Nothing Special   »   [go: up one dir, main page]

WO2022160507A1 - Method for purifying montmorillonite, diosmectite, and preparation method therefor - Google Patents

Method for purifying montmorillonite, diosmectite, and preparation method therefor Download PDF

Info

Publication number
WO2022160507A1
WO2022160507A1 PCT/CN2021/093536 CN2021093536W WO2022160507A1 WO 2022160507 A1 WO2022160507 A1 WO 2022160507A1 CN 2021093536 W CN2021093536 W CN 2021093536W WO 2022160507 A1 WO2022160507 A1 WO 2022160507A1
Authority
WO
WIPO (PCT)
Prior art keywords
montmorillonite
powder
bentonite
dispersant
mass ratio
Prior art date
Application number
PCT/CN2021/093536
Other languages
French (fr)
Chinese (zh)
Inventor
许丹青
余国新
耿亮
朱亚东
Original Assignee
海南海力制药有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 海南海力制药有限公司 filed Critical 海南海力制药有限公司
Publication of WO2022160507A1 publication Critical patent/WO2022160507A1/en

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
    • C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
    • C01B33/40—Clays
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
    • A61K9/145—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic compounds

Definitions

  • the invention relates to the technical field of medicine, in particular to a purification method of montmorillonite, montmorillonite powder and a preparation method thereof.
  • Bentonite is a rock with montmorillonite as the main component.
  • the method of purifying and preparing high-purity montmorillonite from bentonite is very eye-catching, and it has become one of the research hotspots of non-metallic mineral materials at home and abroad.
  • the montmorillonite purified from bentonite is a natural mineral drug and pharmaceutical excipient with less toxic and side effects on the human body and obvious curative effect or auxiliary effect. Montmorillonite was further purified.
  • montmorillonite should not be purified by chemical method, nor should it be purified by adding toxic dispersants and flocculants to avoid the pollution of montmorillonite refined soil by toxic substances introduced by chemical reagents. Therefore, medical montmorillonite generally chooses physical purification. .
  • the existing physical purification method of montmorillonite is generally to grind the montmorillonite raw material and then screen it, then mix the screened montmorillonite raw material with water to form a puree, add a dispersant, and centrifuge after the centrifugation. The upper layer of puree is heated and dried.
  • the purification process of this method is simple and easy to operate, due to the fine grains, poor crystallization, variable composition of montmorillonite minerals, and other impurities such as clay minerals, the montmorillonite obtained from the montmorillonite purified by this method is produced.
  • the particle size and particle size distribution of Toffite powder are unqualified.
  • the technical problem to be solved by the present invention is to overcome the defects of unqualified particle size and particle size distribution in the montmorillonite prepared by the montmorillonite obtained by the purification method of montmorillonite in the prior art, thereby providing a montmorillonite The purification method, montmorillonite powder and preparation method thereof.
  • a method for purifying montmorillonite comprising the steps:
  • Pretreatment and coarse impurity removal drying, grinding and pulverizing the bentonite, and sieving to obtain bentonite powder; adding water and dispersant to the bentonite powder, beating, and sieving to remove coarse sand to obtain slurry;
  • Deep impurity removal the suspension formed by adding water to the slurry is sonicated under agitation, and then subjected to high-speed centrifugal separation to remove impurities, and the obtained thin slurry is concentrated and dried;
  • the amount of dispersant is 0.9-1.1% of the mass of bentonite, and the dispersant is sodium carbonate and trisodium phosphate with a mass ratio of 1:(0.2-0.5).
  • the suspension is ultrasonically treated at a stirring speed of 800-1000r/min for 40-60min; the ultrasonic frequency is 50-60KHz.
  • the mass ratio of slurry to water is 1:(9-10).
  • the mass ratio of bentonite powder to water is 1: (2-3);
  • the beating time is 5-7h.
  • the bentonite is dried at 70-80°C for 4-7h.
  • a universal pulverizer a ball mill, a superfine grinder, a vibration mill or a peeler to grind the dried bentonite.
  • the present invention also provides the montmorillonite obtained by the purification method of the above-mentioned montmorillonite.
  • the present invention also provides the montmorillonite powder obtained by the above-mentioned montmorillonite, including the following raw materials by weight:
  • the montmorillonite powder includes the following raw materials by weight: 100 parts of montmorillonite and 35 parts of glucose.
  • the present invention also provides the preparation method of the above-mentioned montmorillonite powder, comprising the following steps:
  • the mixing time is 25-35 min.
  • the purification method of montmorillonite provided by the present invention by adopting the dispersing agent that the mixture of sodium carbonate and trisodium phosphate with a specific mass ratio of 1: (0.2-0.5) is used, combined with the limited amount of the dispersing agent and grinding and pulverizing.
  • the step of drying bentonite can effectively change the adhesion relationship between the impurities in the bentonite and the montmorillonite, so that the impurities attached to the surface of the montmorillonite particles can be separated from the montmorillonite, reducing the phenomenon of agglomeration, and then beating and sieving to remove the coarse sand and other large particles of impurities; by ultrasonic under stirring, the fine impurities mixed between the montmorillonite flakes and between the montmorillonite grains are quickly separated from the montmorillonite, and then removed by high-speed centrifugation Moreover, the dispersant used in the present invention has mild chemical properties, will not destroy the composition and structure of montmorillonite, and will not introduce toxic substances.
  • the montmorillonite obtained by the method for purifying montmorillonite provided by the invention has high purity and low content of toxic elements, and can be directly used in the field of medicine, especially the montmorillonite powder prepared by using the montmorillonite conforms to the 2015 edition of the Chinese Pharmacopoeia Medium montmorillonite particle size, particle size distribution and other related quality regulations.
  • the purification method of montmorillonite provided by the present invention can further improve the fineness of the montmorillonite lamellae and the montmorillonite crystal grains by limiting the stirring rate of the suspension, the frequency and time of the ultrasonic wave.
  • the separation effect of impurities from montmorillonite improves the purity of montmorillonite.
  • the purification method of montmorillonite provided by the present invention can further improve the effect of removing fine impurities by limiting the mass ratio of slurry to water and combining with the high-speed centrifugation step.
  • the purification method of montmorillonite provided by the present invention, by fully drying the bentonite to remove the moisture therein, so that the montmorillonite is not easy to agglomerate and is easy to grind, so that as many impurities as possible are exposed on the surface of the montmorillonite, combined with the bentonite.
  • the mass ratio of powder to water and the beating time are limited, which is easy to remove coarse sand and other large-particle impurities, and prepares for subsequent deep cleaning.
  • the montmorillonite powder provided by the present invention can not only cover the earthy smell in the montmorillonite by mixing the montmorillonite of a specific weight portion with glucose, so that the patient is easy to accept; and can improve the efficacy; the montmorillonite Shisan conforms to the quality regulations related to montmorillonite powder in the 2015 edition of the Chinese Pharmacopoeia, and is widely used.
  • the preparation method of montmorillonite powder provided by the present invention is simple and convenient.
  • the montmorillonite powder prepared by this method complies with the relevant quality regulations of montmorillonite powder in the 2015 edition of the Chinese Pharmacopoeia.
  • the content of montmorillonite in the following examples and comparative examples is calculated by the loss-on-drying method.
  • the specific operation is as follows: accurately weigh about 0.4 g, put it in a centrifuge tube that is pre-dried to constant weight at 105 ° C, and add the volume fraction of 30 mL of 50% ethanol, stir evenly, centrifuge (about 15 minutes at 3000 rpm), discard the supernatant, add 30 mL of 50% ethanol by volume, stir, centrifuge (about 15 minutes at 3000 rpm), discard The supernatant was removed, and the obtained precipitate was dried at 105° C. to constant weight to obtain the weight of montmorillonite, which was calculated and obtained.
  • the present embodiment provides a preparation method of montmorillonite powder, comprising the following steps:
  • Pretreatment and rough impurity removal After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant (The mass ratio of sodium carbonate and trisodium phosphate is 1:0.2), the mass ratio of bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
  • Deep impurity removal the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 800r/min (ultrasonic frequency is 60KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
  • the montmorillonite obtained by the above purification is off-white, and the diffraction angles (2 ⁇ ) in the X-ray powder diffraction pattern are about 5.8°, 19.8°, and 61.9°, respectively.
  • the purity of the montmorillonite measured by the loss on drying method is 99.8%.
  • the total amount of heavy metals is less than 10 parts per million.
  • the above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
  • the present embodiment provides a preparation method of montmorillonite powder, comprising the following steps:
  • Pretreatment and rough impurity removal After drying the bentonite at 70°C for 7 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 200-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:3, add a dispersant (the mass ratio of sodium carbonate and trisodium phosphate of 1:0.5), the mass ratio of bentonite powder and dispersant is 1:0.9; then stirred for 7h, and passed through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
  • a dispersant the mass ratio of sodium carbonate and trisodium phosphate of 1:0.5
  • Deep impurity removal the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 40min at a stirring speed of 900r/min (ultrasonic frequency is 55KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 68%. Purified montmorillonite.
  • the montmorillonite obtained by the above purification is off-white, and the diffraction angles (2 ⁇ ) in the X-ray powder diffraction pattern are about 5.8°, 19.8°, and 61.9°, respectively.
  • the purity of the montmorillonite measured by the loss on drying method is 99.7%.
  • the total amount of heavy metals is less than 10 parts per million.
  • the above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 30kg of pulverized glucose, then weigh 90kg of pulverized montmorillonite, and mix for 30min. have to.
  • the present embodiment provides a preparation method of montmorillonite powder, comprising the following steps:
  • Pretreatment and coarse impurity removal After drying the bentonite at 80°C for 4 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2, add a dispersant (the mass ratio of sodium carbonate and trisodium phosphate is 1:0.4), the mass ratio of bentonite powder and dispersant is 1:1.1; then stir for 5h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
  • Deep impurity removal the above-mentioned slurry and water are mixed uniformly to form a suspension according to the mass ratio of 1:10, then ultrasonically treated for 60min at a stirring speed of 1000r/min (ultrasonic frequency is 50KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 65%. Purified montmorillonite.
  • the montmorillonite obtained by the above purification is off-white, and the diffraction angles (2 ⁇ ) in the X-ray powder diffraction pattern are about 5.8°, 19.8°, and 61.9°, respectively.
  • the purity of the montmorillonite measured by the loss on drying method is 99.6%.
  • the total amount of heavy metals is less than 10 parts per million.
  • the above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 40kg of the pulverized glucose, then weigh 110kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
  • the present embodiment provides a preparation method of montmorillonite powder, comprising the following steps:
  • Pretreatment and rough impurity removal After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant (The mass ratio of sodium carbonate and trisodium phosphate is 1:0.2), the mass ratio of bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
  • Deep impurity removal the above-mentioned slurry and water are mixed uniformly to form a suspension according to a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 1200r/min (ultrasonic frequency is 70KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
  • the montmorillonite obtained by the above purification is off-white, and the diffraction angles (2 ⁇ ) in the X-ray powder diffraction pattern are about 5.8°, 19.8°, and 61.9°, respectively.
  • the purity of the montmorillonite measured by loss on drying method is 99.2%.
  • the total amount of heavy metals is less than 10 parts per million.
  • the above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
  • the present embodiment provides a preparation method of montmorillonite powder, comprising the following steps:
  • Pretreatment and rough impurity removal After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant (The mass ratio of sodium carbonate and trisodium phosphate is 1:0.2), the mass ratio of bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
  • Deep impurity removal the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 70min at a stirring speed of 700r/min (ultrasonic frequency is 40KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
  • the montmorillonite obtained by the above purification is off-white, and the diffraction angles (2 ⁇ ) in the X-ray powder diffraction pattern are about 5.8°, 19.8° and 61.9°, respectively.
  • the purity of the montmorillonite measured by loss on drying method is 99.3%.
  • the total amount of heavy metals is less than 10 parts per million.
  • the above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
  • This comparative example provides a kind of preparation method of montmorillonite powder, comprising the following steps:
  • Pretreatment and rough impurity removal After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant The mass ratio of sodium carbonate, bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
  • Deep impurity removal the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 800r/min (ultrasonic frequency is 60KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
  • the montmorillonite obtained by the above purification is gray, and the purity of the montmorillonite measured by the loss on drying method is 85.5%.
  • the above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
  • This comparative example provides a kind of preparation method of montmorillonite powder, comprising the following steps:
  • Pretreatment and rough impurity removal After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant The mass ratio of trisodium phosphate, bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
  • Deep impurity removal the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 800r/min (ultrasonic frequency is 60KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
  • the montmorillonite obtained by the above purification is gray, and the purity of the montmorillonite measured by the loss on drying method is 82.6%.
  • the above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
  • This comparative example provides a kind of preparation method of montmorillonite powder, comprising the following steps:
  • Pretreatment and rough impurity removal After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant (the mass ratio of sodium carbonate and trisodium phosphate of 1:0.2), the mass ratio of bentonite powder and dispersant is 1:1.3; then stirred for 6h, and passed through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
  • a dispersant the mass ratio of sodium carbonate and trisodium phosphate of 1:0.2
  • Deep impurity removal the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 800r/min (ultrasonic frequency is 60KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
  • the montmorillonite obtained by the above purification is gray, and the purity of the montmorillonite measured by the loss on drying method is 86.9%.
  • the above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
  • This comparative example provides a kind of preparation method of montmorillonite powder, comprising the following steps:
  • Pretreatment and rough impurity removal After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant The mass ratio of sodium hexametaphosphate, bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
  • Deep impurity removal the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 800r/min (ultrasonic frequency is 60KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
  • the montmorillonite obtained by the above purification is gray, and the purity of the montmorillonite measured by the loss on drying method is 88.1%.
  • the total amount of heavy metals is less than 10 parts per million.
  • the above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
  • the montmorillonite powder obtained by each embodiment and the comparative example is subjected to particle size, particle size distribution, pH test, and the test results are shown in the following table; Concrete test method is as follows:
  • Particle size Take 10g of montmorillonite powder, add 500ml of water, stir vigorously for 15min (rotation speed is 7000 rpm), pour the content after stirring into a sieve (pore size 45 ⁇ m, pre-dried at 105°C to constant weight), After washing the sieve with water until there is no suspension spot, the sieve was dried at 105°C for 3 hours and weighed.
  • Particle size distribution Take an appropriate amount of montmorillonite powder (approximately equivalent to 0.10g of montmorillonite), so that the shading rate of the detector is in the range of 8%-20%, add 800ml of water, stir at a speed of 3000 rpm, and ultrasonically 2- 3 minutes (ultrasonic power 16W, amplitude 3 ⁇ m), check according to the third method of 0982 of the 2015 edition of the Four General Principles, and take the average value of 3 consecutive measurements.
  • the montmorillonite obtained by the purification method of the montmorillonite provided by the present invention has high purity and low content of toxic elements, and can be directly used in the field of medicine, especially the montmorillonite obtained by applying the montmorillonite.
  • Montmorillonite powder complies with the relevant quality regulations of montmorillonite powder particle size, particle size distribution and pH in the 2015 edition of the Chinese Pharmacopoeia.

Landscapes

  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Inorganic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Veterinary Medicine (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Dispersion Chemistry (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The present invention relates to the technical field of medicine, and in particular relates to a method for purifying montmorillonite, diosmectite, and a preparation method therefor. According to the method for purifying montmorillonite, by means of a dispersant which is composed of a mixture of sodium carbonate and trisodium phosphate and which has a specific mass ratio of 1:(0.2-0.5) is used, as well as the step of combining a limited amount of the dispersant with ground, pulverized and dried bentonite, the adhesion relationship between impurities in the bentonite and the montmorillonite may be effectively changed, thereby separating the impurities attached to the surface of montmorillonite particles from the montmorillonite, and reducing the phenomenon of agglomeration. Then, beating and sieving are carried out to remove coarse sand and other large-particle impurities. An ultrasound is performed while stirring, so that fine impurities mixed with montmorillonite flakes and wrapped between montmorillonite grains are quickly separated from the montmorillonite, and are then removed by high-speed centrifugation. Moreover, the dispersant used in the present invention has mild chemical properties, will not destroy the composition and structure of montmorillonite, and will not introduce toxic substances.

Description

蒙脱石的纯化方法、蒙脱石散及其制备方法Method for purifying montmorillonite, montmorillonite powder and preparation method thereof 技术领域technical field
本发明涉及医药技术领域，特别涉及一种蒙脱石的纯化方法、蒙脱石散及其制备方法。The invention relates to the technical field of medicine, in particular to a purification method of montmorillonite, montmorillonite powder and a preparation method thereof.
背景技术Background technique
膨润土是以蒙脱石为主要组分的岩石。近年来，从膨润土中提纯制备高纯蒙脱石的方法非常引人注目，成为国内外非金属矿物材料研究热点之一。膨润土提纯出的蒙脱石是一种对人体毒副作用小，疗效或辅助效果明显的天然矿物药物和药物辅料，用于医药的蒙脱石需要高纯度和很低的有毒元素含量，因此需要对蒙脱石进一步提纯。Bentonite is a rock with montmorillonite as the main component. In recent years, the method of purifying and preparing high-purity montmorillonite from bentonite is very eye-catching, and it has become one of the research hotspots of non-metallic mineral materials at home and abroad. The montmorillonite purified from bentonite is a natural mineral drug and pharmaceutical excipient with less toxic and side effects on the human body and obvious curative effect or auxiliary effect. Montmorillonite was further purified.
医药蒙脱石不宜用化学法提纯，也不宜加入毒性较大的分散剂、絮凝剂进行提纯，以免化学试剂引入的毒性物质对蒙脱石精土的污染，因此医药蒙脱石一般选择物理提纯。Pharmaceutical montmorillonite should not be purified by chemical method, nor should it be purified by adding toxic dispersants and flocculants to avoid the pollution of montmorillonite refined soil by toxic substances introduced by chemical reagents. Therefore, medical montmorillonite generally chooses physical purification. .
现有的蒙脱石的物理纯化方法一般是研磨蒙脱石原料后进行筛选，然后将筛选后的蒙脱石原料和水混合形成原浆并加入分散剂，混合均匀后离心并将离心后的上层原浆加热烘干，即得。虽然该方法提纯工艺简单，易于操作，但是由于蒙脱石矿物晶粒细、结晶差、成分多变，并伴有其他黏土矿物等杂质，导致用该方法提纯得到的蒙脱石制备得到的蒙脱石散的粒度及粒度分布不合格。The existing physical purification method of montmorillonite is generally to grind the montmorillonite raw material and then screen it, then mix the screened montmorillonite raw material with water to form a puree, add a dispersant, and centrifuge after the centrifugation. The upper layer of puree is heated and dried. Although the purification process of this method is simple and easy to operate, due to the fine grains, poor crystallization, variable composition of montmorillonite minerals, and other impurities such as clay minerals, the montmorillonite obtained from the montmorillonite purified by this method is produced. The particle size and particle size distribution of Toffite powder are unqualified.
发明内容SUMMARY OF THE INVENTION
因此，本发明要解决的技术问题在于克服现有技术中蒙脱石的纯化方法得到的蒙脱石制备得到的蒙脱石散存在粒度及粒度分布不合格的缺陷，从而提供一种蒙脱石的纯化方法、蒙脱石散及其制备方法。Therefore, the technical problem to be solved by the present invention is to overcome the defects of unqualified particle size and particle size distribution in the montmorillonite prepared by the montmorillonite obtained by the purification method of montmorillonite in the prior art, thereby providing a montmorillonite The purification method, montmorillonite powder and preparation method thereof.
为此，本发明技术方案如下：For this reason, the technical scheme of the present invention is as follows:
一种蒙脱石的纯化方法，包括如下步骤：A method for purifying montmorillonite, comprising the steps:
预处理及粗除杂：将膨润土干燥、研磨粉碎，过筛得膨润土粉体；向膨润土粉体中加水和分散剂，打浆，过筛去除粗砂，得浆料；Pretreatment and coarse impurity removal: drying, grinding and pulverizing the bentonite, and sieving to obtain bentonite powder; adding water and dispersant to the bentonite powder, beating, and sieving to remove coarse sand to obtain slurry;
深度除杂：向浆料中加水形成的悬浮液在搅拌状态下超声，然后经高速离心分离除杂，所得稀浆料经浓缩干燥即得；Deep impurity removal: the suspension formed by adding water to the slurry is sonicated under agitation, and then subjected to high-speed centrifugal separation to remove impurities, and the obtained thin slurry is concentrated and dried;
其中，分散剂用量为膨润土质量的0.9-1.1％，所述分散剂为质量比为1∶(0.2-0.5)的碳酸钠和磷酸三钠。Wherein, the amount of dispersant is 0.9-1.1% of the mass of bentonite, and the dispersant is sodium carbonate and trisodium phosphate with a mass ratio of 1:(0.2-0.5).
可选地，深度除杂步骤中，悬浮液在800-1000r/min搅拌速度下超声处理40-60min；超声频率为50-60KHz。Optionally, in the deep impurity removal step, the suspension is ultrasonically treated at a stirring speed of 800-1000r/min for 40-60min; the ultrasonic frequency is 50-60KHz.
可选地，深度除杂步骤中，浆料与水的质量比为1∶(9-10)。Optionally, in the deep impurity removal step, the mass ratio of slurry to water is 1:(9-10).
可选地，预处理及粗除杂步骤中，膨润土粉体与水的质量比为1∶(2-3)；Optionally, in the pretreatment and rough impurity removal steps, the mass ratio of bentonite powder to water is 1: (2-3);
打浆时间为5-7h。The beating time is 5-7h.
可选地，将膨润土在70-80℃下干燥4-7h。Optionally, the bentonite is dried at 70-80°C for 4-7h.
可选地，采用万能粉碎机、球磨机、超细研磨机、振动磨或剥片机等对干燥后的膨润土进行研磨。Optionally, use a universal pulverizer, a ball mill, a superfine grinder, a vibration mill or a peeler to grind the dried bentonite.
本发明还提供了上述的蒙脱石的纯化方法纯化得到的蒙脱石。The present invention also provides the montmorillonite obtained by the purification method of the above-mentioned montmorillonite.
本发明还提供了由上述的蒙脱石制得的蒙脱石散，包括如下重量份的原料：The present invention also provides the montmorillonite powder obtained by the above-mentioned montmorillonite, including the following raw materials by weight:
蒙脱石90-110份，葡萄糖30-40份。Montmorillonite 90-110 parts, glucose 30-40 parts.
可选地，蒙脱石散，包括如下重量份的原料：蒙脱石100份，葡萄糖35份。Optionally, the montmorillonite powder includes the following raw materials by weight: 100 parts of montmorillonite and 35 parts of glucose.
本发明还提供了上述的蒙脱石散的制备方法，包括如下步骤：The present invention also provides the preparation method of the above-mentioned montmorillonite powder, comprising the following steps:
将蒙脱石和葡萄糖分别粉碎后过80目筛；然后按选定的重量份数称量、混合、分装，即得。Pulverize the montmorillonite and glucose respectively and pass through an 80-mesh sieve; then weigh, mix and pack according to the selected parts by weight to obtain the obtained product.
可选地，混合时间为25-35min。Optionally, the mixing time is 25-35 min.
与现有技术相比，本发明的优点：Compared with the prior art, the advantages of the present invention:
1.本发明提供的蒙脱石的纯化方法，通过采用特定的质量比为1∶(0.2-0.5)的碳酸钠和磷酸三钠的混合物构成的分散剂，结合分散剂的限定用量及研磨粉碎干燥后膨润土的步骤，能有效改变膨润土中的杂质与蒙脱石的附着关系，使附着在蒙脱石颗粒表面的杂质与蒙脱石分离，减少团聚现象，然后经打浆、过筛除去粗砂及其他大颗粒杂质；通过在搅拌状下进行超声，使得夹杂在蒙脱石片层间以及包裹在蒙脱石晶粒之间的细微杂质从蒙脱石中快速分离出来，然后经高速离心除去；而且，本发明所用的分散剂化学性质温和，不会破坏蒙脱石的成分和结构，更不会引入毒性物质。1. The purification method of montmorillonite provided by the present invention, by adopting the dispersing agent that the mixture of sodium carbonate and trisodium phosphate with a specific mass ratio of 1: (0.2-0.5) is used, combined with the limited amount of the dispersing agent and grinding and pulverizing. The step of drying bentonite can effectively change the adhesion relationship between the impurities in the bentonite and the montmorillonite, so that the impurities attached to the surface of the montmorillonite particles can be separated from the montmorillonite, reducing the phenomenon of agglomeration, and then beating and sieving to remove the coarse sand and other large particles of impurities; by ultrasonic under stirring, the fine impurities mixed between the montmorillonite flakes and between the montmorillonite grains are quickly separated from the montmorillonite, and then removed by high-speed centrifugation Moreover, the dispersant used in the present invention has mild chemical properties, will not destroy the composition and structure of montmorillonite, and will not introduce toxic substances.
本发明提供的蒙脱石的纯化方法得到的蒙脱石纯度高，且有毒元素含量低，可直接用于医药领域，尤其是应用该蒙脱石制得的蒙脱石散符合2015版中国药典中蒙脱石散粒度、粒度分布及其他相关的质量规定。The montmorillonite obtained by the method for purifying montmorillonite provided by the invention has high purity and low content of toxic elements, and can be directly used in the field of medicine, especially the montmorillonite powder prepared by using the montmorillonite conforms to the 2015 edition of the Chinese Pharmacopoeia Medium montmorillonite particle size, particle size distribution and other related quality regulations.
2.本发明提供的蒙脱石的纯化方法，通过限定悬浮液的搅拌速率、超声的频率及时间，可进一步提高夹杂在蒙脱石片层间以及包裹在蒙脱石晶粒之 间的细微杂质从蒙脱石中的分离效果，提高蒙脱石的纯度。2. The purification method of montmorillonite provided by the present invention can further improve the fineness of the montmorillonite lamellae and the montmorillonite crystal grains by limiting the stirring rate of the suspension, the frequency and time of the ultrasonic wave. The separation effect of impurities from montmorillonite improves the purity of montmorillonite.
3.本发明提供的蒙脱石的纯化方法，通过限定浆料与水的质量比，结合高速离心步骤，可进一步提高除去细微杂质的效果。3. The purification method of montmorillonite provided by the present invention can further improve the effect of removing fine impurities by limiting the mass ratio of slurry to water and combining with the high-speed centrifugation step.
4.本发明提供的蒙脱石的纯化方法，通过将膨润土充分干燥除去其中的水分，使蒙脱石不易结块且易于研磨，使得尽可能多的杂质暴露在蒙脱石的表面，结合膨润土粉体与水的质量比以及打浆时间的限定，易于粗砂及其他大颗粒杂质的去除，同时为后续深度除杂做准备。4. The purification method of montmorillonite provided by the present invention, by fully drying the bentonite to remove the moisture therein, so that the montmorillonite is not easy to agglomerate and is easy to grind, so that as many impurities as possible are exposed on the surface of the montmorillonite, combined with the bentonite. The mass ratio of powder to water and the beating time are limited, which is easy to remove coarse sand and other large-particle impurities, and prepares for subsequent deep cleaning.
5.本发明提供的蒙脱石散，通过将特定重量份的蒙脱石与葡萄糖混合，不仅可以遮盖蒙脱石中的土腥味，使患者易于接受；而且可提高药效；该蒙脱石散符合2015版中国药典中蒙脱石散相关的质量规定，且使用人群广泛。5. The montmorillonite powder provided by the present invention can not only cover the earthy smell in the montmorillonite by mixing the montmorillonite of a specific weight portion with glucose, so that the patient is easy to accept; and can improve the efficacy; the montmorillonite Shisan conforms to the quality regulations related to montmorillonite powder in the 2015 edition of the Chinese Pharmacopoeia, and is widely used.
6.本发明提供的蒙脱石散的制备方法，简单方便。该方法制得的蒙脱石散符合2015版中国药典中蒙脱石散相关的质量规定。6. The preparation method of montmorillonite powder provided by the present invention is simple and convenient. The montmorillonite powder prepared by this method complies with the relevant quality regulations of montmorillonite powder in the 2015 edition of the Chinese Pharmacopoeia.
具体实施方式Detailed ways
下述各实施例及对比例中蒙脱石的含量均采用干燥失重法计算，具体操作如下：精密称取约0.4g，置预先经105℃干燥至恒重的离心管中，加体积分数为50％乙醇30mL，搅拌均匀后，离心(每分钟3000转约15分钟)，弃去上清液，再加体积分数为50％乙醇30mL，搅拌，离心(每分钟3000转约15分钟)，弃去上清液，所得沉淀在105℃干燥至恒重，即得蒙脱石的重量，计算，即得。The content of montmorillonite in the following examples and comparative examples is calculated by the loss-on-drying method. The specific operation is as follows: accurately weigh about 0.4 g, put it in a centrifuge tube that is pre-dried to constant weight at 105 ° C, and add the volume fraction of 30 mL of 50% ethanol, stir evenly, centrifuge (about 15 minutes at 3000 rpm), discard the supernatant, add 30 mL of 50% ethanol by volume, stir, centrifuge (about 15 minutes at 3000 rpm), discard The supernatant was removed, and the obtained precipitate was dried at 105° C. to constant weight to obtain the weight of montmorillonite, which was calculated and obtained.
实施例1Example 1
本实施例提供一种蒙脱石散的制备方法，包括如下步骤：The present embodiment provides a preparation method of montmorillonite powder, comprising the following steps:
蒙脱石的纯化：Purification of Montmorillonite:
预处理及粗除杂：将膨润土在75℃下干燥6h后，用万能粉碎机研磨粉碎过100目筛得膨润土粉体；将膨润土粉体和水按照质量比1∶2.5混合后，加入分散剂(质量比为1∶0.2的碳酸钠和磷酸三钠)，膨润土粉体与分散剂的质量比为1∶1.0；然后搅拌6h，过四级水力旋流器去除粗砂，得浆料；Pretreatment and rough impurity removal: After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant (The mass ratio of sodium carbonate and trisodium phosphate is 1:0.2), the mass ratio of bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
深度除杂：将上述的浆料与水按照质量比为1∶9混合均匀形成的悬浮液，然后在800r/min搅拌速度下超声处理50min后(超声频率为60KHz)；经蝶式离心机分离得到的稀料浆进入另一蝶式离心机浓缩，浓缩后的料浆经压滤机压滤得固含量为60％的滤饼，滤饼在120℃烘干，然后粉碎至500目以上即得纯化后的蒙脱石。Deep impurity removal: the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 800r/min (ultrasonic frequency is 60KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
上述纯化得到的蒙脱石为灰白色，其X-射线粉末衍射图谱中衍射角(2θ)分别约为5.8°、19.8°、61.9°，干燥失重法测得蒙脱石纯度为99.8％。参照中国药典2015版第四部通则0812重金属检查法中的第一法进行测试，重金属总量小于百万分之十。The montmorillonite obtained by the above purification is off-white, and the diffraction angles (2θ) in the X-ray powder diffraction pattern are about 5.8°, 19.8°, and 61.9°, respectively. The purity of the montmorillonite measured by the loss on drying method is 99.8%. Refer to the first method in the Chinese Pharmacopoeia 2015 edition of the fourth general rule 0812 heavy metal inspection method to test, the total amount of heavy metals is less than 10 parts per million.
蒙脱石散的制备：Preparation of montmorillonite powder:
将上述的蒙脱石粉碎过80目筛：葡萄糖粉碎过80目筛；在负压称量罩下先称量粉碎后的葡萄糖35kg，然后称量粉碎后的蒙脱石100kg，混合30min，即得。The above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
实施例2Example 2
本实施例提供一种蒙脱石散的制备方法，包括如下步骤：The present embodiment provides a preparation method of montmorillonite powder, comprising the following steps:
蒙脱石的纯化：Purification of Montmorillonite:
预处理及粗除杂：将膨润土在70℃下干燥7h后，用万能粉碎机研磨粉碎过200目筛得膨润土粉体；将膨润土粉体和水按照质量比1∶3混合后，加入分散剂(质量比为1∶0.5的碳酸钠和磷酸三钠)，膨润土粉体与分散剂的质量比为1∶0.9；然后搅拌7h，过四级水力旋流器去除粗砂，得浆料；Pretreatment and rough impurity removal: After drying the bentonite at 70°C for 7 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 200-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:3, add a dispersant (the mass ratio of sodium carbonate and trisodium phosphate of 1:0.5), the mass ratio of bentonite powder and dispersant is 1:0.9; then stirred for 7h, and passed through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
深度除杂：将上述的浆料与水按照质量比为1∶9混合均匀形成的悬浮液，然后在900r/min搅拌速度下超声处理40min后(超声频率为55KHz)；经蝶式离心机分离得到的稀料浆进入另一蝶式离心机浓缩，浓缩后的料浆经压滤机压滤得固含量为68％的滤饼，滤饼在120℃烘干，然后粉碎至500目以上即得纯化后的蒙脱石。Deep impurity removal: the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 40min at a stirring speed of 900r/min (ultrasonic frequency is 55KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 68%. Purified montmorillonite.
上述纯化得到的蒙脱石为灰白色，其X-射线粉末衍射图谱中衍射角(2θ)分别约为5.8°、19.8°、61.9°，干燥失重法测得蒙脱石纯度为99.7％。参照中国药典2015版第四部通则0812重金属检查法中的第一法进行测试，重金属总量小于百万分之十。The montmorillonite obtained by the above purification is off-white, and the diffraction angles (2θ) in the X-ray powder diffraction pattern are about 5.8°, 19.8°, and 61.9°, respectively. The purity of the montmorillonite measured by the loss on drying method is 99.7%. Refer to the first method in the Chinese Pharmacopoeia 2015 edition of the fourth general rule 0812 heavy metal inspection method to test, the total amount of heavy metals is less than 10 parts per million.
蒙脱石散的制备：Preparation of montmorillonite powder:
将上述的蒙脱石粉碎过80目筛：葡萄糖粉碎过80目筛；在负压称量罩下先称量粉碎后的葡萄糖30kg，然后称量粉碎后的蒙脱石90kg，混合30min，即得。The above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 30kg of pulverized glucose, then weigh 90kg of pulverized montmorillonite, and mix for 30min. have to.
实施例3Example 3
本实施例提供一种蒙脱石散的制备方法，包括如下步骤：The present embodiment provides a preparation method of montmorillonite powder, comprising the following steps:
蒙脱石的纯化：Purification of Montmorillonite:
预处理及粗除杂：将膨润土在80℃下干燥4h后，用万能粉碎机研磨粉碎过100目筛得膨润土粉体；将膨润土粉体和水按照质量比1∶2混合后，加 入分散剂(质量比为1∶0.4的碳酸钠和磷酸三钠)，膨润土粉体与分散剂的质量比为1∶1.1；然后搅拌5h，过四级水力旋流器去除粗砂，得浆料；Pretreatment and coarse impurity removal: After drying the bentonite at 80°C for 4 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2, add a dispersant (the mass ratio of sodium carbonate and trisodium phosphate is 1:0.4), the mass ratio of bentonite powder and dispersant is 1:1.1; then stir for 5h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
深度除杂：将上述的浆料与水按照质量比为1∶10混合均匀形成的悬浮液，然后在1000r/min搅拌速度下超声处理60min后(超声频率为50KHz)；经蝶式离心机分离得到的稀料浆进入另一蝶式离心机浓缩，浓缩后的料浆经压滤机压滤得固含量为65％的滤饼，滤饼在120℃烘干，然后粉碎至500目以上即得纯化后的蒙脱石。Deep impurity removal: the above-mentioned slurry and water are mixed uniformly to form a suspension according to the mass ratio of 1:10, then ultrasonically treated for 60min at a stirring speed of 1000r/min (ultrasonic frequency is 50KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 65%. Purified montmorillonite.
上述纯化得到的蒙脱石为灰白色，其X-射线粉末衍射图谱中衍射角(2θ)分别约为5.8°、19.8°、61.9°，干燥失重法测得蒙脱石纯度为99.6％。参照中国药典2015版第四部通则0812重金属检查法中的第一法进行测试，重金属总量小于百万分之十。The montmorillonite obtained by the above purification is off-white, and the diffraction angles (2θ) in the X-ray powder diffraction pattern are about 5.8°, 19.8°, and 61.9°, respectively. The purity of the montmorillonite measured by the loss on drying method is 99.6%. Refer to the first method in the Chinese Pharmacopoeia 2015 edition of the fourth general rule 0812 heavy metal inspection method to test, the total amount of heavy metals is less than 10 parts per million.
蒙脱石散的制备：Preparation of montmorillonite powder:
将上述的蒙脱石粉碎过80目筛：葡萄糖粉碎过80目筛；在负压称量罩下先称量粉碎后的葡萄糖40kg，然后称量粉碎后的蒙脱石110kg，混合30min，即得。The above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 40kg of the pulverized glucose, then weigh 110kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
实施例4Example 4
本实施例提供一种蒙脱石散的制备方法，包括如下步骤：The present embodiment provides a preparation method of montmorillonite powder, comprising the following steps:
蒙脱石的纯化：Purification of Montmorillonite:
预处理及粗除杂：将膨润土在75℃下干燥6h后，用万能粉碎机研磨粉碎过100目筛得膨润土粉体；将膨润土粉体和水按照质量比1∶2.5混合后，加入分散剂(质量比为1∶0.2的碳酸钠和磷酸三钠)，膨润土粉体与分散剂的质量比为1∶1.0；然后搅拌6h，过四级水力旋流器去除粗砂，得浆料；Pretreatment and rough impurity removal: After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant (The mass ratio of sodium carbonate and trisodium phosphate is 1:0.2), the mass ratio of bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
深度除杂：将上述的浆料与水按照质量比为1∶9混合均匀形成的悬浮液，然后在1200r/min搅拌速度下超声处理50min后(超声频率为70KHz)；经蝶式离心机分离得到的稀料浆进入另一蝶式离心机浓缩，浓缩后的料浆经压滤机压滤得固含量为60％的滤饼，滤饼在120℃烘干，然后粉碎至500目以上即得纯化后的蒙脱石。Deep impurity removal: the above-mentioned slurry and water are mixed uniformly to form a suspension according to a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 1200r/min (ultrasonic frequency is 70KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
上述纯化得到的蒙脱石为灰白色，其X-射线粉末衍射图谱中衍射角(2θ)分别约为5.8°、19.8°、61.9°，干燥失重法测得蒙脱石纯度为99.2％。参照中国药典2015版第四部通则0812重金属检查法中的第一法进行测试，重金属总量小于百万分之十。The montmorillonite obtained by the above purification is off-white, and the diffraction angles (2θ) in the X-ray powder diffraction pattern are about 5.8°, 19.8°, and 61.9°, respectively. The purity of the montmorillonite measured by loss on drying method is 99.2%. Refer to the first method in the Chinese Pharmacopoeia 2015 edition of the fourth general rule 0812 heavy metal inspection method to test, the total amount of heavy metals is less than 10 parts per million.
蒙脱石散的制备：Preparation of montmorillonite powder:
将上述的蒙脱石粉碎过80目筛：葡萄糖粉碎过80目筛；在负压称量罩下先称量粉碎后的葡萄糖35kg，然后称量粉碎后的蒙脱石100kg，混合30min，即得。The above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
实施例5Example 5
本实施例提供一种蒙脱石散的制备方法，包括如下步骤：The present embodiment provides a preparation method of montmorillonite powder, comprising the following steps:
蒙脱石的纯化：Purification of Montmorillonite:
预处理及粗除杂：将膨润土在75℃下干燥6h后，用万能粉碎机研磨粉碎过100目筛得膨润土粉体；将膨润土粉体和水按照质量比1∶2.5混合后，加入分散剂(质量比为1∶0.2的碳酸钠和磷酸三钠)，膨润土粉体与分散剂的质量比为1∶1.0；然后搅拌6h，过四级水力旋流器去除粗砂，得浆料；Pretreatment and rough impurity removal: After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant (The mass ratio of sodium carbonate and trisodium phosphate is 1:0.2), the mass ratio of bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
深度除杂：将上述的浆料与水按照质量比为1∶9混合均匀形成的悬浮液，然后在700r/min搅拌速度下超声处理70min后(超声频率为40KHz)；经蝶 式离心机分离得到的稀料浆进入另一蝶式离心机浓缩，浓缩后的料浆经压滤机压滤得固含量为60％的滤饼，滤饼在120℃烘干，然后粉碎至500目以上即得纯化后的蒙脱石。Deep impurity removal: the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 70min at a stirring speed of 700r/min (ultrasonic frequency is 40KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
上述纯化得到的蒙脱石为灰白色，其X-射线粉末衍射图谱中衍射角(2θ)分别约为5.8°、19.8°、61.9°，干燥失重法测得蒙脱石纯度为99.3％。参照中国药典2015版第四部通则0812重金属检查法中的第一法进行测试，重金属总量小于百万分之十。The montmorillonite obtained by the above purification is off-white, and the diffraction angles (2θ) in the X-ray powder diffraction pattern are about 5.8°, 19.8° and 61.9°, respectively. The purity of the montmorillonite measured by loss on drying method is 99.3%. Refer to the first method in the Chinese Pharmacopoeia 2015 edition of the fourth general rule 0812 heavy metal inspection method to test, the total amount of heavy metals is less than 10 parts per million.
蒙脱石散的制备：Preparation of montmorillonite powder:
将上述的蒙脱石粉碎过80目筛：葡萄糖粉碎过80目筛；在负压称量罩下先称量粉碎后的葡萄糖35kg，然后称量粉碎后的蒙脱石100kg，混合30min，即得。The above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
对比例1Comparative Example 1
本对比例提供一种蒙脱石散的制备方法，包括如下步骤：This comparative example provides a kind of preparation method of montmorillonite powder, comprising the following steps:
蒙脱石的纯化：Purification of Montmorillonite:
预处理及粗除杂：将膨润土在75℃下干燥6h后，用万能粉碎机研磨粉碎过100目筛得膨润土粉体；将膨润土粉体和水按照质量比1∶2.5混合后，加入分散剂碳酸钠，膨润土粉体与分散剂的质量比为1∶1.0；然后搅拌6h，过四级水力旋流器去除粗砂，得浆料；Pretreatment and rough impurity removal: After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant The mass ratio of sodium carbonate, bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
深度除杂：将上述的浆料与水按照质量比为1∶9混合均匀形成的悬浮液，然后在800r/min搅拌速度下超声处理50min后(超声频率为60KHz)；经蝶式离心机分离得到的稀料浆进入另一蝶式离心机浓缩，浓缩后的料浆经压滤机压滤得固含量为60％的滤饼，滤饼在120℃烘干，然后粉碎至500目以上 即得纯化后的蒙脱石。Deep impurity removal: the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 800r/min (ultrasonic frequency is 60KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
上述纯化得到的蒙脱石为灰色，干燥失重法测得蒙脱石纯度为85.5％。参照中国药典2015版第四部通则0812重金属检查法中的第一法进行测试，重金属总量大于百万分之十。The montmorillonite obtained by the above purification is gray, and the purity of the montmorillonite measured by the loss on drying method is 85.5%. Refer to the first method in the Chinese Pharmacopoeia 2015 edition of the fourth general chapter 0812 heavy metal inspection method for testing, and the total amount of heavy metals is greater than 10 parts per million.
蒙脱石散的制备：Preparation of montmorillonite powder:
将上述的蒙脱石粉碎过80目筛：葡萄糖粉碎过80目筛；在负压称量罩下先称量粉碎后的葡萄糖35kg，然后称量粉碎后的蒙脱石100kg，混合30min，即得。The above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
对比例2Comparative Example 2
本对比例提供一种蒙脱石散的制备方法，包括如下步骤：This comparative example provides a kind of preparation method of montmorillonite powder, comprising the following steps:
蒙脱石的纯化：Purification of Montmorillonite:
预处理及粗除杂：将膨润土在75℃下干燥6h后，用万能粉碎机研磨粉碎过100目筛得膨润土粉体；将膨润土粉体和水按照质量比1∶2.5混合后，加入分散剂磷酸三钠，膨润土粉体与分散剂的质量比为1∶1.0；然后搅拌6h，过四级水力旋流器去除粗砂，得浆料；Pretreatment and rough impurity removal: After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant The mass ratio of trisodium phosphate, bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
深度除杂：将上述的浆料与水按照质量比为1∶9混合均匀形成的悬浮液，然后在800r/min搅拌速度下超声处理50min后(超声频率为60KHz)；经蝶式离心机分离得到的稀料浆进入另一蝶式离心机浓缩，浓缩后的料浆经压滤机压滤得固含量为60％的滤饼，滤饼在120℃烘干，然后粉碎至500目以上即得纯化后的蒙脱石。Deep impurity removal: the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 800r/min (ultrasonic frequency is 60KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
上述纯化得到的蒙脱石为灰色，干燥失重法测得蒙脱石纯度为82.6％。 参照中国药典2015版第四部通则0812重金属检查法中的第一法进行测试，重金属总量大于百万分之十。The montmorillonite obtained by the above purification is gray, and the purity of the montmorillonite measured by the loss on drying method is 82.6%. Refer to the first method in the Chinese Pharmacopoeia 2015 edition of the fourth general chapter 0812 heavy metal inspection method for testing, and the total amount of heavy metals is greater than 10 parts per million.
蒙脱石散的制备：Preparation of montmorillonite powder:
将上述的蒙脱石粉碎过80目筛：葡萄糖粉碎过80目筛；在负压称量罩下先称量粉碎后的葡萄糖35kg，然后称量粉碎后的蒙脱石100kg，混合30min，即得。The above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
对比例3Comparative Example 3
本对比例提供一种蒙脱石散的制备方法，包括如下步骤：This comparative example provides a kind of preparation method of montmorillonite powder, comprising the following steps:
蒙脱石的纯化：Purification of Montmorillonite:
预处理及粗除杂：将膨润土在75℃下干燥6h后，用万能粉碎机研磨粉碎过100目筛得膨润土粉体；将膨润土粉体和水按照质量比1∶2.5混合后，加入分散剂(质量比为1∶0.2的碳酸钠和磷酸三钠)，膨润土粉体与分散剂的质量比为1∶1.3；然后搅拌6h，过四级水力旋流器去除粗砂，得浆料；Pretreatment and rough impurity removal: After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant (the mass ratio of sodium carbonate and trisodium phosphate of 1:0.2), the mass ratio of bentonite powder and dispersant is 1:1.3; then stirred for 6h, and passed through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
深度除杂：将上述的浆料与水按照质量比为1∶9混合均匀形成的悬浮液，然后在800r/min搅拌速度下超声处理50min后(超声频率为60KHz)；经蝶式离心机分离得到的稀料浆进入另一蝶式离心机浓缩，浓缩后的料浆经压滤机压滤得固含量为60％的滤饼，滤饼在120℃烘干，然后粉碎至500目以上即得纯化后的蒙脱石。Deep impurity removal: the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 800r/min (ultrasonic frequency is 60KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
上述纯化得到的蒙脱石为灰色，干燥失重法测得蒙脱石纯度为86.9％。参照中国药典2015版第四部通则0812重金属检查法中的第一法进行测试，重金属总量大于百万分之十。The montmorillonite obtained by the above purification is gray, and the purity of the montmorillonite measured by the loss on drying method is 86.9%. Refer to the first method in the Chinese Pharmacopoeia 2015 edition of the fourth general chapter 0812 heavy metal inspection method for testing, and the total amount of heavy metals is greater than 10 parts per million.
蒙脱石散的制备：Preparation of montmorillonite powder:
将上述的蒙脱石粉碎过80目筛：葡萄糖粉碎过80目筛；在负压称量罩下先称量粉碎后的葡萄糖35kg，然后称量粉碎后的蒙脱石100kg，混合30min，即得。The above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
对比例4Comparative Example 4
本对比例提供一种蒙脱石散的制备方法，包括如下步骤：This comparative example provides a kind of preparation method of montmorillonite powder, comprising the following steps:
蒙脱石的纯化：Purification of Montmorillonite:
预处理及粗除杂：将膨润土在75℃下干燥6h后，用万能粉碎机研磨粉碎过100目筛得膨润土粉体；将膨润土粉体和水按照质量比1∶2.5混合后，加入分散剂六偏磷酸钠，膨润土粉体与分散剂的质量比为1∶1.0；然后搅拌6h，过四级水力旋流器去除粗砂，得浆料；Pretreatment and rough impurity removal: After drying the bentonite at 75°C for 6 hours, use a universal pulverizer to grind and pulverize the bentonite powder through a 100-mesh sieve; after mixing the bentonite powder and water in a mass ratio of 1:2.5, add a dispersant The mass ratio of sodium hexametaphosphate, bentonite powder and dispersant is 1:1.0; then stir for 6h, and pass through a four-stage hydrocyclone to remove coarse sand to obtain slurry;
深度除杂：将上述的浆料与水按照质量比为1∶9混合均匀形成的悬浮液，然后在800r/min搅拌速度下超声处理50min后(超声频率为60KHz)；经蝶式离心机分离得到的稀料浆进入另一蝶式离心机浓缩，浓缩后的料浆经压滤机压滤得固含量为60％的滤饼，滤饼在120℃烘干，然后粉碎至500目以上即得纯化后的蒙脱石。Deep impurity removal: the above-mentioned slurry and water are mixed uniformly to form a suspension in a mass ratio of 1:9, then ultrasonically treated for 50min at a stirring speed of 800r/min (ultrasonic frequency is 60KHz); separated by a butterfly centrifuge The obtained thin slurry is concentrated in another butterfly centrifuge, and the concentrated slurry is filtered by a filter press to obtain a filter cake with a solid content of 60%. Purified montmorillonite.
上述纯化得到的蒙脱石为灰色，干燥失重法测得蒙脱石纯度为88.1％。参照中国药典2015版第四部通则0812重金属检查法中的第一法进行测试，重金属总量小于百万分之十。The montmorillonite obtained by the above purification is gray, and the purity of the montmorillonite measured by the loss on drying method is 88.1%. Refer to the first method in the Chinese Pharmacopoeia 2015 edition of the fourth general rule 0812 heavy metal inspection method to test, the total amount of heavy metals is less than 10 parts per million.
蒙脱石散的制备：Preparation of montmorillonite powder:
将上述的蒙脱石粉碎过80目筛：葡萄糖粉碎过80目筛；在负压称量罩 下先称量粉碎后的葡萄糖35kg，然后称量粉碎后的蒙脱石100kg，混合30min，即得。The above-mentioned montmorillonite is pulverized through an 80-mesh sieve: the glucose is pulverized through an 80-mesh sieve; under the negative pressure weighing hood, first weigh 35kg of the pulverized glucose, then weigh 100kg of the pulverized montmorillonite, and mix for 30min, that is, have to.
实验例Experimental example
将各实施例和对比例制得的蒙脱石散进行粒度、粒度分布、酸碱度测试，测试结果如下表所示；具体测试方法如下：The montmorillonite powder obtained by each embodiment and the comparative example is subjected to particle size, particle size distribution, pH test, and the test results are shown in the following table; Concrete test method is as follows:
粒度 取蒙脱石散10g，加水500ml，强烈搅拌15min(转速每分钟7000转)，将搅拌后的内容物倾入已用水湿润的药筛(孔径45μm，预先在105℃干燥至恒重)，并用水冲洗药筛至无混悬液斑后，将药筛在105℃干燥3小时，称重。Particle size Take 10g of montmorillonite powder, add 500ml of water, stir vigorously for 15min (rotation speed is 7000 rpm), pour the content after stirring into a sieve (pore size 45μm, pre-dried at 105°C to constant weight), After washing the sieve with water until there is no suspension spot, the sieve was dried at 105°C for 3 hours and weighed.
粒径分布 取蒙脱石散适量(约相当于蒙脱石0.10g)，使检测器遮光率在8％-20％范围，加水800ml，以每分钟3000转的转速搅拌，并同时超声2-3分钟(超声功率16W，振幅3μm)，依2015年版四部通则0982第三法检查，连续测量3次取平均值。Particle size distribution Take an appropriate amount of montmorillonite powder (approximately equivalent to 0.10g of montmorillonite), so that the shading rate of the detector is in the range of 8%-20%, add 800ml of water, stir at a speed of 3000 rpm, and ultrasonically 2- 3 minutes (ultrasonic power 16W, amplitude 3μm), check according to the third method of 0982 of the 2015 edition of the Four General Principles, and take the average value of 3 consecutive measurements.
酸碱度 取蒙脱石散适量(约相当于蒙脱石0.2g)，加水20ml，置水浴上加热2-3分钟后，放冷，滤过，取滤液，依中国药典2015年版四部通则0631中pH值测定法进行测定。pH Take an appropriate amount of montmorillonite powder (approximately equivalent to 0.2g of montmorillonite), add 20ml of water, heat it on a water bath for 2-3 minutes, let it cool, filter, and take the filtrate. value determination method.
表1测试结果Table 1 Test results
Figure PCTCN2021093536-appb-000001
Figure PCTCN2021093536-appb-000001
Figure PCTCN2021093536-appb-000002
Figure PCTCN2021093536-appb-000002
由上表中的数据可知，本发明提供的蒙脱石的纯化方法纯化得到的蒙脱石纯度高，且有毒元素含量低，可直接用于医药领域，尤其是应用该蒙脱石制得的蒙脱石散符合2015版中国药典中蒙脱石散粒度、粒度分布及酸碱度等相关的质量规定。As can be seen from the data in the above table, the montmorillonite obtained by the purification method of the montmorillonite provided by the present invention has high purity and low content of toxic elements, and can be directly used in the field of medicine, especially the montmorillonite obtained by applying the montmorillonite. Montmorillonite powder complies with the relevant quality regulations of montmorillonite powder particle size, particle size distribution and pH in the 2015 edition of the Chinese Pharmacopoeia.

Claims (10)

  1. 一种蒙脱石的纯化方法，其特征在于，包括如下步骤：A method for purifying montmorillonite, comprising the steps of:
    预处理及粗除杂：将膨润土干燥、研磨粉碎，过筛得膨润土粉体；向膨润土粉体中加水和分散剂，打浆，过筛去除粗砂，得浆料；Pretreatment and coarse impurity removal: drying, grinding and pulverizing the bentonite, and sieving to obtain bentonite powder; adding water and dispersant to the bentonite powder, beating, and sieving to remove coarse sand to obtain slurry;
    深度除杂：向浆料中加水形成的悬浮液在搅拌状态下超声，然后经高速离心分离除杂，所得稀浆料经浓缩干燥即得；Deep impurity removal: the suspension formed by adding water to the slurry is sonicated under agitation, and then subjected to high-speed centrifugal separation to remove impurities, and the obtained thin slurry is concentrated and dried;
    其中，分散剂用量为膨润土质量的0.9-1.1％，所述分散剂为质量比为1∶0.2-0.5的碳酸钠和磷酸三钠。Wherein, the dosage of the dispersant is 0.9-1.1% of the mass of the bentonite, and the dispersant is sodium carbonate and trisodium phosphate with a mass ratio of 1:0.2-0.5.
  2. 根据权利要求1所述的蒙脱石的纯化方法，其特征在于，深度除杂步骤中，悬浮液在800-1000r/min搅拌速度下超声处理40-60min；超声频率为50-60KHz。The method for purifying montmorillonite according to claim 1, characterized in that, in the deep impurity removal step, the suspension is ultrasonically treated at a stirring speed of 800-1000r/min for 40-60min; the ultrasonic frequency is 50-60KHz.
  3. 根据权利要求1或2所述的蒙脱石的纯化方法，其特征在于，深度除杂步骤中，浆料与水的质量比为1∶9-10。The method for purifying montmorillonite according to claim 1 or 2, characterized in that, in the deep impurity removal step, the mass ratio of slurry to water is 1:9-10.
  4. 根据权利要求1-3任一项所述的蒙脱石的纯化方法，其特征在于，预处理及粗除杂步骤中，膨润土粉体与水的质量比为1∶2-3；The method for purifying montmorillonite according to any one of claims 1-3, characterized in that, in the pretreatment and rough impurity removal steps, the mass ratio of bentonite powder to water is 1:2-3;
    打浆时间为5-7h。The beating time is 5-7h.
  5. 根据权利要求1-4任一项所述的蒙脱石的纯化方法，其特征在于，将膨润土在70-80℃下干燥4-7h。The method for purifying montmorillonite according to any one of claims 1-4, wherein the bentonite is dried at 70-80° C. for 4-7 hours.
  6. 权利要求1-5任一项所述的蒙脱石的纯化方法纯化得到的蒙脱石。The montmorillonite obtained by the purification method of montmorillonite according to any one of claims 1-5.
  7. 由权利要求6所述的蒙脱石制得的蒙脱石散，其特征在于，包括如下重量份的原料：The montmorillonite powder obtained by the montmorillonite of claim 6 is characterized in that, comprises the raw material of following weight portion:
    蒙脱石90-110份，葡萄糖30-40份。Montmorillonite 90-110 parts, glucose 30-40 parts.
  8. 根据权利要求7所述的蒙脱石散，其特征在于，所述蒙脱石散包括如下重量份的原料：montmorillonite powder according to claim 7, is characterized in that, described montmorillonite powder comprises the raw material of following weight portion:
    蒙脱石100份，葡萄糖35份。100 parts of montmorillonite, 35 parts of glucose.
  9. 一种权利要求7或8所述的蒙脱石散的制备方法，其特征在于，包括如下步骤：A preparation method of the described montmorillonite powder of claim 7 or 8, is characterized in that, comprises the steps:
    将蒙脱石和葡萄糖分别粉碎后过80目筛；然后按选定的重量份数称量、混合、分装，即得。Pulverize the montmorillonite and glucose respectively and pass through an 80-mesh sieve; then weigh, mix and pack according to the selected parts by weight to obtain the obtained product.
  10. 根据权利要求9所述的蒙脱石散的制备方法，其特征在于，混合时间为25-35min。The preparation method of montmorillonite powder according to claim 9, is characterized in that, mixing time is 25-35min.
PCT/CN2021/093536 2021-01-29 2021-05-13 Method for purifying montmorillonite, diosmectite, and preparation method therefor WO2022160507A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202110126294.2A CN112794336A (en) 2021-01-29 2021-01-29 Purification method of montmorillonite, montmorillonite powder and preparation method thereof
CN202110126294.2 2021-01-29

Publications (1)

Publication Number Publication Date
WO2022160507A1 true WO2022160507A1 (en) 2022-08-04

Family

ID=75812867

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2021/093536 WO2022160507A1 (en) 2021-01-29 2021-05-13 Method for purifying montmorillonite, diosmectite, and preparation method therefor

Country Status (2)

Country Link
CN (1) CN112794336A (en)
WO (1) WO2022160507A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116177703A (en) * 2023-01-17 2023-05-30 武汉科莱烯科技有限公司 Preparation method and application of composite two-dimensional montmorillonite paint mist coagulant
CN117446815A (en) * 2023-11-07 2024-01-26 佛山市顺德区特普高实业有限公司 Method for preparing montmorillonite with low ferric oxide content and application thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101774599A (en) * 2009-01-08 2010-07-14 浙江海力生制药有限公司 Modified na-montmorillonite, preparation method and application thereof
CN103848430A (en) * 2012-11-29 2014-06-11 中国地质大学（北京） Method of separating and purifying montmorillonite from calcium bentonite
CN104944430A (en) * 2014-03-31 2015-09-30 中国地质大学（北京） Novel technique for preparing high-purity montmorillonite by deeply purifying bentonite
CN107399742A (en) * 2017-08-25 2017-11-28 芜湖飞尚非金属材料有限公司 A kind of preparation technology of ultra-fine montmorillonite
WO2019120951A1 (en) * 2017-12-22 2019-06-27 Imertech Sas Mineral treatment process

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007051427A1 (en) * 2005-11-04 2007-05-10 Zhejiang Hailisheng Pharmaceutical Limited Co. Modified montmorillonite, method for preparing the same and use thereof
CN101016157A (en) * 2006-02-09 2007-08-15 浙江海力生制药有限公司 Method of purifying montmorillonite, purified montmorillonite and composition thereof
CN100500563C (en) * 2007-03-29 2009-06-17 浙江三鼎科技有限公司 Method for purifying superfine montmorillonite
KR101295204B1 (en) * 2009-01-08 2013-08-09 하이리성 파마수티컬 컴퍼니 리미티드 Modified sodium-montmorillonite, preparing method and uses thereof
CN102406657B (en) * 2010-09-26 2013-03-27 济南康众医药科技开发有限公司 Preparation method of montmorillonite preparations
CN107324351B (en) * 2017-07-06 2018-03-27 四川维奥制药有限公司 A kind of medicinal smectite and its preparation technology

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101774599A (en) * 2009-01-08 2010-07-14 浙江海力生制药有限公司 Modified na-montmorillonite, preparation method and application thereof
CN103848430A (en) * 2012-11-29 2014-06-11 中国地质大学（北京） Method of separating and purifying montmorillonite from calcium bentonite
CN104944430A (en) * 2014-03-31 2015-09-30 中国地质大学（北京） Novel technique for preparing high-purity montmorillonite by deeply purifying bentonite
CN107399742A (en) * 2017-08-25 2017-11-28 芜湖飞尚非金属材料有限公司 A kind of preparation technology of ultra-fine montmorillonite
WO2019120951A1 (en) * 2017-12-22 2019-06-27 Imertech Sas Mineral treatment process

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116177703A (en) * 2023-01-17 2023-05-30 武汉科莱烯科技有限公司 Preparation method and application of composite two-dimensional montmorillonite paint mist coagulant
CN117446815A (en) * 2023-11-07 2024-01-26 佛山市顺德区特普高实业有限公司 Method for preparing montmorillonite with low ferric oxide content and application thereof
CN117446815B (en) * 2023-11-07 2024-06-04 佛山市顺德区特普高实业有限公司 Method for preparing montmorillonite with low ferric oxide content and application thereof

Also Published As

Publication number Publication date
CN112794336A (en) 2021-05-14

Similar Documents

Publication Publication Date Title
WO2022160507A1 (en) Method for purifying montmorillonite, diosmectite, and preparation method therefor
US4166582A (en) Comminution of materials
CN103012850A (en) Process for preparing surface organically modified nano-mineral fibers by one-step method
CN103073010A (en) Environment-friendly production process for high-purity montmorillonite
CN101844772A (en) Process for purifying montmorillonite
CN107902685B (en) A kind of no grinding aid wet-milling, slurry grading system for superfine heavy calcium carbonate technique
CN113979458A (en) Preparation method of boehmite with adjustable particle size
US4119700A (en) Production of pharmaceutical barium sulphate
CN107324351B (en) A kind of medicinal smectite and its preparation technology
CN101139468B (en) Preparation technique of calcination kaoline for butyl rubber plug
CN102951651A (en) Preparation technology of high-purity fine white montmorillonite
CN104510758B (en) A kind of preparation method of PULVIS CORNUS BUBALI CONCEN TRATUS and concentration cornu bubali particle
CN102283860A (en) Preparation method for montmorillonite preparation
CN107413485A (en) A kind of axial-flow type material multi milled processed machinery
CN100418885C (en) High-purity medicinal calcium carbonate and its manufacturing method
CN110669153A (en) Method for extracting agar from gracilaria
CN115057439B (en) Coal gangue activation method without calcination in environment protection
JPH05261262A (en) Preparation of pigment suspension
CN110878014B (en) Method for rapidly extracting gingerol
CN208771624U (en) A kind of flour mill that stability is high
CN108854939B (en) Preparation method and application of modified river sand adsorbent
CN221951387U (en) A Chinese medicine raw material crushing device with impurity separation structure
JP2507571B2 (en) Abrasive manufacturing method
CN111530625A (en) Preparation method of 80-mesh and 200-mesh potassium feldspar dry powder
JP2014065823A (en) Production method of ashless coal

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 21922105

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 21922105

Country of ref document: EP

Kind code of ref document: A1