CN101921487A - Methyl ethylene high temperature vulcanizing silicone rubber production technology - Google Patents
Methyl ethylene high temperature vulcanizing silicone rubber production technology Download PDFInfo
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- CN101921487A CN101921487A CN2009101478363A CN200910147836A CN101921487A CN 101921487 A CN101921487 A CN 101921487A CN 2009101478363 A CN2009101478363 A CN 2009101478363A CN 200910147836 A CN200910147836 A CN 200910147836A CN 101921487 A CN101921487 A CN 101921487A
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Abstract
The invention provides a methyl ethylene high temperature vulcanizing silicone rubber production technology, relating to improvement of the existing methyl ethylene high temperature vulcanizing silicone rubber production technology. The production technology is carried out by the following steps: A, dehydration on major ingredient is carried out; B, polymerization is carried out; C, dehydrated auxiliaries are added I the polymerization process; D, two or more than two polysiloxane polymer raw materials in different molecular weights are placed into a mixing kettle, and fully mixing is carried out; E, low molecule is removed; F, the removed low molecule and low molecule subject to flash evaporation are recycled by condensing and cooling. The methyl ethylene high temperature vulcanizing silicon rubber production technology of the invention can cause residue of catalyst used in the production process after high temperature decomposition to be reduced, odour of rubber is obviously reduced, and equilibration reaction is more perfect.
Description
Technical field
The present invention relates to improvement to present production methyl ethylene high temperature vulcanizing silicone rubber technology.
Background technology
Produce methyl ethylene high temperature vulcanizing silicone rubber at present, the catalyst that uses is many through residue behind the pyrolytic decomposition in process of production, and the foreign odor flavor of sizing material is bigger.There is mechanical workout and the over-all properties difference problem of producing in therefore existing complete processing.
Summary of the invention
The purpose of this invention is to provide a kind of methyl ethylene high temperature vulcanizing silicone rubber production technology, it is many to the invention solves in the production process that existing technology exists residue, the foreign odor flavor of sizing material is bigger, and there be mechanical workout and the over-all properties difference problem of producing in existing complete processing.
Methyl ethylene high temperature vulcanizing silicone rubber production technology of the present invention, carry out according to following steps:
A: major ingredient dehydration, under the condition of vacuum, to carry out, the temperature that requires dehydration is at 45-70 ℃, and the vacuum tightness of requirement is-0.1 to-0.096Mpa, and the time of dehydration is 2-4 hour, blasts nitrogen during dehydration, perhaps imposes stirring; Can improve the dehydration quality like this.
B: polyreaction, the dimethyl cyclosiloxane to be put in the polymerization reaction kettle, the temperature of reaction is 105-115 ℃, under condition of normal pressure, in order to prevent contacting of reaction mass and air, blanketing with inert gas, the time of reaction is 2-4 hour.
C: before above-mentioned polyreaction, add the auxiliary agent that has dewatered;
Comprise following auxiliary agent: 1, molecular weight regulator: alkyl-blocked low polydimethylsiloxane, perhaps have the organopolysiloxane of alkene, the molecular weight ranges of the auxiliary agent of adding is: 0-2000; 2, catalyzer: Tetramethylammonium hydroxide, tetrabutylammonium hydroxide phosphorus etc., add-on be the DMC gross weight 40 to 2000ppm.Alkali metal hydroxide is as potassium hydroxide, cesium hydroxide, its add-on be the DMC gross weight 100 to 2000ppm.3, improve the organic compound of cross-linking set: the methyl ethylene cyclosiloxane, alkyl-blocked poly-ethylene methacrylic siloxanes, add-on is 0 to 15%D of a DMC total amount: the polymer raw material of the different molecular weight of the organopolysiloxane after two kinds or the two or more polymerization is put into mixing kettle, mix fully, the blended time is 1-2 hour, the interior temperature control of mixing kettle is at 140-160 ℃, electronic rotating speed is adjustable to be 0-15rpm, in this mixing kettle catalyzer is destroyed or neutralizes; Can alleviate the pressure that takes off low molecule still like this, and can allow the remnant of catalyzer lower, reduce and adding the peculiar smell in man-hour, improve the quality of product.
E: take off low molecule, the product material after the above-mentioned D step is put into the top of taking off low molecule still, with catalyst breakage, allow material decompose under 150-170 ℃ condition, kept under said temperature 30-60 minute, above-mentioned reaction is to carry out under non-pressurized condition; In taking off low molecular device, realize two kinds of functions, catalyst breakage, allow material under the condition of managing, resolve into other chemical substance on the top of taking off low molecule still.
After above-mentioned broken matchmaker's process was finished, material improved surface-area through card, and under-0.1 to-0.096Mpa condition of negative pressure, the low molecule in the reactant reduces pressure by flash distillation then, and the temperature of flash distillation is 150-170 ℃;
F: the low molecule of deviating from, the low molecule by flash distillation reclaims by condensation and cooling, obtains product at last.The low molecule of above-mentioned recovery can recycle.
Methyl ethylene high temperature vulcanizing silicone rubber production technology of the present invention can make in process of production the catalyst that uses reduce through residue behind the pyrolytic decomposition, the foreign odor flavor of sizing material obviously alleviate and equilibration reaction more perfect.
The present invention has done further improvement to the technology of original methyl ethylene high temperature vulcanizing silicone rubber.For the machinery that improves and improve product and the over-all properties of processing, on production equipment, increased mixing device.So change, just can promptly have the high molecular while that low-molecular-weight high-temperature sulfuration silicon rubber raw rubber is also arranged easily as requested, and can bring great convenience for new Formula Design and production easily according to the requirement of technology.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing and with illustrated embodiments the present invention is done detailed explanation.
Embodiment one: consult Fig. 1, methyl ethylene high temperature vulcanizing silicone rubber production technology, carry out according to following steps:
A: the major ingredient dehydration, under the condition of vacuum, to carry out, the temperature that requires dehydration is at 45 ℃, and the vacuum tightness of requirement is-0.1Mpa that the time of dehydration is 2 hours, blasts nitrogen during dehydration, perhaps imposes stirring;
B: polyreaction, will there be the dimethyl cyclosiloxane to put in the polymerization reaction kettle, the temperature of reaction is 105-℃, under condition of normal pressure, blanketing with inert gas, the time of reaction is 2 hours;
C: before above-mentioned polyreaction, add the auxiliary agent that has dewatered;
Comprise following auxiliary agent: 1, molecular weight regulator: alkyl-blocked low polydimethylsiloxane, perhaps have the organopolysiloxane of alkene, the molecular weight ranges of the auxiliary agent of adding is: 0-2000; 2, catalyzer: alkali metal hydroxide, perhaps organic bases; 3, improve the organic compound of cross-linking set: the ring body that has the organopolysiloxane of alkylene;
D: the polymer raw material of the different molecular weight of the organopolysiloxane after two kinds or the two or more polymerization is put into mixing kettle, mix fully, in this mixing kettle catalyzer is destroyed or neutralize;
E: take off low molecule, the product material after the above-mentioned D step is put into the top of taking off low molecule still, with catalyst breakage, allow material decompose under 160 ℃ condition, kept under said temperature 30 minutes, above-mentioned reaction is to carry out under non-pressurized condition; After above-mentioned broken matchmaker's process was finished, material improved surface-area through card, and under the condition of negative pressure of-0.1Mpa, the low molecule in the reactant reduces pressure by flash distillation then, and the temperature of flash distillation is 160 ℃;
F: the low molecule of deviating from: the low molecule of flash distillation reclaims by condensation and cooling.
Embodiment two: present embodiment and embodiment one difference are:
A: the major ingredient dehydration, under the condition of vacuum, to carry out, the temperature that requires dehydration is at 70 ℃, and the vacuum tightness of requirement is-0.096Mpa that the time of dehydration is 4 hours, blasts nitrogen during dehydration, perhaps imposes stirring;
B: polyreaction, will there be the dimethyl cyclosiloxane to put in the polymerization reaction kettle, the temperature of reaction is 115 ℃, under condition of normal pressure, blanketing with inert gas, the time of reaction is 4 hours;
C: before above-mentioned polyreaction, add the auxiliary agent that has dewatered;
D: the polymer raw material of the different molecular weight of the organopolysiloxane after two kinds or the two or more polymerization is put into mixing kettle, mix fully, in this mixing kettle catalyzer is destroyed or neutralize;
E: take off low molecule, the product material after the above-mentioned D step is put into the top of taking off low molecule still, with catalyst breakage, allow material decompose under 150 ℃ condition, kept under said temperature 60 minutes, above-mentioned reaction is to carry out under non-pressurized condition; After above-mentioned broken matchmaker's process was finished, material improved surface-area through card, and under the condition of negative pressure of-0.096Mpa, the low molecule in the reactant reduces pressure by flash distillation then, and the temperature of flash distillation is 170 ℃;
F: the low molecule of deviating from: the low molecule of flash distillation reclaims by condensation and cooling.
Embodiment three: present embodiment and embodiment one difference are:
A: the major ingredient dehydration, under the condition of vacuum, to carry out, the temperature that requires dehydration is at 50 ℃, and the vacuum tightness of requirement is-0.1Mpa that the time of dehydration is 2.3 hours, blasts nitrogen during dehydration, perhaps imposes stirring;
B: polyreaction, will there be the dimethyl cyclosiloxane to put in the polymerization reaction kettle, the temperature of reaction is 105-115 ℃, under condition of normal pressure, blanketing with inert gas, the time of reaction is 2.6 hours;
C: before above-mentioned polyreaction, add the auxiliary agent that has dewatered;
D: the polymer raw material of the different molecular weight of the organopolysiloxane after two kinds or the two or more polymerization is put into mixing kettle, mix fully, in this mixing kettle catalyzer is destroyed or neutralize;
E: take off low molecule, the product material after the above-mentioned D step is put into the top of taking off low molecule still, with catalyst breakage, allow material decompose under 165 ℃ condition, kept under said temperature 40 minutes, above-mentioned reaction is to carry out under non-pressurized condition; After above-mentioned broken matchmaker's process was finished, material improved surface-area through card, and under the condition of negative pressure of-0.1Mpa, the low molecule in the reactant reduces pressure by flash distillation then, and the temperature of flash distillation is 159 ℃;
F: the low molecule of deviating from: the low molecule of flash distillation reclaims by condensation and cooling.
Embodiment four: present embodiment and embodiment one difference are:
A: the major ingredient dehydration, under the condition of vacuum, to carry out, the temperature that requires dehydration is at 60 ℃, and the vacuum tightness of requirement is-0.093Mpa that the time of dehydration is 3 hours, blasts nitrogen during dehydration, perhaps imposes stirring;
B: polyreaction, will there be the dimethyl cyclosiloxane to put in the polymerization reaction kettle, the temperature of reaction is 110 ℃, under condition of normal pressure, blanketing with inert gas, the time of reaction is 3.5 hours;
C: before above-mentioned polyreaction, add the auxiliary agent that has dewatered;
D: the polymer raw material of the different molecular weight of the organopolysiloxane after two kinds or the two or more polymerization is put into mixing kettle, mix fully, in this mixing kettle catalyzer is destroyed or neutralize;
E: take off low molecule, the product material after the above-mentioned D step is put into the top of taking off low molecule still, with catalyst breakage, allow material decompose under 155 ℃ condition, kept under said temperature 50 minutes, above-mentioned reaction is to carry out under non-pressurized condition; After above-mentioned broken matchmaker's process was finished, material improved surface-area through card, and under the condition of negative pressure of-0.096Mpa, the low molecule in the reactant reduces pressure by flash distillation then, and the temperature of flash distillation is 165 ℃;
F: the low molecule of deviating from: the low molecule of flash distillation reclaims by condensation and cooling.
Embodiment five: present embodiment and embodiment one difference are:
A: the major ingredient dehydration, under the condition of vacuum, to carry out, the temperature that requires dehydration is at 55 ℃, and the vacuum tightness of requirement is-0.096Mpa that the time of dehydration is 3.5 hours, blasts nitrogen during dehydration, perhaps imposes stirring;
B: polyreaction, will there be the dimethyl cyclosiloxane to put in the polymerization reaction kettle, the temperature of reaction is 109 ℃, under condition of normal pressure, blanketing with inert gas, the time of reaction is 3 hours;
C: before above-mentioned polyreaction, add the auxiliary agent that has dewatered;
D: the polymer raw material of the different molecular weight of the organopolysiloxane after two kinds or the two or more polymerization is put into mixing kettle, mix fully, in this mixing kettle catalyzer is destroyed or neutralize;
E: take off low molecule, the product material after the above-mentioned D step is put into the top of taking off low molecule still, with catalyst breakage, allow material decompose under 168 ℃ condition, kept under said temperature 45 minutes, above-mentioned reaction is to carry out under non-pressurized condition; After above-mentioned broken matchmaker's process was finished, material improved the surface and plants through card, and under the condition of negative pressure of-0.097Mpa, the low molecule in the reactant reduces pressure by flash distillation then, and the temperature of flash distillation is 156 ℃;
F: the low molecule of deviating from: the low molecule of flash distillation reclaims by condensation and cooling.
Claims (1)
1. methyl ethylene high temperature vulcanizing silicone rubber production technology is characterized in that, carries out according to following steps:
A: major ingredient dehydration, under the condition of vacuum, to carry out, the temperature that requires dehydration is at 45-70 ℃, and the vacuum tightness of requirement is-0.1 to-0.096Mpa, and the time of dehydration is 2-4 hour, blasts nitrogen during dehydration, perhaps imposes stirring;
B: polyreaction, will there be the dimethyl cyclosiloxane to put in the polymerization reaction kettle, the temperature of reaction is 105-115 ℃, under condition of normal pressure, blanketing with inert gas, the time of reaction is 2-4 hour;
C: before above-mentioned polyreaction, add the auxiliary agent that has dewatered;
Comprise following auxiliary agent: 1, molecular weight regulator: alkyl-blocked low polydimethylsiloxane, perhaps have the organopolysiloxane of alkene, the molecular weight ranges of the auxiliary agent of adding is: 0-2000; 2, catalyzer: alkali metal hydroxide, perhaps organic bases; 3, improve the organic compound of cross-linking set: this organic compound is the ring body that has the organopolysiloxane of alkylene;
D: the polymer raw material of the different molecular weight of the organopolysiloxane after two kinds or the two or more polymerization is put into mixing kettle, mix fully, in this mixing kettle catalyzer is destroyed or neutralize;
E: take off low molecule, the product material after the above-mentioned D step is put into the top of taking off low molecule still, with catalyst breakage, allow material decompose under 150-170 ℃ condition, kept under said temperature 30-60 minute, above-mentioned reaction is to carry out under non-pressurized condition; After above-mentioned broken matchmaker's process was finished, material improved surface-area through card, and under-0.1 to-0.096Mpa condition of negative pressure, the low molecule in the reactant reduces pressure by flash distillation then, and the temperature of flash distillation is 150-170 ℃;
F: the low molecule of deviating from, the low molecule by flash distillation reclaims by condensation and cooling, obtains product at last.
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| CN2009101478363A CN101921487A (en) | 2009-06-15 | 2009-06-15 | Methyl ethylene high temperature vulcanizing silicone rubber production technology |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206348A (en) * | 2011-01-19 | 2011-10-05 | 颜建平 | Secondary flash evaporation low molecular weight removing process and equipment |
| CN103289634A (en) * | 2013-05-24 | 2013-09-11 | 江苏明昊新材料科技有限公司 | Production method of silicone sealant |
| CN103755962A (en) * | 2013-12-20 | 2014-04-30 | 浙江新安化工集团股份有限公司 | Production method for high-vinyl raw rubber |
| CN104610547A (en) * | 2015-02-05 | 2015-05-13 | 东莞新东方科技有限公司 | Crud silicone rubber and preparation method thereof |
| CN107522863A (en) * | 2017-09-15 | 2017-12-29 | 湖北兴瑞化工有限公司 | A kind of method that trifluoro propyl silicone oil is produced using ion exchange resin |
| CN107778488A (en) * | 2017-11-16 | 2018-03-09 | 湖北兴瑞化工有限公司 | A kind of de- low molecule device and the method that production viscosity is 30 1000000cs methyl-silicone oils |
-
2009
- 2009-06-15 CN CN2009101478363A patent/CN101921487A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206348A (en) * | 2011-01-19 | 2011-10-05 | 颜建平 | Secondary flash evaporation low molecular weight removing process and equipment |
| CN102206348B (en) * | 2011-01-19 | 2013-05-08 | 颜建平 | Secondary flash evaporation low molecular weight removing process and equipment |
| CN103289634A (en) * | 2013-05-24 | 2013-09-11 | 江苏明昊新材料科技有限公司 | Production method of silicone sealant |
| CN103755962A (en) * | 2013-12-20 | 2014-04-30 | 浙江新安化工集团股份有限公司 | Production method for high-vinyl raw rubber |
| CN103755962B (en) * | 2013-12-20 | 2016-08-17 | 浙江新安化工集团股份有限公司 | A kind of production method of high-vinyl raw rubber |
| CN104610547A (en) * | 2015-02-05 | 2015-05-13 | 东莞新东方科技有限公司 | Crud silicone rubber and preparation method thereof |
| CN107522863A (en) * | 2017-09-15 | 2017-12-29 | 湖北兴瑞化工有限公司 | A kind of method that trifluoro propyl silicone oil is produced using ion exchange resin |
| CN107778488A (en) * | 2017-11-16 | 2018-03-09 | 湖北兴瑞化工有限公司 | A kind of de- low molecule device and the method that production viscosity is 30 1000000cs methyl-silicone oils |
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Application publication date: 20101222 |