CN113429806A - Preparation method of high-dispersion modified white carbon black for rubber filler - Google Patents
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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
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3045—Treatment with inorganic compounds
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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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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- 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
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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
- C08L7/00—Compositions of natural rubber
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- 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
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3669—Treatment with low-molecular organic compounds
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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
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3676—Treatment with macro-molecular organic compounds
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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
- C09C1/36—Compounds of titanium
- C09C1/3692—Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/21—Attrition-index or crushing strength of granulates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The invention discloses a preparation method of high-dispersion modified white carbon black for rubber filler, which comprises the following steps: s1: mixing sepiolite powder and white carbon black powder to obtain mixed slurry; s2: adjusting the pH value; s3: adding an emulsifier, carrying out suction filtration and drying to obtain mixed powder; s4, weighing the mixed powder, adding the mixed powder into a toluene solution, and dispersing; s5, adding diisocyanate modifier and organic tin catalyst at the same time, and carrying out condensation reflux reaction for 2-4 h; and S6, adding polyethylene glycol-2000, reacting for 3-4h at constant temperature, drying in vacuum, and grinding to obtain the modified sepiolite/white carbon black powder. According to the invention, Toluene Diisocyanate (TDI) grafted polyethylene glycol (PEG) and hydroxyl groups on the surfaces of the white carbon black and the sepiolite are replaced by isocyanate with better reaction activity, so that the surfaces of the white carbon black and the sepiolite contain aliphatic hydrocarbon functional groups, and the dispersibility of the white carbon black and the sepiolite in rubber is improved.
Description
Technical Field
The invention relates to a preparation method of high-dispersion modified white carbon black for a rubber filler, belonging to the field of rubber additives.
Background
One of the reinforcing materials in the rubber industry is mainly carbon black, and accounts for about 60% or more of the rubber filler. However, carbon black has a number of negative effects during its preparation and use. Carbon black is a byproduct of the petroleum industry, and has high cost and serious pollution in the using process. Therefore, alternatives to carbon black have been sought.
The research on the reinforcing performance of inorganic materials mainly focuses on white carbon black and silicon dioxide. The white carbon black is a reinforcing filling modified material with high specific surface area, high structure and high activity. Because of the special surface area structure and particle morphology and the unique physical and chemical characteristics, the surface activity and the reinforcing performance of the composite filler are more excellent than those of other inorganic light-colored fillers.
However, the surface of the silica particles contains many hydroxyl groups, and there are usually 3 kinds of free hydroxyl groups, continuous hydroxyl groups, and double hydroxyl groups. The surface polarity of the particles is very strong, the surface energy is high, and the particles have extremely strong water absorption, so that the particle agglomeration phenomenon is caused. In addition, the modified silica is difficult to disperse in an organic phase and cannot be well compatible with a sizing material, so that various performance indexes are poor, and therefore, the ideal dispersing effect is difficult to obtain by adding the common white carbon black into the blend.
The sepiolite is a natural hydrous magnesium silicate mineral, has the structural characteristics of chain and layered transition, and is characterized in that a layer of magnesium-oxygen octahedron is sandwiched between two layers of silicon-oxygen tetrahedrons to form a 2:1 layered structure, so that the sepiolite has larger specific surface area and excellent adsorption performance, and is an ideal reinforcing agent for rubber.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a preparation method of high-dispersion modified white carbon black for rubber filler, which is characterized in that sepiolite and white carbon black are blended and modified, the special structure of the sepiolite is utilized as a rubber additive to realize two-phase synergistic interaction, the dispersibility of the white carbon black in rubber is improved, the agglomeration is reduced, and the rubber strength is further improved.
The invention mainly adopts the technical scheme that:
a preparation method of high-dispersion modified white carbon black for rubber filler comprises the following specific steps:
s1: mixing sepiolite powder and white carbon black powder according to a certain mass ratio, dispersing and adding into deionized water, and stirring at a certain stirring speed for 5-10min to obtain mixed slurry;
s2: adding 4-6% dilute hydrochloric acid into the mixed slurry to adjust the pH value to 7-8, adjusting the temperature of the solution to be 60 ℃, and stirring at a certain stirring speed for 10-25min to obtain mixed slurry;
s3: adding a certain amount of emulsifier into the mixed slurry obtained in S2, stirring at low speed for 20min, and performing suction filtration and drying to obtain mixed powder;
s4, weighing a certain amount of mixed powder, adding the mixed powder into the toluene solution, and stirring and dispersing at a low speed for 45-60 min;
s5, adding diisocyanate modifier and organic tin catalyst into the mixed solution obtained in S4, heating to 80 ℃ in water bath, and carrying out condensation reflux reaction for 2-4 h;
and S6, adding a certain amount of polyethylene glycol-2000, reacting for 3-4h at constant temperature, washing with absolute ethyl alcohol for multiple times, filtering, drying in vacuum at 120 ℃, and grinding to obtain the modified sepiolite/white carbon black powder.
Preferably, in the S1, the stirring speed is 800-1000 rpm.
Preferably, in S1, the mass ratio of the sepiolite powder to the white carbon black powder is 1-3: 4.
Preferably, the solid-liquid mass ratio in S1 is 1: 4-5.
Preferably, in the S2, the stirring speed is 600-800 rpm.
Preferably, in the S3, the emulsifier is one or more of TX-10, polyoxyethylene lauryl ether and polyoxyethylene 12-14 carbon primary alcohol.
Preferably, in the S3, the addition amount of the emulsifier is 1% to 2% of white carbon black.
Preferably, the diisocyanate modifier and polyethylene glycol-2000 are added in a molar ratio n (diisocyanates): n (PEG) is 1: 0.6-1.
Preferably, the diisocyanate modifier is hexamethylene diisocyanate or toluene diisocyanate.
Preferably, the addition amount of the polyethylene glycol-2000 is 0.95-2.2% of the mass of the mixed powder.
Has the advantages that: the invention provides a preparation method of high-dispersion modified white carbon black for rubber filler, which has the following advantages compared with the prior art:
(1) the white carbon black particles are coated on the surface of the sepiolite through electrostatic force, so that the structure of the sepiolite can be stabilized to a certain extent, and meanwhile, the surface activity of the fiber can be improved, so that the crosslinking degree of the fiber and natural rubber is increased, and a good synergistic effect is generated.
(2) Meanwhile, the surface modification is carried out on the sepiolite and the white carbon black, the isocyanate with better reaction activity is replaced by the hydroxyl on the surfaces of the white carbon black and the sepiolite through the Toluene Diisocyanate (TDI) grafted polyethylene glycol (PEG), and the isocyanate is fully reacted with the hydroxyl on the surfaces of the white carbon black and the sepiolite and the terminal hydroxyl of the PEG, so that the grafting rate of the PEG on the surfaces of the white carbon black and the sepiolite is improved, the surfaces of the white carbon black and the sepiolite contain aliphatic hydrocarbon functional groups, and the dispersibility of the white carbon black and the sepiolite in rubber is improved.
(3) The emulsifier is added into the slurry of the sepiolite and the white carbon black, so that the moisture content on the surfaces of the white carbon black and the sepiolite can be reduced in the previous stage of slurry treatment, the filtering efficiency of the slurry is improved, and the dispersibility and the hydrophobicity of the white carbon black are effectively improved.
(4) The sepiolite has Si-O group outside the structure, has strong affinity to organic matters, can directly act with an organic reactant, is favorable for improving the compatibility of the white carbon black and the organic reactant, has far lower price than the white carbon black, can greatly reduce the production cost of the rubber auxiliary agent by replacing part of the white carbon black, and simultaneously ensures the rubber strength.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present application, 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 application.
Example 1
A preparation method of high-dispersion modified white carbon black for rubber filler comprises the following specific steps:
s1: mixing 1:4 sepiolite powder and white carbon black powder, dispersing and adding into deionized water (the solid-to-liquid ratio is 1:5), and stirring at 800rpm for 10min to obtain mixed slurry;
s2: adding 5% dilute hydrochloric acid into the mixed slurry to adjust the pH value to 8, adjusting the temperature of the solution to be 60 ℃, and stirring at 600rpm for 25min to obtain mixed slurry;
s3: adding 1% of emulsifier TX-10 into the mixed slurry obtained in S2, stirring at low speed for 20min, and performing suction filtration and drying to obtain mixed powder;
s4, weighing a certain amount of mixed powder, adding the mixed powder into the toluene solution, and stirring and dispersing at a low speed for 45 min;
s5, adding hexamethylene diisocyanate and an organic tin catalyst (dibutyltin dilaurate) into the mixed solution obtained in the S4 at the same time, heating to 80 ℃ in a water bath, and carrying out condensation reflux reaction for 3 hours;
and S6, adding 0.9% of polyethylene glycol-2000, reacting for 3 hours at constant temperature, washing with absolute ethyl alcohol for multiple times, filtering, drying in vacuum at 120 ℃, and grinding to obtain modified sepiolite/white carbon black powder, wherein the molar ratio n (diisocyanate) of the diisocyanate modifier to the addition amount of the polyethylene glycol-2000 is as follows: n (PEG) is 1: 0.6.
Example 2
A preparation method of high-dispersion modified white carbon black for rubber filler comprises the following specific steps:
s1: mixing 1:3 sepiolite powder and white carbon black powder, dispersing and adding into deionized water (the solid-to-liquid ratio is 1:4), and stirring at 800rpm for 10min to obtain mixed slurry;
s2: adding 5% dilute hydrochloric acid into the mixed slurry to adjust the pH value to 8, adjusting the temperature of the solution to be 60 ℃, and stirring at 600rpm for 25min to obtain mixed slurry;
s3: adding 2% of emulsifier TX-10 into the mixed slurry obtained in S2, stirring at low speed for 20min, and performing suction filtration and drying to obtain mixed powder;
s4, weighing a certain amount of mixed powder, adding the mixed powder into the toluene solution, and stirring and dispersing at a low speed for 45 min;
s5, adding hexamethylene diisocyanate and an organic tin catalyst (dibutyltin dilaurate) into the mixed solution obtained in the S4 at the same time, heating to 80 ℃ in a water bath, and carrying out condensation reflux reaction for 3 hours;
and S6, adding 1.2% of polyethylene glycol-2000, reacting for 3 hours at constant temperature, washing with absolute ethyl alcohol for multiple times, filtering, drying in vacuum at 120 ℃, and grinding to obtain modified sepiolite/white carbon black powder, wherein the molar ratio n (diisocyanate) of the diisocyanate modifier to the addition amount of the polyethylene glycol-2000 is as follows: n (PEG) is 1: 0.8.
Example 3
A preparation method of high-dispersion modified white carbon black for rubber filler comprises the following specific steps:
s1: mixing 1:4 sepiolite powder and white carbon black powder, dispersing and adding into deionized water (the solid-to-liquid ratio is 1:5), and stirring at 800rpm for 10min to obtain mixed slurry;
s2: adding 5% dilute hydrochloric acid into the mixed slurry to adjust the pH value to 8, adjusting the temperature of the solution to be 60 ℃, and stirring at 600rpm for 25min to obtain mixed slurry;
s3: adding 1.2% of emulsifier laurinol polyoxyethylene ether into the mixed slurry obtained in the step S2, stirring at a low speed for 20min, and performing suction filtration and drying to obtain mixed powder;
s4, weighing a certain amount of mixed powder, adding the mixed powder into the toluene solution, and stirring and dispersing at a low speed for 45 min;
s5, adding toluene diisocyanate and an organic tin catalyst (dibutyltin dilaurate) into the mixed solution obtained in the S4 at the same time, heating to 80 ℃ in a water bath, and carrying out condensation reflux reaction for 3 hours;
and S6, adding 2.2% of polyethylene glycol-2000, reacting for 3 hours at constant temperature, washing with absolute ethyl alcohol for multiple times, filtering, drying in vacuum at 120 ℃, and grinding to obtain modified sepiolite/white carbon black powder, wherein the molar ratio n (diisocyanate) of the diisocyanate modifier to the addition amount of the polyethylene glycol-2000 is as follows: n (PEG) is 1: 1.
Examples 1, 2 and 3 and ordinary white carbon were kneaded and vulcanized according to the kneading formulations shown in table 1, as shown in table 1, to obtain sample 1, sample 2, sample 3 and sample 4, respectively.
Table 1: the addition amount of each component in the mixing formula
The physical and mechanical properties of the rubber compounds obtained by mixing the above samples 1, 2, 3 and 4 were measured according to the national standards, and the results are shown in table 2.
TABLE 2 results of measuring physical and mechanical properties of each sample
| Sample No. 1 | Sample No. 2 | Sample No. 3 | Sample No. 4 | |
| Tensile stress (100%)/MPa | 7.23 | 7.53 | 7.11 | 4.69 |
| Stretching stressForce (300%)/MPa | 12.81 | 13.01 | 12.64 | 10.65 |
| Tensile strength/MPa | 15.81 | 16.56 | 16.21 | 11.57 |
| Elongation at break/% | 385.21 | 365.32 | 373.56 | 421.25 |
| Tear Strength/kN/m | 68.36 | 75.23 | 69.95 | 51.03 |
According to the experimental results, the tensile strength and the tearing strength of the rubber added with the modified white carbon black are greatly improved. In addition, the elongation at break of the modified rubber is reduced to a certain extent, because the modified powder improves the crosslinking degree of the rubber, thereby enhancing the tensile strength of the rubber but also limiting the movement of rubber molecular chains, and further reducing the elongation at break of the rubber.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of high-dispersion modified white carbon black for rubber filler is characterized by comprising the following specific steps:
s1: mixing sepiolite powder and white carbon black powder according to a certain mass ratio, dispersing and adding into deionized water, and stirring at a certain stirring speed for 5-10min to obtain mixed slurry;
s2: adding 4-6% dilute hydrochloric acid into the mixed slurry to adjust the pH value to 7-8, adjusting the temperature of the solution to be 60 ℃, and stirring at a certain stirring speed for 10-25min to obtain mixed slurry;
s3: adding a certain amount of emulsifier into the mixed slurry obtained in S2, stirring at low speed for 20min, and performing suction filtration and drying to obtain mixed powder;
s4, weighing a certain amount of mixed powder, adding the mixed powder into the toluene solution, and stirring and dispersing at a low speed for 45-60 min;
s5, adding diisocyanate modifier and organic tin catalyst into the mixed solution obtained in S4, heating to 80 ℃ in water bath, and carrying out condensation reflux reaction for 2-4 h;
and S6, adding a certain amount of polyethylene glycol-2000, reacting for 3-4h at constant temperature, washing with absolute ethyl alcohol for multiple times, filtering, drying in vacuum at 120 ℃, and grinding to obtain the modified sepiolite/white carbon black powder.
2. The method for preparing high-dispersion modified white carbon black for the rubber filler according to claim 1, wherein the stirring speed in S1 is 800-1000 rpm.
3. The method for preparing high-dispersion modified white carbon black for the rubber filler according to claim 2, wherein in the step S1, the mass ratio of the sepiolite powder to the white carbon black powder is 1-3: 4.
4. The method for preparing high-dispersion modified white carbon black for the rubber filler according to claim 3, wherein the solid-liquid mass ratio in S1 is 1: 4-5.
5. The method for preparing high dispersion modified white carbon black for rubber filler according to claim 4, wherein in S2, the stirring speed is 600-800 rpm.
6. The method for preparing high dispersion modified silica white for rubber filler according to claim 5, wherein in S3, the emulsifier is one or more of TX-10, polyoxyethylene lauryl ether and polyoxyethylene 12-14 carbon primary alcohol.
7. The method for preparing high-dispersion modified white carbon black for the rubber filler according to claim 6, wherein in the S3, the addition amount of the emulsifier is 1% -2% of white carbon black.
8. The method for preparing high-dispersion modified white carbon black for rubber fillers according to claim 7, wherein the molar ratio n (diisocyanates) of the addition amounts of the diisocyanate modifier and the polyethylene glycol-2000 is as follows: n (PEG) is 1: 0.6-1.
9. The method for preparing high-dispersion modified white carbon black for the rubber filler according to claim 8, wherein the diisocyanate modifier is hexamethylene diisocyanate or toluene diisocyanate.
10. The method for preparing high-dispersion modified white carbon black for the rubber filler according to claim 9, wherein the addition amount of the polyethylene glycol-2000 is 0.9-2.2% of the mass of the mixed powder.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114539814A (en) * | 2022-02-26 | 2022-05-27 | 江苏爱特恩高分子材料有限公司 | Preparation method of high-dispersion white carbon black |
| CN115368755A (en) * | 2022-10-07 | 2022-11-22 | 江苏爱特恩高分子材料有限公司 | Preparation method of vermiculite/white carbon black composite material for rubber filling |
| CN116751411A (en) * | 2023-07-10 | 2023-09-15 | 青岛众祥高分子材料有限公司 | Application of modified sepiolite in rubber |
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| 于清溪: "橡胶填料技术的进步(四)", 《世界橡胶工业》 * |
| 周勇等: "海泡石高填充丁苯橡胶的性能初探", 《特种橡胶制品》 * |
| 崔小明: "白炭黑的生产及改性技术进展", 《中国橡胶》 * |
| 李玉芳: "橡胶填充剂白炭黑的生产及改性技术进展", 《精细化工原料及中间体》 * |
| 李金玲等: "纳米二氧化硅表面改性研究", 《材料开发与应用》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114539814A (en) * | 2022-02-26 | 2022-05-27 | 江苏爱特恩高分子材料有限公司 | Preparation method of high-dispersion white carbon black |
| CN115368755A (en) * | 2022-10-07 | 2022-11-22 | 江苏爱特恩高分子材料有限公司 | Preparation method of vermiculite/white carbon black composite material for rubber filling |
| CN116751411A (en) * | 2023-07-10 | 2023-09-15 | 青岛众祥高分子材料有限公司 | Application of modified sepiolite in rubber |
| CN116751411B (en) * | 2023-07-10 | 2023-12-08 | 青岛众祥高分子材料有限公司 | Application of modified sepiolite in rubber |
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Application publication date: 20210924 |