CN113307290B - Agglomerated magnesium hydroxide with large particle size and preparation method thereof - Google Patents
Agglomerated magnesium hydroxide with large particle size and preparation method thereof Download PDFInfo
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- CN113307290B CN113307290B CN202110553030.5A CN202110553030A CN113307290B CN 113307290 B CN113307290 B CN 113307290B CN 202110553030 A CN202110553030 A CN 202110553030A CN 113307290 B CN113307290 B CN 113307290B
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Abstract
The invention discloses a preparation method of agglomerated magnesium hydroxide with large granularity, which comprises the following steps: preparing a first solution containing magnesium ions, wherein the concentration of the magnesium ions is 0.2-2 mol/L; preparing a second solution containing hydroxide ions, wherein the concentration of the hydroxide ions is 0.1-1.5 mol/L; dropwise adding the second solution into the first solution for reaction to obtain a mixed solution, wherein the molar ratio of the second solution to the first solution is 1.6-3.5, the dropwise adding speed is 0.2-1.0 mol/h, and the pH of the mixed solution is controlled within the range of 6.2-12.5; and filtering, washing and drying the mixed solution to obtain the magnesium hydroxide. The method utilizes a normal-temperature reaction method to control the concentration of magnesium ions and the concentration of hydroxyl ions, controls the reaction process to control the particle size of a magnesium hydroxide product on the premise of accurately controlling the pH value of the reaction, does not add any chemical auxiliary agent, does not heat or pressurize, directly synthesizes the agglomerated magnesium hydroxide with large particle size in one step, and quickly separates and washes the agglomerated magnesium hydroxide.
Description
Technical Field
The invention relates to the technical field of magnesium hydroxide preparation, in particular to an agglomerated magnesium hydroxide with large granularity and a preparation method thereof.
Background
Currently, the most widespread industrial production processes of magnesium hydroxide are hydrothermal method and alkali precipitation method. The hydrothermal method is mainly used for producing ultrafine-particle magnesium hydroxide, and the reaction conditions are strong alkali and high temperature, so that the process control difficulty is high. The alkali liquor precipitation method is usually adopted for production at normal temperature or in a heating mode, the produced magnesium hydroxide is flocculent precipitate, has small particle size and is difficult to filter and wash, and the magnesium hydroxide with large particle size of more than 20 micrometers or even about 80 micrometers is difficult to produce.
Disclosure of Invention
The invention aims to provide an agglomerated magnesium hydroxide with large particle size and a preparation method thereof, which are used for solving the problems of small particle size and difficult filtration of the magnesium hydroxide prepared by the existing production method.
In order to achieve the above purpose, the invention provides the following technical scheme: a preparation method of agglomerated large-particle-size magnesium hydroxide comprises the following steps:
the first step is as follows: preparing a first solution containing magnesium ions, wherein the concentration of the magnesium ions is 0.2-2 mol/L;
the second step is as follows: preparing a second solution containing hydroxide ions, wherein the concentration of the hydroxide ions is 0.1-1.5 mol/L;
the third step: dropwise adding the second solution into the first solution to react to obtain a mixed solution, wherein the molar ratio of the second solution to the first solution is 1.6-3.5, the dropwise adding speed is 0.2-1.0 mol/h, and the pH of the mixed solution is controlled within the range of 6.2-12.5;
the fourth step: and filtering, washing and drying the mixed solution to obtain the agglomerated magnesium hydroxide with large granularity.
According to one embodiment of the invention, in the third step, the second solution is added dropwise at a constant rate.
According to one embodiment of the present invention, in the third step, stirring is performed during the reaction at a stirring rate of 1000 to 3000rpm.
According to an embodiment of the present invention, in the third step, after the dropping of the second solution is completed, the stirring is performed for 10 to 20min.
According to an embodiment of the present invention, in the third step, the reaction conditions are normal temperature and normal pressure.
According to one embodiment of the present invention, the normal temperature is 18 ℃ to 30 ℃, and the normal pressure is a standard atmospheric pressure.
According to one embodiment of the present invention, in the fourth step, the drying temperature is 100 to 150 ℃.
According to one embodiment of the invention, the first solution is waste brine from potash fertilizer production, and is filtered before being prepared.
According to one embodiment of the invention, the second solution is formulated from sodium hydroxide or potassium hydroxide.
The invention also provides magnesium hydroxide prepared by the preparation method of the agglomerated large-particle-size magnesium hydroxide.
Compared with the prior art, the agglomerated large-particle-size magnesium hydroxide and the preparation method thereof provided by the invention have the following advantages:
according to the invention, the concentration of magnesium ions and the concentration of hydroxide ions are both very low, according to the theory of ion mutual attraction, strong electrolyte is completely dissociated in a low-concentration solution, ions are only influenced by coulomb force, the magnesium ions and the hydroxide ions are completely ionized, when the low-concentration hydroxide ions are dripped into the low-concentration magnesium ion solution, the magnesium ions can rapidly react with the corresponding equivalent amount of hydroxide ions to form magnesium hydroxide microcrystals under the influence of coulomb force, the microcrystals mutually attract to form crystal nuclei, because the concentration of the magnesium ions and the hydroxide ions is very low, the generation amount of the crystal nuclei is small, when the hydroxide ions are dripped continuously, the growth rate of the crystal nuclei is greater than the generation rate of the crystal nuclei, the magnesium ions and the hydroxide ions are directionally arranged according to a certain crystal lattice by taking the formed crystal nuclei as the center, and are crystallized to form crystals with larger particles continuously, the D50 particle size range is 20-100 mu m, the dehydration property is good, the filtering and the separation are easy, and the purity of the magnesium hydroxide obtained by filtering and washing reaches more than 99.0%.
The method utilizes a normal-temperature reaction method to control the concentration of magnesium ions and the concentration of hydroxyl ions, controls the reaction process to control the particle size of a magnesium hydroxide product on the premise of accurately controlling the pH value of the reaction, does not add any chemical auxiliary agent, does not heat or pressurize, directly synthesizes the agglomerated magnesium hydroxide with large particle size in one step, and quickly separates and washes the agglomerated magnesium hydroxide.
Drawings
Various additional advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. In the drawings:
FIG. 1 is a process flow diagram of a method for preparing agglomerated large-particle-size magnesium hydroxide according to a preferred embodiment of the present invention;
FIG. 2 is a graph showing the results of a particle size test on magnesium hydroxide prepared in example 1;
FIG. 3 is a graph showing the results of a particle size test on magnesium hydroxide prepared in example 2;
FIG. 4 is a graph showing the results of a particle size test of magnesium hydroxide prepared in comparative example 1.
Detailed Description
The present invention provides many applicable inventive concepts that can be embodied in a wide variety of specific contexts. The specific examples described in the following embodiments of the present invention are merely illustrative of specific embodiments of the present invention and do not limit the scope of the invention.
The invention is further described with reference to the following figures and detailed description of embodiments.
As shown in fig. 1, fig. 1 is a process flow diagram of a method for preparing agglomerated large-particle-size magnesium hydroxide according to a preferred embodiment of the present invention.
The preparation method of the agglomerated large-particle-size magnesium hydroxide comprises the following steps of:
first step S1: preparing a first solution containing magnesium ions, wherein the concentration of the magnesium ions is 0.2-2 mol/L;
a second step S2: preparing a second solution containing hydroxide ions, wherein the concentration of the hydroxide ions is 0.1-1.5 mol/L;
a third step S3: dropwise adding the second solution into the first solution to react to obtain a mixed solution, wherein the molar ratio of the second solution to the first solution is 1.6-3.5, the dropwise adding speed is 0.2-1.0 mol/h, and the pH of the mixed solution is controlled within the range of 6.2-12.5;
fourth step S4: and filtering, washing and drying the mixed solution to obtain the agglomerated magnesium hydroxide with large granularity.
According to the invention, the concentration of magnesium ions and the concentration of hydroxide ions are both very low, according to the theory of ion mutual attraction, strong electrolyte is completely dissociated in a low-concentration solution, ions are only influenced by coulomb force, the magnesium ions and the hydroxide ions are completely ionized, when the low-concentration hydroxide ions are dripped into the low-concentration magnesium ion solution, the magnesium ions can rapidly react with the corresponding equivalent amount of hydroxide ions to form magnesium hydroxide microcrystals under the influence of coulomb force, the microcrystals mutually attract to form crystal nuclei, because the concentration of the magnesium ions and the hydroxide ions is very low, the generation amount of the crystal nuclei is small, when the hydroxide ions are dripped continuously, the growth rate of the crystal nuclei is greater than the generation rate of the crystal nuclei, the magnesium ions and the hydroxide ions are directionally arranged according to a certain crystal lattice by taking the formed crystal nuclei as the center, and are crystallized to form crystals with larger particles continuously, the D50 particle size range is 20-100 mu m, the dehydration property is good, the filtering and the separation are easy, and the purity of the magnesium hydroxide obtained by filtering and washing reaches more than 99.0%.
The method utilizes a normal-temperature reaction method to control the concentration of magnesium ions and the concentration of hydroxyl ions, controls the reaction process to control the particle size of a magnesium hydroxide product on the premise of accurately controlling the pH value of the reaction, does not add any chemical auxiliary agent, does not heat or pressurize, directly synthesizes the agglomerated magnesium hydroxide with large particle size in one step, and quickly separates and washes the agglomerated magnesium hydroxide.
The steps are explained in detail below.
In the first step S1, the first solution containing magnesium ions may be prepared alone, or may be wastewater from other industrial production, such as waste brine from potash fertilizer production, and may contain magnesium ions, and certainly, may not contain other cations capable of producing precipitates with hydroxide ions.
Before the first solution is prepared by using the waste brine produced by the potash fertilizer, filtration is firstly carried out to remove insoluble impurities in the first solution, so as to ensure the purity of the magnesium hydroxide.
In the second step S2, the second solution containing hydroxide ions is prepared from sodium hydroxide or potassium hydroxide, which may be prepared from sodium hydroxide or potassium hydroxide solid, or from a concentrated solution of sodium hydroxide or potassium hydroxide.
In the third step S3, the amount of the second solution added is determined by controlling the PH of the mixed solution.
And slowly dripping the second solution at a constant speed when dripping the second solution, wherein the dripping speed is 0.2-1.0 mol/h, so that local over-concentration is avoided, excessive crystal nucleus is prevented from being generated, and the preparation of the agglomerated magnesium hydroxide with large particle size is ensured.
And continuously stirring in the reaction process, wherein the stirring speed is 1000-3000 rpm, so that the first solution and the second solution are uniformly mixed.
And after the second solution is dropwise added, continuously stirring for 10-20min, enabling hydroxyl ions and magnesium ions to completely react and age, dissolving tiny crystals, depositing the tiny crystals on large crystals to grow, and continuously performing the dissolving-depositing process to obtain the aggregated magnesium hydroxide with large particle size.
The reaction conditions are normal temperature and normal pressure. The normal temperature is 18-30 ℃, and the normal pressure is a standard atmospheric pressure. The reaction process flow is short and easy to operate due to the normal temperature and pressure reaction, and the method is suitable for large-scale industrial production.
In the fourth step S4, the drying temperature is 100 to 150 ℃.
The invention also provides magnesium hydroxide prepared by the preparation method of the agglomerated large-particle-size magnesium hydroxide.
Example 1
Taking waste brine discharged in potassium fertilizer production of a salt lake of Cherokee rose as a raw material, filtering to remove insoluble impurities, taking 100ml of filtered brine, diluting by 10 times according to the volume ratio to obtain 1000ml of diluted first solution, wherein the concentration of magnesium ions in the first solution is 11.2g/L (namely 0.467 mol/L);
taking 50.25g of flake sodium hydroxide analytically pure, preparing the flake sodium hydroxide into a volumetric flask with 1000ml of constant volume to obtain a second solution, wherein the concentration of hydroxyl ions is 1.26mol/L;
stirring 500ml of the first solution at normal temperature and normal pressure, measuring the PH value to be 6.0 at the rotation speed of 2000rpm, taking 1000ml of the prepared second solution, slowly and uniformly dropwise adding the prepared second solution into the first solution through a separating funnel for reaction, wherein the dropwise adding speed is about 12ml/min, the adding is completed after 47.5min, the total amount of the second solution is 570ml, and the molar ratio of the second solution to the first solution is 3.08:1, continuously stirring for 20min, and obtaining a mixed solution after the reaction is finished, wherein the pH value of the mixed solution is 11;
filtering the mixed solution after reaction for 10min, separating, washing, and drying at 100 ℃ for 6h to obtain the agglomerated magnesium hydroxide with large particle size.
The results of the particle size measurement of the magnesium hydroxide by a MasterSIZE-2000 laser particle sizer are shown in FIG. 2. As shown in figure 2, the magnesium hydroxide prepared by the method is an agglomerated large-particle-size product, and the D50 particle size is in the range of 20-100 mu m.
Example 2
Taking waste brine discharged in potassium fertilizer production of a salt lake of Kerr as a raw material, filtering to remove insoluble impurities, taking 100ml of filtered brine, and diluting by 20 times according to the volume ratio to obtain 2000ml of diluted first solution, wherein the concentration of magnesium ions in the first solution is 5.5g/L (namely 0.23 mol/L);
taking 50.25g of flake sodium hydroxide analytically pure, preparing the flake sodium hydroxide into a volumetric flask with 1000ml of constant volume to obtain a second solution, wherein the concentration of hydroxyl ions is 1.26mol/L;
stirring 500ml of the first solution at normal temperature and normal pressure, wherein the rotating speed is 2000rpm, taking 500ml of the prepared second solution, slowly and uniformly dropwise adding the second solution into the first solution through a separating funnel for reaction, wherein the dropwise adding speed is about 10ml/min, after 28min, the second solution is added to account for 280ml, and the molar ratio of the second solution to the first solution is 3.07:1, continuously stirring for 20min, and obtaining a mixed solution after the reaction is finished, wherein the pH value of the mixed solution is 10.5;
filtering and washing the mixed solution after reaction, and drying for 6h at 100 ℃ to obtain the agglomerated magnesium hydroxide with large particle size.
The results of the particle size measurement of the magnesium hydroxide by a MasterSIZE-2000 laser particle sizer are shown in FIG. 3. As shown in figure 3, the magnesium hydroxide prepared by the method is an agglomerated large-particle-size product, and the D50 particle size is in the range of 20-100 microns.
Example 3
Prepared according to the procedure of example 1, except that the concentration of magnesium ions in the first solution was 0.2mol/L, the second solution was prepared from potassium hydroxide solid, the concentration of hydroxide ions was 0.1mol/L, and the dropping rate of the second solution was 0.2mol/h; during the reaction, the end point of the addition of the second solution is that the pH of the mixed solution reaches 6.2.
Example 4
Prepared according to the procedure of example 1, but the concentration of magnesium ions in the first solution is 2mol/L, the second solution is prepared from potassium hydroxide solution, the concentration of hydroxide ions is 1.5mol/L, and the dropping speed of the second solution is 0.69mol/h; during the reaction, the end point of the addition of the second solution is that the pH of the mixed solution reaches 12.5.
Example 5
Prepared according to the procedure of example 1, but the concentration of magnesium ions in the first solution is 1.2mol/L, the second solution is prepared from a sodium hydroxide solution, the concentration of hydroxide ions is 0.9mol/L, and the dropping speed of the second solution is 1mol/h; during the reaction, the end point of the addition of the second solution is that the pH of the mixed solution reaches 8.8.
Example 6
Prepared according to the procedure of example 1, but the concentration of magnesium ions in the first solution is 0.8mol/L, the second solution is prepared from a sodium hydroxide solution, the concentration of hydroxide ions is 0.5mol/L, and the dropping speed of the second solution is 0.58mol/h; during the reaction, the end point of the addition of the second solution is that the pH of the mixed solution reaches 7.5.
Example 7
Prepared according to the procedure of example 1, but the concentration of magnesium ions in the first solution is 1.65mol/L, the second solution is prepared from a sodium hydroxide solution, the concentration of hydroxide ions is 1.08mol/L, and the dropping speed of the second solution is 0.43mol/h; in the reaction process, the addition end point of the second solution is that the pH value of the mixed solution reaches 9.
The magnesium hydroxide prepared in the above examples 3 to 7 has a D50 particle size of 20 to 100 μm, which is measured by a MASTERSIZE-2000 laser particle size analyzer, requires only about 10 minutes for filtration, and has good dehydration property, easy filtration, and easy separation.
Comparative example 1
Taking waste brine discharged in potassium fertilizer production of a salt lake of Kerr as a raw material, filtering to remove insoluble impurities, taking 500ml of filtered brine, and obtaining a first solution without diluting, wherein the concentration of magnesium ions in the first solution is 112.0g/L (namely 4.67 mol/L);
taking 48.00g of flake sodium hydroxide analytically pure, preparing the flake sodium hydroxide into a 200ml volumetric flask with constant volume to obtain a second solution, wherein the concentration of hydroxide ions is 6mol/L;
stirring 500ml of the first solution at normal temperature, wherein the rotating speed is 2000rpm, taking 200ml of the prepared second solution, slowly adding the second solution into the first solution through a separating funnel at the speed of about 100ml/min, after 2min, continuously stirring for 20min without controlling the reaction pH, and obtaining a mixed solution after the reaction;
after the reaction is finished, the generated white precipitate cannot be layered for a long time, and when the filtering operation is carried out, the separation difficulty of solid and liquid is very high. Filtering the reacted mixed solution for a long time, washing, and drying at 100 ℃ for 6 hours to obtain the magnesium hydroxide.
The results of the particle size measurement of the magnesium hydroxide by a MasterSIZE-2000 laser particle sizer are shown in FIG. 4. As shown in FIG. 4, when the first solution containing magnesium ions at a higher concentration is reacted with the second solution containing hydroxide ions at a higher concentration, the particle size D50 of the obtained product is about 11 μm, the settling rate of the particles is slow, and the difficulty of filtration is high without controlling the pH value of the reaction.
Comparative example 2
Prepared according to the procedure in example 1, with the difference that: the concentration of magnesium ions in the first solution was 0.18mol/L.
Comparative example 3
Prepared according to the procedure in example 1, with the difference that: in the first solution, the concentration of magnesium ions was 2.3mol/L.
Comparative example 4
Prepared according to the procedure in example 1, with the difference that: in the second solution, the concentration of hydroxide ions was 0.08mol/L.
Comparative example 5
Prepared according to the procedure in example 1, with the difference that: in the second solution, the concentration of hydroxide ions was 1.7mol/L.
Comparative example 6
Prepared according to the procedure in example 1, with the difference that: the first solution is added dropwise to the second solution.
Comparative example 7
Prepared according to the procedure in example 1, with the difference that: the molar ratio of the second solution to the first solution is 1.5.
Comparative example 8
Prepared according to the procedure in example 1, with the only difference that: the molar ratio of the second solution to the first solution was 3.8.
Comparative example 9
Prepared according to the procedure in example 1, with the difference that: the dropping rate was 1.5mol/h.
Comparative example 10
Prepared according to the procedure in example 1, with the difference that: the dropping rate was 0.1mol/h.
The magnesium hydroxide prepared in the above comparative examples 2 to 9 has a D50 particle size of less than 20 μm, and requires at least 30 minutes for filtration, and is difficult to filter and separate, as measured by a MASTERSIZE-2000 laser particle sizer; in comparative example 10, the reaction time was too long.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and that those skilled in the art will be able to design alternative embodiments without departing from the scope of the appended claims. In the claims, any reference signs placed between parentheses shall not be construed as limiting the claim. The word "comprising" does not exclude the presence of elements or steps not listed in a claim.
Claims (4)
1. A preparation method of agglomerated large-particle-size magnesium hydroxide is characterized by comprising the following steps: the method comprises the following steps:
first step (S1): preparing a first solution containing magnesium ions, wherein the concentration of the magnesium ions is 0.2-2 mol/L;
second step (S2): preparing a second solution containing hydroxide ions, wherein the concentration of the hydroxide ions is 0.1-1.5 mol/L;
third step (S3): dropwise adding the second solution into the first solution at a constant speed for reaction to obtain a mixed solution, wherein the molar ratio of the second solution to the first solution is 1.6-3.5, the dropwise adding speed is 0.2-1.0 mol/h, stirring is carried out in the reaction process, the stirring speed is 1000-3000 rpm, and the pH of the mixed solution is controlled within the range of 6.2-12.5;
fourth step (S4): filtering, washing and drying the mixed solution to obtain agglomerated magnesium hydroxide with large granularity,
wherein, in the third step, the reaction condition is normal temperature and normal pressure, the normal temperature is 18 ℃ to 30 ℃, the normal pressure is a standard atmospheric pressure,
the second solution is prepared from sodium hydroxide or potassium hydroxide.
2. The method for preparing agglomerated large-particle-size magnesium hydroxide according to claim 1, characterized in that: in the third step, stirring for 10-20min after the second solution is dropwise added.
3. The method for preparing agglomerated large-particle-size magnesium hydroxide according to claim 1, wherein: wherein, in the fourth step, the drying temperature is 100-150 ℃.
4. The method for preparing agglomerated large-particle-size magnesium hydroxide according to claim 1, characterized in that: wherein the first solution is waste brine produced in potash fertilizer production, and is filtered before being prepared.
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| JPS60155529A (en) * | 1984-01-20 | 1985-08-15 | Asahi Glass Co Ltd | Production of high-purity magnesium hydroxide |
| IE921328A1 (en) * | 1992-04-23 | 1993-11-03 | Defped Ltd | Particulate magnesium hydroxide |
| WO2008120746A1 (en) * | 2007-03-30 | 2008-10-09 | Ube Material Industries, Ltd. | Magnesium hydroxide powder and method for producing the same |
| CN101234769B (en) * | 2008-03-04 | 2010-08-11 | 贵州大学 | Technique for preparing high purity ultra-fine magnesium hydroxide by sodium hydroxide method |
| CN101362603A (en) * | 2008-09-03 | 2009-02-11 | 河北科技大学 | A kind of method for preparing high-purity magnesium hydroxide |
| CN101700899A (en) * | 2009-10-28 | 2010-05-05 | 钟辉 | Technology for producing and preparing high-purity lamellar magnesium hydroxide |
| CN101857248B (en) * | 2010-06-01 | 2011-11-09 | 浙江海虹控股集团有限公司 | Method for preparing large-grain magnesium hydroxide by taking highly acid ammonium salt as crystal control agent |
| CN102815729A (en) * | 2012-09-18 | 2012-12-12 | 清华大学深圳研究生院 | High-dispersity magnesium hydroxide powder and preparation method thereof in oil phase |
| CN103803598A (en) * | 2012-11-15 | 2014-05-21 | 潘洪海 | Preparation method of micron-sized magnesium hydroxide particles |
| CN103408045B (en) * | 2013-08-01 | 2015-11-18 | 四川龙蟒磷化工有限公司 | A kind of method utilizing phosphorus ore de-magging waste liquid to prepare magnesium hydroxide |
| CN104261442A (en) * | 2014-07-08 | 2015-01-07 | 云天化集团有限责任公司 | Method for preparing magnesium hydroxide |
| JP7132800B2 (en) * | 2018-09-12 | 2022-09-07 | 神島化学工業株式会社 | Magnesium hydroxide particles and method for producing the same |
| CN110642274B (en) * | 2019-10-24 | 2022-04-22 | 西部矿业集团有限公司 | A method for preparing hexagonal flake magnesium hydroxide for flame retardants by a large particle size magnesium hydroxide hydrothermal method |
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