CN109354876A - A kind of preparation method of silicon rubber modified white carbon black - Google Patents
A kind of preparation method of silicon rubber modified white carbon black Download PDFInfo
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- CN109354876A CN109354876A CN201811174035.1A CN201811174035A CN109354876A CN 109354876 A CN109354876 A CN 109354876A CN 201811174035 A CN201811174035 A CN 201811174035A CN 109354876 A CN109354876 A CN 109354876A
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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Abstract
The present invention discloses a kind of preparation method of silicon rubber modified white carbon black, comprise the steps of: 1) by main chain contain aromatic ring, the coupling agent of heterocycle or hetero atom rigid radical, organic solvent and water by volume example be 1 ︰ (1~10) ︰ (0.5~2) be hydrolyzed, obtain modified agent emulsion；2) the modified agent emulsion of step 1) is added into white carbon black suspension, at 40~100 DEG C, stirring 0.5~for 24 hours, obtain modified white carbon black suspension；3) by the filtering of step 2) modified white carbon black suspension, dry, crushing, modified white carbon black is obtained.Modified white carbon black produced by the present invention can be improved and be filled into the mechanical property in silicon rubber with silicone rubber matrix compatibility, white carbon black and be also improved.
Description
Technical field
The invention belongs to the preparation technical fields of white carbon black.
Background technique
The production technology of white carbon black is divided into vapor phase method and the precipitation method, and white carbon black has large specific surface area, partial size small, chemical steady
The features such as qualitative good, high temperature resistant and good electrical insulation capability, obtains wide in the industries such as rubber, tire, adhesive, coating, plastics
General application, but a large amount of active silicone hydroxyl is contained on its surface, keeps white carbon black hydrophily stronger, and then make white carbon black in organic group
Wetability is poor in body, it is uneven to disperse.Simultaneously because white carbon black surface energy with higher, is easy to reunite, leads to white carbon black
Aggregate particle size is bigger than normal, cannot reach good reinforcing effect in application.Therefore, surface treatment modification need to be carried out to white carbon black,
Raising and organic matrix compatibility, drop low-surface-energy, increase reinforcing effect, expand its application range.
Silicon rubber during the preparation process, is usually added into white carbon black appropriate to improve the intensity of silicon rubber, improves silicon rubber
Physical property, thus effectively improve silicon rubber application performance.In certain special dimensions, the intensity of silicon rubber is proposed
Higher requirement, this just needs that special modifying agent is selected to be modified white carbon black, to improve the intensity and modulus of silicon rubber.
China Patent Publication No. CN107033630A is by the way that 4,6-diamino isophthalic two are added dropwise into white carbon black dispersion
Silicon rubber white carbon black is made in phenol modifying agent under conditions of high-speed stirred, but surface treatment effect is bad, and white carbon black cannot be very
Good is dispersed in inside silicon rubber organic matrix.China Patent Publication No. CN102731834 A by aerosol with potassium by being mixed
Miscellaneous pyrolytic silicon dioxide is reacted with hexamethyldisilazane, be made silicon rubber white carbon black, but complex process, energy consumption it is higher,
It is not easy to control, and stability is poor.
Therefore, it selects modifying agent and modified technique appropriate to be modified research to white carbon black, improves white carbon black in silicon
Application performance in rubber is of great significance.
Summary of the invention
It is an object of that present invention to provide a kind of preparation methods of silicon rubber modified white carbon black.
Based on above-mentioned purpose, the present invention takes following technical scheme:
A kind of preparation method of silicon rubber modified white carbon black comprising the steps of:
1) by main chain contain aromatic ring, the coupling agent of heterocycle or hetero atom rigid radical, organic solvent and water by volume example be 1 ︰
(1~10) ︰ (0.5~2) is hydrolyzed, and obtains modified agent emulsion；
2) the modified agent emulsion of step 1) is added into white carbon black suspension, at 40~100 DEG C, stirring 0.5~for 24 hours, obtain modification
White carbon black suspension；
3) by the filtering of step 2) modified white carbon black suspension, dry, crushing, modified white carbon black is obtained.
The mass fraction of white carbon black is 5~25% in step 2) white carbon black suspension, and white carbon black suspension takes the precipitation method
It is made.
The additive amount of step 1) coupling agent is the 0.5~10% of step 2 white carbon black quality, and coupling agent is phenyl triethoxy
Silane, phenyltrimethoxysila,e, aryl imide silane, alcyl acid imide silane, anacardol titanate esters, polyethers titanate esters
One or more of mixture.
Organic solvent is one or both of ethyl alcohol, methanol, isopropanol, atoleine, toluene, dimethylbenzene in step 1)
Above mixture.
White carbon black suspension is made by following methods in step 2): bottom liquid and dispersing agent are sequentially added in a kettle, in
At 60-95 DEG C, by concentration be 15-30% sodium silicate aqueous solution and concentration be 40-90% sulfuric acid solution and meanwhile be added in the liquid of bottom,
2-4h is reacted, white carbon black suspension is obtained, the mass ratio of the sulfuric acid in sodium metasilicate and sulfuric acid solution in sodium silicate aqueous solution is 1 ︰
(0.3-0.6) 。
The dispersing agent is macromolecule sodium salt.
The dispersing agent is one of Sodium Polyacrylate, sodium carboxymethylcellulose, sodium alginate, polyglutamic acid sodium or two
Kind or more mixture.
The bottom liquid is water.
Compared with prior art, the invention has the following advantages:
1) coupling agent that main chain contains the rigid radicals such as aromatic ring, heterocycle or hetero atom is modified white carbon black, above-mentioned coupling
One end of agent and the silicone hydroxyl on white carbon black surface occur chemical action and form hydrogen bond, and the organo-functional group of the other end of coupling agent can
It is combined in the form of covalent bond with silicon rubber, between white carbon black and silicon rubber through organic group in the form of so-called " molecular bridge "
It is formed in conjunction with molecule on inorganic interface organic, to improve white carbon black and silicone rubber matrix compatibility, and is contained by main chain
There is the coupling agent modified white carbon black of rigid radical to be filled into silicon rubber the hardness that can significantly improve silicon rubber and stretch strong
Degree；
2) dispersant with high efficiency-macromolecule sodium salt is added in the present invention in the synthesis process of white carbon black, is able to suppress white carbon black synthesis
The reunion of primary partical in the process, making the hard charcoal black track producing particle generated, carefully small ﹑ is uniform, when being filled into silicon rubber, can play and receive
Small-size effect and quantum tunneling effect specific to rice material.
Specific embodiment
Embodiment 1
White carbon black suspension is made by following methods: being sequentially added 519.4 water and 2.6g Sodium Polyacrylate in a kettle, is heated up
To 75 DEG C, it is the sodium silicate aqueous solution that 3.3 concentration are 20% and the sulfuric acid solution that 165g concentration is 60% by 1313g modulus while adds
Enter in water, react 3h, obtain 2000g white carbon black suspension, the mass fraction of white carbon black is 10% in white carbon black suspension.
A kind of preparation method of silicon rubber modified white carbon black comprising the steps of:
1) under ultrasonic wave, by volume it is that 1 ︰, 4 ︰ 1 is hydrolyzed by 6g phenyl triethoxysilane, dehydrated alcohol and water, obtains
Modified agent emulsion；
2) the modified agent emulsion of step 1) is added into 2000g white carbon black suspension to stir 2.5h at 50 DEG C, obtain modified hard charcoal
Black suspension；
3) by the filtering of step 2) modified white carbon black suspension, dry, supersonic jet mill, it is white to obtain the modification that partial size is 4.5 μm
Carbon black.
Embodiment 2
White carbon black suspension is made by following methods: being sequentially added 14.5g water and 3g sodium carboxymethylcellulose in a kettle, is risen
1050.5g modulus is that the sodium silicate aqueous solution that 3.3 concentration are 30% and the sulfuric acid solution that 132g concentration is 90% are same to 85 DEG C by temperature
When be added to the water, react 2h, obtain 1200g white carbon black suspension, in white carbon black suspension the mass fraction of white carbon black be 20%.
A kind of preparation method of silicon rubber modified white carbon black comprising the steps of:
1) under ultrasonic wave, by volume it is that 1 ︰, 5 ︰ 1 is hydrolyzed by 8g phenyltrimethoxysila,e, first alcohol and water, obtains modification
Agent emulsion；
2) the modified agent emulsion of step 1) is added into 1200g white carbon black suspension to stir 1.5h at 60 DEG C, obtain modified hard charcoal
Black suspension；
3) by the filtering of step 2) modified white carbon black suspension, dry, supersonic jet mill, it is white to obtain the modification that partial size is 4.0 μm
Carbon black.
Embodiment 3
White carbon black suspension is made by following methods: being sequentially added 498g water and 3.1g sodium alginate in a kettle, is warming up to
70 DEG C, by 1134.4g modulus be the sodium silicate aqueous solution that 3.3 concentration are 25% and the sulfuric acid solution that 164.5g concentration is 65% simultaneously
It is added to the water, reacts 3.5h, obtain 1800g white carbon black suspension, the mass fraction of white carbon black is 12% in white carbon black suspension.
A kind of preparation method of silicon rubber modified white carbon black comprising the steps of:
1) under ultrasonic wave, by volume it is that 1 ︰, 7 ︰ 1 is hydrolyzed by 9g aryl imide silane, isopropyl alcohol and water, obtains modification
Agent emulsion；
2) the modified agent emulsion of step 1) is added into 1800g white carbon black suspension to stir 2h at 65 DEG C, obtain modified white carbon black
Suspension；
3) by the filtering of step 2) modified white carbon black suspension, dry, supersonic jet mill, it is white to obtain the modification that partial size is 3.5 μm
Carbon black.
Embodiment 4
White carbon black suspension is made by following methods: being sequentially added 136g water and 3.5g Sodium Polyacrylate in a kettle, is heated up
It is that the sodium silicate aqueous solution that 3.3 concentration are 30% and the sulfuric acid solution that 136.2g concentration is 85% are same by 1024.3g modulus to 85 DEG C
When be added to the water, react 2.5h, obtain 1300g white carbon black suspension, in white carbon black suspension the mass fraction of white carbon black be 18%.
A kind of preparation method of silicon rubber modified white carbon black comprising the steps of:
1) under ultrasonic wave, by volume it is that 1 ︰, 8 ︰ 2 is hydrolyzed by 7g alcyl acid imide silane, atoleine and water, obtains
Modified agent emulsion；
2) the modified agent emulsion of step 1) is added into 1300g white carbon black suspension to stir 3.5h at 70 DEG C, obtain modified hard charcoal
Black suspension；
3) by the filtering of step 2) modified white carbon black suspension, dry, supersonic jet mill, the modification hard charcoal that partial size is 5 μm is obtained
It is black.
Embodiment 5
White carbon black suspension is made by following methods: being sequentially added 118g water and 3g sodium carboxymethylcellulose in a kettle, is risen
1149.2g modulus is the sodium silicate aqueous solution that 3.3 concentration are 24% and the sulfuric acid solution that 129.8g concentration is 80% to 90 DEG C by temperature
It is added to the water simultaneously, reacts 2h, obtain 1400g white carbon black suspension, the mass fraction of white carbon black is 15% in white carbon black suspension.
A kind of preparation method of silicon rubber modified white carbon black comprising the steps of:
1) under ultrasonic wave, by volume it is that 1 ︰, 5 ︰ 0.5 is hydrolyzed by 10g anacardol titanate esters, toluene and water, obtains modification
Agent emulsion；
2) the modified agent emulsion of step 1) is added into 1400g white carbon black suspension to stir 2h at 80 DEG C, obtain modified white carbon black
Suspension；
3) by the filtering of step 2) modified white carbon black suspension, dry, supersonic jet mill, it is white to obtain the modification that partial size is 2.5 μm
Carbon black.
Embodiment 6
White carbon black suspension is made by following methods: being sequentially added 97.9g water and 2g sodium alginate in a kettle, is warming up to 65
DEG C, it is the sodium silicate aqueous solution that 3.3 concentration are 28% and the sulfuric acid solution that 123.3g concentration is 75% by 876.8g modulus while adds
Enter in water, react 4h, obtain 1100g white carbon black suspension, the mass fraction of white carbon black is 17% in white carbon black suspension.
A kind of preparation method of silicon rubber modified white carbon black comprising the steps of:
1) under ultrasonic wave, by volume it is that 1 ︰, 6 ︰ 1 is hydrolyzed by 8.5g polyethers titanate esters, dimethylbenzene and water, obtains modifying agent
Lotion；
2) the modified agent emulsion of step 1) is added into 1100g white carbon black suspension to stir 1h at 75 DEG C, obtain modified white carbon black
Suspension；
3) by the filtering of step 2) modified white carbon black suspension, dry, supersonic jet mill, the modification hard charcoal that partial size is 3 μm is obtained
It is black.
In order to further demonstrate that meaning of the present invention, provides and do the comparative example compared, comparative example with 1-6 of the embodiment of the present invention
It is modified in 1 using general silane coupling agent (vinyl three (2- methoxy ethoxy) silane)；It is not added in comparative example 2
Macromolecule sodium salt；Without using supersonic jet mill in comparative example 3.It is specific as follows.
Comparative example 1
White carbon black suspension is made by following methods: being sequentially added 122g water and 3.6g Sodium Polyacrylate in a kettle, is heated up
To 75 DEG C, by 1697g modulus be the sodium silicate aqueous solution that 3.3 concentration are 26% and the sulfuric acid solution that 277.2g concentration is 60% simultaneously
It is added to the water, reacts 3h, obtain 2100g white carbon black suspension, the mass fraction of white carbon black is 16% in white carbon black suspension.
A kind of preparation method of modified white carbon black comprising the steps of:
It 1) is by volume 1 ︰ by 11g vinyl three (2- methoxy ethoxy) silane, dehydrated alcohol and water under ultrasonic wave
6 ︰ 1 are hydrolyzed, and obtain modified agent emulsion；
2) the modified agent emulsion of step 1) is added into white carbon black suspension and stirs 4h at 70 DEG C, obtains modified white carbon black suspension
Liquid；
3) by the filtering of step 2) modified white carbon black suspension, dry, supersonic jet mill, the modification hard charcoal that partial size is 3 μm is obtained
It is black.
Comparative example 2
White carbon black suspension is made by following methods: 102.6g water sequentially added in a kettle, is warming up at 80 DEG C, it will
1149.2g modulus is the sodium silicate aqueous solution that 3.3 concentration are 24% and 148.2g concentration is 70% sulfuric acid solution while water is added
In, 3h is reacted, 1400g white carbon black suspension is obtained, the mass fraction of white carbon black is 15% in white carbon black suspension.
A kind of preparation method of modified white carbon black comprising the steps of:
1) under ultrasonic wave, by volume it is that 1 ︰, 5 ︰ 0.5 is hydrolyzed by 10g anacardol titanate esters, toluene and water, obtains modification
Agent emulsion；
2) the modified agent emulsion of step 1) is added into white carbon black suspension and stirs 2h at 80 DEG C, obtains modified white carbon black suspension
Liquid；
3) by the filtering of step 2) modified white carbon black suspension, dry, supersonic jet mill, it is white to obtain the modification that partial size is 2.5 μm
Carbon black.
Comparative example 3
White carbon black suspension is made by following methods: 176.1g water and 3g sodium carboxymethylcellulose are sequentially added in a kettle,
It is the sodium silicate aqueous solution that 3.3 concentration are 28% and the sulfuric acid solution that 118.8g concentration is 85% by 902.1g modulus at 85 DEG C
It is added to the water simultaneously, reacts 2.5h, obtain the suspension of 1200g white carbon black, the mass fraction of white carbon black in the suspension of white carbon black
It is 17%.
A kind of preparation method of silicon rubber modified white carbon black comprising the steps of:
1) under ultrasonic wave, by volume it is that 1 ︰, 5 ︰ 1 is hydrolyzed by 8g phenyltrimethoxysila,e, first alcohol and water, obtains modification
Agent emulsion；
2) the modified agent emulsion of step 1) is added into white carbon black suspension and stirs 1.5h at 60 DEG C, obtains modified white carbon black suspension
Liquid；
3) by the filtering of step 2) modified white carbon black suspension, dry, crushing, modified white carbon black is obtained.
The performance of the modified white carbon black of testing example 1-6, comparative example 1-3.Test result is as shown in table 1.
As shown in Table 1, hardness, tensile strength and tearing strength of modified white carbon black obtained by the present invention etc. performance
White carbon black better than in comparative example improves the application performance of white carbon black, is particularly suitable for silicon rubber technical field.
Claims (8)
1. a kind of preparation method of silicon rubber modified white carbon black, which is characterized in that comprise the steps of:
1) by main chain contain aromatic ring, the coupling agent of heterocycle or hetero atom rigid radical, organic solvent and water by volume example be 1 ︰
(1~10) ︰ (0.5~2) is hydrolyzed, and obtains modified agent emulsion；
2) the modified agent emulsion of step 1) is added into white carbon black suspension, at 40~100 DEG C, stirring 0.5~for 24 hours, obtain modification
White carbon black suspension；
3) by the filtering of step 2) modified white carbon black suspension, dry, crushing, modified white carbon black is obtained.
2. the preparation method of silicon rubber modified white carbon black as described in claim 1, which is characterized in that step 2) white carbon black
The mass fraction of white carbon black is 5~25% in suspension, and white carbon black suspension takes the precipitation method to be made.
3. the preparation method of silicon rubber modified white carbon black as claimed in claim 2, which is characterized in that step 1) coupling agent
Additive amount be step 2 white carbon black quality 0.5~10%, coupling agent be phenyl triethoxysilane, phenyltrimethoxysila,e,
One or more of aryl imide silane, alcyl acid imide silane, anacardol titanate esters, polyethers titanate esters are mixed
Close object.
4. the preparation method of silicon rubber modified white carbon black as described in claim 1, which is characterized in that organic molten in step 1)
Agent is the mixture of one or more of ethyl alcohol, methanol, isopropanol, atoleine, toluene, dimethylbenzene.
5. the preparation method of silicon rubber modified white carbon black as claimed in claim 2, which is characterized in that white carbon black in step 2)
Suspension is made by following methods: being sequentially added bottom liquid and dispersing agent in a kettle, is 15- by concentration at 60-95 DEG C
The sulfuric acid solution that 30% sodium silicate aqueous solution and concentration is 40-90% is added in the liquid of bottom simultaneously, reacts 2-4h, obtains white carbon black suspension
Liquid, the mass ratio of the sulfuric acid in sodium metasilicate and sulfuric acid solution in sodium silicate aqueous solution are 1 ︰ (0.3-0.6).
6. the preparation method of silicon rubber modified white carbon black as claimed in claim 5, which is characterized in that the dispersing agent is height
Molecule sodium salt.
7. the preparation method of silicon rubber modified white carbon black as claimed in claim 6, which is characterized in that the dispersing agent is poly-
The mixture of one or more of sodium acrylate, sodium carboxymethylcellulose, sodium alginate, polyglutamic acid sodium.
8. the preparation method of silicon rubber modified white carbon black as claimed in claim 5, which is characterized in that the bottom liquid is water.
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Cited By (5)
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|---|---|---|---|---|
| CN110387145A (en) * | 2019-07-18 | 2019-10-29 | 常州大学 | A kind of preparation method of the high abrasion white carbon black for butadiene-styrene rubber reinforcement |
| CN110734653A (en) * | 2019-10-23 | 2020-01-31 | 浙江新纳材料科技股份有限公司 | Preparation method of chemically-coated hydrophobic white carbon black |
| CN112574599A (en) * | 2020-12-31 | 2021-03-30 | 常州市五洲化工有限公司 | Preparation method of modified white carbon black |
| CN113755032A (en) * | 2020-12-16 | 2021-12-07 | 安徽进化硅纳米材料科技有限公司 | Method for refining silicon dioxide, ultrafine silicon dioxide powder and use |
| CN115521502A (en) * | 2021-06-25 | 2022-12-27 | 济南优纳泰克新材料科技有限公司 | Modified white carbon black micron aggregate and preparation method and application thereof |
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| US20130131357A1 (en) * | 2011-06-02 | 2013-05-23 | Beijing University Of Chemical Technology | Method for preparing white carbon black modified by silane coupling agent |
| CN106883453A (en) * | 2017-03-20 | 2017-06-23 | 北京化工大学 | The preparation method of the modified white carbon black with chemical isolation structure |
| CN107973935A (en) * | 2017-12-07 | 2018-05-01 | 沈阳化工大学 | A kind of modified white carbon black and preparation method thereof |
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| US20130131357A1 (en) * | 2011-06-02 | 2013-05-23 | Beijing University Of Chemical Technology | Method for preparing white carbon black modified by silane coupling agent |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110387145A (en) * | 2019-07-18 | 2019-10-29 | 常州大学 | A kind of preparation method of the high abrasion white carbon black for butadiene-styrene rubber reinforcement |
| CN110734653A (en) * | 2019-10-23 | 2020-01-31 | 浙江新纳材料科技股份有限公司 | Preparation method of chemically-coated hydrophobic white carbon black |
| CN113755032A (en) * | 2020-12-16 | 2021-12-07 | 安徽进化硅纳米材料科技有限公司 | Method for refining silicon dioxide, ultrafine silicon dioxide powder and use |
| CN112574599A (en) * | 2020-12-31 | 2021-03-30 | 常州市五洲化工有限公司 | Preparation method of modified white carbon black |
| CN112574599B (en) * | 2020-12-31 | 2022-03-22 | 常州市五洲化工有限公司 | Preparation method of modified white carbon black |
| CN115521502A (en) * | 2021-06-25 | 2022-12-27 | 济南优纳泰克新材料科技有限公司 | Modified white carbon black micron aggregate and preparation method and application thereof |
| CN115521502B (en) * | 2021-06-25 | 2024-01-26 | 济南优纳泰克新材料科技有限公司 | Modified white carbon black micron aggregate and preparation method and application thereof |
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