CN108948661A - A kind of activated Calcium carbonate - Google Patents
A kind of activated Calcium carbonate Download PDFInfo
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- CN108948661A CN108948661A CN201810643866.2A CN201810643866A CN108948661A CN 108948661 A CN108948661 A CN 108948661A CN 201810643866 A CN201810643866 A CN 201810643866A CN 108948661 A CN108948661 A CN 108948661A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L21/00—Compositions of unspecified rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to technical field of composite materials, and in particular to a kind of activated Calcium carbonate.This kind of activated Calcium carbonate is made of following raw material according to parts by weight: 65 ~ 75 parts of calcium carbonate, 20 ~ 36 parts of epoxy resin, 6 ~ 15 parts of triethyl citrate, 11 ~ 18 parts of plant ash, 2 ~ 13 parts of graphene, 1 ~ 9 part of glass fibre, 4 ~ 8 parts of stearic acid, 1 ~ 6 part and 7 ~ 15 parts of activator of silane coupling agent.This kind of activated Calcium carbonate raw material is cheap and easy to get, and production cost is low, excellent with rubber matrix compatibility, has good mechanical performance, wear-resisting property, and reinforcing effect is good.The preparation method of this kind of activated Calcium carbonate is simple, is suitable for industrialized production.
Description
Technical field
The present invention relates to technical field of composite materials, and in particular to a kind of activated Calcium carbonate.
Background technique
Calcium carbonate is a kind of important functional inorganic filling, and nontoxic, tasteless and nonirritant has cheap, storage
The advantages that amount is abundant, chemical stability is good, easy drying, easy coloring, big loading, can significantly improve material processing performance,
Physical property simultaneously reduces production cost, is widely used in the fields such as plastics, rubber, coating, papermaking.
In rubber product, calcium carbonate substituting for carbon black, White Carbon black are used as filler and reinforcing agent and has become reduction
A kind of effective scheme of rubber product production cost.However, calcium carbonate be hydrophilic compounds, surface hydrophilic oleophobic,
Aggregation is easily formed in use, and insufficient with Polymers Phase capacitive, dispersion performance and reinforcing effect are poor, special as filler
It is that can reduce the material performance of material when largely filling, common calcium carbonate has been unable to satisfy the use demand of people.
In order to improve the functional characteristic of calcium carbonate, improve performance indicator, now mainly pass through stearic acid in the industrial production
And its salt, coupling agent, or realize that surface is modified by absorption, surface coating and surface chemistry bonding.But change by these
The processing of property agent, the compatibility between rubber matrix and pearl filler is still undesirable, and interface binding power is weaker, to rubber material
Performance adversely affect.
Activated Calcium carbonate of the invention enhances calcium carbonate surface and rubber-based by being activated to calcium carbonate surface
The compatibility of body promotes the reinforcing property of calcium carbonate, to meet the use demand of people.
Summary of the invention
In order to solve the problems, such as to mention in above-mentioned background, it is an object of that present invention to provide a kind of activated Calcium carbonates.
To achieve the above object, the invention provides the following technical scheme:
A kind of activated Calcium carbonate is made of following raw material according to parts by weight: 65 ~ 75 parts of calcium carbonate, epoxy resin 20 ~ 36
Part, 6 ~ 15 parts of triethyl citrate, 11 ~ 18 parts of plant ash, 2 ~ 13 parts of graphene, 1 ~ 9 part of glass fibre, 4 ~ 8 parts of stearic acid, silicon
1 ~ 6 part and 7 ~ 15 parts of activator of alkane coupling agent.
As a further solution of the present invention: the activated Calcium carbonate is made of: carbon following raw material according to parts by weight
68 ~ 72 parts of sour calcium, 25 ~ 31 parts of epoxy resin, 9 ~ 13 parts of triethyl citrate, 12 ~ 15 parts of plant ash, 6 ~ 10 parts of graphene, glass
3 ~ 7 parts of glass fiber, 5 ~ 7 parts of stearic acid, 2 ~ 5 parts and 10 ~ 14 parts of activator of silane coupling agent.
As a further solution of the present invention: the activated Calcium carbonate is made of: carbon following raw material according to parts by weight
70 parts of sour calcium, it is 29 parts of epoxy resin, 12 parts of triethyl citrate, 14 parts of plant ash, 8 parts of graphene, 4 parts of glass fibre, stearic
6 parts of acid, 3 parts and 11 parts of activator of silane coupling agent.
As a further solution of the present invention: the activator of the activated Calcium carbonate is by zinc oxide, Aluminate, dodecyl
Benzene sulfonic acid sodium salt composition.
As a further solution of the present invention: zinc oxide, Aluminate, dodecyl in the activator of the activated Calcium carbonate
The weight ratio of benzene sulfonic acid sodium salt is 1 ~ 5:3 ~ 10:2 ~ 8.
A kind of preparation method of activated Calcium carbonate, comprising the following steps:
(1) it is uniformly mixed after crushing calcium carbonate with plant ash, is put into high-speed mixer, stirs and heat up, when in mixing machine
When temperature is 80 DEG C, stops heating and silane coupling agent is added, continues to stir 30min, be heated to 110 DEG C, citric acid three is added
Ethyl ester, glass fibre stir 10min, are cooled to room temperature, obtain modified calcium carbonate；
(2) epoxy resin is heated to 75 DEG C, graphene, stearic acid is added, after keeping the temperature 1h, modified calcium carbonate is added, is cooled to
60 DEG C, activator is added, keeps the temperature 1h to get activated Calcium carbonate.
Activated Calcium carbonate of the invention uses calcium carbonate, epoxy resin, plant ash as primary raw material, and raw material is inexpensively easy
, production cost is low, has used plant ash, triethyl citrate, glass fibre to be modified calcium carbonate, has effectively improved carbon
The compatibility of sour calcium and rubber matrix, and then improve the reinforcing property of calcium carbonate；It is added to graphene, glass fibre effectively mentions
The mechanical performance and wear-resisting property for having risen calcium carbonate, used stearic acid as surfactant make calcium carbonate and graphene it
Between combination it is even closer；The activator being made of zinc oxide, Aluminate, neopelex has been used, calcium carbonate is made
Surface active can generate stronger interaction with rubber interface, further promote the mechanical performance and reinforcement of activated Calcium carbonate
Performance.Each ingredient, which cooperates, can the compatibility of play promotion activated Calcium carbonate and rubber matrix.The system of this kind of activated Calcium carbonate
Preparation Method is simple, is suitable for industrialized production.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of activated Calcium carbonate is made of following raw material according to parts by weight: 70 parts of calcium carbonate, ring
29 parts of oxygen resin, 12 parts of triethyl citrate, 14 parts of plant ash, 8 parts of graphene, 4 parts of glass fibre, 6 parts of stearic acid, silane is even
Join 3 parts and 11 parts of activator of agent.
The activator of activated Calcium carbonate is made of zinc oxide, Aluminate, neopelex.
Zinc oxide in the activator of activated Calcium carbonate, Aluminate, neopelex weight ratio be 1:3:2.
A kind of preparation method of activated Calcium carbonate, comprising the following steps:
(1) it is uniformly mixed after crushing calcium carbonate with plant ash, is put into high-speed mixer, stirs and heat up, when in mixing machine
When temperature is 80 DEG C, stops heating and silane coupling agent is added, continues to stir 30min, be heated to 110 DEG C, citric acid three is added
Ethyl ester, glass fibre stir 10min, are cooled to room temperature, obtain modified calcium carbonate；
(2) epoxy resin is heated to 75 DEG C, graphene, stearic acid is added, after keeping the temperature 1h, modified calcium carbonate is added, is cooled to
60 DEG C, activator is added, keeps the temperature 1h to get activated Calcium carbonate.
Embodiment 2
In the embodiment of the present invention, a kind of activated Calcium carbonate is made of following raw material according to parts by weight: 65 parts of calcium carbonate, ring
20 parts of oxygen resin, 6 parts of triethyl citrate, 11 parts of plant ash, 2 parts of graphene, 1 part of glass fibre, 4 parts of stearic acid, silane is even
Join 1 part and 7 parts of activator of agent.
The activator of activated Calcium carbonate is made of zinc oxide, Aluminate, neopelex.
Zinc oxide in the activator of activated Calcium carbonate, Aluminate, neopelex weight ratio be 1:2:1.
A kind of preparation method of activated Calcium carbonate, comprising the following steps:
(1) it is uniformly mixed after crushing calcium carbonate with plant ash, is put into high-speed mixer, stirs and heat up, when in mixing machine
When temperature is 80 DEG C, stops heating and silane coupling agent is added, continues to stir 30min, be heated to 110 DEG C, citric acid three is added
Ethyl ester, glass fibre stir 10min, are cooled to room temperature, obtain modified calcium carbonate；
(2) epoxy resin is heated to 75 DEG C, graphene, stearic acid is added, after keeping the temperature 1h, modified calcium carbonate is added, is cooled to
60 DEG C, activator is added, keeps the temperature 1h to get activated Calcium carbonate.
Embodiment 3
In the embodiment of the present invention, a kind of activated Calcium carbonate is made of following raw material according to parts by weight: 75 parts of calcium carbonate, ring
36 parts of oxygen resin, 15 parts of triethyl citrate, 18 parts of plant ash, 13 parts of graphene, 9 parts of glass fibre, 8 parts of stearic acid, silane
6 parts and 15 parts of activator of coupling agent.
The activator of activated Calcium carbonate is made of zinc oxide, Aluminate, neopelex.
Zinc oxide in the activator of activated Calcium carbonate, Aluminate, neopelex weight ratio be 1:3:3.
A kind of preparation method of activated Calcium carbonate, comprising the following steps:
(1) it is uniformly mixed after crushing calcium carbonate with plant ash, is put into high-speed mixer, stirs and heat up, when in mixing machine
When temperature is 80 DEG C, stops heating and silane coupling agent is added, continues to stir 30min, be heated to 110 DEG C, citric acid three is added
Ethyl ester, glass fibre stir 10min, are cooled to room temperature, obtain modified calcium carbonate；
(2) epoxy resin is heated to 75 DEG C, graphene, stearic acid is added, after keeping the temperature 1h, modified calcium carbonate is added, is cooled to
60 DEG C, activator is added, keeps the temperature 1h to get activated Calcium carbonate.
Embodiment 4
In the embodiment of the present invention, a kind of activated Calcium carbonate is made of following raw material according to parts by weight: 72 parts of calcium carbonate, ring
31 parts of oxygen resin, 13 parts of triethyl citrate, 15 parts of plant ash, 10 parts of graphene, 7 parts of glass fibre, 7 parts of stearic acid, silane
5 parts and 14 parts of activator of coupling agent.
The activator of activated Calcium carbonate is made of zinc oxide, Aluminate, neopelex.
Zinc oxide in the activator of activated Calcium carbonate, Aluminate, neopelex weight ratio be 2:4:1.
A kind of preparation method of activated Calcium carbonate, comprising the following steps:
(1) it is uniformly mixed after crushing calcium carbonate with plant ash, is put into high-speed mixer, stirs and heat up, when in mixing machine
When temperature is 80 DEG C, stops heating and silane coupling agent is added, continues to stir 30min, be heated to 110 DEG C, citric acid three is added
Ethyl ester, glass fibre stir 10min, are cooled to room temperature, obtain modified calcium carbonate；
(2) epoxy resin is heated to 75 DEG C, graphene, stearic acid is added, after keeping the temperature 1h, modified calcium carbonate is added, is cooled to
60 DEG C, activator is added, keeps the temperature 1h to get activated Calcium carbonate.
Embodiment 5
In the embodiment of the present invention, a kind of activated Calcium carbonate is made of following raw material according to parts by weight: 68 parts of calcium carbonate, ring
25 parts of oxygen resin, 9 parts of triethyl citrate, 12 parts of plant ash, 6 parts of graphene, 3 parts of glass fibre, 5 parts of stearic acid, silane is even
Join 2 parts and 10 parts of activator of agent.
The activator of activated Calcium carbonate is made of zinc oxide, Aluminate, neopelex.
Zinc oxide in the activator of activated Calcium carbonate, Aluminate, neopelex weight ratio be 1:5:4.
A kind of preparation method of activated Calcium carbonate, comprising the following steps:
(1) it is uniformly mixed after crushing calcium carbonate with plant ash, is put into high-speed mixer, stirs and heat up, when in mixing machine
When temperature is 80 DEG C, stops heating and silane coupling agent is added, continues to stir 30min, be heated to 110 DEG C, citric acid three is added
Ethyl ester, glass fibre stir 10min, are cooled to room temperature, obtain modified calcium carbonate；
(2) epoxy resin is heated to 75 DEG C, graphene, stearic acid is added, after keeping the temperature 1h, modified calcium carbonate is added, is cooled to
60 DEG C, activator is added, keeps the temperature 1h to get activated Calcium carbonate.
Each 400g of activated Calcium carbonate is prepared according to the formula and preparation method of embodiment 1 ~ 5, control group is set, control group makes
With ordinary calcium carbonate 400g, 1 ~ 5 group of embodiment and control group are separately added into 600g nitrile rubber, obtained using identical technique
To rubber product, the rubber product of each group is tested for the property, test result is as shown in table 1.
The performance of 1 each group rubber product of table
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, and do not carrying on the back
In the case where from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter from which
From the point of view of a bit, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is wanted by appended right
Ask rather than above description limit, it is intended that by all changes that come within the meaning and range of equivalency of the claims
It is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (6)
1. a kind of activated Calcium carbonate, which is characterized in that be made of following raw material according to parts by weight: 65 ~ 75 parts of calcium carbonate, ring
20 ~ 36 parts of oxygen resin, 6 ~ 15 parts of triethyl citrate, 11 ~ 18 parts of plant ash, 2 ~ 13 parts of graphene, 1 ~ 9 part of glass fibre, firmly
4 ~ 8 parts of resin acid, 1 ~ 6 part and 7 ~ 15 parts of activator of silane coupling agent.
2. activated Calcium carbonate according to claim 1, which is characterized in that be made of following raw material according to parts by weight:
68 ~ 72 parts of calcium carbonate, 25 ~ 31 parts of epoxy resin, 9 ~ 13 parts of triethyl citrate, 12 ~ 15 parts of plant ash, 6 ~ 10 parts of graphene,
3 ~ 7 parts of glass fibre, 5 ~ 7 parts of stearic acid, 2 ~ 5 parts and 10 ~ 14 parts of activator of silane coupling agent.
3. activated Calcium carbonate according to claim 1, which is characterized in that be made of following raw material according to parts by weight:
70 parts of calcium carbonate, 29 parts of epoxy resin, 12 parts of triethyl citrate, 14 parts of plant ash, 8 parts of graphene, 4 parts of glass fibre, firmly
6 parts of resin acid, 3 parts and 11 parts of activator of silane coupling agent.
4. activated Calcium carbonate according to claim 1 to 3, it is characterised in that: activator is by zinc oxide, Aluminate, ten
Dialkyl benzene sulfonic acids sodium composition.
5. activated Calcium carbonate according to claim 4, it is characterised in that: zinc oxide, Aluminate, dodecyl in activator
The weight ratio of benzene sulfonic acid sodium salt is 1 ~ 5:3 ~ 10:2 ~ 8.
6. a kind of preparation method of activated Calcium carbonate, which comprises the following steps:
(1) it is uniformly mixed after crushing calcium carbonate with plant ash, is put into high-speed mixer, stirs and heat up, when in mixing machine
When temperature is 80 DEG C, stops heating and silane coupling agent is added, continues to stir 30min, be heated to 110 DEG C, citric acid three is added
Ethyl ester, glass fibre stir 10min, are cooled to room temperature, obtain modified calcium carbonate；
(2) epoxy resin is heated to 75 DEG C, graphene, stearic acid is added, after keeping the temperature 1h, modified calcium carbonate is added, is cooled to
60 DEG C, activator is added, keeps the temperature 1h to get activated Calcium carbonate.
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| CN201810643866.2A CN108948661A (en) | 2018-06-21 | 2018-06-21 | A kind of activated Calcium carbonate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110804250A (en) * | 2019-12-04 | 2020-02-18 | 苏州炜隆灿防静电包装有限公司 | Improved high-strength scratch-resistant polypropylene material and preparation method thereof |
| CN111500089A (en) * | 2020-04-20 | 2020-08-07 | 池州市贵兴非矿新材料有限公司 | Active calcium carbonate and preparation method thereof |
| CN113121905A (en) * | 2021-04-23 | 2021-07-16 | 江西恒东管业有限公司 | Novel steel-plastic composite Krah pipe and preparation method thereof |
| CN113461725A (en) * | 2021-07-05 | 2021-10-01 | 浙江钦堂钙业有限公司 | Long-chain siloxane glyceride, blended calcium carbonate powder activator and preparation method |
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| CN103923365A (en) * | 2014-03-19 | 2014-07-16 | 南京固柏橡塑制品有限公司 | Rubber filler and rubber containing rubber filler |
| CN104910547A (en) * | 2015-05-28 | 2015-09-16 | 青阳县恒源化工原料有限责任公司 | Glass fiber compounded high-strength active calcium carbonate |
| 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 |
| CN107698801A (en) * | 2017-09-30 | 2018-02-16 | 广西华洋矿源材料有限公司 | A kind of modified and light calcium carbonate |
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Patent Citations (5)
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| CN103408795A (en) * | 2013-07-03 | 2013-11-27 | 青阳县永诚钙业有限责任公司 | Modified calcium carbonate with fireproof ceilings and preparation method thereof |
| CN103923365A (en) * | 2014-03-19 | 2014-07-16 | 南京固柏橡塑制品有限公司 | Rubber filler and rubber containing rubber filler |
| CN104910547A (en) * | 2015-05-28 | 2015-09-16 | 青阳县恒源化工原料有限责任公司 | Glass fiber compounded high-strength active calcium carbonate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110804250A (en) * | 2019-12-04 | 2020-02-18 | 苏州炜隆灿防静电包装有限公司 | Improved high-strength scratch-resistant polypropylene material and preparation method thereof |
| CN111500089A (en) * | 2020-04-20 | 2020-08-07 | 池州市贵兴非矿新材料有限公司 | Active calcium carbonate and preparation method thereof |
| CN113121905A (en) * | 2021-04-23 | 2021-07-16 | 江西恒东管业有限公司 | Novel steel-plastic composite Krah pipe and preparation method thereof |
| CN113461725A (en) * | 2021-07-05 | 2021-10-01 | 浙江钦堂钙业有限公司 | Long-chain siloxane glyceride, blended calcium carbonate powder activator and preparation method |
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