CN114369290A - Surface organic modified talcum powder filler and preparation method and application thereof - Google Patents

Surface organic modified talcum powder filler and preparation method and application thereof Download PDF

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Publication number
CN114369290A
CN114369290A CN202111521710.5A CN202111521710A CN114369290A CN 114369290 A CN114369290 A CN 114369290A CN 202111521710 A CN202111521710 A CN 202111521710A CN 114369290 A CN114369290 A CN 114369290A
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talcum powder
organically
parts
aqueous solution
modified talc
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董诗琪
董大洋
胡飞
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Maanshan Goody Plastic Co ltd
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Maanshan Goody Plastic Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The embodiment of the invention relates to the technical field of material processing, and particularly discloses a surface organic modified talcum powder filler and a preparation method and application thereof, wherein the surface organic modified talcum powder filler comprises the following raw materials: talcum powder, surface treating agent and solvent; wherein the surface treatment agent is an aqueous solution of an alkyl silicate. According to the embodiment of the invention, the talc powder is treated by adopting a wet process and taking an alkyl silicate aqueous solution as a surface treatment agent, so that the phenomenon of insufficient surface treatment uniformity effect in dry treatment is avoided, a large amount of waste water is not generated, the production cost is low, and the problem that the surface treatment uniformity effect cannot be ensured while the production cost is reduced in the existing talc powder filler surface treatment process is solved. Moreover, the preparation method provided by the embodiment of the invention is simple and has wide market prospect.

Description

Surface organic modified talcum powder filler and preparation method and application thereof
Technical Field
The embodiment of the invention relates to the technical field of material processing, in particular to a surface organic modified talcum powder filler and a preparation method and application thereof.
Background
With the continuous progress of science and technology, the performance requirements of the market for materials are also continuously improved. Among them, the polymer material is also generally called a polymer material, is a material having a polymer compound as a matrix, and generally comprises a polymer compound, an inorganic filler and an auxiliary agent. At present, high polymer materials are generally applied to the fields of buildings, the electrical and electronic industry, transportation, agriculture and the like.
The inorganic filler has important significance in the preparation of high polymer materials: on one hand, the method has the effect of reducing the cost, and on the other hand, the method has the effect of improving the mechanical properties such as hardness, strength and the like of the material. Among them, talc is a common filler in the field of polymer material processing due to its low price, and has wide applications in polypropylene, polyethylene, polycarbonate, ABS (Acrylonitrile Butadiene Styrene) plastics, rubber and paint. The talcum powder mainly contains magnesium silicate hydroxide (Mg)3Si4O10(OH)2) The inorganic compound has strong polarity on the surface, so that the inorganic compound is difficult to be uniformly mixed with a low-polarity or non-polar polymer matrix, effective bonding and combination are difficult to form between the filler and the interface of the resin matrix, the improvement of the material strength is not facilitated, and the dispersion of the filler in the resin matrix is also not facilitated.
In order to solve the problems, a silane coupling agent, a titanate coupling agent, an aluminate coupling agent and the like are commonly used for carrying out surface treatment on the talcum powder filler by adopting a dry method or a wet method process. However, the above technical solutions have the following disadvantages in practical use: the dry method is to carry out surface reaction on the atomized coupling agent and the filler or directly carry out mixed reaction on the coupling agent and the inorganic filler, but because the dosage of the coupling agent is very small, the surface treatment of the filler is difficult to be uniform in the dry treatment process, the uniform effect of the surface treatment cannot be ensured, and the oil absorption of the product is too high. In addition, the wet process is also called solution process, and is to stir talc powder and aqueous solution of coupling agent for reaction and treatment, but most of the coupling agents undergo hydrolysis reaction in the aqueous solution to polymerize, which not only affects the treatment effect of the filler, but also shortens the service life of the aqueous solution of the coupling agent, thereby generating a large amount of wastewater to be treated and increasing the production cost.
Disclosure of Invention
The embodiment of the invention aims to provide a surface organic modified talcum powder filler, which solves the problem that the surface treatment uniformity effect cannot be ensured while the production cost is reduced in the conventional talcum powder filler surface treatment process proposed in the background art.
In order to achieve the above purpose, the embodiments of the present invention provide the following technical solutions:
the surface organic modified talcum powder filler comprises the following raw materials: talcum powder, surface treating agent and proper amount of solvent; wherein the surface treatment agent is an aqueous solution of an alkyl silicate.
As a further scheme of the embodiment of the invention: the surface organic modified talcum powder filler comprises the following components in parts by weight:
10-60 parts of talcum powder
5-70 parts of surface treating agent
50-350 parts of deionized water
Wherein the surface treating agent is an alkyl silicate aqueous solution.
As a further scheme of the embodiment of the invention: the surface treating agent is alkyl silicate aqueous solution with the mass percentage concentration of 20-40%.
As a further scheme of the embodiment of the invention: the surface treating agent is a sodium methyl silicate aqueous solution with the mass percentage concentration of 30 percent.
Another object of an embodiment of the present invention is to provide a method for preparing a surface-organically-modified talc filler, including the following steps:
1) weighing the surface treating agent and the solvent, and uniformly mixing to obtain a mixture (namely surface treating agent diluent);
2) weighing talcum powder, adding the talcum powder into the mixture, and stirring to obtain a stirred material (namely a reaction mixed solution);
3) and carrying out suction filtration on the stirred material, carrying out filtration drying, placing a filter cake in an environment of 60-125 ℃ for heat preservation for 0.5-4 hours, and grinding into powder to obtain the surface organic modified talcum powder filler.
The embodiment of the invention also aims to provide an application of the surface organic modified talcum powder filler in preparation of high polymer materials.
Compared with the prior art, the embodiment of the invention has the beneficial effects that:
the surface organic modified talcum powder filler provided by the embodiment of the invention is prepared by adopting a wet process and treating talcum powder by taking alkyl silicate aqueous solution as a surface treating agent, so that the phenomenon of insufficient surface treatment uniformity effect in dry treatment is avoided, and meanwhile, a large amount of waste water is not generated and the production cost is low; compared with the traditional process, the embodiment of the invention has the following effective effects: (1) the traditional silane coupling agent belongs to organic matters, volatile organic matters such as methanol and the like can be generated during hydrolysis, the stability of the aqueous solution is poor, the aqueous solution cannot be used for a long time, and the formed wastewater treatment difficulty is higher. According to the invention, a wet process is adopted to organically modify the talcum powder, the adopted alkyl silicate aqueous solution has high storage stability, can be used for a long time, does not generate organic volatile matters in the treatment process, and has excellent environmental protection performance; (2) the price of the alkyl silicate adopted by the invention is far lower than that of the traditional coupling agent, and the production cost can be effectively reduced. (3) Compared with the traditional coupling agent treatment process, the talcum powder surface treatment process adopted by the embodiment of the invention has the advantages of simple and convenient and quick process operation, can be used for preparing other types of surface organic modified inorganic fillers, and has wide market prospect.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the embodiments of the present invention, but are not intended to limit the embodiments of the present invention in any way. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the embodiments of the present invention. These are all within the scope of the embodiments of the present invention.
The embodiment of the invention provides a surface organic modified talcum powder filler, which comprises the following raw materials: talcum powder, surface treating agent and proper amount of solvent; wherein the surface treatment agent is an aqueous solution of an alkyl silicate. The surface organic modified talcum powder filler provided by the embodiment of the invention has the characteristics of excellent environmental protection performance, low production cost and simple and convenient process operation. Because the coupling agent and the inorganic filler are not mixed and reacted by a dry method, but are treated by a wet method process and alkyl silicate aqueous solution as a surface treating agent, the phenomenon of insufficient surface treatment uniformity effect in the dry method treatment is avoided, simultaneously, a large amount of waste water is not generated, the production cost is low, and the problem that the surface treatment uniformity effect cannot be ensured while the production cost is reduced in the existing talcum powder filler surface treatment process is solved.
As another preferred embodiment of the present invention, the surface-organized modified talc powder filler comprises the following raw materials in parts by weight: 1-70 parts of talcum powder, 1-80 parts of surface treating agent and 0-500 parts of solvent.
As another preferred embodiment of the present invention, the surface-organized modified talc powder filler comprises the following raw materials in parts by weight: 10-60 parts of talcum powder, 5-70 parts of surface treating agent and 50-350 parts of solvent.
As another preferred embodiment of the present invention, the solvent is selected from deionized water, mineral water, distilled water, and soft water, which is not limited herein and may be selected as needed.
Preferably, the solvent is selected from deionized water. At the moment, the surface organic modified talcum powder filler is composed of the following components in parts by weight:
10-60 parts of talcum powder
5-70 parts of surface treating agent
50-350 parts of deionized water
Wherein the surface treating agent is an alkyl silicate aqueous solution.
As another preferable embodiment of the present invention, the surface treatment agent is an alkyl silicate aqueous solution having a mass percentage concentration of 20 to 40%.
As another preferred embodiment of the present invention, the alkyl silicate structure in the aqueous solution of alkyl silicate is represented by the following formula:
Figure BDA0003407739410000051
wherein, R is alkyl (specifically alkyl chains with different lengths), and M is univalent metal ions.
As another preferred example of the embodiment of the present invention, the monovalent metal ion is any one of a sodium ion and a potassium ion.
Preferably, the monovalent metal ion is a sodium ion.
As another preferred example of the present invention, the alkyl group is any one or more of methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, and tert-butyl.
Preferably, the alkyl group is methyl.
Further preferably, the surface treatment agent is a sodium methyl silicate aqueous solution with a mass percentage concentration of 30%.
The embodiment of the invention also provides a preparation method of the surface organic modified talcum powder filler, which comprises the following steps:
1) weighing the surface treating agent and the solvent according to the proportion, and uniformly mixing to obtain a mixture (namely surface treating agent diluent);
2) weighing talcum powder (in proportion) and adding the talcum powder into the mixture to be stirred to obtain a stirred material (namely reaction mixed liquid);
3) carrying out suction filtration on the stirred material so as to separate the talcum powder from the surface treating agent diluent; and (3) after filtration, placing the filter cake in an environment of 60-125 ℃ for heat preservation for 0.5-4 hours, and grinding into powder to obtain the surface organic modified talcum powder filler.
As another preferred embodiment of the invention, in the preparation method of the surface organic modified talcum powder filler, the heat preservation is carried out by drying according to the conditions of heat preservation at 60 ℃ for 0.5 hour, heat preservation at 110 ℃ for 1-3 hours and heat preservation at 125 ℃ for 2-4 hours in sequence.
As another preferred embodiment of the present invention, the solvent is deionized water. In this case, preferably, the method for preparing the surface-organized modified talc powder filler comprises the following steps:
1) mixing deionized water and alkyl silicate water solution, and stirring uniformly to obtain surface treating agent diluent;
2) adding talcum powder into the surface treating agent diluent prepared in the step 1) at room temperature, and stirring for 0.5-2 hours to obtain a stirred material;
3) carrying out suction filtration on the stirred material obtained in the step 2) to separate the talcum powder from the diluent of the surface treating agent; after being dried by filtration, the filter cake is directly put into an oven to be dried according to the conditions of heat preservation for 0.5 hour at 60 ℃, 1 to 3 hours at 110 ℃ and 2 to 4 hours at 125 ℃;
4) and (3) grinding the dried product in the step 3) into fine powder in an agate mortar to obtain the surface organically modified talcum powder, namely the surface organically modified talcum powder filler.
Preferably, the alkyl silicate aqueous solution is an alkyl silicate solution having a concentration of 30% by mass, more preferably an alkyl sodium silicate solution, and still more preferably a methyl sodium silicate solution. After the talcum powder is mixed and contacted with the sodium alkyl silicate solution, hydroxyl on the surface of talcum powder particles and hydroxyl in alkyl silicate anions are subjected to condensation reaction to introduce alkyl to the surfaces of the talcum powder particles, alkyl silicate on the surfaces of the talcum powder particles generates alkyl silanol under the action of water and carbon dioxide (the carbon dioxide can be air or carbon dioxide contained in water, or carbon dioxide additionally blown in the stirring and mixing process according to needs, or carbon dioxide introduced in the heat preservation process), and an organic silicon film can be formed on the surfaces of the talcum powder particles by the condensation reaction between the alkyl silanol and the condensation reaction with the hydroxyl on the surfaces of the talcum powder particles, so that the organic modification of the surfaces of the talcum powder particles is realized. The organic modification can reduce the oil absorption of the talcum powder, thereby being beneficial to forming a stronger interface layer with a high polymer matrix.
The embodiment of the invention also provides the surface organic modified talcum powder filler prepared by the preparation method of the surface organic modified talcum powder filler.
The embodiment of the invention also provides an application of the surface organic modified talcum powder filler in preparation of high polymer materials. In particular to the preparation of products such as rubber, fiber, plastic, polymer adhesive, polymer coating, polymer-based composite material and the like.
As another preferred embodiment of the present invention, the polymer material is any one of a polypropylene composite material, a polyethylene composite material, a polycarbonate composite material, ABS plastic, rubber, or paint.
The technical effects of the surface-organized modified talc filler of the present invention will be further described below by referring to specific examples.
Example 1
The surface organic modified talcum powder filler comprises the following raw materials: 30 g of talcum powder, 10 g of sodium methyl silicate aqueous solution with the mass percentage concentration of 30 percent and 290 g of deionized water.
In this embodiment, the method for preparing the surface-organized modified talc powder filler specifically includes the following steps:
(1) mixing and stirring deionized water and sodium methyl silicate aqueous solution uniformly to obtain surface treating agent diluent;
(2) adding talcum powder into the surface treating agent diluent prepared in the step (1) at room temperature, and stirring for 0.75 hour to complete the reaction to obtain a reaction mixed solution;
(3) carrying out suction filtration on the reaction mixed liquid in the step (2) to separate the talcum powder from the surface treating agent diluent; after being dried by filtration, the filter cake is directly put into an oven to be dried according to the conditions of heat preservation for 0.5 hour at 60 ℃, 2 hours at 110 ℃ and 3 hours at 125 ℃;
(4) and (4) grinding the dried product obtained in the step (3) into fine powder in an agate mortar to obtain the surface organic modified talcum powder filler.
Example 2
Compared to example 1, except that the raw material composition was: the procedure of example 1 was repeated except that 50 g of talc, 20 g of a 30% sodium methyl silicate aqueous solution, 280 g of deionized water, and a diluent of a surface treatment agent were mixed with talc and reacted for 1 hour with stirring.
Example 3
Compared to example 1, except that the raw material composition was: the procedure of example 1 was repeated except that 15 g of talc, 60 g of a 30% aqueous solution of sodium methylsilicate, 240 g of deionized water, and a diluent of a surface treatment agent were mixed with talc and reacted for 1.5 hours under stirring.
Example 4
The unmodified talc starting material from example 1 was used as a reference for comparison with the other examples.
Specifically, the formulations of the above examples are shown in table 1:
table 1 composition of the formulations
Group of Talcum powder 30% aqueous sodium methylsilicate solution Deionized water
Example 1 30 10 290
Example 2 50 20 280
Example 3 15 60 240
Reference sample 30 0 0
As can be seen from the data in Table 1, the surface-organized modified talcum powder filler provided by the embodiments 1-3 of the invention is treated by a wet process and alkyl silicate aqueous solution as a surface treating agent, and has the advantages of simple and rapid process operation compared with the traditional coupling agent treatment process.
Example 5
Compared with the example 1, the method is the same as the example 1 except that the mass percent concentration of the sodium methylsilicate aqueous solution is 20 percent.
Example 6
Compared with the example 1, the method is the same as the example 1 except that the mass percent concentration of the sodium methylsilicate aqueous solution is 25 percent.
Example 7
Compared with the example 1, the method is the same as the example 1 except that the mass percent concentration of the sodium methylsilicate aqueous solution is 35 percent.
Performance detection
Performance testing was performed on the surface organically modified talc fillers prepared in examples 1 to 3 and the unmodified talc of example 4. Specifically, according to GB/T5211.15-2014 Universal test method part 15: measurement of oil absorption the oil absorption was measured and the results are shown in table 2, which shows that the talc surface treatment technique of the present invention can reduce the oil absorption of talc and thus prove that the surface organic modification of talc is achieved.
TABLE 2 shear impact Strength test results Table
Figure BDA0003407739410000091
As can be seen from the data in Table 2, the surface-organically modified talc filler prepared in example 1 of the present invention has a lower oil absorption than unmodified talc, indicating that the surface of the talc has been covered with organic groups; is favorable for forming effective bonding and combination with the basic interface of the macromolecular compound, improves the material strength and is also favorable for the dispersion of the filler in the macromolecular compound matrix material.
The oil absorption has important guiding significance for selecting the filler, and the oil absorption directly influences the processing performance of the high polymer material, and the high oil absorption of the filler can reduce the fluidity of the high polymer material and deteriorate the molding process performance. The talcum powder surface treatment technology of treating talcum powder by adopting a wet process and taking alkyl silicate aqueous solution as a surface treatment agent can reduce the oil absorption of the talcum powder, realize the surface organic modification of the talcum powder, and is favorable for forming effective bonding and combination with a high molecular compound matrix material interface.
To further illustrate the technical advantages of the surface organically modified talc filler of example 1 of the present invention, the storage stability of the aqueous silane coupling agent solution used in the prior art and the aqueous sodium methyl silicate solution of the present invention example are compared as follows: the storage period of the silane coupling agent treatment solution is about 1 week, while the sodium methyl silicate aqueous solution of the embodiment of the invention can be stored for about 1 month, so that the storage period is greatly prolonged; in addition, the silane coupling agent treatment solution can also cause the problem of wastewater treatment, the embodiment of the invention adopts the sodium methylsilicate aqueous solution, so that the environment is protected, the problem of wastewater treatment is reduced, and the cost is greatly reduced, compared with a talcum powder filler product organically modified by adopting the silane coupling agent, the cost of the surface organically modified talcum powder filler prepared by the embodiment of the invention is reduced by about 90%. According to the invention, the talc powder is organically modified by adopting a wet process, the adopted alkyl silicate aqueous solution has high storage stability, can be used for a long time, does not generate organic volatile matters in the treatment process, and has excellent environmental protection performance.
According to the above results, the beneficial effects of the embodiment of the invention are as follows, the surface organic modified talcum powder filler provided by the embodiment of the invention is prepared by adopting a wet process and treating talcum powder by taking an alkyl silicate aqueous solution as a surface treatment agent, compared with the traditional process, the phenomenon of insufficient surface treatment uniformity effect in dry treatment is avoided, meanwhile, a large amount of waste water is not generated, the production cost is low, the problem that the surface treatment uniformity effect cannot be ensured while the production cost is reduced in the existing talcum powder filler surface treatment process is solved, and the market prospect is wide.
While the preferred embodiments of the present invention have been described in detail, the embodiments of the present invention are not limited to the above embodiments, and various changes can be made without departing from the spirit of the embodiments of the present invention within the knowledge of those skilled in the art. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the embodiments of the present invention are still within the scope of the embodiments of the present invention as thus claimed.

Claims (10)

1. The surface organic modified talcum powder filler is characterized by comprising the following raw materials: talcum powder, surface treating agent and solvent; wherein the surface treatment agent is an aqueous solution of an alkyl silicate.
2. The surface-organically-modified talc filler according to claim 1, wherein said surface-organically-modified talc filler comprises the following raw materials in parts by weight: 1-70 parts of talcum powder, 1-80 parts of surface treating agent and 0-500 parts of solvent.
3. The surface-organically-modified talc filler according to claim 2, characterized in that said surface-organically-modified talc filler comprises the following raw materials in parts by weight: 10-60 parts of talcum powder, 5-70 parts of surface treating agent and 50-350 parts of solvent.
4. The surface-organically modified talc filler according to claim 1, wherein said aqueous solution of alkyl silicate is 20 to 40% by mass.
5. The surface-organically modified talc filler according to claim 1, wherein said alkyl silicate is a monovalent metal ion silicate, and said monovalent metal ion is any one of sodium ion and potassium ion.
6. The surface-organically modified talc filler according to claim 1, wherein said surface treatment agent is an aqueous solution of sodium methyl silicate having a concentration of 30% by mass.
7. A process for the preparation of an organically surface-modified talc filler according to any one of claims 1 to 6, characterized by the steps of:
1) weighing a surface treating agent and a solvent, and uniformly mixing to obtain a mixture;
2) weighing talcum powder, adding the talcum powder into the mixture, and stirring to obtain a stirred material;
3) and carrying out suction filtration on the stirred material, carrying out filtration drying, then placing a filter cake in an environment of 60-125 ℃, preserving heat, and grinding to obtain the surface organic modified talcum powder filler.
8. The method for preparing surface-organized modified talcum powder filler according to claim 7, wherein the heat preservation is performed by drying according to the conditions of heat preservation at 60 ℃ for 0.5 hour, heat preservation at 110 ℃ for 1-3 hours and heat preservation at 125 ℃ for 2-4 hours in sequence.
9. Use of a surface organically modified talc as defined in claim 1, 2, 3, 4, 5 or 6 for the preparation of a polymeric material.
10. The use of the surface-organically modified talc filler according to claim 9 for the preparation of a polymer material, wherein said polymer material is any one of polypropylene composite, polyethylene composite, polycarbonate composite, ABS plastic, rubber or paint.
CN202111521710.5A 2021-12-13 2021-12-13 Surface organic modified talcum powder filler and preparation method and application thereof Pending CN114369290A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115386247A (en) * 2022-08-26 2022-11-25 马鞍山顾地塑胶有限公司 In-situ surface coating modified calcium carbonate filler and preparation method and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU1233070A (en) * 1969-03-13 1971-09-16 Laporte Industries Limited Improvements in and relating tothe manufacture of oxides
JPH0848910A (en) * 1994-08-03 1996-02-20 Asahi Glass Co Ltd Surface-treated metal oxide and its production

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU1233070A (en) * 1969-03-13 1971-09-16 Laporte Industries Limited Improvements in and relating tothe manufacture of oxides
JPH0848910A (en) * 1994-08-03 1996-02-20 Asahi Glass Co Ltd Surface-treated metal oxide and its production

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115386247A (en) * 2022-08-26 2022-11-25 马鞍山顾地塑胶有限公司 In-situ surface coating modified calcium carbonate filler and preparation method and application thereof
CN115386247B (en) * 2022-08-26 2023-06-27 马鞍山顾地塑胶有限公司 In-situ surface-coated modified calcium carbonate filler and preparation method and application thereof

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