CN1978491A - Method for preparing fluoro-silicone elastomer - Google Patents
Method for preparing fluoro-silicone elastomer Download PDFInfo
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- CN1978491A CN1978491A CN 200510111206 CN200510111206A CN1978491A CN 1978491 A CN1978491 A CN 1978491A CN 200510111206 CN200510111206 CN 200510111206 CN 200510111206 A CN200510111206 A CN 200510111206A CN 1978491 A CN1978491 A CN 1978491A
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Abstract
This invention discloses the preparation method of a kind of fluosilicic elastomer. The invention includes the preparation processes of the fluochloride silane, the fluosilicicone, the fluosilicic collagen and the fluosilicic elastomer. It is characterized in that the alkene and the chlorohydrocarbon reacted additionally, and fluorinated directly, then reacted with silane. The fluochloride silane was then obtained. All the technological processes in this invention have no bottleneck, and were carried under suitable temperature and press. The technological processes are convenience and easy to control, thus it has the industrial exploitation prospect.
Description
Technical field
The present invention relates to a kind of method for preparing fluoro silicone elastomers, particularly relate to the method for preparing fluorosilicone.
Background technology
Fluorosilicone is the main raw material of fluorine silicon liquid glue, fluoro silicone elastomers, fluorine silicon grease, fluorine silicon thermal insulating fluid, fluorine silicon defoaming agent, fluorine silicon fabric finishing agent.Fluoro silicone elastomers has good chemically-resistant solvent (except that ketone), anti-fuel oil, high-low temperature resistant (70～+ 250 ℃) performance, is widely used in the sealing of space shuttle fuel tank, automotive oil tank sealing, artificial organ, instrument industry.
Originally preparation fluochloride silane method is with after carbon enpara and the alkene addition, flaorination process by a complicated step, two steps obtains fluoroolefin through the rectification and purification of 3～6 towers then, and addition reaction generation fluochloride silane takes place under High Temperature High Pressure for fluoroolefin and chlorosilane then.Step in this technology, two step fluorizated yields are low, the rectification and purification process energy consumption height of 3～6 towers, and yield poorly.The complete process that fluochloride silane prepares fluorosilicone, fluorosilicone prepares fluorine silicon raw rubber and rubber is mixing, be sulfided into fluoro silicone elastomers is report not almost, and at present domestic all is laboratory process, is difficult to break through produce amplify bottleneck, and output is very low.As document US 2,596,967, US3,288,712, US772,484, US1,075,101 grade is laboratory process.
The shortcoming of technology is that production bottleneck is many at present, and output is little, and the energy consumption height is unwell to industry's enlarging production.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of method for preparing fluoro silicone elastomers, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the preparation process of fluochloride silane, the preparation process of fluorosilicone, the preparation process of fluorine silicon raw rubber and the preparation process of fluoro silicone elastomers, it is characterized in that, fluochloride silane is directly fluoridized with the silane hydrocarbon reaction after by carbon enpara and alkene addition reaction and is obtained, and comprises the steps:
(1) carbon enpara and alkene under causing, catalyzer were reacted 14～18 hours under 110～160 ℃ the temperature, obtain the affixture of carbon enpara and alkene, the molar ratio of carbon enpara and alkene is: the carbon enpara: alkene=1: 0.8～2.5, said catalyzer chosen from Fe system or copper are a kind of in the muriate, catalyst levels is 0.5～5% of a carbon enpara molar weight, and reaction expression is as follows:
RCXYZ+R
1CH＝CBD＝C(R
1BD)C(HZ)C(XYR)
RCXYZ is the carbon enpara, wherein:
R is-H-CH
3,-Cl;
X is-H-CH
3,-Cl;
Y is-H-CH
3,-Cl;
Z is-H-CH
3,-Cl;
Preferably R is-H ,-C1, and preferably X is-H ,-Cl, preferred Y is-CH
3Or-Cl, preferred Z is-CH
3,-Cl.；
R
1CH=CBD is an alkene, wherein:
R
1For-H ,-CH
3
B is-CH
3,-H;
D is-CH
3,-H;
Preferred R
1For-H, B is-H that D is-CH
3,-H;
(2) the carbon enpara of fluorizating agent and step (1) and the affixture of alkene are carried out fluoridation, directly fluoridize into Fluorine containing olefine, the temperature of fluoridation is 190～300 ℃, and optimum temperature is 200～290 ℃, reaction times is 4～6 hours, obtains Fluorine containing olefine;
Fluorizating agent is selected from a kind of or its mixture in Sodium Fluoride, aluminum fluoride or the cuprous chloride;
The molar ratio of the affixture of fluorizating agent and carbon enpara and alkene is: fluorizating agent: the affixture of carbon enpara and alkene=1: 5～20, and reaction expression is as follows:
C(R
1BD)C(HZ)C(XYR)+3-F→C(BD)＝C(H)CFFF
(3) Fluorine containing olefine and chlorosilane addition reaction are generated fluochloride silane;
The temperature of reaction is 140～200 ℃, and optimum temperature is 140～170 ℃, and the reaction times is 10～12 hours, and the molar ratio of Fluorine containing olefine and chlorosilane is a Fluorine containing olefine: chlorosilane=1: 2～4;
The molecular formula of said chlorosilane is: R
2R
3SiCl, wherein:
R
2For-CH=CH
2,-H ,-C
6H
5,-CH
3Or-Cl;
Preferred R
2For-H ,-CH
3Or-Cl, preferred R
3For-CH=CH
2,-C
6H
5,-CH
3Or-Cl, reaction expression is as follows:
C(BD)＝C(H)CFFF+R
2R
3SiCl＝C(BD)C(HR
3)CFFFR
2SiCl
Following step is adopted in the preparation of fluorosilicone:
With fluochloride silane directly and water carry out dechlorination reaction, the temperature of reaction is 30～90 ℃, reaction times is 7～11 hours, collection is with the dechlorination material, in having the reactor of water distilling apparatus, carry out dehydration reaction, the temperature of dehydration reaction is 100～350 ℃, and optimum temperature is 120～350 ℃, obtains fluorosilicone.
The method of the preparation of fluorine silicon raw rubber and methyl silicone rubber preparation method are similar, as Kirk N.Ind EngChem, and 1959,51:515 document disclosed method, the present invention adopts following step:
With fluorosilicone at 70～200 ℃, optimum temperature is under 80～180 ℃ the condition, dropped into catalyst reaction 6～10 hours, the fluorosilicone direct polymerization is a fluorine silicon raw rubber, said catalyzer is selected from a kind of in tetrahydroxy ammonium hydroxide, silanol lithium or the mineral acid, and the mole dosage of catalyzer is 0.1～3% of a fluorosilicone.
The method of the preparation of method for preparing fluoro-silicone elastomer and silicone elastomer is similar, and as EP382370 document disclosed method, the present invention adopts following step:
With fluorine silicon raw rubber in rubber mixing machine with auxiliary agent after mixing 2～20 minutes, add reinforced filling, mixing again 20～40 minutes, added vulcanizing agent mixing again 1～10 minute, melting temperature is 30～80 ℃, film is taken out from rubber mixing machine, vulcanize in vulcanizing press, curing temperature is 100～200 ℃, and optimum temperature is 120～170 ℃, curing time is 10～15 minutes, obtains fluoro silicone elastomers.
Said auxiliary agent is the auxiliary agent of this area routine, a kind of or mixture in preferred dimethyl silicone oil, silanol or the phenyl silicone oil, and the weight consumption of auxiliary agent is 2～10% of a fluorine silicon raw rubber;
Said reinforced filling is the reinforced filling of this area routine, a kind of or mixture in preferred white carbon black, lime carbonate, the Calcium hydrogen carbonate, and the weight consumption of reinforced filling is 10～60% of a fluorine silicon raw rubber;
Said vulcanizing agent is the peroxide vulcanizing agent of this area routine, and the weight consumption of vulcanizing agent is 0.5～4% of a fluorine silicon raw rubber;
The whole technological process of the present invention does not have production bottleneck, and carries out under suitable temperature, pressure, the convenient easily control of technological operation, thus make this technology have the prospect of commercial exploitation.
Embodiment
Example given below is used for illustrating the invention that is provided.The detection method of the product of embodiment adopts the method for standard codes such as GB/T528, GB/T529, GB/T531, GB/T7759, GB/T1682.
Embodiment 1
Have in chuck and the steam-heated stainless steel still at 150L and to add the carbon enpara (wherein trichloromethane 10%, tetrachloromethane 80%, trichloroethane 10%) 90 kilograms, catalyzer iron(ic) chloride 800 grams, high-speed stirring 2 hours, stirring velocity is 100 rev/mins, and steam is warmed up to 80 ℃, and (wherein propylene 5% to feed alkene in the stainless steel still, ethene 85%, butylene 10%), 10 kilograms/hour of input speeds, feed time are 6 hours.150 ℃ of insulations 4 hours, cooling then, directly pump into the stainless steel fixed bed of 300L, the 200L fluorizating agent is housed, fluorizating agent is a Sodium Fluoride, pumping into speed is 5 kilograms/hour, fixed bed is warming up to 270 ℃, and the Fluorine containing olefine of generation is packed in the surge tank, adds 60 kilograms of chlorosilane (therein ethylene base chlorosilanes 15% in the reactor of 80L, dimethyl dichlorosilane (DMCS) 80%, phenyl chlorosilane 5%), progressively add Fluorine containing olefine then, feed rate is 5 kilograms/hour, the reinforced time is 4 hours, and reinforced 160 ℃ of the insulations of finishing obtained 40 kilograms of fluochloride silanes after 2 hours.40 kilograms of fluochloride silanes are joined in the reactor of 100L, drop into 80 kilograms in water then, stir and separate byproduct hydrochloric acid after 2 hours, the material that will take off chlorine adds in the 100L reactor of band water distilling apparatus, be warmed up to 100 ℃ and begin dehydration, progressively be warmed up to 130 ℃, stablize 3 hours after, obtain 30 kilograms of purity and be 99.0% fluorosilicone.30 kilograms fluorosilicones are dropped in the stainless steel cauldron of 40L, be warming up to 140 ℃, add 10 gram tetrahydroxy ammonium hydroxide then, fluorosilicone aggregates into 30 kilograms of fluorine silicon raw rubbers rapidly.It is in 150 liang of roller rubber mixing machines of that 10 kilograms of fluorine silicon raw rubbers are joined diameter, mixing 3 minutes, adds 200 gram dimethyl silicone oils and 200 gram silanols then, after mixing 5 minutes, add 2 kilograms of white carbon blacks, mixing 20 minutes, added vulcanizing agent mixing again 5 minutes, film can be taken out from rubber mixing machine, vulcanize in vulcanizing press, curing temperature is at 160 ℃, and curing time is 10 minutes, obtain fluoro silicone elastomers FSY001, elastomer performance sees Table 1 after testing.
Table 1
Density: 1.3
Hardness: 42 Shaos
Tensile strength: 8.0Mpa
Elongation: 250%
Tear strength: 10Mpa
Setafter break: 10%
Compression set: 28%
250 ℃ * 22h hot air aging
Hardness :+4
Tensile strength-32%
Tensile strength at yield-37%
150 ℃ * 70h 30# standard oil is aging
Hardness :-2
Tensile strength :-18%
Tensile strength at yield :-14%
23 ℃ * 24h fuel oil B is aging
Mass change: 9%
Temperature limit of brittleness-60 ℃ non-cracking is qualified
Embodiment 2
Have in chuck and the steam-heated stainless steel still at 150L and to add the carbon enpara (wherein trichloromethane 40%, tetrachloromethane 40%, trichloroethane 20%) 90 kilograms, catalyzer iron(ic) chloride 950 grams, high-speed stirring 2 hours, stirring velocity is 100 rev/mins, steam is warmed up to 80 ℃, feeds alkene (wherein propylene 5%, ethene 95%) in the stainless steel still, 10 kilograms/hour of input speeds, feed time are 6 hours.150 ℃ of insulations 4 hours, cooling then, directly pump into the stainless steel fixed bed of 300L, the 200L fluorizating agent of packing into, fluorizating agent is an aluminum fluoride, pumping into speed is 5 kilograms/hour, fixed bed is warming up to 300 ℃, and the Fluorine containing olefine of generation is packed in the surge tank, adds 50 kilograms of chlorosilane (therein ethylene base chlorosilanes 5% in the reactor of 80L, dimethyl dichlorosilane (DMCS) 90%, phenyl chlorosilane 5%), progressively add Fluorine containing olefine then, feed rate is 5 kilograms/hour, the reinforced time is 3 hours, and reinforced 160 ℃ of the insulations of finishing obtained 35 kilograms of fluochloride silanes after 2 hours.35 kilograms of fluochloride silanes are joined in the reactor of 100L, drop into 70 kilograms in water then, stir and separate byproduct hydrochloric acid after 2 hours, the material that will take off chlorine adds in the 100L reactor of band water distilling apparatus, be warmed up to 100 ℃ and begin dehydration, progressively be warmed up to 150 ℃, stablize 3 hours after, obtain 25 kilograms of purity and be 99.0% fluorosilicone.25 kilograms fluorosilicones are dropped in the stainless steel cauldron of 40L, be warming up to 140 ℃, add 5 gram tetrahydroxy ammonium hydroxide then, fluorosilicone aggregates into 25 kilograms of fluorine silicon raw rubbers rapidly.It is in 150 liang of roller rubber mixing machines of that 10 kilograms of fluorine silicon raw rubbers are joined diameter, mixing 3 minutes, adds 200 gram dimethyl silicone oils and 150 gram silanols then, after mixing 5 minutes, add 2 kilograms of white carbon blacks, mixing 20 minutes, added vulcanizing agent mixing again 5 minutes, film can be taken out from rubber mixing machine, vulcanize in vulcanizing press, curing temperature is at 180 ℃, and curing time is 10 minutes, obtain fluoro silicone elastomers FSY002, elastomer performance sees Table 2 after testing.
Table 2
Density: 1.35
Hardness: 45 Shaos
Tensile strength: 9.0Mpa
Elongation: 300%
Tear strength: 10Mpa
Setafter break: 11%
Compression set: 29%
250 ℃ * 22h hot air aging
Hardness :+3
Tensile strength-35%
Tensile strength at yield-36%
150 ℃ * 70h 30# standard oil is aging
Hardness :-2
Tensile strength :-19%
Tensile strength at yield :-13%
23 ℃ * 24h fuel oil B is aging
Mass change: 10%
Temperature limit of brittleness-60 ℃ non-cracking is qualified
Embodiment 3
Have in chuck and the steam-heated stainless steel still at 150L and to add the carbon enpara (wherein tetrachloromethane 95%, trichloroethane 5%) 90 kilogram, catalyzer iron(ic) chloride 1050 grams, high-speed stirring 2 hours, stirring velocity are 100 rev/mins, and steam is warmed up to 80 ℃, (wherein propylene 5% to feed alkene in the stainless steel still, ethene 95%), 10 kilograms/hour of input speeds, feed time are 6 hours.150 ℃ of insulations 4 hours, cooling then, directly pump into stainless steel fixed bed (the 200L fluorizating agent of packing into of 300L, fluorizating agent is the mixture of Sodium Fluoride and cuprous chloride, mol ratio is 1: 1, pumping into speed is 5 kilograms/hour, fixed bed is warming up to 280 ℃, the Fluorine containing olefine that produces is packed in the surge tank, adds 60 kilograms of chlorosilanes (wherein dimethyl dichlorosilane (DMCS) 95%, phenyl chlorosilane 5%) in the reactor of 80L, progressively add Fluorine containing olefine then, feed rate is 5 kilograms/hour, and the reinforced time is 4 hours, and reinforced 160 ℃ of the insulations of finishing obtained 50 kilograms of fluochloride silanes after 2 hours.50 kilograms of fluochloride silanes are joined in the reactor of 100L, drop into 90 kilograms in water then, stir and separate byproduct hydrochloric acid after 2 hours, the material that will take off chlorine adds in the 100L reactor of band water distilling apparatus, be warmed up to 100 ℃ and begin dehydration, progressively be warmed up to 160 ℃, stablize 3 hours after, obtain 41 kilograms of purity and be 99.0% fluorosilicone.41 kilograms fluorosilicones are dropped in the stainless steel cauldron of 50L, be warming up to 140 ℃, add 12 gram silanol lithiums then, fluorosilicone aggregates into 41 kilograms of fluorine silicon raw rubbers rapidly.It is in 150 liang of roller rubber mixing machines of that 10 kilograms of fluorine silicon raw rubbers are joined diameter, mixing 3 minutes, adds 200 gram dimethyl silicone oils and 200 gram silanols then, after mixing 5 minutes, add 4 kilograms of white carbon blacks, mixing 20 minutes, added vulcanizing agent mixing again 5 minutes, film can be taken out from rubber mixing machine, vulcanize in vulcanizing press, curing temperature is at 160 ℃, and curing time is 10 minutes, obtain fluoro silicone elastomers FSY003, elastomer performance sees Table 3 after testing.
Table 3
Density: 1.4
Hardness: 65 Shaos
Tensile strength: 9.5Mpa
Elongation: 350%
Tear strength: 12Mpa
Setafter break: 10%
Compression set: 25%
250 ℃ * 22h hot air aging
Hardness :+4
Tensile strength-30%
Tensile strength at yield-31%
150 ℃ * 70h 30# standard oil is aging
Hardness :-2
Tensile strength :-12%
Tensile strength at yield :-11%
23 ℃ * 24h fuel oil B is aging
Mass change: 11%
Temperature limit of brittleness-60 ℃ non-cracking is qualified
Embodiment 4
Have in chuck and the steam-heated stainless steel still at 150L and to add the carbon enpara (wherein trichloromethane 75%, tetrachloromethane 15%, trichloroethane 10%) 90 kilograms, catalyzer iron(ic) chloride 1350 grams, high-speed stirring 2 hours, stirring velocity is 100 rev/mins, and steam is warmed up to 80 ℃, and (wherein propylene 65% to feed alkene in the stainless steel still, ethene 25%, butylene 10%), 10 kilograms/hour of input speeds, feed time are 6 hours.150 ℃ of insulations 4 hours, cooling then, directly pump into the stainless steel fixed bed of 300L, the 200L fluorizating agent of packing into, fluorizating agent is a cuprous chloride, pumping into speed is 5 kilograms/hour, fixed bed is warming up to 290 ℃, and the Fluorine containing olefine of generation is packed in the surge tank, adds 40 kilograms of chlorosilane (therein ethylene base chlorosilanes 75% in the reactor of 80L, dimethyl dichlorosilane (DMCS) 20%, phenyl chlorosilane 5%), progressively add Fluorine containing olefine then, feed rate is 5 kilograms/hour, the reinforced time is 2 hours, and reinforced 160 ℃ of the insulations of finishing obtained 20 kilograms of fluochloride silanes after 2 hours.20 kilograms of fluochloride silanes are joined in the reactor of 100L, drop into 50 kilograms in water then, stir and separate byproduct hydrochloric acid after 2 hours, the material that will take off chlorine adds in the 100L reactor of band water distilling apparatus, be warmed up to 100 ℃ and begin dehydration, progressively be warmed up to 130 ℃, stablize 3 hours after, obtain 17 kilograms of purity and be 99.0% fluorosilicone.17 kilograms fluorosilicones are dropped in the stainless steel cauldron of 30L, be warming up to 140 ℃, add 6 gram tetrahydroxy ammonium hydroxide then, fluorosilicone aggregates into 17 kilograms of fluorine silicon raw rubbers rapidly.It is in 150 liang of roller rubber mixing machines of that 10 kilograms of fluorine silicon raw rubbers are joined diameter, mixing 3 minutes, adds 200 gram dimethyl silicone oils and 200 gram silanols then, after mixing 5 minutes, add 4 kilograms of white carbon blacks, mixing 20 minutes, added vulcanizing agent mixing again 5 minutes, film can be taken out from rubber mixing machine, vulcanize in vulcanizing press, curing temperature is at 160 ℃, and curing time is 10 minutes, obtain fluoro silicone elastomers FSY004, elastomer performance sees Table 4 after testing.
Table 4
Density: 1.4
Hardness: 67 Shaos
Tensile strength: 8.5Mpa
Elongation: 290%
Tear strength: 10Mpa
Setafter break: 15%
Compression set: 30%
250 ℃ * 22h hot air aging
Hardness :+4
Tensile strength-36%
Tensile strength at yield-37%
150 ℃ * 70h 30# standard oil is aging
Hardness :-2
Tensile strength :-17%
Tensile strength at yield :-14%
23 ℃ * 24h fuel oil B is aging
Mass change: 13%
Temperature limit of brittleness-60 ℃ non-cracking is qualified
Embodiment 5
Have in chuck and the steam-heated stainless steel still at 150L and to add the carbon enpara (wherein tetrachloromethane 5%, trichloroethane 95%) 90 kilogram, catalyzer iron(ic) chloride 950 grams, high-speed stirring 2 hours, stirring velocity are 100 rev/mins, and steam is warmed up to 80 ℃, (wherein propylene 95% to feed alkene in the stainless steel still, ethene 5%), 10 kilograms/hour of input speeds, feed time are 6 hours.150 ℃ of insulations 4 hours, cooling then, directly pump into the stainless steel fixed bed of 300L, the 200L fluorizating agent of packing into, fluorizating agent is a Sodium Fluoride, pumping into speed is 5 kilograms/hour, fixed bed is warming up to 270 ℃, the Fluorine containing olefine that produces is packed in the surge tank, adds 60 kilograms of chlorosilanes (wherein dimethyl dichlorosilane (DMCS) 95%, phenyl chlorosilane 5%) in the reactor of 80L, progressively add Fluorine containing olefine then, feed rate is 5 kilograms/hour, and the reinforced time is 3 hours, and reinforced 160 ℃ of the insulations of finishing obtained 25 kilograms of fluochloride silanes after 2 hours.25 kilograms of fluochloride silanes are joined in the reactor of 100L, drop into 60 kilograms in water then, stir and separate byproduct hydrochloric acid after 2 hours, the material that will take off chlorine adds in the 100L reactor of band water distilling apparatus, be warmed up to 100 ℃ and begin dehydration, progressively be warmed up to 130 ℃, stablize 3 hours after, obtain 20 kilograms of purity and be 99.0% fluorosilicone.20 kilograms fluorosilicones are dropped in the stainless steel cauldron of 30L, be warming up to 140 ℃, add 7 gram tetrahydroxy ammonium hydroxide then, fluorosilicone aggregates into 20 kilograms of fluorine silicon raw rubbers rapidly.It is in 150 liang of roller rubber mixing machines of that 10 kilograms of fluorine silicon raw rubbers are joined diameter, mixing 3 minutes, adds 200 gram dimethyl silicone oils and 200 gram silanols then, after mixing 5 minutes, add 2 kilograms of white carbon blacks, mixing 20 minutes, added vulcanizing agent mixing again 5 minutes, film can be taken out from rubber mixing machine, vulcanize in vulcanizing press, curing temperature is at 170 ℃, and curing time is 10 minutes, obtain fluoro silicone elastomers FSY005, elastomer performance sees Table 5 after testing.
The performance of gained fluoro silicone elastomers of the present invention is as follows:
Table 5
Density: 1.3
Hardness: 42 Shaos
Tensile strength: 7.5Mpa
Elongation: 250%
Tear strength: 9Mpa
Setafter break: 19%
Compression set: 33%
250 ℃ * 22h hot air aging
Hardness :+4
Tensile strength-39%
Tensile strength at yield-42%
150 ℃ * 70h 30# standard oil is aging
Hardness :-2
Tensile strength :-22%
Tensile strength at yield :-17%
23 ℃ * 24h fuel oil B is aging
Mass change: 15%
Temperature limit of brittleness-60 ℃ non-cracking is qualified
Claims (10)
1. method for preparing fluoro-silicone elastomer, comprise the preparation process of fluochloride silane, the preparation process of fluorosilicone, the preparation process of fluorine silicon raw rubber and the preparation process of fluoro silicone elastomers, it is characterized in that fluochloride silane is directly fluoridized with the silane hydrocarbon reaction after by carbon enpara and alkene addition reaction and obtained.
2. method according to claim 1 is characterized in that the preparation method of fluochloride silane comprises the steps:
(1) carbon enpara and alkene were reacted 14～18 hours under 110～160 ℃ the temperature under catalyzer causes, obtain the affixture of carbon enpara and alkene;
The molecular formula of carbon enpara is RCXYZ, wherein:
R is-H ,-CH
3Or-Cl, X is-H ,-CH
3Or-Cl, Y is-H ,-CH
3Or-Cl, Z is-H ,-CH
3Or-Cl;
The molecular formula of alkene is R
1CH=CBD, wherein:
R
1For-H or-CH
3, B is-CH
3Or-H, D is-CH
3Or-H;
(2) the carbon enpara of fluorizating agent and step (1) and the affixture of alkene are carried out fluoridation, directly fluoridize into Fluorine containing olefine, the temperature of fluoridation is 190～300 ℃, reaction times is 4～6 hours, obtain Fluorine containing olefine, fluorizating agent is selected from a kind of or its mixture in Sodium Fluoride, aluminum fluoride or the cuprous chloride;
(3) Fluorine containing olefine and chlorosilane addition reaction are generated fluochloride silane;
The temperature of reaction is 140～200 ℃, and the reaction times is 10～12 hours;
The molecular formula of said chlorosilane is: R
2R
3SiCl, wherein:
R
2For-CH=CH
2,-H ,-C
6H
5,-CH
3Or-Cl.
3. method according to claim 2 is characterized in that, the molar ratio of carbon enpara and alkene is: the carbon enpara: alkene=1: 0.8～2.5.
4. method according to claim 2 is characterized in that, it is a kind of in the muriate that said catalyzer is selected from from iron system or copper, and catalyst levels is 0.5～5% of a carbon enpara molar weight.
5. method according to claim 2 is characterized in that, R is-H or-Cl, X is-H or-Cl, Y is-CH
3Or-Cl, Z is-CH
3Or-Cl, R
1For-H, B is-H that D is-CH
3Or-H, R
2For-H ,-CH
3Or-Cl, R
3For-CH=CH
2,-C
6H
5,-CH
3Or-Cl.
6. method according to claim 2 is characterized in that, the molar ratio of the affixture of fluorizating agent and carbon enpara and alkene is: fluorizating agent: the affixture of carbon enpara and alkene=1: 5～20.
7. method according to claim 2 is characterized in that, the molar ratio of Fluorine containing olefine and chlorosilane is a Fluorine containing olefine: chlorosilane=1: 2～4.
8. method according to claim 1, the preparation that it is characterized in that fluorosilicone comprises following step: with fluochloride silane directly and water carry out dechlorination reaction, the temperature of reaction is 30～90 ℃, reaction times is 7～11 hours, collection is with the dechlorination material, carry out dehydration reaction in having the reactor of water distilling apparatus, the temperature of dehydration reaction is 100～350 ℃, obtains fluorosilicone.
9. method according to claim 1, the preparation that it is characterized in that fluorine silicon raw rubber comprises following step: with fluorosilicone under 70～200 ℃ condition, dropped into catalyst reaction 6～10 hours, the fluorosilicone direct polymerization is a fluorine silicon raw rubber, said catalyzer is selected from a kind of in tetrahydroxy ammonium hydroxide, silanol lithium or the mineral acid, and the mole dosage of catalyzer is 0.1～3% of a fluorosilicone.
10. method according to claim 1, the preparation that it is characterized in that fluoro silicone elastomers comprises following step: with fluorine silicon raw rubber in rubber mixing machine with auxiliary agent after mixing 2～20 minutes, add reinforced filling, mixing again 20～40 minutes, added vulcanizing agent mixing again 1～10 minute, melting temperature is 30～80 ℃, film is taken out from rubber mixing machine, vulcanize in vulcanizing press, curing temperature is 100～200 ℃, curing time is 10～15 minutes, obtains fluoro silicone elastomers.
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|---|---|---|---|
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| CN100469818C CN100469818C (en) | 2009-03-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4028338A (en) * | 1975-10-09 | 1977-06-07 | General Electric Company | Fluorosiloxydiphenylsiloxy block copolymers |
| US5041588A (en) * | 1989-07-03 | 1991-08-20 | Dow Corning Corporation | Chemically reactive fluorinated organosilicon compounds and their polymers |
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