CN105061767B - A kind of hydrolysis process and its equipment of dimethyldichlorosilane - Google Patents
A kind of hydrolysis process and its equipment of dimethyldichlorosilane Download PDFInfo
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Abstract
The invention discloses a kind of Processes and apparatus of dimethyldichlorosilane hydrolysis.Present invention process has 5 steps：1st step is that the hydrochloric acid that the hydrochloric acid, dimethyldichlorosilane and the 2nd one-step hydrolysis of 35%-60% generates is hydrolyzed by scheduled mass ratio at 10-60 DEG C of temperature, 0-0.35MPa.2nd step is that the hydrolysate that the 1st step obtains is hydrolyzed with the dilute hydrochloric acid from the 3rd step in static mixer again, and reaction temperature is less than 35 DEG C, and reaction pressure is normal pressure.3rd step is that hydrolysate is extracted in static mixer with process water and reacted.4th step be hydrolysate with lye in static mixer mixing neutralization reaction.5th step is hydrolysate deactivation carbon filter purified treatment.The present invention obtains hydrolysate chloride ion content and is less than 10ppm, and loop wire is than being about 1.5-0.6, and hydrogen chloride gas impurity content is less than 10ppm, and hydrolysate viscosity is less than 50mm2/s。
Description
Technical field
The invention belongs to organic silicon monomer production technical fields, and in particular to dimethyldichlorosilane hydrolysis process and set
It is standby.
Background technology
Organosilicon material is a kind of new material that recent decades just grow up, and is commonly called as " industrial monosodium glutamate ", mainly divides silicon
Rubber, silicone oil, silane coupling agent, silicones four are main kind of, are widely used in the industries such as space flight, pharmaceutical engineering, machine-building.It is raw
The raw material of production organosilicon material is most commonly that the polysiloxanes that dimethyldichlorosilane hydrolysis, cracking obtain.
Most common dimethyldichlorosilane hydrolysis process is a large amount of water hydrolysis and azeotropic acid hydrolysis, generates the silicon containing terminal hydroxy group
Oxygen alkane wire body and siloxanes ring body, and the hydrochloric acid solution of by-product 30% or so.In hydrolytic process, the hydrogen chloride of generation is dissolved in water
A large amount of heat is released, needs in time to remove heat, consumes a large amount of cold.30% or so the hydrochloric acid generated removes synthesis chloromethanes
It must first desorb and release hydrogen chloride gas, consume a large amount of heat again in this way.Not only equipment investment is big for both techniques, and disappears
The a large amount of energy is consumed, operating cost is higher, and economic benefit is low.
As methylchlorosilane yield and product variety increase, the progress of separating and purifying technology and the improvement of polymerization technique,
Cyclic annular and linear polysiloxanes exploitations and application have pushed dimethyldichlorosilane hydrolysis process from azeotropic acid hydrolysis to saturation
Acid-hydrolyzed development.Foreign countries develop since the 1980s and apply being saturated acid hydrolysis process patent, domestic each organosilicon
Manufacturer also continually develops and has applied respective hydrolysis patented technology in last decade.
French Patent (FRP) 2,512,028 reports the method for hydrolysis of organic chloride silane, especially dimethyldichlorosilane, has
Machine halogenated silane hydrolyzes in the hydrochloric acid solution more than 35%, and the molar ratio of water and organochlorosilane is one between 10 and 30
One-step hydrolysis.The technique cannot get hydrogen chloride gas.French Patent (FRP) 2,518,099 carries out dimethyl dichloro using the water of accurate measurement
One one-step hydrolysis of silane, to obtain anhydrous hydrogen chloride and polysiloxane hydrolyzates.United States Patent (USP) US5075479 is using saturation hydrochloric acid
Solution, cycle, which hydrolyzes, generates hydrogen chloride gas, 24-100 DEG C of reaction temperature, pressure 0.1-1.0MPa, water and dimethyl two in acid
The ratio of chlorosilane is 5-50：1.United States Patent (USP) US5169970 reports methylchlorosilane two step hydrolysis method, first step useization
The water for learning metering hydrolyzes organochlorosilane, and second step passes through same treatment by the hydrolysate that step 1 obtains, but second step makes
Source with metering water is the hydrogen chloride solution for subscribing concentration, and this method generates low pressure hydrogen chloride gas, it is difficult to recycling and increment.
Patent No. CN101148510A discloses a kind of multi-stage continuously hydrolyzing of organodichlorosilane and prepares poly organo
The method of alkane and gas phase hydrogen chloride.It is to recycle hydrolysising reacting system at least three-level, every grade of hydrolysising reacting system includes interior follow again
Ring element and outer circulation unit obtain the few silicone products of chloride ion-containing and hydrogen chloride gas with pressure.The invention flow is multiple
It is miscellaneous.Patent No. CN101323666A discloses a kind of method of methylchlorosilane concentrated acid hydrolysis production hydrolysate, and this method uses
Two-stage phase separator carries out acid oil separation, isolated acidic hydrolysis object devaporation tower boiling, steam consumption and methyl chloride silicon
Alkane addition molar ratio is 0.12-0.18:1, the hydrolysate after boiling obtains qualified hydrolysate using two-stage phase separator
Product.Patent No. CN101875726A discloses a kind of method of preparing polysiloxane by hydrolyzing dimethyl dichlorosilane, and two
A continuous hydrolysis step and a neutralization procedure, hydrogen chloride purifying and alkali neutralization have been all made of resin cation filter device.Specially
Profit CN101619072A discloses a kind of technique of saturation hydrolyzing dimethyl dichlorosilane by using concentrated hydrochloric acid loop, is urged in phase transfer
It is carried out under the conditions of agent is existing, the molar ratio of the water and dimethyldichlorosilane that are saturated contained by concentrated hydrochloric acid is 200-1000：1,
Reaction is hydrolyzed in gained mixture in packed tower, is then produced hydrogen chloride gas by falling film separator.
Invention content
The present invention be directed to the problem on existing technology for hydrolyzing, a whole set of hydrolysis process route that optimizes.
Technical solution of the present invention：
A kind of hydrolysis process of dimethyldichlorosilane, includes the following steps,
1）Hydrochloric acid, dimethyldichlorosilane and two level the hydrolysis hydrochloric acid of 35%-60% is placed in mixer, after mixing
It is 10-60 DEG C in temperature, reaction is hydrolyzed under 0-0.35MPa, hydrolyzes 10-60s, obtains hydrolysate I；
2）Hydrolysate I and three-level hydrolysis hydrochloric acid are placed in static mixer one, in excessive water, (step is reacted
Without in addition adding water, the water for hydrolyzing needs is provided by the water in three-level hydrolysis hydrochloric acid, and the water in three-level hydrolysis hydrochloric acid is excessive
) after carry out excessive water hydrolysis in the case where temperature is 10-35 DEG C and normal pressure, obtain hydrolysate II after hydrolyzing 10-60s；
3）Hydrolysate II and process water are placed in static mixer two, is extracted at being 60-100 DEG C in temperature, goes phase
Separator is layered to obtain extract III；
4）It is 1 by weight by the sodium carbonate liquor of extract III and 5%-25%：2-5 is placed in static mixer three,
Temperature is to carry out neutralization reaction at 60-100 DEG C, obtains neutralization reaction product IV；
5）Chloride ion content, which is obtained, by neutralization reaction product IV in active carbon filter, after removing impurity is less than 10ppm,
Loop wire is than being about 1.5-0.6, and viscosity is less than 50mm2The hydrolysate of/s, the hydrolysate be siloxanes ring body and wire body mixture,
In, the content of siloxanes ring body ring body accounts for the 30-50% of total weight of the mixture.
The step 1）In, the weight ratio of concentration of hydrochloric acid 40%-50%, hydrochloric acid and dimethyldichlorosilane are 30-
100:1, the weight ratio of dimethyldichlorosilane and two level hydrolysis hydrochloric acid is 1-10:1, wherein it is step 2 that two level, which hydrolyzes hydrochloric acid,）
In further hydrolyze after the hydrochloric acid that generates, the mass concentration control which hydrolyzes hydrochloric acid is 20%-35%.Hydrochloric acid and dimethyl two
Chlorosilane reaction with pressure in mixer and the pipeline being connect with mixer generates hydrogen chloride gas, reaction pressure in reaction process
Power, that is, hydrogen chloride gas pressure is 0.1-0.35MPa, 10-50 DEG C of reaction temperature.
The step 2）In, hydrolysate I and the weight ratio of three-level hydrolysis hydrochloric acid are 1:1-15, wherein three-level hydrolyzes
Hydrochloric acid is step 3）In further hydrolyze after the hydrochloric acid that generates, the mass concentration control which hydrolyzes hydrochloric acid is 0.1%-22%.
Step 5）In, activated carbon is provided in active carbon filter, wherein the specific surface area of activated carbon is 900-1500
㎡/g。
The present invention also provides a kind of hydrolysis devices of dimethyldichlorosilane, specifically include as follows：
The conveying pipeline of dimethyldichlorosilane is connect with mixer one, and mixer one is connect with heat exchanger, heat exchanger and gas
Liquid/gas separator connects, and gas-liquid separator is connect with phase separator one；
Phase separator one is connect with static mixer one, and static mixer one is connect with phase separator two；
Phase separator two is connect with static mixer two, and static mixer two is connect with phase separator three；
Phase separator three is connect with static mixer three, and static mixer three is connect with phase separator four；
Phase separator four is connect with active carbon filter, and active carbon filter is connect with hydrolysate conveying pipeline.
Gas-liquid separator is connect through conveying pipeline with condenser one, and condenser one is connect with condenser two, condenser two with remove
Day with fog connects, and demister is connect with hydrogen chloride gas conveying pipeline.
Phase separator one is also connect with mixer one；Phase separator two is also connect with static mixer one through conveying pipeline, tool
Body is that phase separator two is connected through conveying pipeline and phase separator one to the conveying pipeline between static mixer one；On phase separator also
It is provided with conveying pipeline, process water feed pipe is provided on the conveying pipeline, which divides two-way, connects all the way with static mixer one
It connects, is connect all the way with static mixer two.
It is additionally provided with conveying pipeline on static mixer one, the conveying pipeline and phase separator one to the conveying between mixer one
Pipe connects.
The advantages of the content of present invention：
The present invention has carried out tuning to a whole set of hydrolysis process, in hydrolytic process, is added without any additive, number of devices
It is few and simple in structure, it is easy to operate, reduce loss of the hydrolysate in each technical process, hydrolysate high income, hydrolysate silicon
Oxygen alkane ring body and the total recovery of wire body mixture are 98%-99.5%, and siloxanes ring body content reaches 30-50%.
Qualified products are obtained by being simply layered.Product chlorinated gas pressure is stablized, and impurity is few, to subsequent technique control
It makes highly beneficial.Externally discharged waste water amount is less, and environmental protection pressure is small.Small investment, low energy consumption, and economic benefit is very notable.
Description of the drawings
Fig. 1 is the process equipment figure of the present invention.
Specific implementation mode
It is the non-limiting examples of the present invention below：
Embodiment 1
5 steps of process program point are completed, and the 1st step is that the hydrochloric acid, dimethyldichlorosilane and the 2nd one-step hydrolysis of 35%-60% generates
Hydrochloric acid be hydrolyzed at 10-60 DEG C of temperature, 0-0.35MPa by certain mass ratio.2nd step is the hydrolysis that the 1st step obtains
Object is hydrolyzed with dilute hydrochloric acid in static mixer again, and reaction temperature is less than 35 DEG C, and reaction pressure is normal pressure.3rd step is hydrolysis
Object, which is extracted with process water in static mixer, to react.4th step be hydrolysate with lye in static mixer mixing neutralization reaction.
5th step is that hydrolysate deactivation carbon filter purified treatment obtains qualified products.
In above-mentioned technique, the 1st step reacts concentration of hydrochloric acid prior to 40%-50%, the weight of hydrochloric acid and dimethyldichlorosilane
Compare 30-100：1, the weight ratio of dimethyldichlorosilane and two level hydrolysis hydrochloric acid is 1-10：1.Three strands of materials is abundant through mixer
Hybrid reaction supplements certain 10-50 DEG C of heat maintaining reaction temperature using heater, and the acid of generation, oil, gas mixture are in gas
Liquid/gas separator is into separation.Obtained hydrogen chloride gas pressure 0.1-0.35MPa, hydrogen chloride gas pass through first-stage condenser and two level
Condensing gas removes most of siloxanes and water, then hydrogen chloride gas of the impurity content less than 10ppm is obtained after demister.Chlorination
Hydrogen is adjusted by pressure is sent into chloromethanes synthesis battery limit (BL).The sour oil mixture obtained through gas-liquid separator is naturally heavy in phase separator
Drop separation, acidic hydrolysis object go to participate in reaction in next step, and the hydrochloric acid continuation of 40%-50% recycles in systems.
In above-mentioned technique, the 2nd step looped cycle reaction process, hydrolysate is the diluted acid and ring of 0.1%-22% with mass concentration
Cycle acid solution in the system of road, which is sufficiently mixed in static mixture under normal pressure, reacts, and reaction temperature is less than 35 DEG C, and what is obtained is anti-
It answers mixture that phase separator is gone to detach, obtains supplement water of the hydrochloric acid of 20%-35% as the 1st one-step hydrolysis, obtained acidic hydrolysis
Object goes the 3rd step to extract.
In above-mentioned technique, the extraction reaction of the 3rd step, soft water and the acidic hydrolysis object from the 2nd step phase separator are mixed in static state
It is sufficiently mixed in clutch, temperature is controlled at 60-100 DEG C, then goes the mass concentration that phase separator natural subsidence is layered to be
The diluted acid of 0.1%-22% is used for the supplement water of the 2nd step reaction, and hydrolysate goes the 4th step neutralization reaction.
In above-mentioned technique, the sodium carbonate liquor of hydrolysate and the 5%-25% configured from extraction phase separator is with weight
Compare 2-5：1, reaction is sufficiently mixed in static mixer, then 60-100 DEG C of reaction temperature is passed through phase separator and detached, lye follows
Ring utilizes.Obtained hydrolysate deactivation carbon filter purification, the water of lower layer are sent into extracting system.Hydrolysate chloride ion content is small
In 10ppm, loop wire is than being about 1.5-0.6, and viscosity is less than 50mm2/s.
Embodiment 2
The dimethyldichlorosilane concentrated hydrochloric acid with 40% and 30% mixed in hydrochloric acid from the 2nd step reaction system after metering
Reaction, the quality of concentrated hydrochloric acid and the mass ratio of dimethyldichlorosilane are 40：1, dimethyl base dichlorosilane and 30% hydrochloric acid
Mass ratio is 5：1,40 DEG C of maintaining reaction temperature.Acid, oil, gas three-phase mixture are detached by gas-liquid separator and phase separator,
Obtained hydrogen chloride gas adjusts dechlorination methane synthesis device after condensed in two stages, demisting, by pressure, and hydrogen chloride impurity contains
Measure 10ppm.Obtained acidic hydrolysis object goes in the 2nd step reaction system to be reacted, and the dilute hydrochloric acid of supplement concentration 5% is hydrolyzed,
30 DEG C of reaction temperature is detached in reaction mixture in phase separator, and bottom obtains 30% hydrochloric acid, and the acidic hydrolysis object at top is gone
Then extracting system, 85 DEG C of reaction temperature go the diluted acid that the mass concentration that phase separator natural subsidence is layered is 5% to be used for
The supplement water of 2nd step reaction, hydrolysate go the 4th step neutralization reaction.Neutralize the sodium carbonate liquor using 15%, hydrolysate and carbonic acid
Sodium solution weight ratio is 3：1,85 DEG C of reaction temperature.Then pass through phase separator to detach, lye recycles, hydrolysate deactivation
Carbon filter obtains hydrolysate chloride ion content and is less than 7ppm, and loop wire is than about 1.1, viscosity 45mm2/s。
Embodiment 3
The conveying pipeline of a kind of hydrolysis device of dimethyldichlorosilane, dimethyldichlorosilane is connect with mixer one, is mixed
Clutch one is connect with heat exchanger, and heat exchanger is connect with gas-liquid separator, and gas-liquid separator is connect with phase separator one；
Phase separator one is connect with static mixer one, and static mixer one is connect with phase separator two；
Phase separator two is connect with static mixer two, and static mixer two is connect with phase separator three；
Phase separator three is connect with static mixer three, and static mixer three is connect with phase separator four；
Phase separator four is connect with active carbon filter, and active carbon filter is connect with hydrolysate conveying pipeline.
The gas-liquid separator is connect through conveying pipeline with condenser one, and condenser one is connect with condenser two, condenser
Two connect with demister, and demister is connect with hydrogen chloride gas conveying pipeline.
The phase separator one is also connect with mixer one；Phase separator two also connects with static mixer one through conveying pipeline
It connects, specifically phase separator two is connected through conveying pipeline and phase separator one to the conveying pipeline between static mixer one；Phase separation
Be additionally provided with conveying pipeline on device, process water feed pipe be provided on the conveying pipeline, which divides two-way, all the way with static mixing
Device one connects, and is connect all the way with static mixer two.
It is additionally provided with conveying pipeline on the static mixer one, the conveying pipeline and phase separator one are between mixer one
Conveying pipeline connection.
Claims (6)
1. a kind of hydrolysis process of dimethyldichlorosilane, which is characterized in that include the following steps,
(1) hydrochloric acid, dimethyldichlorosilane and two level hydrolysis hydrochloric acid are placed in mixer, are hydrolyzed after mixing anti-
It answers, hydrolyzes 10-60s, obtain hydrolysate I, the hydrochloric acid and dimethyldichlorosilane are connect in mixer and with mixer
Pipeline in reaction with pressure, hydrogen chloride gas is generated in reaction process, reaction pressure, that is, hydrogen chloride gas pressure is 0.1-
0.35MPa, 10-50 DEG C of reaction temperature；
(2) hydrolysate I and three-level hydrolysis hydrochloric acid are placed in static mixer one, in excessive water, temperature is 10-35 DEG C
And excessive water hydrolysis is carried out under normal pressure, obtain hydrolysate II after hydrolyzing 10-60s；
(3) hydrolysate II and process water are placed in static mixer two, are extracted at being 60-100 DEG C in temperature, goes to be separated
Device is layered to obtain extract III；
(4) it is 1 by weight by the sodium carbonate liquor of extract III and 5%-25%：2-5 is placed in static mixer three, in temperature
Degree is to carry out neutralization reaction at 60-100 DEG C, obtains neutralization reaction product IV；
(5) by neutralization reaction product IV in active carbon filter, chloride ion content is obtained less than 10ppm, ring after removing impurity
Line ratio is 1.5-0.6, and viscosity is less than 50mm2The hydrolysate of/s, the hydrolysate are siloxanes ring body and wire body mixture, wherein
The content of siloxanes ring body ring body accounts for the 30-50% of total weight of the mixture；
Step（1）In, the weight ratio of concentration of hydrochloric acid 40%-50%, hydrochloric acid and dimethyldichlorosilane are 30-100:1, dimethyl
The weight ratio of dichlorosilane and two level hydrolysis hydrochloric acid is 1-10：1, wherein it is step that two level, which hydrolyzes hydrochloric acid,（2）In further hydrolyze
The hydrochloric acid generated afterwards, the mass concentration control which hydrolyzes hydrochloric acid are 20%-35%, hydrolysate I and three-level hydrolysis hydrochloric acid
Weight ratio is 1:1-15, it is step that three-level, which hydrolyzes hydrochloric acid,（3）In further hydrolyze after the hydrochloric acid that generates, which hydrolyzes hydrochloric acid
Mass concentration control is 0.1%-22%；Excessive water hydrolyzes the water in hydrochloric acid by three-level and provides in the step (2), and three-level hydrolyzes salt
Water in acid is excessive, and step reaction is without in addition addition water.
2. the hydrolysis process of dimethyldichlorosilane according to claim 1, which is characterized in that step 5）In, activated carbon
Activated carbon is provided in filter, wherein the specific surface area of activated carbon is 900-1500 ㎡/g.
3. the hydrolysis process of dimethyldichlorosilane as claimed in claim 1 or 2, which is characterized in that used in the hydrolysis process
Hydrolysis device it is as follows,
The conveying pipeline of dimethyldichlorosilane is connect with mixer one, and mixer one is connect with heat exchanger, heat exchanger and gas-liquid point
It is connected from device, gas-liquid separator is connect with phase separator one；
Phase separator one is connect with static mixer one, and static mixer one is connect with phase separator two；
Phase separator two is connect with static mixer two, and static mixer two is connect with phase separator three；
Phase separator three is connect with static mixer three, and static mixer three is connect with phase separator four；
Phase separator four is connect with active carbon filter, and active carbon filter is connect with hydrolysate conveying pipeline.
4. the hydrolysis process of dimethyldichlorosilane according to claim 3, which is characterized in that gas-liquid separator is through conveying
Pipe is connect with condenser one, and condenser one is connect with condenser two, and condenser two is connect with demister, demister and hydrogen chloride gas
Body conveying pipeline connects.
5. the hydrolysis process of dimethyldichlorosilane according to claim 3, which is characterized in that phase separator one also with it is mixed
Clutch one connects；Phase separator two is also connect with static mixer one through conveying pipeline, specifically phase separator two through conveying pipeline with
Phase separator one to the conveying pipeline between static mixer one connects；Conveying pipeline is additionally provided on phase separator, on the conveying pipeline
It is provided with process water feed pipe, which divides two-way, is connect all the way with static mixer one, connects all the way with static mixer two
It connects.
6. the hydrolysis process of dimethyldichlorosilane according to claim 3, which is characterized in that on static mixer one also
It is provided with conveying pipeline, the conveying pipeline and phase separator one to the conveying pipeline between mixer one connect.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106317095B (en) * | 2016-08-16 | 2018-09-07 | 湖北兴发化工集团股份有限公司 | A kind of concentrated hydrochloric acid hydrolysis technique and device |
| CN107177344A (en) * | 2017-05-27 | 2017-09-19 | 湖北兴瑞化工有限公司 | A kind of method that the glue of the high grade of transparency 107 is produced by raw material of Dimethyldichlorosilane hydrolysate |
| CN109880119B (en) * | 2019-01-31 | 2021-08-10 | 山东东岳有机硅材料股份有限公司 | Method for eliminating phenomena of no delamination and equipment adhesion of organosilicon crude monomer hydrolysate |
| CN110845734B (en) * | 2019-10-15 | 2021-06-15 | 中国化学赛鼎宁波工程有限公司 | System and method for hydrolyzing organochlorosilane and refining hydrochloric acid |
| CN114011356B (en) * | 2021-11-12 | 2023-05-26 | 新疆晶硕新材料有限公司 | Method and device for treating dimethyl dichlorosilane hydrolysate |
| CN114516976B (en) * | 2022-01-28 | 2024-01-12 | 云南能投硅材科技发展有限公司 | Pretreatment process for hydrolysis waste of dimethyl dichlorosilane |
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| CN101323666A (en) * | 2008-07-24 | 2008-12-17 | 山东东岳有机硅材料有限公司 | Method for continuous production hydrolysate by methylchlorosilane concentrated acid hydrolyzing |
| CN101875726A (en) * | 2009-04-30 | 2010-11-03 | 中国石油天然气股份有限公司 | Method for preparing polysiloxane by hydrolyzing dimethyl dichlorosilane |
| CN104163922A (en) * | 2014-07-21 | 2014-11-26 | 鲁西化工集团股份有限公司硅化工分公司 | Concentrated-acid hydrolysis technology for dimethyl dichlorosilane under balance state |
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| CN101875726A (en) * | 2009-04-30 | 2010-11-03 | 中国石油天然气股份有限公司 | Method for preparing polysiloxane by hydrolyzing dimethyl dichlorosilane |
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