CN114058082A - Novel modified silicon dioxide and preparation method thereof - Google Patents
Novel modified silicon dioxide and preparation method thereof Download PDFInfo
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- CN114058082A CN114058082A CN202111335572.1A CN202111335572A CN114058082A CN 114058082 A CN114058082 A CN 114058082A CN 202111335572 A CN202111335572 A CN 202111335572A CN 114058082 A CN114058082 A CN 114058082A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 54
- JOLVYUIAMRUBRK-UHFFFAOYSA-N 11',12',14',15'-Tetradehydro(Z,Z-)-3-(8-Pentadecenyl)phenol Natural products OC1=CC=CC(CCCCCCCC=CCC=CCC=C)=C1 JOLVYUIAMRUBRK-UHFFFAOYSA-N 0.000 claims abstract description 43
- YLKVIMNNMLKUGJ-UHFFFAOYSA-N 3-Delta8-pentadecenylphenol Natural products CCCCCCC=CCCCCCCCC1=CC=CC(O)=C1 YLKVIMNNMLKUGJ-UHFFFAOYSA-N 0.000 claims abstract description 43
- FAYVLNWNMNHXGA-UHFFFAOYSA-N Cardanoldiene Natural products CCCC=CCC=CCCCCCCCC1=CC=CC(O)=C1 FAYVLNWNMNHXGA-UHFFFAOYSA-N 0.000 claims abstract description 43
- PTFIPECGHSYQNR-UHFFFAOYSA-N cardanol Natural products CCCCCCCCCCCCCCCC1=CC=CC(O)=C1 PTFIPECGHSYQNR-UHFFFAOYSA-N 0.000 claims abstract description 43
- JOLVYUIAMRUBRK-UTOQUPLUSA-N Cardanol Chemical compound OC1=CC=CC(CCCCCCC\C=C/C\C=C/CC=C)=C1 JOLVYUIAMRUBRK-UTOQUPLUSA-N 0.000 claims abstract description 42
- 229920000642 polymer Polymers 0.000 claims abstract description 38
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 29
- 239000012043 crude product Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 9
- 238000000967 suction filtration Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 19
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 8
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 4
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000012808 vapor phase Substances 0.000 claims 1
- 230000004048 modification Effects 0.000 abstract description 7
- 238000012986 modification Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 6
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000003607 modifier Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 8
- 239000006087 Silane Coupling Agent Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229910021485 fumed silica Inorganic materials 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 244000226021 Anacardium occidentale Species 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 235000020226 cashew nut Nutrition 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- -1 Cardanol modified white carbon Chemical class 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012767 functional filler Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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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
- C08K9/10—Encapsulated ingredients
-
- 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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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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- 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)
- Silicon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses novel modified silicon dioxide and a preparation method thereof, and the novel modified silicon dioxide mainly comprises the following preparation steps: (1) respectively weighing silicon dioxide, cardanol-based polymer, catalyst and organic solvent; (2) adding silicon dioxide into an organic solvent, uniformly mixing, adding a cardanol-based polymer and a catalyst into the mixture, and reacting at constant temperature; (3) and carrying out suction filtration and drying on the crude product to obtain the modified silicon dioxide particles. According to the invention, the cardanol-based polymer is used as a surfactant to carry out surface modification on the silicon dioxide, so that the agglomeration phenomenon of the silicon dioxide is effectively improved, and the dispersion performance of the silicon dioxide in a polymer matrix is improved. The method is simple, the cardanol-based polymer is used as the surface modifier, the source is wide, the synthesis cost is low, and the method is environment-friendly.
Description
Technical Field
The invention belongs to the technical field of inorganic material preparation, and particularly relates to novel modified silicon dioxide and a preparation method thereof.
Background
Silica is often produced by Chemical Vapor Deposition (CVD) and precipitation processes and has the chemical formula SiO2·nH2O is a porous non-metal nano material, is amorphous white powder at normal temperature, and is non-toxic and pollution-free. Silica has excellent properties such as high dispersibility, good chemical stability, high temperature resistance, and electrical insulation, and is widely used as a functional filler, a catalyst carrier, and the like. However, because a large number of silicon hydroxyl groups exist on the surface of the silicon dioxide, the silicon dioxide is easy to agglomerate in a polymer matrix, the dispersion performance of the silicon dioxide is influenced, and the improvement of the performance of the matrix is further influenced. Therefore, there is a need for surface modification of silica to reduce agglomeration of silica and improve its dispersion in the matrix.
Cardanol, a by-product of the cashew industry, is a natural phenolic substance with a long C15 unsaturated side chain in the meta position. The molecular structure of the material has a plurality of reactive sites, and the material has the advantages of strong chemical modification, wide application, abundant sources, low price, nature, environmental protection and the like. In recent years, cardanol and derivatives thereof have been used to replace a part of chemical raw materials and successfully synthesize various chemical products through research.
At present, most of the modification of silica is carried out by using silane coupling agent, but the traditional silane coupling agent such as silane coupling agent Si-69 and silane coupling agent SI-75 can generate a large amount of volatile organic gas when reacting with the hydroxyl on the surface of silica, and have great harm to industrial production and human health, so researchers are searching for novel environment-friendly and pollution-free surface modifying agents. Influences of Shenmei, Zhang bo, Xin Zhu Xiang, Cardanol modified white carbon black/nano chitin on performances of styrene butadiene rubber/butadiene rubber composite material [ J ] synthetic rubber industry, 2017,40(5):5.) through direct mixing, silicon dioxide is physically modified by cardanol, and dispersing performances of the silicon dioxide are improved to a certain extent. But in the physical modification process, the reaction time is short, the cardanol and silicon dioxide are not tightly combined, and the modification effect is not obvious.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide novel modified silicon dioxide and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme.
A preparation method of novel modified silicon dioxide comprises the following steps:
(1) respectively weighing silicon dioxide, cardanol-based polymer, catalyst and organic solvent;
(2) pouring silicon dioxide and an organic solvent into a three-neck flask with a thermometer and a condenser, uniformly mixing, adding a cardanol-based polymer and a catalyst, uniformly stirring, and reacting at constant temperature;
(3) and carrying out suction filtration and drying on the reaction crude product to obtain the modified silicon dioxide particles.
Preferably, the silica in step (1) is precipitated silica or fumed silica.
Preferably, the cardanol-based polymer in the step (1) is a processed product of refined cardanol, the polymerization degree is 5-20, and the molecular weight is 1500-6000.
Preferably, the catalyst in step (1) is one or more of dibutyltin dilaurate, stannous octoate or dibutyltin diacetate.
Preferably, the mass ratio of the cardanol-based polymer to the silicon dioxide in the step (1) is (0.1-1): 1.
preferably, the mass ratio of the cardanol-based polymer to the silicon dioxide in the step (1) is 0.1:1, 0.2:1, 0.4:1, 0.6:1, 0.8:1, 1: 1.
Preferably, the mass ratio of the cardanol-based polymer to the catalyst in the step (1) is 1: (0.001-0.01).
Preferably, the mass ratio of the cardanol-based polymer to the catalyst in the step (1) is 1:0.001, 1:0.002, 1:0.004, 1:0.006, 1:0.008 or 1: 0.01.
Preferably, the organic solvent in step (2) is one or more of absolute ethyl alcohol, toluene, xylene, ethyl acetate and acetone.
Preferably, the mass ratio percentage of the silicon dioxide to the organic solvent in the step (2) is 20-50%.
Preferably, the rate of agitation is 250-.
Preferably, the isothermal reaction in the step (2) is carried out at the temperature of 60-100 ℃ for 6-12 h.
The novel modified silicon dioxide is prepared by the preparation method.
The novel modified silicon dioxide is modified silicon dioxide by a cardanol-based polymer through a double mechanism of physical adsorption and chemical reaction. The chemical reaction principle of the cardanol-based polymer and silicon dioxide is as follows:
wherein the polymerization degree n is 1-20;
R1is a straight carbon chain- (CH)2)7-、-(CH2)7-CH＝CH-CH2-、-(CH2)7-CH＝CH-CH2-CH＝CH-CH2-one or more of;
R2is-H or a linear carbon chain- (CH)2)2-CH3、-(CH2)5-CH3One or more of (a).
Compared with the prior art, the invention has the advantages and positive effects that:
1. according to the invention, the cardanol-based polymer is directly used for surface modification of silicon dioxide under the condition of not using a silane coupling agent. The cardanol-based polymer modifies the surface of the silicon dioxide through double reactions of physical adsorption and chemical combination, and the silicon dioxide particles are wrapped. The modified silicon dioxide has obviously improved dispersion performance, reduces the agglomeration phenomenon in a polymer matrix, and improves the processing performance and mechanical property of the polymer.
2. The surface modifier used in the invention is a cardanol-based polymer, and the cardanol is used as a raw material and is prepared through a simple synthesis process. The cardanol is a natural phenolic substance extracted from cashew shells, and has the advantages of being renewable, wide in source, low in price, green, environment-friendly and the like.
3. The preparation process has the advantages of simple synthesis and separation steps, high reaction load rate, low toxicity of the solvent, recyclability and contribution to low-cost industrial production.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of silica.
FIG. 2 is a Scanning Electron Microscope (SEM) image of a modified silica of example 1 of the present invention.
Fig. 3 is a Transmission Electron Microscope (TEM) image of silica.
FIG. 4 is a Transmission Electron Microscope (TEM) image of a modified silica in example 2 of the present invention.
FIG. 5 is a graph comparing the infrared spectra of silica and modified silica of example 3 of the present invention.
Detailed Description
The following examples further illustrate the present disclosure, but the embodiments of the present disclosure are not limited thereto. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and substance of the invention.
The starting materials used in the examples are all commercially available.
Example 1
Step (1): 50g of fumed silica, 5g of cardanol-based polymer, 0.05g of dibutyltin dilaurate and 250g of absolute ethyl alcohol are weighed.
Step (2): the silicon dioxide and the absolute ethyl alcohol are poured into a three-neck flask with a thermometer and a condenser, and are stirred for 1 hour at room temperature and mixed uniformly. Then adding cardanol-based polymer and dibutyltin dilaurate, stirring uniformly at 250rpm, heating to 60 ℃, and reacting for 6 h.
And (3): and (3) after the reaction crude product is subjected to suction filtration, putting the reaction crude product into a vacuum oven for drying to obtain powdery modified silicon dioxide particles with the load rate of 4.59%.
Comparing the SEM image of the silica of fig. 1 with the SEM image of the modified silica of example 1 of fig. 2, it can be seen that the unmodified silica is not uniformly dispersed and obvious aggregates appear, while the aggregation of the modified silica is significantly improved and the dispersion effect is enhanced. This is because silica has abundant silicon hydroxyl groups on its surface, high surface energy, and is very prone to agglomeration. After the cardanol-based polymer is modified, the number of silicon hydroxyl groups on the surface of the silicon dioxide is reduced, the surface energy is reduced, and the dispersion condition of the silicon dioxide is improved.
Example 2
Step (1): 50g of fumed silica, 10g of cardanol-based polymer, 0.05g of dibutyltin dilaurate and 250g of absolute ethyl alcohol are weighed.
Step (2): the silicon dioxide and the absolute ethyl alcohol are poured into a three-neck flask with a thermometer and a condenser, and are stirred for 1 hour at room temperature and mixed uniformly. Then adding cardanol-based polymer and dibutyltin dilaurate, stirring uniformly at the stirring speed of 300rpm, heating to 60 ℃, and reacting for 8 h.
And (3): and (3) after the reaction crude product is subjected to suction filtration, putting the reaction crude product into a vacuum oven for drying, and obtaining powdery modified silicon dioxide particles after drying, wherein the loading rate is 8.03%.
Comparing the TEM image of the silica of fig. 3 with the TEM image of the example 2 of fig. 4, it can be seen that the surface energy of the modified silica is reduced and the agglomeration phenomenon is significantly reduced compared to the silica, and the result is in accordance with the observation phenomenon of the SEM image.
Example 3
Step (1): 50g of fumed silica, 20g of cardanol-based polymer, 0.05g of dibutyltin dilaurate and 100g of toluene were weighed.
Step (2): the silicon dioxide and the absolute ethyl alcohol are poured into a three-neck flask with a thermometer and a condenser, and are stirred for 1 hour at room temperature and mixed uniformly. Then adding cardanol-based polymer and dibutyltin dilaurate, stirring uniformly at the stirring speed of 350rpm, heating to 80 ℃, and reacting for 8 h.
And (3): and (3) after the reaction crude product is subjected to suction filtration, putting the reaction crude product into a vacuum oven for drying, and obtaining powdery modified silicon dioxide particles after drying, wherein the loading rate is 15.95%.
FIG. 5 is a graph of a comparison of the infrared spectra of silica and modified silica of example 3 of the present invention, from which it can be observed that: 2930cm-1、2850cm-1And 1450cm-1The peak is a characteristic peak of C-H on the cardanol-based polymer, which indicates that the cardanol-based polymer is successfully loaded on the surface of silicon dioxide.
Example 4
Step (1): weighing 50g of precipitation-process silicon dioxide, 30g of cardanol-based polymer, 0.1g of stannous octoate and 200g of ethyl acetate.
Step (2): the silica and the ethyl acetate are poured into a three-neck flask with a thermometer and a condenser, and stirred for 1 hour at room temperature to be uniformly mixed. Then adding the cardanol-based polymer and stannous octoate, stirring uniformly at the stirring speed of 350rpm, heating to 80 ℃, and reacting for 10 hours.
And (3): and (3) after the reaction crude product is subjected to suction filtration, putting the reaction crude product into a vacuum oven for drying to obtain powdery modified silicon dioxide particles with the loading rate of 24.56%.
Example 5
Step (1): 50g of precipitation-process silica, 50g of cardanol-based polymer, 0.05g of dibutyltin diacetate and 200g of ethyl acetate were weighed.
Step (2): the silica and the toluene are poured into a three-neck flask with a thermometer and a condenser, and are stirred for 1 hour at room temperature and mixed uniformly. Then adding cardanol-based polymer and dibutyltin diacetate, stirring uniformly at the stirring speed of 400rpm, heating to 100 ℃, and reacting for 12 h.
And (3): and (3) after the reaction crude product is subjected to suction filtration, putting the reaction crude product into a vacuum oven for drying, and obtaining powdery modified silicon dioxide particles after drying, wherein the loading rate is 40.09%.
Claims (10)
1. A preparation method of novel modified silicon dioxide is characterized by comprising the following steps:
(1) respectively weighing silicon dioxide, cardanol-based polymer, catalyst and organic solvent;
(2) pouring silicon dioxide and an organic solvent into a three-neck flask with a thermometer and a condenser, uniformly mixing, adding a cardanol-based polymer and a catalyst, uniformly stirring, and reacting at constant temperature;
(3) and carrying out suction filtration and drying on the reaction crude product to obtain the modified silicon dioxide particles.
2. The method according to claim 1, wherein the silica in the step (1) is precipitated silica or vapor phase silica.
3. The method as claimed in claim 1, wherein the cardanol-based polymer in step (1) is a processed product of refined cardanol, and has a polymerization degree of 5-20 and a molecular weight of 1500-6000.
4. The preparation method according to claim 1, wherein the catalyst in step (1) is one or more of dibutyltin dilaurate, stannous octoate or dibutyltin diacetate.
5. The method according to claim 1, wherein the mass ratio of the cardanol-based polymer to the silica in step (1) is (0.1-1): 1.
6. the preparation method according to claim 1, wherein the mass ratio of the cardanol-based polymer to the catalyst in step (1) is 1: (0.001-0.01).
7. The preparation method according to claim 1, wherein the organic solvent in step (2) is one or more of absolute ethanol, toluene, xylene, ethyl acetate and acetone.
8. The preparation method according to claim 1, wherein the mass ratio percentage of the silica to the organic solvent in the step (2) is 20 to 50%.
9. The method as claimed in claim 1, wherein the stirring rate in step (2) is 400 rpm; the temperature of the constant temperature reaction in the step (2) is 60-100 ℃, and the time of the constant temperature reaction is 6-12 h.
10. A novel modified silica produced by the production method according to any one of claims 1 to 9.
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| CN117327373A (en) * | 2023-12-01 | 2024-01-02 | 广州豫顺新材料科技有限公司 | Preparation method of modified nano silicon dioxide toughened epoxy resin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117327373A (en) * | 2023-12-01 | 2024-01-02 | 广州豫顺新材料科技有限公司 | Preparation method of modified nano silicon dioxide toughened epoxy resin |
| CN117327373B (en) * | 2023-12-01 | 2024-02-13 | 广州豫顺新材料科技有限公司 | Preparation method of modified nano silicon dioxide toughened epoxy resin |
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Application publication date: 20220218 |