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CN114231053A - Preparation method of needle-shaped cluster calcium carbonate-silver composite antibacterial material - Google Patents

Preparation method of needle-shaped cluster calcium carbonate-silver composite antibacterial material Download PDF

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Publication number
CN114231053A
CN114231053A CN202111345248.8A CN202111345248A CN114231053A CN 114231053 A CN114231053 A CN 114231053A CN 202111345248 A CN202111345248 A CN 202111345248A CN 114231053 A CN114231053 A CN 114231053A
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calcium carbonate
silver
antibacterial material
composite antibacterial
cluster
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Inventor
田兴友
孙俊
李潇潇
王化
刘研研
张海宝
袁云
袁丽
曹宇翔
高丽
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Zhongke Lemei Technology Group Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02Compounds of alkaline earth metals or magnesium
    • C09C1/021Calcium carbonates
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16Heavy metals; Compounds thereof
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02Compounds of alkaline earth metals or magnesium
    • C09C1/021Calcium carbonates
    • C09C1/022Treatment with inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Zoology (AREA)
  • Plant Pathology (AREA)
  • Pest Control & Pesticides (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Wood Science & Technology (AREA)
  • Agronomy & Crop Science (AREA)
  • Environmental Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material, belonging to the technical field of preparation of antibacterial materials2Carbonizing for more than 2 hours to obtain calcium carbonate slurry, adding the prepared silver-ammonia solution into the calcium carbonate slurry, stirring for reaction for more than 5 hours, and finally performing suction filtration, washing and drying to obtain the calcium carbonate-silver composite antibacterial material. The invention provides a method for feeding materials step by step without changing reaction volumeThe method for preparing the acicular cluster calcium carbonate-silver composite antibacterial material by using the device has the advantages of simple purification and drying of reaction products, uniform powder structure size, acicular cluster morphology, and adjustable product color from white to light brown to brown, and can be applied to the fields of papermaking fillers, plastic modification and the like.

Description

Preparation method of needle-shaped cluster calcium carbonate-silver composite antibacterial material
Technical Field
The invention relates to the technical field of calcium carbonate composite materials, in particular to a preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material.
Background
Calcium carbonate is one of the most widely used inorganic carbonate raw materials in industrial production, has excellent and unique physical and chemical properties, wide sources and low price, is used as a filler and a modifier with excellent performance, is widely applied to industries such as building materials, rubber, plastics, papermaking, coatings, printing ink, food, medicines and the like, can improve the wear resistance, glossiness, dimensional stability, mechanical properties, processability, thickening and anti-settling of products and the like, and improves the comprehensive performance of products. With the development of science and technology, the calcium carbonate industry has developed from the situation of initial extensive mineral exploitation and utilization to the explosive development of large-scale chemical control synthesis production nowadays. The development of nanotechnology leads people to realize that the quality of the performance of calcium carbonate mainly depends on parameters such as the morphology structure, the particle size distribution, the chemical composition, the surface characteristic and the like of a calcium carbonate product, the development of the technology for regulating and controlling the preparation of the calcium carbonate with different morphology characteristics and particle size distribution is a research hotspot in the industry, the research in recent years shows that the calcium carbonate product with unique morphology and performance can be prepared by adding a crystal form control agent, but the introduction of various crystal form control agents increases the production cost on one hand, and introduces impurity ions into the calcium carbonate on the other hand, thereby bringing influences on the purification and the application of subsequent products; in addition, some studies have used soluble calcium salts as precursors for the preparation of calcium carbonate, which obviously also increases the cost of synthetic calcium carbonate. Therefore, the method starts from calcium oxide with wide raw materials and low price, and the method for exploring the preparation process of the low-cost and simple calcium carbonate product is urgent need in the industry. With the improvement of living standard and the enhancement of safety, health and hygiene consciousness of people, people put higher requirements on safety and hygiene of articles such as plastics, paper, food, building materials and the like in daily work and life, and calcium carbonate widely applied as a filler in the fields endows the calcium carbonate with effective antibacterial performance, greatly improves the added value of calcium carbonate products and widens the application field of the calcium carbonate products.
Disclosure of Invention
In order to solve the technical problems in the background technology, the invention provides a preparation method of the needle-shaped cluster calcium carbonate-silver composite antibacterial material, inorganic salt is not required to be added as a crystal form control agent, the needle-shaped cluster calcium carbonate-silver composite antibacterial material is directly prepared by step feeding without changing a reaction container, the preparation method is relatively simple, the operation is simple and convenient, the powder structure is in the shape of the needle-shaped cluster, and the color of the product can be adjusted from white to light brown to brown.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material comprises the following steps:
the method comprises the following steps: firstly, adding calcium oxide and sucrose into water, fully and uniformly mixing, and then fully reacting the mixed solution in a water bath for more than 1 hour;
step two: regulating and controlling the reaction temperature, and introducing CO into the solution2Carbonizing for more than 2 hours to obtain calcium carbonate slurry;
step three: adding the prepared silver-ammonia solution into the calcium carbonate slurry, stirring and reacting for more than 5 hours, and finally performing suction filtration, washing and drying to obtain the calcium carbonate-silver composite antibacterial material
In the technical scheme, further, the concentration of calcium oxide in the first step is 0.1-5mol/L, the concentration of sucrose is 0.001-0.05mol/L, and the temperature of the water bath is 100 ℃.
Further, the reaction temperature in the second step is regulated to be 60-100 ℃, and CO is introduced2The rate of (b) is 2-30 mL/min.
Further, the silver-ammonia solution in the third step is prepared from silver nitrate and ammonia water, and the silver ion concentration is 0.001-0.2 mol/L.
Furthermore, the volume ratio of the calcium oxide and sucrose mixed solution to the silver ammonia solution is 3: 1.
Compared with the prior art for preparing the calcium carbonate material, the method has the outstanding characteristics that inorganic salt is not required to be added as a crystal form control agent, impurity ions are not introduced, the production cost is reduced, and the product is simple to purify; the needle-shaped cluster calcium carbonate-silver composite antibacterial material is directly prepared by feeding materials step by step without changing a reaction container, the production equipment is simple, and the investment cost is low; the product is powder with needle-shaped cluster morphology, has uniform structure size, needle-shaped diameter of hundreds of nanometers, micron-sized length and good compatibility, and can be applied to the fields of papermaking fillers, plastic modification and the like; the color of the product can be adjusted from white to light brown, and meanwhile, the calcium carbonate has antibacterial performance, can be applied to products with antibacterial requirements in industries such as rubber, plastic, papermaking, paint, printing ink and the like, improves the added value of the product, and widens the application field.
Drawings
Fig. 1 is a scanning electron microscope image of the acicular cluster calcium carbonate-silver composite antibacterial material provided by the invention.
Fig. 2 is an EDS energy spectrum of the acicular cluster calcium carbonate-silver composite antibacterial material provided by the present invention.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material comprises the following steps:
the method comprises the following steps: firstly, adding 4.2g of calcium oxide and 0.2565g of cane sugar into 150mL of water, fully and uniformly mixing, and then fully reacting the mixed solution in a water bath at 100 ℃ for 2 hours;
step two: introducing CO into the solution at the speed of 10mL/min in a water bath at 100 DEG C2Carbonizing for 2 hours to obtain calcium carbonate slurry;
step three: weighing 0.17g of silver nitrate, adding the silver nitrate into 50mL of water, uniformly stirring, dropwise adding 1mL of concentrated ammonia water to prepare a silver-ammonia solution, adding the silver-ammonia solution into the calcium carbonate slurry, stirring and reacting for 5 hours, and finally performing suction filtration, washing and drying to obtain the calcium carbonate-silver composite antibacterial material, wherein the product is brown.
FIG. 1 is a scanning electron microscope image of the acicular cluster calcium carbonate-silver composite antibacterial material prepared under the conditions of example 1, and it can be seen from the image that the product is an acicular cluster, the diameter of the needle is about 60-100 nm, and the length is 1-3 microns. Fig. 2 is an EDS energy spectrum of the acicular cluster calcium carbonate-silver composite antibacterial material prepared under the conditions of example 1, and it can be seen from the spectrum that the product mainly consists of Ca, C, O and Ag elements.
Example 2
A preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material comprises the following steps:
the method comprises the following steps: firstly, adding 4.2g of calcium oxide and 0.2565g of cane sugar into 150mL of water, fully and uniformly mixing, and then fully reacting the mixed solution in a water bath at 100 ℃ for 2 hours;
step two: introducing CO into the solution at the speed of 10mL/min in a water bath at 100 DEG C2Carbonizing for 2 hours to obtain calcium carbonate slurry;
step three: weighing 0.034g of silver nitrate, adding the silver nitrate into 50mL of water, uniformly stirring, dropwise adding 0.2mL of concentrated ammonia water to prepare a silver-ammonia solution, adding the silver-ammonia solution into the calcium carbonate slurry, stirring and reacting for 5 hours, and finally performing suction filtration, washing and drying to obtain the calcium carbonate-silver composite antibacterial material, wherein the product is light brown.
Example 3
A preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material comprises the following steps:
the method comprises the following steps: firstly, adding 4.2g of calcium oxide and 0.2565g of cane sugar into 150mL of water, fully and uniformly mixing, and then fully reacting the mixed solution in a water bath at 100 ℃ for 2 hours;
step two: introducing CO into the solution at the speed of 10mL/min in a water bath at 100 DEG C2Carbonizing for 2 hours to obtain calcium carbonate slurry;
step three: weighing 0.0085g of silver nitrate, adding the silver nitrate into 50mL of water, uniformly stirring, dropwise adding 0.05mL of concentrated ammonia water to prepare a silver-ammonia solution, adding the silver-ammonia solution into the calcium carbonate slurry, stirring and reacting for 5 hours, and finally performing suction filtration, washing and drying to obtain the calcium carbonate-silver composite antibacterial material, wherein the product is white.
Example 4
A preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material comprises the following steps:
the method comprises the following steps: adding 4.2g of calcium oxide and 0.0513g of cane sugar into 150mL of water, fully and uniformly mixing, and fully reacting the mixed solution in a water bath at 100 ℃ for 2 hours;
step two: introducing CO2 into the solution at the speed of 10mL/min in a water bath at the temperature of 60 ℃ for carbonization for 2 hours to obtain calcium carbonate slurry;
step three: weighing 0.0085g of silver nitrate, adding the silver nitrate into 50mL of water, uniformly stirring, dropwise adding 0.05mL of concentrated ammonia water to prepare a silver-ammonia solution, adding the silver-ammonia solution into the calcium carbonate slurry, stirring and reacting for 5 hours, and finally performing suction filtration, washing and drying to obtain the calcium carbonate-silver composite antibacterial material, wherein the product is white.
Example 5
A preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material comprises the following steps:
the method comprises the following steps: adding 0.804g of calcium oxide and 0.0513g of cane sugar into 150mL of water, fully and uniformly mixing, and fully reacting the mixed solution in a water bath at 100 ℃ for 1 hour;
step two: introducing the solution into a water bath at 100 ℃ at a rate of 2mL/minInto CO2Carbonizing for 3 hours to obtain calcium carbonate slurry;
step three: weighing 0.0085g of silver nitrate, adding the silver nitrate into 50mL of water, uniformly stirring, dropwise adding 2 drops of concentrated ammonia water to prepare a silver-ammonia solution, adding the silver-ammonia solution into the calcium carbonate slurry, stirring and reacting for 6 hours, and finally performing suction filtration, washing and drying to obtain the calcium carbonate-silver composite antibacterial material, wherein the product is white.
Example 6
A preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material comprises the following steps:
the method comprises the following steps: adding 21g of calcium oxide and 2.565g of cane sugar into 150mL of water, fully and uniformly mixing, and fully reacting the mixed solution in a water bath at 100 ℃ for 5 hours;
step two: introducing CO into the solution at the speed of 30mL/min in a water bath at 100 DEG C2Carbonizing for 5 hours to obtain calcium carbonate slurry;
step three: 1.6987g of silver nitrate is weighed and added into 50mL of water, the mixture is stirred evenly, 10mL of concentrated ammonia water is dripped to prepare silver ammonia solution, then the silver ammonia solution is added into the calcium carbonate slurry, the mixture is stirred and reacts for 10 hours, and finally the calcium carbonate-silver composite antibacterial material is obtained through suction filtration, washing and drying, and the product is brown.
Example 7
A preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material comprises the following steps:
the method comprises the following steps: adding 8.4g of calcium oxide and 0.2565g of cane sugar into 150mL of water, fully and uniformly mixing, and fully reacting the mixed solution in a water bath at 100 ℃ for 2 hours;
step two: introducing CO into the solution at the speed of 20mL/min in a water bath at 100 DEG C2Carbonizing for 3 hours to obtain calcium carbonate slurry;
step three: weighing 0.034g of silver nitrate, adding the silver nitrate into 50mL of water, uniformly stirring, dropwise adding 0.4mL of concentrated ammonia water to prepare a silver-ammonia solution, adding the silver-ammonia solution into the calcium carbonate slurry, stirring and reacting for 6 hours, and finally performing suction filtration, washing and drying to obtain the calcium carbonate-silver composite antibacterial material, wherein the product is light brown.
Group of Quality of calcium oxide Quality of sucrose Quality of silver nitrate Color of antibacterial material
Example 1 4.2g 0.2565g 0.17g Brown colour
Example 2 4.2g 0.2565g 0.034g Light brown
Example 3 4.2g 0.2565g 0.0085g White colour
Example 4 4.2g 0.0513g 0.0085g White colour
Example 5 0.804g 0.0513g 0.0085g White colour
Example 6 21g 2.565g 1.6987g Brown colour
Example 7 8.4g 0.2565g 0.034g Light brown
Compared with the prior art for preparing the calcium carbonate material, the method has the outstanding characteristics that inorganic salt is not required to be added as a crystal form control agent, impurity ions are not introduced, the production cost is reduced, and the product is simple to purify; the needle-shaped cluster calcium carbonate-silver composite antibacterial material is directly prepared by feeding materials step by step without changing a reaction container, the production equipment is simple, and the investment cost is low; the product is powder with needle-shaped cluster morphology, has uniform structure size, needle-shaped diameter of hundreds of nanometers, micron-sized length and good compatibility, and can be applied to the fields of papermaking fillers, plastic modification and the like; the color of the product can be adjusted from white to light brown, and meanwhile, the calcium carbonate has antibacterial performance, can be applied to products with antibacterial requirements in industries such as rubber, plastic, papermaking, paint, printing ink and the like, improves the added value of the product, and widens the application field.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (5)

1. A preparation method of a needle-shaped cluster calcium carbonate-silver composite antibacterial material is characterized by comprising the following steps:
the method comprises the following steps: firstly, adding calcium oxide and sucrose into water, fully and uniformly mixing, and then fully reacting the mixed solution in a water bath for more than 1 hour;
step two: regulating and controlling the reaction temperature, and introducing CO into the solution2Carbonizing for more than 2 hours to obtain calcium carbonate slurry;
step three: and adding a prepared silver-ammonia solution into the calcium carbonate slurry, stirring and reacting for more than 5 hours, and finally performing suction filtration, washing and drying to obtain the calcium carbonate-silver composite antibacterial material.
2. The method for preparing an acicular cluster calcium carbonate-silver composite antibacterial material according to claim 1, characterized in that the calcium oxide concentration in the first step is 0.1-5mol/L, the sucrose concentration is 0.001-0.05mol/L, and the water bath temperature is 100 ℃.
3. The method for preparing the acicular cluster calcium carbonate-silver composite antibacterial material according to claim 1, wherein the reaction temperature in the second step is controlled to be 60-100 ℃, and CO is introduced2The rate of (b) is 2-30 mL/min.
4. The method for preparing an acicular cluster calcium carbonate-silver composite antibacterial material according to claim 1, wherein the silver ammonia solution in step three is prepared from silver nitrate and ammonia water, and the silver ion concentration is 0.001-0.2 mol/L.
5. The method for preparing the acicular cluster calcium carbonate-silver composite antibacterial material according to claim 1, wherein the volume ratio of the calcium oxide and sucrose mixed solution to the silver ammonia solution is 3: 1.
CN202111345248.8A 2021-11-15 2021-11-15 Preparation method of needle-shaped cluster calcium carbonate-silver composite antibacterial material Pending CN114231053A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5169682A (en) * 1990-03-28 1992-12-08 Coral Biotech Co., Ltd. Method of providing silver on calcium carbonate material such as coral sand
JPH0717803A (en) * 1991-03-27 1995-01-20 Shiraishi Chuo Kenkyusho:Kk Antimicrobial calcium carbonate powder
JPH11236304A (en) * 1998-02-20 1999-08-31 Dowa Mining Co Ltd Silver-based antimicrobial composition and its production
JP2006096953A (en) * 2004-09-30 2006-04-13 Nisshin Steel Co Ltd Metal-coated calcium carbonate powder, pigment and resin composition
CN101108741A (en) * 2006-07-21 2008-01-23 北京市化工建材厂 Industrial process for preparing nm-class active calcium carbonate
CN101480194A (en) * 2009-01-22 2009-07-15 河北工业大学 Method for preparing antimicrobial material using nano calcium carbonate as substrate
CN112340763A (en) * 2020-12-07 2021-02-09 江西华明纳米碳酸钙有限公司 Preparation method of special nano calcium carbonate for water-based ink
CN113461042A (en) * 2021-07-19 2021-10-01 合肥工业大学 Optimization method of modification process of nano calcium carbonate

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5169682A (en) * 1990-03-28 1992-12-08 Coral Biotech Co., Ltd. Method of providing silver on calcium carbonate material such as coral sand
JPH0717803A (en) * 1991-03-27 1995-01-20 Shiraishi Chuo Kenkyusho:Kk Antimicrobial calcium carbonate powder
JPH11236304A (en) * 1998-02-20 1999-08-31 Dowa Mining Co Ltd Silver-based antimicrobial composition and its production
JP2006096953A (en) * 2004-09-30 2006-04-13 Nisshin Steel Co Ltd Metal-coated calcium carbonate powder, pigment and resin composition
CN101108741A (en) * 2006-07-21 2008-01-23 北京市化工建材厂 Industrial process for preparing nm-class active calcium carbonate
CN101480194A (en) * 2009-01-22 2009-07-15 河北工业大学 Method for preparing antimicrobial material using nano calcium carbonate as substrate
CN112340763A (en) * 2020-12-07 2021-02-09 江西华明纳米碳酸钙有限公司 Preparation method of special nano calcium carbonate for water-based ink
CN113461042A (en) * 2021-07-19 2021-10-01 合肥工业大学 Optimization method of modification process of nano calcium carbonate

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PRAKASH CHANDRA SAHOO: "Facile fabrication of silver nanoparticle embedded CaCO3 microspheres via microalgae-templated CO2 biomineralization application in antimicrobial paint development", 《RSC ADVANCES》 *
伊昌: "蔗糖、柠檬酸及其复配对合成纳米碳酸钙的影响", 《功能材料》 *
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