CN107936574A - A kind of preparation method of precipitated silica reinforcement silicon rubber - Google Patents
A kind of preparation method of precipitated silica reinforcement silicon rubber Download PDFInfo
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- CN107936574A CN107936574A CN201711248431.XA CN201711248431A CN107936574A CN 107936574 A CN107936574 A CN 107936574A CN 201711248431 A CN201711248431 A CN 201711248431A CN 107936574 A CN107936574 A CN 107936574A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of preparation method of precipitated silica reinforcement silicon rubber, it is characterised in that the silicone rubber material weight is as follows:100 parts of methyl vinyl silicon kautschuk, 0.2 0.4 parts of 0.3 0.8 parts of 3 3.6 parts of 40 50 parts of white carbon, antistructurizing agent, containing hydrogen silicone oil, the releasing agent of precipitated silica reinforcement.Its preparation method is, first by load weighted 100 parts of methyl vinyl silicon kautschuk, 0.2 0.4 parts of releasing agent, in 0.3 0.8 parts of input mixers of containing hydrogen silicone oil;Again by 40 50 parts of points of 35 addition mixers of white carbon, 3 3.6 parts of hydroxy silicon oil, afterwards mixing is mediated, and is controlled 50 80 degree of temperature, after mixing is agglomerating, is heated up and evacuate after parking;Finally by the back mixing on a mill of the silicone rubber compounds after evacuation, product is filtered and packaged into after sizing material is smooth.The present invention has the advantages that simple production process, tearing strength is high, and effect is good.
Description
Technical field
The present invention relates to silicon rubber production technical field, is mended more particularly, to a kind of precipitated silica of high-tear strength
The preparation method and production technology of strong silicon rubber.
Background technology
Silicon rubber is one of most important organosilicon product, has good heat resistance, lower temperature resistance and processing performance, extensively
It is general to be applied to the fields such as electronics, aviation, food, health.It is the linear polysiloxanes of high molecular weight before vulcanization, becomes after vulcanization
The elastomer of net structure.Uncured crosslinked basic polysiloxanes is known as silicon raw rubber, it is the line of a kind of high molecular weight
Type polydiorganosiloxanepolyurea, since cohesion energy density is low between dividing, the tensile strength only 0.3-0.5MPa after vulcanization.By to life
The improvement of glue, using reinforced filling and corresponding mixed technology etc., present tensile strength is up to 13MPa;And silicon rubber system
Product are mostly baroque small parts, are easily torn when hot-die molds after product vulcanization;Product is in compared with harsh environment
Using tear is also be easy to cause, the performance of product is then influenced, therefore the tearing strength for improving silicon rubber has important meaning
Justice.The tearing toughness of the silicon rubber of early stage only has 5-10KN/M, and scientific progress and silicon rubber production and mixed technology change therewith
It is good, 50KN/M is had reached now, but gas-phase silicon rubber is also only limited to, the existing precipitated silica reinforcement of in the market
The tearing strength of silicon rubber is also simply in 20KN/M or so;Therefore the tear resistance of the silicon rubber of precipitated silica reinforcement is improved
Can have great importance to the perfect and market demand of silicon rubber technology.
The content of the invention
The purpose of the present invention is exactly and the precipitation method of a kind of high-tear strength provided in order to solve the deficiency of the prior art
The silicon rubber of white carbon reinforcement, while a kind of preparation method of the special silicone rubber is provided, by existing product differing ethylene
The collocation of base content raw rubber, obtains low cost and the product with gas phase silicon rubber high-tear strength performance.
The present invention is to realize above-mentioned purpose using following technical solution:
A kind of preparation method of precipitated silica reinforcement silicon rubber, it is characterised in that the silicone rubber material parts by weight
Proportioning is as follows:100 parts of methyl vinyl silicon kautschuk, 40-50 parts of the white carbon of precipitated silica reinforcement, structuring control
3-3.6 parts of agent, 0.3-0.8 parts of containing hydrogen silicone oil, 0.2-0.4 parts of releasing agent.
The methyl vinyl silicon kautschuk molecular weight is 55-65 ten thousand, and fugitive constituent is not higher than 0.8%.
The white carbon is the white carbon of precipitated silica reinforcement;The white carbon of the precipitated silica reinforcement passes through
Silazane processing, can effectively reduce Si-OH, and be transformed into hydrophobic surface by hydrophilic surface, so as to improve in raw rubber
Dispersiveness and the purpose of sizing material recurring structure is reduced or avoided;And gas-phase silica particle diameter is smaller, specific surface area is big, and silicon
Rubber raw rubber is combined fully, to improve Silicone Rubber such as tensile strength etc..
The antistructurizing agent is hydroxy silicon oil, its chain link is about 8-10, its cap hydroxyl groups can be with white carbon table
The Si-OH effects in face, lose the latter amount of activated, to obtain the superior silicon rubber of processing performance.
The releasing agent is stearic acid or magnesium stearate or aluminum stearate or calcium stearate etc..
The containing hydrogen silicone oil, its hydrogen content are 0.7%-1.5%.
The invention also discloses the preparation method of precipitated silica reinforcement silicon rubber, concretely comprise the following steps;It will weigh first
100 parts good of methyl vinyl silicon kautschuk, 0.2-0.4 parts of releasing agent, in 0.3-0.8 parts of input mixers of containing hydrogen silicone oil;
Again by white carbon 40-50 parts divide in 3-5 addition mixer, 3-3.6 parts of hydroxy silicon oil, afterwards mixing is mediated, control temperature 50-
80 degree, after mixing is agglomerating, after parking a period of time, heats up and evacuate;Finally silicone rubber compounds by after evacuation on a mill
Back mixing, product is filtered and packaged into after sizing material is smooth.
Wherein white carbon needs a point 3-5 addition, ensures that mixing space is sufficient, it is ensured that raw rubber, white carbon, silicones and knot
The combination of structure controlling agent is abundant, is conducive to the reinforcement of silicon rubber.
High temperature is needed to evacuate a period of time after wherein mixing is agglomerating in mixing step, to remove the low molecule in rubber compound,
The more preferable hydroxyl for making hydroxy silicon oil dialogue carbon blacksurface acts on fully, it is ensured that the processing performance of follow-up silicon rubber is excellent.
In 150-180 degree, vacuum is -0.08Mpa for wherein evacuation temperature control;
Wherein open mill refining glue when unsuitable excessive, silicon rubber edge-smoothing when beginning to pratise of temperature;Added during mill,
Pigment, additive, other auxiliary agents.
It is of the invention to be using the attainable beneficial effect of above-mentioned technical solution institute:Product of the present invention is in existing precipitation
Improved on the basis of the silicone rubber products of method white carbon reinforcement, the requirement of high tear energy and low cost is taken into account, close
The white carbon of extraordinary precipitated silica reinforcement is added when refining feeds intake, different types of raw rubber is equipped with, obtains precipitated silica
The silicon rubber of reinforcement also has high tensile strength and tearing strength, has good market value.
Brief description of the drawings
Fig. 1 is the preparation technology flow chart of the present invention.
Embodiment
With reference to attached drawing 1, it is explained in detail below for the specific preparation process of the present invention;
Embodiment 1
A kind of precipitated silica reinforcement silicon rubber and preparation method thereof is as follows, its raw material weight component is ethylene methacrylic
100 parts of base raw-silastic continuously, 45 parts of the white carbon of precipitated silica reinforcement, 3.5 parts of hydroxy silicon oil, 0.2 part of magnesium stearate, contains
0.6 part of hydrogen silicone oil, the wherein hydroxy radical content of hydroxy silicon oil are 8.5%, and the content of the hydrogen of containing hydrogen silicone oil is 0.7%;Material component
In can also add a small amount of anti-yellowing dose;Its preparation method is as follows:
1. by 100 parts of methyl vinyl silicon kautschuk, 10 parts of white carbon, 3.5 parts of hydroxy silicon oil, 0.2 part of magnesium stearate,
0.6 part of containing hydrogen silicone oil, anti-yellowing dose puts into mixing kneader, and 10-20min is mediated in mixing.
2. dividing 3-4 times after follow-up sizing material kneading is agglomerating and adding 35 parts of reinforced filling white carbon, mixer temperature is adjusted to 50-80
Degree, sizing material mediates agglomerating rear reduction mixer temperature, and starts to evacuate parking a few hours time, and evacuation temperature is adjusted to 150-
180 degree, goes out sizing material after evacuating 1.5-2h.
3. treating that temperature is cooled to room temperature in beginning to pratise on open mill, added during mill, pigment, additive, other auxiliary agents;
After beginning to pratise uniformly, uniformity coefficient is smooth for edge sizing material, is filtered and packaged afterwards by rubber strainer.
Embodiment 2
A kind of preparation method of precipitated silica reinforcement silicon rubber, its raw material weight component are methyl ethylene silicon rubber
100 parts of glue raw rubber, 50 parts of white carbon, 3 parts of hydroxy silicon oil, 0.3 part of magnesium stearate, 0.5 part of containing hydrogen silicone oil, wherein hydroxy silicon oil
Hydroxy radical content is 8.5%, and the content of the hydrogen of containing hydrogen silicone oil is 1.5%;Its preparation method is as follows:
1. by 100 parts of methyl vinyl silicon kautschuk, 20 parts of white carbon, 1.1 parts of hydroxy silicon oil, 0.3 part of magnesium stearate,
In 0.8 part of input mixing kneader of containing hydrogen silicone oil, 10-20min is mediated in mixing.
2. subsequently mediate it is agglomerating after divide 3-4 times addition 30 parts of white carbon, mixer temperature adjustment 50-80 degree, finally mediate
Mixer temperature is reduced after agglomerating, a few hours time is parked and starts to evacuate, evacuation temperature is adjusted to 150-180 degree, evacuates 1.5-2h
After go out sizing material.
3. after temperature be cooled to room temperature in begin to pratise on the machine of beginning to pratise uniformly after, uniformity coefficient for edge sizing material it is smooth, after pass through
Filter is crossed to filter and package.
Embodiment 3
A kind of preparation method of precipitated silica reinforcement silicon rubber is as follows, its raw material weight component is methyl ethylene
100 parts of raw-silastic continuously, 40 parts of white carbon, 1.1 parts of hydroxy silicon oil, 0.4 part of magnesium stearate, wherein 0.7 part of containing hydrogen silicone oil, hydroxyl
The hydroxy radical content of silicone oil is 8.5%, and the content of the hydrogen of containing hydrogen silicone oil is 1.5%;Its preparation method is as follows:
1. by 100 parts of methyl vinyl silicon kautschuk, 10 parts of white carbon, 1.1 parts of hydroxy silicon oil, 0.2 part of magnesium stearate,
In 0.7 part of input mixing kneader of containing hydrogen silicone oil, 10-15min is mediated in mixing.
2. subsequently mediate it is agglomerating after divide 3-4 times addition 30 parts of white carbon, mixer temperature adjustment 50-80 degree, finally mediate
Mixer temperature is reduced after agglomerating, a few hours time is parked and starts to evacuate, evacuation temperature is adjusted to 150-180 degree, evacuates 1.5-2h
After go out sizing material.
3. after temperature be cooled to room temperature in begin to pratise on the machine of beginning to pratise uniformly after, uniformity coefficient for edge sizing material it is smooth, after pass through
Filter is crossed to filter and package.
The examination criteria and performance of the high-temperature mixing silicon rubber of the next resulting three kinds of softs of three kinds of above-mentioned examples are such as
Under:Hardness:GB/T531-92;Tensile strength and elongation:GB/T528-92;Tearing strength (crescent sample):GB/T529-
91。
Above-described is only the preferred embodiment of the present invention, it is noted that for those of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the present invention
Protection domain.
Claims (9)
1. a kind of preparation method of precipitated silica reinforcement silicon rubber, it is characterised in that the silicone rubber material parts by weight are matched somebody with somebody
Than as follows:100 parts of methyl vinyl silicon kautschuk, 40-50 parts of white carbon, the antistructurizing agent of precipitated silica reinforcement
3-3.6 parts, 0.3-0.8 parts of containing hydrogen silicone oil, 0.2-0.4 parts of releasing agent.
2. the preparation method of precipitated silica reinforcement silicon rubber according to claim 1, it is characterised in that in composition of raw materials
The methyl vinyl silicon kautschuk molecular weight is 55-65 ten thousand, and fugitive constituent is not higher than 0.8%.
3. the preparation method of precipitated silica reinforcement silicon rubber according to claim 1, it is characterised in that the white carbon
For the white carbon of the precipitated silica reinforcement by silazane processing.
4. the preparation method of precipitated silica reinforcement silicon rubber according to claim 1, it is characterised in that the structuring
Controlling agent is hydroxy silicon oil, its chain link is about 8-10.
5. the preparation method of precipitated silica reinforcement silicon rubber according to claim 1, it is characterised in that the Silicon Containing Hydrogen
Oil, its hydrogen content are 0.7%-1.5%.
6. the preparation method of precipitated silica reinforcement silicon rubber according to claim 1, it is characterised in that the releasing agent
For stearic acid or magnesium stearate or aluminum stearate or calcium stearate.
7. according to the preparation method of precipitated silica reinforcement silicon rubber described in claim 1 to 6 any one, its feature exists
In preparation method concretely comprises the following steps;First by load weighted 100 parts of methyl vinyl silicon kautschuk, releasing agent 0.2-0.4
Part, in 0.3-0.8 parts of input mixers of containing hydrogen silicone oil;Again by white carbon 40-50 parts divide in 3-5 addition mixer, hydroxyl silicon
3-3.6 parts oily, mixing afterwards is mediated, and is controlled temperature 50-80 degree, after mixing is agglomerating, after parking a period of time, is heated up and evacuate;
Finally by the back mixing on a mill of the silicone rubber compounds after evacuation, product is filtered and packaged into after sizing material is smooth.
8. the preparation method of precipitated silica reinforcement silicon rubber according to claim 7, it is characterised in that wherein park
Afterwards, in 150-180 degree, vacuum is -0.08Mpa for evacuation temperature control.
9. the preparation method of precipitated silica reinforcement silicon rubber according to claim 7, it is characterised in that wherein in mill
On machine during back mixing, pigment, additive, auxiliary agent are added.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109096550A (en) * | 2018-06-25 | 2018-12-28 | 确成硅化学股份有限公司 | A method of it is dispersed in rubber to improve white carbon black |
CN109679353A (en) * | 2019-01-21 | 2019-04-26 | 广德鸣生新材料有限公司 | A kind of ice machine silicon rubber connector and preparation method thereof |
CN110551395A (en) * | 2018-05-30 | 2019-12-10 | 厦门明钜科技有限公司 | formula and preparation method of extrusion type mixing silicone rubber |
CN111154268A (en) * | 2019-12-20 | 2020-05-15 | 江西双龙硅材料科技有限公司 | High-tear-resistance precipitation-process silicone rubber and preparation method thereof |
CN112341823A (en) * | 2020-11-12 | 2021-02-09 | 江西蓝星星火有机硅有限公司 | Rice hull ash precipitated silica reinforced high-temperature-resistant silicon rubber compound and preparation method and application thereof |
CN113122004A (en) * | 2021-04-19 | 2021-07-16 | 青岛惠陆有机硅有限公司 | Biological silicon rubber and preparation method thereof |
CN113337124A (en) * | 2021-05-28 | 2021-09-03 | 浙江恒业成有机硅有限公司 | Platinum vulcanization extrusion precipitation silicone rubber and preparation method thereof |
CN115894937A (en) * | 2022-11-23 | 2023-04-04 | 新纳奇材料科技江苏有限公司 | High-strength silicone resin and preparation method thereof |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110551395A (en) * | 2018-05-30 | 2019-12-10 | 厦门明钜科技有限公司 | formula and preparation method of extrusion type mixing silicone rubber |
CN109096550A (en) * | 2018-06-25 | 2018-12-28 | 确成硅化学股份有限公司 | A method of it is dispersed in rubber to improve white carbon black |
CN109679353A (en) * | 2019-01-21 | 2019-04-26 | 广德鸣生新材料有限公司 | A kind of ice machine silicon rubber connector and preparation method thereof |
CN111154268A (en) * | 2019-12-20 | 2020-05-15 | 江西双龙硅材料科技有限公司 | High-tear-resistance precipitation-process silicone rubber and preparation method thereof |
CN112341823A (en) * | 2020-11-12 | 2021-02-09 | 江西蓝星星火有机硅有限公司 | Rice hull ash precipitated silica reinforced high-temperature-resistant silicon rubber compound and preparation method and application thereof |
CN113122004A (en) * | 2021-04-19 | 2021-07-16 | 青岛惠陆有机硅有限公司 | Biological silicon rubber and preparation method thereof |
CN113337124A (en) * | 2021-05-28 | 2021-09-03 | 浙江恒业成有机硅有限公司 | Platinum vulcanization extrusion precipitation silicone rubber and preparation method thereof |
CN115894937A (en) * | 2022-11-23 | 2023-04-04 | 新纳奇材料科技江苏有限公司 | High-strength silicone resin and preparation method thereof |
CN115894937B (en) * | 2022-11-23 | 2023-09-22 | 新纳奇材料科技江苏有限公司 | High-strength silicone resin and preparation method thereof |
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Application publication date: 20180420 |