CN104558003B - A kind of method that liquid phase chlorination reaction prepares Chloromethyltrichlorosilane - Google Patents
A kind of method that liquid phase chlorination reaction prepares Chloromethyltrichlorosilane Download PDFInfo
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- CN104558003B CN104558003B CN201510040387.8A CN201510040387A CN104558003B CN 104558003 B CN104558003 B CN 104558003B CN 201510040387 A CN201510040387 A CN 201510040387A CN 104558003 B CN104558003 B CN 104558003B
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- chlorine
- methyl trichlorosilane
- chloromethyltrichlorosilane
- chlorination reaction
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- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 29
- FYTPGBJPTDQJCG-UHFFFAOYSA-N Trichloro(chloromethyl)silane Chemical compound ClC[Si](Cl)(Cl)Cl FYTPGBJPTDQJCG-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000007791 liquid phase Substances 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 title claims abstract description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000460 chlorine Substances 0.000 claims abstract description 41
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 41
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000005055 methyl trichlorosilane Substances 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000019400 benzoyl peroxide Nutrition 0.000 claims abstract description 10
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000004342 Benzoyl peroxide Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000009835 boiling Methods 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 13
- 239000012043 crude product Substances 0.000 claims description 12
- 238000004821 distillation Methods 0.000 claims description 7
- 238000002309 gasification Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000005485 electric heating Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 125000004218 chloromethyl group Chemical group [H]C([H])(Cl)* 0.000 abstract description 3
- 238000005286 illumination Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- 239000003507 refrigerant Substances 0.000 description 4
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 4
- 239000005052 trichlorosilane Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- KSRPSVLVRQICHA-UHFFFAOYSA-N C[Si](Cl)(Cl)Cl.[Cl] Chemical compound C[Si](Cl)(Cl)Cl.[Cl] KSRPSVLVRQICHA-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 125000001309 chloro group Chemical group Cl* 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 150000004756 silanes Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 229910006024 SO2Cl2 Inorganic materials 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229920002631 room-temperature vulcanizate silicone Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 125000003866 trichloromethyl group Chemical group ClC(Cl)(Cl)* 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Abstract
The present invention relates to a kind of method that liquid phase chlorination reaction prepares Chloromethyltrichlorosilane, belong to technical field of organic chemistry.The present invention is used as catalyst using benzoyl peroxide and iron chloride mixture, using methyl trichlorosilane as raw material, uniformly chlorine is passed through to it, pass through the logical chlorine dose of control, so that the conversion ratio of methyl trichlorosilane is up to 70 80%, the selectivity of chloromethyl trichlorine is significantly improved, and reaches 95%, the total content of many Chloromethyltrichlorosilanes<5%.The present invention can be smoothed out under conditions of lower temperature, no light, or illumination are insufficient, and equipment requirement is simple, reduces the input of reaction unit, makes its industrialized production more cost advantage.
Description
Technical field
The present invention relates to a kind of method that liquid phase chlorination reaction prepares Chloromethyltrichlorosilane, category technique of organic chemistry neck
Domain.
Background technology
Chloromethyltrichlorosilane is the important source material for preparing α functional silanes coupling agents, and it is with alcohol reagent such as methanol, second
Many useful organosilicon products can be generated after the reaction such as alcohol, glycol monoethyl ether.Relative to traditional γ functional silanes,
The Si atoms of Chloromethyltrichlorosilane are only separated by a carbon atom with its functional group, and chemical property is more active, hydrolysis rate and contracting
Faster, chemical reaction or coupling reaction easily occur for poly- speed；In addition, γ-functional group's coupling agent Si atoms are separated by with functional group
Three carbon atoms, the carbon-carbon bond of these three carbon atoms is easily broken off at high temperature, and the heat endurance of α functional groups is then preferable, because
This can be used as a kind of excellent RTV silicone rubber crosslinking agent.
GE companies of U.S. Krieble R H and Elliott J R are in reaction temperature using 4w bactericidal lamps as light source within 1945
Under the conditions of 20-40 DEG C, to (CH3)3C1 is passed through in SiCl2Chlorination is carried out, reaction forms Me2(C1CH2) SiCl, Me2
(C12CH) SiCI and Me (C1CH2)2SiCl。
Russia scholar ponomarenko V A and Mironov V F in 1954 are under ultraviolet light, to MeSiCl3
In be passed through chlorine, the reaction time is 22 h, and reactant flow back in system, available 53% C1CH2SiCl3In the meantime, it is beautiful
State, German, the scholar of the country such as Russia, as initiator, is passed through chlorine with different light in the case of different temperatures,
All obtain chloro hydrocarbyl si lanes.
Nineteen fifty-two, U.S. Tamborski C and Post H W were in O-C6H4Cl dicyandiamide solutions, passed through SO2Cl2 or chlorine
As chlorinating agent, 78 degree of back flow reactions, obtain 2.6% ClCH2SiCl3.This is the synthesis first of Chloromethyltrichlorosilane.
Germany Runge F and Zirneremann W in 1954 uses mercury lamp as light source, at 20 DEG C of reaction temperature, to
Chlorine is passed through in MeSiCl and CHCl3 mixed systems, the HCl of generation is absorbed in -40 DEG C of water, 95% trichloromethyl is obtained
Trichlorosilane.
1956, Chinese Academy of Sciences's chemistry have studied CH3SiCl3Liquid-phase vaporization reaction.It uses low temperature when have compared with
The azodiisobutyronitrile of big capacity of decomposition is catalyst as radical initiator, yttrium chloride, lanthanum chloride etc., makes CH3SiCl3
With ClSO under boiling point2Generation substitution reaction, so as to prepare Chloromethyltrichlorosilane.The reaction uses a large amount of expensive initiations
Agent and catalyst, are unfavorable for industrialized production.
Voronkov MG in 2001 et al. have studied thermal chlorination and prepare Chloromethyltrichlorosilane.In the anti-of 300-400 degree
At a temperature of answering, using chlorinated with chlorine methyl trichlorosilane, reaction is carried out by free radical mechanism, and yield is in 63-82%.
In summary, the more difficult control of chloride solution, and many chloro accessory substances are more；Thermal chlorination, reaction temperature mistake
Height, explosive is dangerous big, it is more difficult to industrialize, cost is higher.
It is an object of the invention to：Chlorination reaction can be smoothed out under non-illuminated conditions by providing one kind, and equipment will
Ask simple, reduce the input of reaction unit, the liquid phase chlorination reaction that industrialized production has more cost advantage is prepared chloromethyl
The method of trichlorosilane.
The technical scheme is that：
A kind of method that liquid phase chlorination reaction prepares Chloromethyltrichlorosilane, it is characterised in that：It comprises the following steps：
1）, with tail gas collecting device, thermometer, reflux condensing tube, electric heating cover, cl gas flow gauge, and equipped with hiding
Methyl trichlorosilane is firstly added in the reaction vessel of light shield, catalyst is then added and opens condenser pipe, then be to slowly warm up to
40-50 DEG C, so that methyl trichlorosilane reaches that boiling point gasifies；
2）, when methyl trichlorosilane reach boiling point gasification after and condenser pipe effect under produce backflow when, pass through cl gas flow
Gauge is passed through chlorine, and to carry out chlorination reaction, the intake velocity of chlorine is 0.15-0.35L/min；The temperature of chlorination reaction is
55—65℃；
3）, with the progress of reaction, the capacity of returns of methyl trichlorosilane is gradually reduced, now slow lifting kettle temperature to 70-
80℃；After chlorine, which is passed through the time, reaches 1-2.5h, you can stop logical chlorine, cooling obtains Chloromethyltrichlorosilane crude product；
4）, crude product is transferred to distilling apparatus air-distillation；What temperature was less than 117 DEG C of fractions be before evaporate, put into next pot again
Carry out chlorination reaction；117-119 DEG C of fraction is product Chloromethyltrichlorosilane finished product.
Described catalyst is the weight of the mixture of iron chloride and benzoyl peroxide, iron chloride and benzoyl peroxide
Than for 2 ︰ 1.
Described methyl trichlorosilane and the mol ratio of chlorine are 1:0.6-0.9.
Advantages of the present invention：
The present invention is using benzoyl peroxide and iron chloride mixture as catalyst, using methyl trichlorosilane as raw material, to
It is uniformly passed through chlorine, passes through the logical chlorine dose of control so that the conversion ratio of methyl trichlorosilane up to 70-80%, chloromethyl trichlorine
Selectivity is significantly improved, and reaches 95%, the total content of many Chloromethyltrichlorosilanes<5%.The present invention can in lower temperature, no light,
Or illumination it is insufficient under conditions of be smoothed out, and equipment requirement is simple, reduces the input of reaction unit, makes its industrial metaplasia
Production has more cost advantage.
Embodiment
Embodiment 1
With exhaust collection bottle, thermometer, reflux condensing tube（Using ethylene glycol-frozen water refrigerant）, electric heating cover,
Methyl trichlorosilane 300g is firstly added in cl gas flow gauge, and the 1000ml four-hole boiling flasks equipped with light shield, 2g is then added
Iron chloride and 1g benzoyl peroxides simultaneously open condenser pipe, then are to slowly warm up to 40-50 DEG C, so that methyl trichlorosilane reaches
Boiling point gasifies.When methyl trichlorosilane is reached after boiling point gasification and produces backflow under condenser pipe effect, pass through chlorine flowrate
Meter is passed through chlorine, and to carry out chlorination reaction, the intake velocity of chlorine is 0.15L/min；Mole of methyl trichlorosilane and chlorine
Than for 1:0.6-0.9；The temperature of chlorination reaction is 55 DEG C.
With the progress of reaction, the capacity of returns of methyl trichlorosilane is gradually reduced, and now slow lifting kettle temperature is to 70 DEG C；When
Chlorine is passed through the time and reached after 1h, you can stop logical chlorine, and cooling obtains Chloromethyltrichlorosilane crude product.Crude product is transferred to distillation dress
Put air-distillation；What temperature was less than 117 DEG C of fractions be before evaporate, put into next pot and carry out chlorination reaction again；117-119 DEG C of fraction be
Product Chloromethyltrichlorosilane finished product.Detected through GC, purity is more than 99%, and yield is 80%.It is many chloro first that temperature, which is more than 119 DEG C,
Base trichlorosilane.
Embodiment 2
With exhaust collection bottle, thermometer, reflux condensing tube（Using ethylene glycol-frozen water refrigerant）, electric heating cover,
Methyl trichlorosilane 300g is firstly added in cl gas flow gauge, and the 1000ml four-hole boiling flasks equipped with light shield, 2g is then added
Iron chloride and 1g benzoyl peroxides simultaneously open condenser pipe, then are to slowly warm up to 40-50 DEG C, so that methyl trichlorosilane reaches
Boiling point gasifies.When methyl trichlorosilane is reached after boiling point gasification and produces backflow under condenser pipe effect, pass through chlorine flowrate
Meter is passed through chlorine, and to carry out chlorination reaction, the intake velocity of chlorine is 0.25L/min；Mole of methyl trichlorosilane and chlorine
Than for 1:0.6-0.9；The temperature of chlorination reaction is 60 DEG C.With the progress of reaction, the capacity of returns of methyl trichlorosilane gradually subtracts
Small, now slow lifting kettle temperature is to 75 DEG C；After chlorine, which is passed through the time, reaches 1.5h, you can stop logical chlorine, cooling obtains chloromethyl
Trichlorosilane crude product.Crude product is transferred to distilling apparatus air-distillation；What temperature was less than 117 DEG C of fractions be before evaporate, put into next pot
Chlorination reaction is carried out again；117-119 DEG C of fraction is product Chloromethyltrichlorosilane finished product；Detect, purity is more than 99%, receive through GC
Rate is 80%.It is many chloromethyl trichlorosilanes that temperature, which is more than 119 DEG C,.
Embodiment 3
With exhaust collection bottle, thermometer, reflux condensing tube（Using ethylene glycol-frozen water refrigerant）, electrical heating
Methyl trichlorosilane 300g is firstly added in set, cl gas flow gauge, and the 1000ml four-hole boiling flasks equipped with light shield, is then added
2g iron chloride and 1g benzoyl peroxides simultaneously open condenser pipe, then are to slowly warm up to 40-50 DEG C, so that methyl trichlorosilane reaches
To boiling point gasification.When methyl trichlorosilane is reached after boiling point gasification and produces backflow under condenser pipe effect, pass through cl gas flow
Gauge is passed through chlorine, and to carry out chlorination reaction, the intake velocity of chlorine is 0.30L/min；Methyl trichlorosilane and chlorine rub
You are than being 1:0.6-0.9；The temperature of chlorination reaction is 65 DEG C.With the progress of reaction, the capacity of returns of methyl trichlorosilane is gradually
Reduce, now slow lifting kettle temperature is to 80 DEG C；After chlorine, which is passed through the time, reaches 2.5h, you can stop logical chlorine, cooling obtains chloromethane
Base trichlorosilane crude product.Crude product is transferred to distilling apparatus air-distillation；What temperature was less than 117 DEG C of fractions be before evaporate, put into next
Pot carries out chlorination reaction again；117-119 DEG C of fraction is product Chloromethyltrichlorosilane finished product；Detected through GC, purity is more than 99%,
Yield is 75%.It is many chloromethyl trichlorosilanes that temperature, which is more than 119 DEG C,
Embodiment 4
With exhaust collection bottle, thermometer, reflux condensing tube（Using ethylene glycol-frozen water refrigerant）, electric heating cover,
Methyl trichlorosilane 300g is firstly added in cl gas flow gauge, and the 1000ml four-hole boiling flasks equipped with light shield, then adds and adds
Enter 2g iron chloride and 1g benzoyl peroxides and open condenser pipe, then be to slowly warm up to 40-50 DEG C, so that methyl trichlorosilane
Reach that boiling point gasifies.When methyl trichlorosilane is reached after boiling point gasification and produces backflow under condenser pipe effect, pass through chlorine
Flowmeter is passed through chlorine, and to carry out chlorination reaction, the intake velocity of chlorine is 0.35L/min；Methyl trichlorosilane and chlorine
Mol ratio is 1:0.6-0.9；The temperature of chlorination reaction is 65 DEG C.With the progress of reaction, the capacity of returns of methyl trichlorosilane by
Decrescence small, now slow lifting kettle temperature is to 80 DEG C；After chlorine, which is passed through the time, reaches 2.5h, you can stop logical chlorine, cooling obtains chlorine
Methyl trichlorosilane crude product.Crude product is transferred to distilling apparatus air-distillation；What temperature was less than 117 DEG C of fractions be before evaporate, under input
One pot carries out chlorination reaction again；117-119 DEG C of fraction is product Chloromethyltrichlorosilane finished product；Detected through GC, purity is more than
99%, yield is 68%.It is many chloromethyl trichlorosilanes that temperature, which is more than 119 DEG C,.
Claims (1)
1. a kind of method that liquid phase chlorination reaction prepares Chloromethyltrichlorosilane, it is characterised in that：It comprises the following steps：
1）, with tail gas collecting device, thermometer, reflux condensing tube, electric heating cover, cl gas flow gauge, and equipped with light shield
Reaction vessel in be firstly added methyl trichlorosilane, then add catalyst and open condenser pipe, then be to slowly warm up to 40-
50 DEG C, so that methyl trichlorosilane reaches that boiling point gasifies；Catalyst is the mixture of iron chloride and benzoyl peroxide, iron chloride
Weight ratio with benzoyl peroxide is 2 ︰ 1；
2）, when methyl trichlorosilane reach boiling point gasification after and condenser pipe effect under produce backflow when, pass through cl gas flow gauge
Chlorine is passed through, to carry out chlorination reaction, the intake velocity of chlorine is 0.15-0.35L/min；The temperature of chlorination reaction be 55-
65℃；The mol ratio of methyl trichlorosilane and chlorine is 1:0.6-0.9；
3）, with the progress of reaction, the capacity of returns of methyl trichlorosilane is gradually reduced, and now slow lifting kettle temperature is to 70-80
℃；After chlorine, which is passed through the time, reaches 1-2.5h, you can stop logical chlorine, cooling obtains Chloromethyltrichlorosilane crude product；
4）, crude product is transferred to distilling apparatus air-distillation；What temperature was less than 117 DEG C of fractions be before evaporate, put into next pot and carry out again
Chlorination reaction；117-119 DEG C of fraction is product Chloromethyltrichlorosilane finished product.
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| CN106957330B (en) * | 2016-01-08 | 2019-01-22 | 溧阳市智行新材料有限公司 | A kind of method that chlorination rectification process prepares chloromethyl trichlorosilane |
| CN118852233A (en) * | 2024-07-03 | 2024-10-29 | 浙江硕而博化工有限公司 | Dimethylvinyl chlorosilane and preparation method thereof |
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|---|---|---|---|---|
| SU154543A1 (en) * | ||||
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2015
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| PL155571B1 (en) * | 1988-05-09 | 1991-12-31 | Politechnika Gdanska | A method of selective chlorination of methylchlorosilanes |
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| Title |
|---|
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