CN110183481A - The technique of catalytic pyrolysis organosilicon high-boiling product - Google Patents
The technique of catalytic pyrolysis organosilicon high-boiling product Download PDFInfo
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- CN110183481A CN110183481A CN201910215202.0A CN201910215202A CN110183481A CN 110183481 A CN110183481 A CN 110183481A CN 201910215202 A CN201910215202 A CN 201910215202A CN 110183481 A CN110183481 A CN 110183481A
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- 238000009835 boiling Methods 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000007233 catalytic pyrolysis Methods 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000000178 monomer Substances 0.000 claims abstract description 11
- 230000003197 catalytic effect Effects 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 23
- 238000000354 decomposition reaction Methods 0.000 claims description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 18
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 12
- 239000012535 impurity Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 9
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000011863 silicon-based powder Substances 0.000 claims description 8
- 238000012805 post-processing Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 7
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- KTQYJQFGNYHXMB-UHFFFAOYSA-N dichloro(methyl)silicon Chemical compound C[Si](Cl)Cl KTQYJQFGNYHXMB-UHFFFAOYSA-N 0.000 claims description 6
- 239000008246 gaseous mixture Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000004005 microsphere Substances 0.000 claims description 6
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- 238000004523 catalytic cracking Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000007781 pre-processing Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 2
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 abstract description 18
- 238000010924 continuous production Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 24
- 238000005336 cracking Methods 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 description 2
- 229910008045 Si-Si Inorganic materials 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- 229910006411 Si—Si Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- KQHIGRPLCKIXNJ-UHFFFAOYSA-N chloro-methyl-silylsilane Chemical compound C[SiH]([SiH3])Cl KQHIGRPLCKIXNJ-UHFFFAOYSA-N 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/121—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20
- C07F7/128—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20 by reactions covered by more than one of the groups C07F7/122 - C07F7/127 and of which the starting material is unknown or insufficiently determined
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a kind of techniques of catalytic pyrolysis organosilicon high-boiling product, catalytic pyrolysis is carried out to organosilicon high-boiling product using composite catalyst, convert it in atmospheric conditions the mix products based on dimethyldichlorosilane monomer, technical solution of the present invention, composite catalyst catalytic activity is good, it can recycle, reaction condition is mild, can be realized smoothly continuous production, easily realizes industrialization, high-boiling components high conversion rate is up to 96%, and the selection rate of dimethyldichlorosilane is up to 76%.
Description
Technical field
The present invention relates to organic silicon byproduct technical field of comprehensive utilization, and in particular to organosilicon high-boiling product catalytic pyrolysis turns
The technique for turning to dimethyldichlorosilane.
Background technique
Organosilicon high-boiling product is the by-product in methyl chlorosilane monomer synthesis process, usually contains a small amount of solid content and not
The metallic compounds such as soluble copper, aluminium, zinc contain multiple compounds, concrete composition simultaneously containing a small amount of superfine silicon powder
Closely related with silicon powder, the purity of chloromethanes, the type of catalyst and reaction condition etc. in organic silicon monomer production, difference is raw
The composition of organosilicon high-boiling product and content are all different in the production. art even different batches of same production technology, therefore, closely
Report over year about organosilicon high-boiling product composition is also not quite similar, and thinks that it is mainly organized as Si-Si, Si-O-Si substantially,
Si-CH3Compound.With the rapid development of silicone industry, the yield of methyl chlorosilane monomer is increasing, high-boiling components
Output also increase therewith, be not easy to store because its is inflammable and explosive, processing can bring very big security risk not in time, domestic
Enterprise Integrated is using the approach of high-boiling components mainly include the following types: preparing silicone oil, preparing waterproofing agent of organosilicon, prepare organosilicon
Resin prepares defoaming agent, cracking preparation single silane etc..
In the prior art, the seventies mainly use thermal-cracking method to cracking preparation single silane, and reaction temperature is up to
300-900 DEG C, carbon distribution is serious, and dimethyldichlorosilane selectivity is very low, and therefore, catalytic pyrolysis gradually replaces pyrolysis technology
And it is in leading position.
Dow Corning Corporation by being added a certain amount of trim,ethylchlorosilane and dimethyl dichlorosilane (DMCS) in a kettle, using chlorine
Change aluminium as catalyst, hydrogen chloride is cracked gas, at 325 DEG C, is reacted 3 hours under 4.8-6.9MPa, high-boiling components conversion ratio can
Up to 81.2%, however its high-temperature and high-pressure conditions is very high to reaction equipment requirement, and production cost is higher, and operation is also dangerous, separately
Outside, based on intermittently operated, the ability for handling high-boiling components is limited to for the reaction.
Chinese patent CN1560056A discloses high as catalyst cracking organic silicon using n,N-Dimethylaniline
The method that boiling object prepares methylchlorosilane, controls 90-110 DEG C of reaction temperature, the selectivity of dimethyldichlorosilane reaches 29-
37%, the selectivity of tri-methyl-chlorosilane is very low, less than 2%.The technical solution can only crack in high-boiling components containing Si-Si bond
Methylchlorodisilane, cannot crack containing Si-O-Si, the other components of Si-C-Si, therefore high-boiling components conversion ratio is lower.
For at present, in place of all kinds of Deep Catalytic Cracking process of organosilicon high-boiling product all Shortcomings or catalytic effect is bad,
Or cannot achieve continuous production or reaction process complexity, production cost is higher, and many techniques are only capable of through a series of catalysis
Single product is made in cracking reaction, how reasonably to be comprehensively utilized to the high-boiling components component of these high added values, is organic
Silicon enterprise technical problem in the urgent need to address.
Summary of the invention
Aiming at the problems and shortcomings existing in the prior art, the purpose of the present invention is to provide a kind of catalytic pyrolysis organosilicons
The technique of high-boiling components carries out catalytic pyrolysis to organosilicon high-boiling product using composite catalyst, is translated into dimethyl dichloro silicon
Mix products based on alkane monomer, using technical solution of the present invention, composite catalyst catalytic activity is good, can recycle circulation benefit
With, reaction condition is mild, and smoothly continuous production may be implemented, easily realize industrialization, high-boiling components high conversion rate up to 96%,
The selection rate of dimethyldichlorosilane is up to 76%.
To achieve the above object and technical effect, the technique of catalytic pyrolysis organosilicon high-boiling product of the present invention, including following step
It is rapid:
(1) it is proportionally added into tri-n-octyl amine, triphenylphosphine and polyacrylamide microsphere, in mass ratio 1 in a kettle:
0.1-2.5: 1.5-5.5, it is warming up to 60-120 DEG C of reaction 6-18 hours, obtains composite catalyst；
(2) removal of impurities processing is carried out to organosilicon high-boiling product, removes high boiling silicon powder and metal impurities in advance, obtain pre- place
Manage high-boiling components；
(3) reactor is added in pretreatment high-boiling components, and composite catalyst and inert gas is added, control reaction temperature
90-160 DEG C, it is then passed through decomposition agent into reactor, catalytic cracking reaction occurs under the catalytic condition of composite catalyst, it is raw
At dimethyldichlorosilane, tri-methyl-chlorosilane and monomethyl dichlorosilane three kinds of monomers based on mix products, pass through
Postprocessing working procedures are isolated recycling.
Wherein, the reaction temperature is at 105-130 DEG C.
Wherein, the molar ratio of the pretreatment high-boiling components and decomposition agent is 1: 1-3.5, pre-processes high-boiling components and composite catalyzing
The mass ratio of agent is 1: 0.03-0.45.In preferred scheme, the mass ratio of the pretreatment high-boiling components and composite catalyst is 1
∶0.15-0.3。
Wherein, the decomposition agent is the mixture of hydrogen chloride, chlorine and hydrogen, mole accounting of the hydrogen chloride in gaseous mixture
For 45-80%.
Wherein, the reactor is selected from one of packed tower, fluidized bed, agitated bed.
Wherein, the inert gas is selected from one of nitrogen, argon gas or a variety of.
Technical solution of the present invention can realize continous way catalytic pyrolysis organosilicon high-boiling product, reaction condition in atmospheric conditions
Mildly, industrialization is easily realized, the tail gas of generation may be recovered utilization based on hydrogen chloride, and three-waste pollution is few.
Composite catalyst of the present invention has both the function of catalyst and compatilizer, reduces the trend of side reaction, catalyst is easy
It separates, can be recycled with other substances, effectively reduce pollution of traditional volatile organic solvent to environment.
Compared with traditional two-step method, technical solution of the present invention good catalyst activity, by-product are few, and conversion can be improved
Rate, high-boiling components cracking conversion per pass are up to 96%, and dimethyldichlorosilane selectivity is up to 76%.
Specific embodiment
Below with reference to embodiment, the invention will be further described.Must it should be noted that, protection scope of the present invention is not
It is limited to these specific embodiments, specifically proportion and response parameter and material selection involved in specific embodiment
It is to enumerate in this embodiment to illustrate the invention, is not any limitation of the invention.
The technique of catalytic pyrolysis organosilicon high-boiling product of the present invention, comprising the following steps:
(1) it is proportionally added into tri-n-octyl amine, triphenylphosphine and polyacrylamide microsphere, in mass ratio 1 in a kettle:
0.1-2.5: 1.5-5.5, it is warming up to 60-120 DEG C of reaction 6-18 hours, obtains composite catalyst；
(2) removal of impurities processing is carried out to organosilicon high-boiling product, removes high boiling silicon powder and metal impurities in advance, obtain pre- place
Manage high-boiling components；
(3) reactor is added in pretreatment high-boiling components, and composite catalyst and inert gas is added, control reaction temperature
90-160 DEG C, it is then passed through decomposition agent into reactor, catalytic cracking reaction occurs under the catalytic condition of composite catalyst, it is raw
At dimethyldichlorosilane, tri-methyl-chlorosilane and monomethyl dichlorosilane three kinds of monomers based on mix products, pass through
Postprocessing working procedures are isolated recycling.
In actual production operation, the catalytic activity of reaction temperature in cracking reactor view composite catalyst is strong and weak, can be with
Temperature range is controlled at 90-160 DEG C, in the preferred scheme, reaction temperature is controlled at 105-130 DEG C.Temperature is too low, unfavorable
In composite catalyst and decomposition agent reaction activation, temperature is excessively high, then is unfavorable for the stabilization of catalyst, may cause side reaction and adds
Play is unfavorable for the heat balance of system.In terms of the dosage of reaction mass, mole of the pretreatment high-boiling components and decomposition agent
Than being 1: 1-3.5, the mass ratio for pre-processing high-boiling components and composite catalyst is 1: 0.03-0.45, in the preferred scheme, in advance
The mass ratio for handling high-boiling components and composite catalyst is 1: 0.15-0.3.
Inventor in experiments it is found that, using the mixture of hydrogen chloride, chlorine and hydrogen as decomposition agent, and control chlorination
When mole accounting of the hydrogen in gaseous mixture is 45-80%, the conversion ratio of raw material organosilicon high-boiling product is higher, dimethyl in product
The selectivity of dichlorosilane is higher.
For those skilled in the art, the reactor that catalytic cracking reaction can be occurred for organosilicon high-boiling product can
To be selected from packed tower, fluidized bed or agitated bed, the inert gas is selected from one of nitrogen, argon gas or its mixing.Other are pre-
Processing, postprocessing working procedures are conventional treatment process, such as can be using filter progress, removal of impurities process, rectification working process, recycling point
From process etc., as long as required equipment and device may be implemented its technical purpose and obtain relevant art effect.
Embodiment 1
Processing is filtered to organosilicon high-boiling product, removes solid silicon powder and metal impurities, obtains pretreatment high-boiling components.?
It is proportionally added into tri-n-octyl amine 100g, triphenylphosphine 85g and polyacrylamide microsphere 550g in reaction kettle, reacts 7 at 80 DEG C
Hour, obtain composite catalyst.Select fluidized bed as cracking reactor, by pretreatment high-boiling components 1000g and composite catalyst
150g is added in fluidized bed, and is passed through inert gas argon gas and decomposition agent, mole accounting of the hydrogen chloride in decomposition agent gaseous mixture
It is 45%, decomposition agent and pretreatment high-boiling components dosage molar ratio 1: 1,105 DEG C of reaction temperature, fluidized bed is interior to occur catalytic pyrolysis
Reaction generates the mixing based on three kinds of monomers of dimethyldichlorosilane, tri-methyl-chlorosilane and monomethyl dichlorosilane and produces
Object eventually passes through postprocessing working procedures and is isolated recycling.
It is computed, high-boiling components crack conversion per pass up to 91%, and dimethyldichlorosilane selectivity is up to 69%.
Embodiment 2
Processing is filtered to organosilicon high-boiling product, removes solid silicon powder and metal impurities, obtains pretreatment high-boiling components.?
Tri-n-octyl amine 100g, triphenylphosphine 150g and polyacrylamide microsphere 500g are proportionally added into reaction kettle, it is anti-at 100 DEG C
It answers 12 hours, obtains composite catalyst.It selects fluidized bed as cracking reactor, pretreatment high-boiling components 1000g and compound will urge
Agent 200g is added in fluidized bed, and is passed through inert gas argon gas and decomposition agent, mole of the hydrogen chloride in decomposition agent gaseous mixture
Accounting is 60%, decomposition agent and pretreatment high-boiling components dosage molar ratio 2: 1, and 130 DEG C of reaction temperature, fluidized bed is interior to be catalyzed
Cracking reaction generates mixed based on three kinds of monomers of dimethyldichlorosilane, tri-methyl-chlorosilane and monomethyl dichlorosilane
Product is closed, postprocessing working procedures is eventually passed through and is isolated recycling.
It is computed, high-boiling components cracking conversion per pass is up to 93%, and dimethyldichlorosilane selectivity is up to 71%.
Embodiment 3
Processing is filtered to organosilicon high-boiling product, removes solid silicon powder and metal impurities, obtains pretreatment high-boiling components.?
Tri-n-octyl amine 100g, triphenylphosphine 250g and polyacrylamide microsphere 550g are proportionally added into reaction kettle, it is anti-at 120 DEG C
It answers 16 hours, obtains composite catalyst.It selects fluidized bed as cracking reactor, pretreatment high-boiling components 1000g and compound will urge
Agent 300g is added in fluidized bed, and is passed through inert gas argon gas and decomposition agent, mole of the hydrogen chloride in decomposition agent gaseous mixture
Accounting is 75%, decomposition agent and pretreatment high-boiling components dosage molar ratio 3.5: 1, and 130 DEG C of reaction temperature, fluidized bed is interior to urge
Change cracking reaction, based on three kinds of monomers for generating dimethyldichlorosilane, tri-methyl-chlorosilane and monomethyl dichlorosilane
Mix products eventually pass through postprocessing working procedures and are isolated recycling.
It is computed, high-boiling components cracking conversion per pass is up to 96%, and dimethyldichlorosilane selectivity is up to 76%.
Claims (7)
1. a kind of technique of catalytic pyrolysis organosilicon high-boiling product, which comprises the following steps:
(1) it is proportionally added into tri-n-octyl amine, triphenylphosphine and polyacrylamide microsphere, in mass ratio 1: 0.1- in a kettle
2.5: 1.5-5.5, it is warming up to 60-120 DEG C of reaction 6-18 hours, obtains composite catalyst；
(2) removal of impurities processing is carried out to organosilicon high-boiling product, removes high boiling silicon powder and metal impurities in advance, it is high to obtain pretreatment
Boil object；
(3) reactor is added in pretreatment high-boiling components, and composite catalyst and inert gas is added, control reaction temperature 90-160
DEG C, it is then passed through decomposition agent into reactor, catalytic cracking reaction occurs under the catalytic condition of composite catalyst, generates diformazan
Mix products based on three kinds of monomers of base dichlorosilane, tri-methyl-chlorosilane and monomethyl dichlorosilane, pass through post-processing
Process is isolated recycling.
2. the technique of catalytic pyrolysis organosilicon high-boiling product according to claim 1, which is characterized in that the reaction temperature exists
105-130℃。
3. the technique of catalytic pyrolysis organosilicon high-boiling product according to claim 2, which is characterized in that the pretreatment high-boiling components
Molar ratio with decomposition agent is 1: 1-3.5, and the mass ratio for pre-processing high-boiling components and composite catalyst is 1: 0.03-0.45.
4. the technique of catalytic pyrolysis organosilicon high-boiling product according to claim 3, which is characterized in that the pretreatment high-boiling components
Mass ratio with composite catalyst is 1: 0.15-0.3.
5. the technique of catalytic pyrolysis organosilicon high-boiling product according to claim 3, which is characterized in that the decomposition agent is chlorination
The mixture of hydrogen, chlorine and hydrogen, mole accounting of the hydrogen chloride in gaseous mixture are 45-80%.
6. the technique of catalytic pyrolysis organosilicon high-boiling product according to claim 2, which is characterized in that the reactor is selected from and fills out
Expect one of tower, fluidized bed, agitated bed.
7. the technique of catalytic pyrolysis organosilicon high-boiling product according to claim 2, which is characterized in that the inert gas is selected from
One of nitrogen, argon gas are a variety of.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111348652A (en) * | 2020-04-29 | 2020-06-30 | 中国恩菲工程技术有限公司 | Chlorosilane high-boiling-point substance catalytic cracking reactor and polycrystalline silicon device |
| CN114573629A (en) * | 2020-11-30 | 2022-06-03 | 新疆硅基新材料创新中心有限公司 | Organic silicon monomer preparation method and system and polycrystalline silicon system |
-
2019
- 2019-03-14 CN CN201910215202.0A patent/CN110183481A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111348652A (en) * | 2020-04-29 | 2020-06-30 | 中国恩菲工程技术有限公司 | Chlorosilane high-boiling-point substance catalytic cracking reactor and polycrystalline silicon device |
| CN114573629A (en) * | 2020-11-30 | 2022-06-03 | 新疆硅基新材料创新中心有限公司 | Organic silicon monomer preparation method and system and polycrystalline silicon system |
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