CN107033630B - A kind of preparation method of silicon rubber white carbon black - Google Patents
A kind of preparation method of silicon rubber white carbon black Download PDFInfo
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- CN107033630B CN107033630B CN201710271458.4A CN201710271458A CN107033630B CN 107033630 B CN107033630 B CN 107033630B CN 201710271458 A CN201710271458 A CN 201710271458A CN 107033630 B CN107033630 B CN 107033630B
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- carbon black
- white carbon
- silicon rubber
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- phenol
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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
- C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- 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
- C09C1/3009—Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
- C09C1/3018—Grinding
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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
- C09C1/3009—Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
- C09C1/3027—Drying, calcination
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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
- C09C1/3063—Treatment with low-molecular organic compounds
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- Organic Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of silicon rubber white carbon black comprising following step: (1) by white carbon black ultrasonic disperse Yu Shuizhong, being sufficiently formed dispersion, the mass ratio of white carbon black and water is 1:15-20；(2) while high-speed stirred, phenol-modified dose is added dropwise into reaction system, rate of addition 2-4ml/30min；The white carbon black and phenol-modified dose of mass ratio are 10 ~ 20:1；(3) after completion of dropwise addition, the reaction was continued 30-60 minutes, drying, grinds to obtain silicon rubber white carbon black.Using white carbon black produced by the present invention as silicon rubber made from additive, excellent hardness and tearing strength can be obtained.
Description
Technical field
The present invention relates to the preparation fields of white carbon black, and in particular to a kind of preparation method of silicon rubber white carbon black.
Background technique
Organic silicon rubber has many characteristics for being different from General Purpose Rubber, such as resistance to ozone as one of specific rubber kind
Property, heat resistance, resistance to ag(e)ing, electric insulation, oil resistant, solvent resistant etc., physical property influenced by environment temperature and humidity it is little,
Weatherability is relatively good.In recent years, the application field of organic silicon rubber is constantly expanded, and is not singly military product, many civilian products
Industry is more and more to use silicon rubber as raw material.
Simple organic silicon rubber molecule backbone linear in the shape of a spiral, intermolecular force are weak, it is difficult to crystallize, wrap
The physical mechanical property included including hardness, tearing strength is very poor, and filler reinforcement material can effectively improve crosslinking silicone polymer
Hardness and cured properties.
On the other hand, white carbon black is a kind of common supporting material, according to preparation method difference, can be divided into gas phase hard charcoal
Black and precipitated silica.Favor since white carbon black is cheap, by vast white carbon black producer and silicon rubber user.However,
Current existing white carbon black is not very ideal the improvement result of the physical mechanical properties such as silicon rubber hardness and tearing strength.
Summary of the invention
Therefore, to solve above-mentioned problems of the prior art, the present invention provides a kind of system of silicon rubber white carbon black
Preparation Method, white carbon black made from the preparation method is to the hardness of silicon rubber, the improvement of tearing strength through the invention
It is more obvious.
The present invention provides a kind of preparation method of silicon rubber white carbon black, which is characterized in that includes the following steps:
(1) by white carbon black ultrasonic disperse Yu Shuizhong, it is sufficiently formed dispersion, the mass ratio of white carbon black and water is 1:15-
20；
(2) while high-speed stirred, phenol-modified dose is added dropwise into reaction system, rate of addition 2-4ml/30min；
The white carbon black and phenol-modified dose of mass ratio are 10 ~ 20:1；
(3) after completion of dropwise addition, the reaction was continued 30-60 minutes, drying, grinds to obtain silicon rubber white carbon black.
According to preparation method as described above, described phenol-modified dose is 4,6-diaminoresorcinol.
According to preparation method as described above, entire reaction process is maintained at 70-80 DEG C.
According to preparation method as described above, which is characterized in that the high-speed stirred is 2000rpm.
The preparation method of silicon rubber white carbon black of the invention, by the way that 4,6-diaminoresorcinol is added as modifying agent
White carbon black is modified, using white carbon black as the hydrogen bond quantity that when reinforcing agent, can be greatly increased between silicon rubber, thus right
The hardness and tearing strength of silicon rubber are improved.
Specific embodiment
A specific embodiment of the invention is explained in detail below, but the present invention is not limited to these embodiments.Ability
Field technique personnel are it is found that the substitution of conventional means is all contained in scope of the invention.
One, preparation example
Embodiment 1
At 70 DEG C, by 200g white carbon black (be purchased from Dongying City Xin Da Chemical Co., Ltd., model WH-93) ultrasonic disperse in
In 3000ml deionized water, it is sufficiently formed dispersion；Kept for 70 DEG C of reaction system；That stirs under the revolving speed of 2000rpm is same
When, 13ml modifying agent 4,6-diaminoresorcinol is added dropwise into reaction system and (is purchased from the happy Industrial Co., Ltd. of Shanghai Jin Jin, divides
Analyse pure), rate of addition 4ml/30min；After completion of dropwise addition, the reaction was continued 60 minutes, drying, grinds to obtain silicon rubber hard charcoal
It is black.
Embodiment 2
At 80 DEG C, by 200g white carbon black (be purchased from Dongying City Xin Da Chemical Co., Ltd., model WH-93) ultrasonic disperse in
In 3000ml deionized water, it is sufficiently formed dispersion；Kept for 80 DEG C of reaction system；That stirs under the revolving speed of 2000rpm is same
When, into reaction system be added dropwise 6.5ml modifying agent 4,6-diaminoresorcinol (be purchased from the happy Industrial Co., Ltd. of Shanghai Jin Jin,
Analyze pure), rate of addition 2ml/30min；After completion of dropwise addition, the reaction was continued 30 minutes, drying, grinds to obtain silicon rubber hard charcoal
It is black.
Embodiment 3
At 70 DEG C, by 200g white carbon black (be purchased from Dongying City Xin Da Chemical Co., Ltd., model WH-93) ultrasonic disperse in
In 4000ml deionized water, it is sufficiently formed dispersion；Kept for 70 DEG C of reaction system；That stirs under the revolving speed of 2000rpm is same
When, into reaction system be added dropwise 9.7ml modifying agent 4,6-diaminoresorcinol (be purchased from the happy Industrial Co., Ltd. of Shanghai Jin Jin,
Analyze pure), rate of addition 3ml/30min；After completion of dropwise addition, the reaction was continued 45 minutes, drying, grinds to obtain silicon rubber hard charcoal
It is black.
Embodiment 4
At 80 DEG C, by 200g white carbon black (be purchased from Dongying City Xin Da Chemical Co., Ltd., model WH-93) ultrasonic disperse in
In 4000ml deionized water, it is sufficiently formed dispersion；Kept for 80 DEG C of reaction system；That stirs under the revolving speed of 2000rpm is same
When, into reaction system be added dropwise 11.7ml modifying agent 4,6-diaminoresorcinol (be purchased from the happy Industrial Co., Ltd. of Shanghai Jin Jin,
Analyze pure), rate of addition 3ml/30min；After completion of dropwise addition, the reaction was continued 45 minutes, drying, grinds to obtain silicon rubber hard charcoal
It is black.
Comparative example
At 70 DEG C, by 200g white carbon black (be purchased from Dongying City Xin Da Chemical Co., Ltd., model WH-93) ultrasonic disperse in
In 3000ml deionized water, it is sufficiently formed dispersion；Kept for 70 DEG C of reaction system；That stirs under the revolving speed of 2000rpm is same
When, the sodium dodecyl benzene sulfonate aqueous solution that 100ml mass fraction is 13.3% is added into reaction system (is purchased from Tianjin Jin Hui
Chemical reagent Co., Ltd, the Pacific-Asian, SILVER REAGENT), rate of addition 4ml/30min；After completion of dropwise addition, the reaction was continued 30 minutes, does
It is dry, grind to obtain silicon rubber white carbon black.
Two, performance test
Using white carbon black obtained in the embodiment of the present invention and comparative example as reinforcing agent, silicon rubber is made, performance is carried out to it
Measurement, as a result as shown in the table.
Tearing strength is measured according to GB/T531 measurement shore hardness, according to GB/T529.
Silicon rubber made from silicon rubber white carbon black produced by the present invention is added it can be seen from Examples and Comparative Examples,
Hardness and tearing strength are good.
Claims (1)
1. a kind of preparation method of silicon rubber white carbon black, which is characterized in that include the following steps:
(1) by white carbon black ultrasonic disperse Yu Shuizhong, it is sufficiently formed dispersion, the mass ratio of white carbon black and water is 1:15-20；
(2) while high-speed stirred, phenol-modified dose is added dropwise into reaction system, rate of addition 2-4ml/30min；It is described
White carbon black and phenol-modified dose of mass ratio are 10~20:1；
(3) after completion of dropwise addition, the reaction was continued 30-60 minutes, drying, grinds to obtain silicon rubber white carbon black；
Described phenol-modified dose is 4,6- diamino resorcin；
Entire reaction process is maintained at 70-80 DEG C；
The high-speed stirred is 2000rpm.
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| CN107033630B true CN107033630B (en) | 2019-03-29 |
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Citations (7)
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| JPH03143914A (en) * | 1989-10-30 | 1991-06-19 | Toshiba Chem Corp | Epoxy resin composition and sealed semiconductor device |
| CN1597531A (en) * | 2004-07-21 | 2005-03-23 | 华南理工大学 | Modified nanometer calcium carbonate and its preparation method |
| CN1657410A (en) * | 2005-01-20 | 2005-08-24 | 辽宁大学 | Method for modifying surface of manometer |
| WO2011002672A1 (en) * | 2009-06-30 | 2011-01-06 | The Gates Corporation | Bonded part with laminated rubber member and method of making |
| CN104194405A (en) * | 2014-08-28 | 2014-12-10 | 确成硅化学股份有限公司 | Modification method of silicon dioxide |
| CN104212204A (en) * | 2014-08-19 | 2014-12-17 | 确成硅化学股份有限公司 | Production method for modified silicon dioxide |
| CN105131331A (en) * | 2015-07-21 | 2015-12-09 | 大连新绿州化学工业有限公司 | Modified precipitated white carbon black and application thereof |
-
2017
- 2017-04-24 CN CN201710271458.4A patent/CN107033630B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03143914A (en) * | 1989-10-30 | 1991-06-19 | Toshiba Chem Corp | Epoxy resin composition and sealed semiconductor device |
| CN1597531A (en) * | 2004-07-21 | 2005-03-23 | 华南理工大学 | Modified nanometer calcium carbonate and its preparation method |
| CN1657410A (en) * | 2005-01-20 | 2005-08-24 | 辽宁大学 | Method for modifying surface of manometer |
| WO2011002672A1 (en) * | 2009-06-30 | 2011-01-06 | The Gates Corporation | Bonded part with laminated rubber member and method of making |
| CN104212204A (en) * | 2014-08-19 | 2014-12-17 | 确成硅化学股份有限公司 | Production method for modified silicon dioxide |
| CN104194405A (en) * | 2014-08-28 | 2014-12-10 | 确成硅化学股份有限公司 | Modification method of silicon dioxide |
| CN105131331A (en) * | 2015-07-21 | 2015-12-09 | 大连新绿州化学工业有限公司 | Modified precipitated white carbon black and application thereof |
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| 间苯二酚甲醛树脂粘合剂的制备及其在橡胶工业中的应用;王峰，等;《山东科学》;20121031;第83-87页 |
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