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 PDF

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Publication number
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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carbon black
white carbon
silicon rubber
preparation
suspension
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CN201811174035.1A
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刘旭
王恩伟
郑强
李冬
孙浩杰
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HENAN JUNHUA DEVELOPMENT Co Ltd
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HENAN JUNHUA DEVELOPMENT Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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
    • C08L83/04Polysiloxanes

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

A kind of preparation method of silicon rubber modified white carbon black
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.
CN201811174035.1A 2018-10-09 2018-10-09 A kind of preparation method of silicon rubber modified white carbon black Withdrawn CN109354876A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
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
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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CN102951649A (en) * 2012-11-15 2013-03-06 北京橡胶工业研究设计院 Preparation method of modified precipitated white carbon black
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130131357A1 (en) * 2011-06-02 2013-05-23 Beijing University Of Chemical Technology Method for preparing white carbon black modified by silane coupling agent
CN102951649A (en) * 2012-11-15 2013-03-06 北京橡胶工业研究设计院 Preparation method of modified precipitated white carbon black
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

Cited By (7)

* Cited by examiner, † Cited by third party
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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