CN107603230A - Silicon rubber prepared using organosilicon low boiling hydrolysate and preparation method thereof - Google Patents
Silicon rubber prepared using organosilicon low boiling hydrolysate and preparation method thereof Download PDFInfo
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- CN107603230A CN107603230A CN201710742448.4A CN201710742448A CN107603230A CN 107603230 A CN107603230 A CN 107603230A CN 201710742448 A CN201710742448 A CN 201710742448A CN 107603230 A CN107603230 A CN 107603230A
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Abstract
The invention belongs to silicon rubber preparing technical field, and in particular to a kind of silicon rubber prepared using organosilicon low boiling hydrolysate and preparation method thereof.The silicon rubber prepared using organosilicon low boiling hydrolysate is made up of the raw material of following parts by weight：100 parts of vinyl polysiloxane, 20 60 parts of nano-calcium carbonate, 30 60 parts of organosilicon low boiling hydrolysate, the addition of platinum catalyst are 1 6ppm of raw material gross mass, and the addition of inhibitor is 0.1 6ppm of raw material gross mass.The invention provides a kind of method that no catalyst, low energy consumption utilize organic silicon low-boiling-point substance, under conditions of silicon rubber aging speed is not influenceed, strengthen the mechanical property of silicon rubber, substantially reduce the production cost of silicon rubber.
Description
Technical field
The invention belongs to silicon rubber preparing technical field, and in particular to a kind of silicon prepared using organosilicon low boiling hydrolysate
Rubber and preparation method thereof.
Background technology
Drastically expand along with domestic methylchlorosilane is production-scale, the yield of its accessory substance organic silicon low-boiling-point substance is also fast
Speed increase.The quantity in stock of organic silicon low-boiling-point substance increased dramatically carrys out enormous pressure to environment and safety belt.
During using direct synthesis methylchlorosilane, except target product Me2SiCL2Outside, the organosilicon of meeting by-product about 2% is low
Boil thing.Organic silicon low-boiling-point substance refers to silane mixture of the boiling point below 40 DEG C, mainly contains tetramethylsilane (molecular formula：Si
(CH3)4), trichlorosilane (molecular formula：SiHCl3), dimethyl dichlorosilane (DMCS) (CH3Cl2SiH), chlorodimethyl silane (molecular formula：
Si(CH3)2) and some alkane HCl.Because each component boiling point approaches, it is used it is difficult to separate.
Sun Feng exists《Organic silicon low-boiling-point substance progress》In point out：Organic silicon low-boiling-point substance processing method has two kinds, first, essence
Method of purification is evaporated, by chemically or physically acting on, changes iso-amylene and Me2SiHCl boiling-point difference is away from purifying Me2SiMe2SiHCl,
The major defect of this technology is to separate these low-boiling-point substance components to need very high fractionating column at present, and energy consumption is very big, and only purifies
A kind of important component.Second, redistribution procedure, the principle that redistribution procedure prepares single silane is to utilize being the richest in organic silicon low-boiling-point substance
The displacement that Si-Cl and Si-Me occurs with rich chlorine component in methylchlorosilane under high temperature and Louis acid catalysis for base component is reacted,
And high-boiling components are made to be cracked into single silane；Disproportionated reaction occurs between the single silane and low-boiling-point substance of cracking, changes into valuable silicon
Alkane monomer, such as Me2SiCl2、Me3SiCl, the current major defect of the technique are to need to consume many catalyst, these catalyst
It is cleaved product to be covered, recycling rate of waterused is very low, and often completes redistribution reaction under higher temperature, pressure.
The content of the invention
It is an object of the invention to provide a kind of silicon rubber prepared using organosilicon low boiling hydrolysate, both can effectively solve the problem that
The Utilizing question of organic silicon low-boiling-point substance, and energy consumption is low, it is not necessary to spent catalyst, can hydrolysis, avoids height at room temperature
Temperature and high pressure, and can strengthen the mechanical property of silicon rubber, substantially reduce the production cost of silicon rubber；Present invention simultaneously provides
The preparation method of the silicon rubber prepared using organosilicon low boiling hydrolysate, it is scientific and reasonable, simple and easy.
The silicon rubber of the present invention prepared using organosilicon low boiling hydrolysate, by the raw material system of following parts by weight
Into：
100 parts of vinyl polysiloxane
Nano-calcium carbonate 20-60 parts
Organosilicon low boiling hydrolysate 30-60 parts,
The addition of platinum catalyst is the 1-6ppm of raw material gross mass, and the addition of inhibitor is raw material gross mass
0.1-6ppm。
The silicon rubber of the present invention prepared using organosilicon low boiling hydrolysate, preferably by the raw material of following parts by weight
It is made：
100 parts of vinyl polysiloxane
20 parts of nano-calcium carbonate
30 parts of organosilicon low boiling hydrolysate,
The addition of platinum catalyst is the 1-6ppm of raw material gross mass, and the addition of inhibitor is raw material gross mass
0.1-6ppm。
Described vinyl polysiloxane is one or both of methyl vinyl silicone rubber or vinyl silicone oil, is
Commercially available prod.
The preparation method of described organosilicon low boiling hydrolysate is to take organic silicon low-boiling-point substance to be put into 1000mL beakers, Xiang Qi
Excessive water is added, after hydrolysis, by the white flock powder of generation and the mixed liquor of water, with Bush's funnel separating and filtering, 100-150
DEG C oven for drying is put into, continued to employ.
Described inhibitor is 1- acetenyl -1- cyclohexanol.
The aobvious alkalescence of nano-calcium carbonate, the acidity of organosilicon low boiling hydrolysate can be neutralized, keep the neutrality of silicon rubber, energy
Enough delaying aging speeds.
Described platinum catalyst, inhibitor are commercially available prod.
The preparation method of the silicon rubber of the present invention prepared using organosilicon low boiling hydrolysate, step are as follows：
(1) vinyl polysiloxane is added in mill；
(2) then, add the ground organosilicon low boiling hydrolysate of drying and nano-calcium carbonate be kneaded uniformly, then add
Enter platinum catalyst, inhibitor mixing uniformly, discharging, make semisolid elastomeric compound, place；Can hydrolyze organosilicon low boiling
The acidity of thing and the alkalescence of nano-calcium carbonate, neutralization reaction is thorough, silicone rubber products is turned into neutrality, after not influenceing silicon rubber
Service life or do not change the aging speed of silicon rubber；
(3) vulcanization tabletting and test are finally carried out in 150 DEG C on vulcanizing press；
Described vinyl polysiloxane is methyl vinyl silicone rubber.
The temperature of mill described in step (1) is 40 DEG C.
The particle diameter of grinding described in step (2) is 0.01-10 μm.
Standing time described in step (2) is 12h.
The preparation method of the silicon rubber of the present invention prepared using organosilicon low boiling hydrolysate, step are as follows：
(1) vinyl polysiloxane is added in the stirred tank of planetary mixer at room temperature；
(2) add and dry ground organosilicon low boiling hydrolysate and nano-calcium carbonate, be uniformly mixed, add platinum
Au catalyst, inhibitor, are uniformly mixed, and discharge, and place；The acidity and nano-calcium carbonate of organosilicon low boiling hydrolysate can be made
The alkalescence of calcium, neutralization reaction is thorough, silicone rubber products is turned into neutrality, does not influence the later service life of silicon rubber or do not change
The aging speed of silicon rubber；
(3) natural levelling in mould is finally poured into carry out vulcanizing tabletting and test in 150 DEG C；
Described vinyl polysiloxane is vinyl silicone oil.
The particle diameter of grinding described in step (2) is 0.01-10 μm, standing time 12h.
The present invention need not add crosslinking agent, because containing the Si -- H bond that can be crosslinked in organosilicon low boiling hydrolysate.
The cross-linking agent that white is obtained after organic silicon low-boiling-point substance is hydrolyzed is separated, the white cross-linking agent density very little,
Present powdered, therefore, may be used as the filler of silicon rubber, the production cost of silicon rubber can be substantially reduced, improve silicon rubber
Mechanical property, solve the Utilizing question of organic silicon low-boiling-point substance, in machine silicon low-boiling-point substance, most of chlorosilane such as trichlorosilane
(SiHCl3), dimethyl dichlorosilane (DMCS) (CH3Cl2SiH), the chlorosilane of diformazan one (Si (CH3)2HCl) can be hydrolyzed, after hydrolysis
Cross-linking agent can be easily separated, safe, energy consumption is low, and does not need spent catalyst, at room temperature can hydrolyze, avoid
High-temperature and high pressure.At present, organosilicon low boiling hydrolyses applying is used as filler, had not been reported into silicon rubber.
The present invention compared with prior art, has the advantages that：
1st, a kind of no catalyst is provided, the method that low energy consumption utilizes organic silicon low-boiling-point substance.
2nd, under conditions of silicon rubber aging speed is not influenceed, strengthen the mechanical property of silicon rubber, substantially reduce silicon rubber
Production cost.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
It is prepared by organosilicon low boiling hydrolysate：500g organic silicon low-boiling-point substances are taken to be put into 1000mL beakers, it is excessive to its addition
Water, the chlorosilane that at this moment organic silicon low-boiling-point substance contains include trichlorosilane, dimethyl dichlorosilane (DMCS), chlorodimethyl silane hydrolysis
Afterwards, further crosslinking, forms the white flock powder of density very little, and the white flock powder is mainly to be obtained after Si-Cl is hydrolyzed
Si-OH, Si-OH continue what is be cross-linked to form under sour environment, by the white flock powder of generation and the mixed liquor of water, use Bush
Funnel separating and filtering, 100 DEG C are put into oven for drying, continue to employ.
It is 40 DEG C by mill temperature setting, 90 parts of methyl vinyl silicone rubbers is added in mill, add 10
Part vinyl silicone oil, adds 60 parts ground of organosilicon low boiling hydrolysate of drying and 60 parts of nano-calcium carbonate be kneaded
Even, the addition of platinum catalyst is the 1ppm of raw material gross mass, and the addition of inhibitor is the 0.1ppm of raw material gross mass, is mixed
Refining is uniform, discharging, makes semisolid elastomeric compound, places 12h, can make the acidity and nano-calcium carbonate of organosilicon low boiling hydrolysate
The alkalescence of calcium, neutralization reaction is thorough, silicone rubber products is turned into neutrality, does not influence the later service life of silicon rubber or do not change
The aging speed of silicon rubber, finally carry out vulcanizing tabletting and test in 150 DEG C on vulcanizing press.
Embodiment 2
It is prepared by organosilicon low boiling hydrolysate：500g organic silicon low-boiling-point substances are taken to be put into 1000mL beakers, it is excessive to its addition
Water, the chlorosilane that at this moment organic silicon low-boiling-point substance contains include trichlorosilane, dimethyl dichlorosilane (DMCS), chlorodimethyl silane hydrolysis
Afterwards, further crosslinking, forms the white flock powder of density very little, and the white flock powder is mainly to be obtained after Si-Cl is hydrolyzed
Si-OH, Si-OH continue what is be cross-linked to form under sour environment, by the white flock powder of generation and the mixed liquor of water, use Bush
Funnel separating and filtering, 150 DEG C are put into oven for drying, continue to employ.
It is 40 DEG C by mill temperature setting, 100 parts of methyl vinyl silicone rubbers is added in mill；Then, add
Enter to dry 30 parts of ground organosilicon low boiling hydrolysate and 20 parts of nano-calcium carbonate be kneaded uniformly, platinum catalyst adds
Enter the 6ppm that amount is raw material gross mass, the addition of inhibitor is the 1ppm of raw material gross mass, is kneaded uniformly, discharging, makes half
The elastomeric compound of solid, 12h is placed, the acidity of organosilicon low boiling hydrolysate and the alkalescence of nano-calcium carbonate, neutralization reaction can be made
Thoroughly, silicone rubber products is turned into neutrality, do not influence the later service life of silicon rubber or do not change the aging speed of silicon rubber,
Finally carry out vulcanizing tabletting and test in 150 DEG C on vulcanizing press.
Embodiment 3
It is prepared by organosilicon low boiling hydrolysate：500g organic silicon low-boiling-point substances are taken to be put into 1000mL beakers, it is excessive to its addition
Water, the chlorosilane that at this moment organic silicon low-boiling-point substance contains include trichlorosilane, dimethyl dichlorosilane (DMCS), chlorodimethyl silane hydrolysis
Afterwards, further crosslinking, forms the white flock powder of density very little, and the white flock powder is mainly to be obtained after Si-Cl is hydrolyzed
Si-OH, Si-OH continue what is be cross-linked to form under sour environment, by the white flock powder of generation and the mixed liquor of water, use Bush
Funnel separating and filtering, 120 DEG C are put into oven for drying, continue to employ.
100 parts of vinyl silicone oils are added in the stirred tank of planetary mixer at room temperature, addition drying is ground to be had
40 parts of 45 parts of machine silicon low boiling hydrolysate and nano-calcium carbonate, are uniformly mixed, the addition of platinum catalyst is the total matter of raw material
The 1ppm of amount, the addition of inhibitor are the 6ppm of raw material gross mass, are uniformly mixed, discharge, place 12h, can make to have
The acidity of machine silicon low boiling hydrolysate and the alkalescence of nano-calcium carbonate, neutralization reaction is thorough, silicone rubber products is turned into neutrality, not shadow
Ring the later service life of silicon rubber or do not change the aging speed of silicon rubber, finally pour into mould natural levelling in 150 DEG C
Carry out vulcanizing tabletting and test.
The tensile strength of product test sample and elongation at break are tested according to GB/T528-1998 made from embodiment 1-3,
Tearing strength is tested according to GB/T529-1999, and hardness is tested according to GB/T531-1999.Test result is shown in Table 1.
Product test result made from the embodiment 1-3 of table 1
Claims (10)
1. a kind of silicon rubber prepared using organosilicon low boiling hydrolysate, it is characterised in that by the raw material system of following parts by weight
Into：
100 parts of vinyl polysiloxane
Nano-calcium carbonate 20-60 parts
Organosilicon low boiling hydrolysate 30-60 parts,
The addition of platinum catalyst is the 1-6ppm of raw material gross mass, and the addition of inhibitor is the 0.1- of raw material gross mass
6ppm。
2. the silicon rubber according to claim 1 prepared using organosilicon low boiling hydrolysate, it is characterised in that described second
Alkenyl polysiloxanes is one or both of methyl vinyl silicone rubber or vinyl silicone oil.
3. the silicon rubber according to claim 1 prepared using organosilicon low boiling hydrolysate, it is characterised in that described has
The preparation method of machine silicon low boiling hydrolysate is to take organic silicon low-boiling-point substance to be put into 1000mL beakers, and excessive water, hydrolysis are added to it
Afterwards, by the white flock powder of generation and the mixed liquor of water, with Bush's funnel separating and filtering, 100-150 DEG C is put into oven for drying,
Continue to employ.
4. the silicon rubber according to claim 1 prepared using organosilicon low boiling hydrolysate, it is characterised in that described suppression
Preparation is 1- acetenyl -1- cyclohexanol.
5. a kind of preparation method of any described silicon rubber prepared using organosilicon low boiling hydrolysate of claim 1-4, its
It is characterised by that step is as follows：
(1) vinyl polysiloxane is added in mill；
(2) then, add the ground organosilicon low boiling hydrolysate of drying and nano-calcium carbonate be kneaded uniformly, add platinum
Au catalyst, inhibitor are kneaded uniformly, discharging, make semisolid elastomeric compound, are placed；
(3) vulcanization tabletting and test are finally carried out in 150 DEG C on vulcanizing press；
Described vinyl polysiloxane is methyl vinyl silicone rubber.
6. the preparation method of the silicon rubber according to claim 5 prepared using organosilicon low boiling hydrolysate, its feature are existed
The temperature of mill described in step (1) is 40 DEG C.
7. the preparation method of the silicon rubber according to claim 5 prepared using organosilicon low boiling hydrolysate, its feature are existed
The particle diameter of grinding described in step (2) is 0.01-10 μm.
8. the preparation method of the silicon rubber according to claim 5 prepared using organosilicon low boiling hydrolysate, its feature are existed
Standing time described in step (2) is 12h.
9. a kind of preparation method of any described silicon rubber prepared using organosilicon low boiling hydrolysate of claim 1-4, its
It is characterised by that step is as follows：
(1) vinyl polysiloxane is added in the stirred tank of planetary mixer at room temperature；
(2) add and dry ground organosilicon low boiling hydrolysate and nano-calcium carbonate, be uniformly mixed, add platinum and urge
Agent, inhibitor, are uniformly mixed, and discharge, and place；
(3) natural levelling in mould is finally poured into carry out vulcanizing tabletting and test in 150 DEG C；
Described vinyl polysiloxane is vinyl silicone oil.
10. the preparation method of the silicon rubber according to claim 9 prepared using organosilicon low boiling hydrolysate, its feature are existed
The particle diameter of grinding described in step (2) is 0.01-10 μm, standing time 12h.
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| US4408030A (en) * | 1982-03-22 | 1983-10-04 | Dow Corning Corporation | Waste chlorosilane treatment |
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Address after: Tangshan Huantai County town of 256401 Shandong city of Zibo province Shandong Dongyue Group Technology Management Center Applicant after: Shandong Dongyue organosilicon material Limited by Share Ltd Address before: Tangshan Huantai County town of 256401 Shandong city of Zibo province Shandong Dongyue Group Technology Management Center Applicant before: Shandong Dongyue Silicon Material co., Ltd. |
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