CN113943497A - Modified calcium carbonate and preparation method thereof - Google Patents
Modified calcium carbonate and preparation method thereof Download PDFInfo
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- CN113943497A CN113943497A CN202010693367.1A CN202010693367A CN113943497A CN 113943497 A CN113943497 A CN 113943497A CN 202010693367 A CN202010693367 A CN 202010693367A CN 113943497 A CN113943497 A CN 113943497A
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- calcium carbonate
- modified calcium
- stabilizer
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
Abstract
The invention provides modified calcium carbonate and a preparation method thereof, wherein the modified calcium carbonate comprises the following raw materials in parts by weight: calcium carbonate, benzoate, a catalyst, an initiator, potassium acetamino sulfonate, sodium bicarbonate, styrene, a plasticizer, sodium persulfate, hydrosol aluminum hydroxide, a compatilizer, a dispersing agent, fumed silica, organic bentonite, polyimide, ammonium bicarbonate, high-abrasion-resistance carbon black, an ultraviolet absorbent, a light stabilizer, an anti-aging agent and a stabilizer. Compared with the prior art, the modified calcium carbonate and the preparation method thereof provided by the invention have the advantages of uniform dispersion, good stability, cost saving and easiness in popularization.
Description
Technical Field
The invention relates to the technical field of calcium carbonate preparation, in particular to modified calcium carbonate and a preparation method thereof.
Background
Calcium carbonate is an important functional inorganic filler, has the advantages of low price, abundant reserves, stable performance, easy processing, no toxicity and the like, can obviously improve the processing performance and physical performance of materials, reduces the production cost and the like, is widely applied to the fields of plastics, rubber, coatings, papermaking and the like, has the defects of insufficient compatibility with high polymers, poor dispersibility and the like in practical application because the calcium carbonate is a hydrophilic compound, cannot achieve a satisfactory filling reinforcing effect, and needs to be modified to improve the dispersibility and compatibility in the coatings so as to achieve the effect of improving the product performance.
In order to improve the reinforcing effect of calcium carbonate, the dispersing performance of the calcium carbonate in the composite material and the physical performance of the modified calcium carbonate filled composite material, different surface modifiers and treatment methods are necessary to modify the surface of calcium carbonate powder, so that the application field of the calcium carbonate is widened.
Therefore, there is a need to provide a novel modified calcium carbonate and a method for preparing the same, which overcomes the above-mentioned drawbacks.
Disclosure of Invention
The invention aims to provide novel modified calcium carbonate and a preparation method thereof, which have the advantages of uniform dispersion, good stability, cost saving and easy popularization.
In order to achieve the purpose, the invention provides modified calcium carbonate which comprises the following raw materials in parts by weight: 200 parts of calcium carbonate, 46-60 parts of benzoate, 0.4-0.6 part of catalyst, 0.2-0.4 part of initiator, 2-4 parts of potassium acetamino sulfonate, 2-3 parts of sodium bicarbonate, 6-10 parts of styrene, 0.5-1 part of plasticizer, 1-3 parts of sodium persulfate, 4-6 parts of hydrosol aluminum hydroxide, 0.3-0.6 part of compatilizer, 0.3-0.5 part of dispersant, 3-5 parts of fumed silica, 2-3 parts of organic bentonite, 2-3 parts of polyimide, 0.4-1 part of ammonium bicarbonate, 2-4 parts of high-wear-resistant carbon black, 0.1-0.4 part of ultraviolet absorbent, 0.2-0.5 part of light stabilizer, 0.3-0.8 part of anti-aging agent and 0.3-0.7 part of stabilizer.
Further, the modified calcium carbonate comprises the following raw materials in parts by weight: 150 parts of calcium carbonate, 46 parts of benzoate, 0.4 part of catalyst, 0.2 part of initiator, 2 parts of potassium acetamino sulfonate, 2 parts of sodium bicarbonate, 6 parts of styrene, 0.5 part of plasticizer, 1 part of sodium persulfate, 4 parts of hydrosol aluminum hydroxide, 0.3 part of compatilizer, 0.3 part of dispersant, 3 parts of fumed silica, 2 parts of organic bentonite, 2 parts of polyimide, 0.4 part of ammonium bicarbonate, 2 parts of high-wear-resistance carbon black, 0.1 part of ultraviolet absorbent, 0.2 part of light stabilizer, 0.3 part of anti-aging agent and 0.3 part of stabilizer.
Further, the modified calcium carbonate comprises the following raw materials in parts by weight: 200 parts of calcium carbonate, 60 parts of benzoate, 0.6 part of catalyst, 0.4 part of initiator, 4 parts of potassium acetamino sulfonate, 3 parts of sodium bicarbonate, 10 parts of styrene, 1 part of plasticizer, 3 parts of sodium persulfate, 6 parts of hydrosol aluminum hydroxide, 0.6 part of compatilizer, 0.5 part of dispersant, 5 parts of fumed silica, 3 parts of organic bentonite, 3 parts of polyimide, 1 part of ammonium bicarbonate, 4 parts of high-abrasion-resistance carbon black, 0.4 part of ultraviolet absorbent, 0.5 part of light stabilizer, 0.8 part of anti-aging agent and 0.7 part of stabilizer.
The invention provides a method for preparing modified calcium carbonate, which comprises the following steps:
step one, crushing calcium carbonate, and screening the crushed calcium carbonate through a 2000-3000-mesh screen to obtain a crushed calcium carbonate;
step two, preparing the crushed calcium carbonate into slurry with the concentration of 4-6%, adding benzoate, a catalyst and an initiator into the slurry, stirring at the temperature of 70-80 ℃ and the rotation speed of 450-800r/min for 30-50min, stopping stirring, adding potassium acetamido sulfonate, sodium bicarbonate and a plasticizer, stirring for 20-30min under the nitrogen atmosphere, adding styrene, heating the mixture to 80 ℃, dropwise adding a potassium persulfate aqueous solution, keeping the temperature at 75 ℃, centrifuging after 2-3h, washing with deionized water, drying in an oven, and crushing into 300-400 meshes to obtain a material A;
step three, uniformly mixing organic bentonite and fumed silica, adding 3-5 times of methanol solution for activation for 30min, grinding in a grinding machine for 2-3h until the particle size is less than 5 mu m, adding deionized water for ultrasonic dispersion uniformly, adding the material A, raising the temperature to 80-100 ℃, performing ultrasonic reflux until the methanol volatilizes, and drying the product to obtain a material B;
and step four, mixing the rest materials, heating to 40-60 ℃, uniformly stirring, adding the material B, stirring for 10-20min at the rotating speed of 1000-1200 rpm, drying at 82-88 ℃ until the water content is less than or equal to 3%, naturally cooling to room temperature, and grinding into nano powder.
Compared with the related technology, the modified calcium carbonate surface is organized, so that the surface of calcium carbonate particles has certain hydrophobicity, the compatibility of calcium carbonate and a polymer is enhanced, the modified calcium carbonate is easy to disperse, difficult to agglomerate, high in mechanical strength, difficult to settle, uniform in dispersion and good in suspension stability, the surface of the calcium carbonate is wear-resistant, oleophilic and hydrophobic, extinguishes fire and the like, the modified calcium carbonate has good compatibility with the polymer, and the interface effect is enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment I is modified calcium carbonate which comprises the following raw materials in parts by weight: 200 parts of calcium carbonate, 46-60 parts of benzoate, 0.4-0.6 part of catalyst, 0.2-0.4 part of initiator, 2-4 parts of potassium acetamino sulfonate, 2-3 parts of sodium bicarbonate, 6-10 parts of styrene, 0.5-1 part of plasticizer, 1-3 parts of sodium persulfate, 4-6 parts of hydrosol aluminum hydroxide, 0.3-0.6 part of compatilizer, 0.3-0.5 part of dispersant, 3-5 parts of fumed silica, 2-3 parts of organic bentonite, 2-3 parts of polyimide, 0.4-1 part of ammonium bicarbonate, 2-4 parts of high-wear-resistant carbon black, 0.1-0.4 part of ultraviolet absorbent, 0.2-0.5 part of light stabilizer, 0.3-0.8 part of anti-aging agent and 0.3-0.7 part of stabilizer.
The compatilizer is modified polyacrylate, the catalyst is a platinum catalyst, the initiator is tert-butyl peroxybenzoate, the plasticizer is di (2-ethylhexyl) phthalate, the ultraviolet absorber is 2-hydroxy-4-methoxybenzophenone, the light stabilizer is a light stabilizer 770, the anti-aging agent is BASF UV-234 anti-aging agent, and the stabilizer is dibasic lead phosphite.
Example two, the modified calcium carbonate comprises the following raw materials in parts by weight: 150 parts of calcium carbonate, 46 parts of benzoate, 0.4 part of catalyst, 0.2 part of initiator, 2 parts of potassium acetamino sulfonate, 2 parts of sodium bicarbonate, 6 parts of styrene, 0.5 part of plasticizer, 1 part of sodium persulfate, 4 parts of hydrosol aluminum hydroxide, 0.3 part of compatilizer, 0.3 part of dispersant, 3 parts of fumed silica, 2 parts of organic bentonite, 2 parts of polyimide, 0.4 part of ammonium bicarbonate, 2 parts of high-wear-resistance carbon black, 0.1 part of ultraviolet absorbent, 0.2 part of light stabilizer, 0.3 part of anti-aging agent and 0.3 part of stabilizer.
The compatilizer is modified polyacrylate, the catalyst is a platinum catalyst, the initiator is tert-butyl peroxybenzoate, the plasticizer is di (2-ethylhexyl) phthalate, the ultraviolet absorber is 2-hydroxy-4-methoxybenzophenone, the light stabilizer is a light stabilizer 770, the anti-aging agent is BASF UV-234 anti-aging agent, and the stabilizer is dibasic lead phosphite.
In the third embodiment, the modified calcium carbonate comprises the following raw materials in parts by weight: 200 parts of calcium carbonate, 60 parts of benzoate, 0.6 part of catalyst, 0.4 part of initiator, 4 parts of potassium acetamino sulfonate, 3 parts of sodium bicarbonate, 10 parts of styrene, 1 part of plasticizer, 3 parts of sodium persulfate, 6 parts of hydrosol aluminum hydroxide, 0.6 part of compatilizer, 0.5 part of dispersant, 5 parts of fumed silica, 3 parts of organic bentonite, 3 parts of polyimide, 1 part of ammonium bicarbonate, 4 parts of high-abrasion-resistance carbon black, 0.4 part of ultraviolet absorbent, 0.5 part of light stabilizer, 0.8 part of anti-aging agent and 0.7 part of stabilizer.
The compatilizer is modified polyacrylate, the catalyst is a platinum catalyst, the initiator is tert-butyl peroxybenzoate, the plasticizer is di (2-ethylhexyl) phthalate, the ultraviolet absorber is 2-hydroxy-4-methoxybenzophenone, the light stabilizer is a light stabilizer 770, the anti-aging agent is BASF UV-234 anti-aging agent, and the stabilizer is dibasic lead phosphite.
The invention provides a method for preparing modified calcium carbonate, which comprises the following steps:
step one, crushing calcium carbonate, and screening the crushed calcium carbonate through a 2000-3000-mesh screen to obtain a crushed calcium carbonate;
step two, preparing the crushed calcium carbonate into slurry with the concentration of 4-6%, adding benzoate, a catalyst and an initiator into the slurry, stirring at the temperature of 70-80 ℃ and the rotation speed of 450-800r/min for 30-50min, stopping stirring, adding potassium acetamido sulfonate, sodium bicarbonate and a plasticizer, stirring for 20-30min under the nitrogen atmosphere, adding styrene, heating the mixture to 80 ℃, dropwise adding a potassium persulfate aqueous solution, keeping the temperature at 75 ℃, centrifuging after 2-3h, washing with deionized water, drying in an oven, and crushing into 300-400 meshes to obtain a material A;
step three, uniformly mixing organic bentonite and fumed silica, adding 3-5 times of methanol solution for activation for 30min, grinding in a grinding machine for 2-3h until the particle size is less than 5 mu m, adding deionized water for ultrasonic dispersion uniformly, adding the material A, raising the temperature to 80-100 ℃, performing ultrasonic reflux until the methanol volatilizes, and drying the product to obtain a material B;
and step four, mixing the rest materials, heating to 40-60 ℃, uniformly stirring, adding the material B, stirring for 10-20min at the rotating speed of 1000-1200 rpm, drying at 82-88 ℃ until the water content is less than or equal to 3%, naturally cooling to room temperature, and grinding into nano powder.
Comparing the performances of the modified calcium carbonate and the unmodified calcium carbonate produced in the embodiments 1 to 3 of the invention, the obtained modified calcium carbonate has the oil absorption value reduced by 52.08 to 53.12 percent compared with the unmodified calcium carbonate, the sedimentation volume reduced by 58.89 to 62.05 percent, the viscosity reduced by 57.58 to 60.79 percent, the bulk density reduced by 20.12 to 21.18 percent, the activation rate improved by 30.09 to 32.58 percent, and the modified calcium carbonate is oleophilic and hydrophobic, has good compatibility with coating, has small bulk density, and has good dispersibility and difficult agglomeration.
Compared with the related technology, the modified calcium carbonate surface is organized, so that the surface of calcium carbonate particles has certain hydrophobicity, the compatibility of calcium carbonate and a polymer is enhanced, the modified calcium carbonate is easy to disperse, difficult to agglomerate, high in mechanical strength, difficult to settle, uniform in dispersion and good in suspension stability, the surface of the calcium carbonate is wear-resistant, oleophilic and hydrophobic, extinguishes fire and the like, the modified calcium carbonate has good compatibility with the polymer, and the interface effect is enhanced.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (4)
1. The modified calcium carbonate is characterized by comprising the following raw materials in parts by weight: 200 parts of calcium carbonate, 46-60 parts of benzoate, 0.4-0.6 part of catalyst, 0.2-0.4 part of initiator, 2-4 parts of potassium acetamino sulfonate, 2-3 parts of sodium bicarbonate, 6-10 parts of styrene, 0.5-1 part of plasticizer, 1-3 parts of sodium persulfate, 4-6 parts of hydrosol aluminum hydroxide, 0.3-0.6 part of compatilizer, 0.3-0.5 part of dispersant, 3-5 parts of fumed silica, 2-3 parts of organic bentonite, 2-3 parts of polyimide, 0.4-1 part of ammonium bicarbonate, 2-4 parts of high-wear-resistant carbon black, 0.1-0.4 part of ultraviolet absorbent, 0.2-0.5 part of light stabilizer, 0.3-0.8 part of anti-aging agent and 0.3-0.7 part of stabilizer.
2. The modified calcium carbonate according to claim 1, comprising the following raw materials in parts by weight: 150 parts of calcium carbonate, 46 parts of benzoate, 0.4 part of catalyst, 0.2 part of initiator, 2 parts of potassium acetamino sulfonate, 2 parts of sodium bicarbonate, 6 parts of styrene, 0.5 part of plasticizer, 1 part of sodium persulfate, 4 parts of hydrosol aluminum hydroxide, 0.3 part of compatilizer, 0.3 part of dispersant, 3 parts of fumed silica, 2 parts of organic bentonite, 2 parts of polyimide, 0.4 part of ammonium bicarbonate, 2 parts of high-wear-resistance carbon black, 0.1 part of ultraviolet absorbent, 0.2 part of light stabilizer, 0.3 part of anti-aging agent and 0.3 part of stabilizer.
3. The modified calcium carbonate according to claim 1, comprising the following raw materials in parts by weight: 200 parts of calcium carbonate, 60 parts of benzoate, 0.6 part of catalyst, 0.4 part of initiator, 4 parts of potassium acetamino sulfonate, 3 parts of sodium bicarbonate, 10 parts of styrene, 1 part of plasticizer, 3 parts of sodium persulfate, 6 parts of hydrosol aluminum hydroxide, 0.6 part of compatilizer, 0.5 part of dispersant, 5 parts of fumed silica, 3 parts of organic bentonite, 3 parts of polyimide, 1 part of ammonium bicarbonate, 4 parts of high-abrasion-resistance carbon black, 0.4 part of ultraviolet absorbent, 0.5 part of light stabilizer, 0.8 part of anti-aging agent and 0.7 part of stabilizer.
4. A method of making the modified calcium carbonate of claim 1, comprising the steps of:
step one, crushing calcium carbonate, and screening the crushed calcium carbonate through a 2000-3000-mesh screen to obtain a crushed calcium carbonate;
step two, preparing the crushed calcium carbonate into slurry with the concentration of 4-6%, adding benzoate, a catalyst and an initiator into the slurry, stirring at the temperature of 70-80 ℃ and the rotation speed of 450-800r/min for 30-50min, stopping stirring, adding potassium acetamido sulfonate, sodium bicarbonate and a plasticizer, stirring for 20-30min under the nitrogen atmosphere, adding styrene, heating the mixture to 80 ℃, dropwise adding a potassium persulfate aqueous solution, keeping the temperature at 75 ℃, centrifuging after 2-3h, washing with deionized water, drying in an oven, and crushing into 300-400 meshes to obtain a material A;
step three, uniformly mixing organic bentonite and fumed silica, adding 3-5 times of methanol solution for activation for 30min, grinding in a grinding machine for 2-3h until the particle size is less than 5 mu m, adding deionized water for ultrasonic dispersion uniformly, adding the material A, raising the temperature to 80-100 ℃, performing ultrasonic reflux until the methanol volatilizes, and drying the product to obtain a material B;
and step four, mixing the rest materials, heating to 40-60 ℃, uniformly stirring, adding the material B, stirring for 10-20min at the rotating speed of 1000-1200 rpm, drying at 82-88 ℃ until the water content is less than or equal to 3%, naturally cooling to room temperature, and grinding into nano powder.
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| CN202010693367.1A CN113943497A (en) | 2020-07-17 | 2020-07-17 | Modified calcium carbonate and preparation method thereof |
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| CN202010693367.1A CN113943497A (en) | 2020-07-17 | 2020-07-17 | Modified calcium carbonate and preparation method thereof |
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Citations (7)
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| CN104927401A (en) * | 2015-06-05 | 2015-09-23 | 安徽雪城超细碳酸钙有限公司 | Modified calcium carbonate and preparation method thereof |
| CN105153750A (en) * | 2015-07-02 | 2015-12-16 | 青阳县恒祥炉料有限公司 | Wear-resistant surface modified calcium carbonate filler and preparation method thereof |
| CN106221292A (en) * | 2016-07-13 | 2016-12-14 | 凤台县泓瀚建筑防水材料厂 | A kind of wear-resisting span carrys out polyimide modified pearl filler |
| CN106397838A (en) * | 2016-09-29 | 2017-02-15 | 贺州钟山县双文碳酸钙新材料有限公司 | Modified calcium carbonate for cables |
| CN106496638A (en) * | 2016-09-29 | 2017-03-15 | 贺州钟山县双文碳酸钙新材料有限公司 | A kind of plastics modified calcium carbonate |
| CN106496637A (en) * | 2016-09-29 | 2017-03-15 | 贺州钟山县双文碳酸钙新材料有限公司 | A kind of rubber modified calcium carbonate |
| CN106519775A (en) * | 2016-09-29 | 2017-03-22 | 贺州钟山县双文碳酸钙新材料有限公司 | Modified calcium carbonate for coating |
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2020
- 2020-07-17 CN CN202010693367.1A patent/CN113943497A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927401A (en) * | 2015-06-05 | 2015-09-23 | 安徽雪城超细碳酸钙有限公司 | Modified calcium carbonate and preparation method thereof |
| CN105153750A (en) * | 2015-07-02 | 2015-12-16 | 青阳县恒祥炉料有限公司 | Wear-resistant surface modified calcium carbonate filler and preparation method thereof |
| CN106221292A (en) * | 2016-07-13 | 2016-12-14 | 凤台县泓瀚建筑防水材料厂 | A kind of wear-resisting span carrys out polyimide modified pearl filler |
| CN106397838A (en) * | 2016-09-29 | 2017-02-15 | 贺州钟山县双文碳酸钙新材料有限公司 | Modified calcium carbonate for cables |
| CN106496638A (en) * | 2016-09-29 | 2017-03-15 | 贺州钟山县双文碳酸钙新材料有限公司 | A kind of plastics modified calcium carbonate |
| CN106496637A (en) * | 2016-09-29 | 2017-03-15 | 贺州钟山县双文碳酸钙新材料有限公司 | A kind of rubber modified calcium carbonate |
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Application publication date: 20220118 |