CN109650339A - Hydrolyzing chlorosilane prepares the technique and device of hydrogen chloride - Google Patents

Hydrolyzing chlorosilane prepares the technique and device of hydrogen chloride Download PDF

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Publication number
CN109650339A
CN109650339A CN201910041456.5A CN201910041456A CN109650339A CN 109650339 A CN109650339 A CN 109650339A CN 201910041456 A CN201910041456 A CN 201910041456A CN 109650339 A CN109650339 A CN 109650339A
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Prior art keywords
hydrogen chloride
chlorosilane
scrubbing tower
technique
prepares
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CN201910041456.5A
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仇晓丰
童新阳
姜思炜
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Hangzhou East Energy Saving Technology Co Ltd
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Hangzhou East Energy Saving Technology Co Ltd
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Priority to CN201910041456.5A priority Critical patent/CN109650339A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/01Chlorine; Hydrogen chloride
    • C01B7/03Preparation from chlorides
    • C01B7/035Preparation of hydrogen chloride from chlorides

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)

Abstract

The present invention provides the technique that a kind of hydrolyzing chlorosilane prepares hydrogen chloride, chlorosilane is dimethyldichlorosilane, can dissolve organosilan by using the detergent of chloride containing benzene derivative and reach purification hydrogen chloride gas purpose.This process unit is by hydrogen chloride flow to successively with hydrolysis device, hydrolysate container, hydrogen chloride scrubbing tower, hydrogen chloride collector.Separately there is the detergent reclaiming device being connected to sink, there is spray equipment on hydrogen chloride scrubbing tower top.The present invention changes the traditional handicraft of hydrogen chloride gas production recycling, and hydrogen chloride purity is high is alleviated environmental protection pressure, is recycled using cleaning solution, and equipment investment is few, and detergent consumption is few.

Description

Hydrolyzing chlorosilane prepares the technique and device of hydrogen chloride
Technical field
The present invention relates to the technologies of preparing of hydrogen chloride.
Background technique
Product in laboratory chlorine-hydride method:
It is usually reacted with salt and the concentrated sulfuric acid, do not heated or slightly heated, generate sodium bisulfate and hydrogen chloride, NaCl+ H2SO4→NaHSO4+HCl .Industrial producing chlorine-hydride method:
2NaCl+2H2O==energization==2NaOH+H2 ↑+Cl2, H2+Cl2==light==2HCl.
But the former is only suitable for a small amount of production, for the latter to the more demanding of equipment, energy consumption is larger, and there are biggish danger Property and environmental issue.
A kind of dimethyldichlorosilane of the disclosure of the invention that number of patent application is 2014102906400 hydrolyzes by-product hydrochloric acid and mentions Pure method, using siloxanes in hydride modified macropore polyvinylidene chloride absorption resin removing hydrochloric acid, the program is used Resin is adsorbed, consumption raw material is more, adsorbs the limited sorption capacity of resin.
The invention that number of patent application is 2010102728693 is related to a kind of Alkylchlorosilane hydrolysis device and hydrolysis process. The hydrolysis device includes strengthening mass transfer reaction device, gas condenser, gas purifier, phase separator, storage tank.The hydrolysis work Skill is to strengthen alkylchlorosilane and saturation hydrochloric acid in mass transfer reaction device, after liquid distribution trough tentatively mixes, is sprayed onto reinforcing Mass transfer reaction device internal rotor inner edge is cut by rotor and is collided, is further atomized hybrid reaction;The hydrogen chloride generated is reacted from reaction Device releases after gas condenser and gas purifier, obtains hydrogen chloride gas;The equipment that the invention uses is more, cost It is higher.
Summary of the invention
Summary of the invention
Goal of the invention: providing a kind of no high pressure-temperature technique requirement, and detergent is recycled, and can obtain high-purity hydrogen chloride The hydrolyzing chlorosilane of gas prepares the technique and its device of hydrogen chloride.
Technical solution:
The present invention provides the techniques that a kind of dimethylchlorosilane hydrolysis prepares hydrogen chloride, have following technical process:
1) hydrolyzing chlorosilane generates dimethyl siloxane and hydrogen chloride, have in hydrolysis device dimethyldichlorosilane raw material and Water, a large amount of hydrogen chloride of association generate when hydrolysis generates siloxanes, and 1000 ~ 2000ppm siloxanes is contained in hydrogen chloride gas, need Carrying out purification can be back to use in the production technologies such as chloromethanes;Its reaction equation is as follows:
n(CH3)2SiCl2 + nH2O = [ (CH3)2SiO ]n + 2nHCl
2) liquid product hydrolyzed is flowed out from hydrolysis device bottom;The gaseous products of hydrolysis are washed by hydrogen chloride scrubbing tower, are washed Gas collection after washing is pure hydrogen chloride;
3) contain siloxanes, hydrogen chloride, cleaning solution in the cleaning solution after washing;It first passes through at the recycling function of reclaiming device Reason generates pure detergent, and remaining gaseous material is back to use technical process 2 again) in hydrogen chloride scrubbing tower in, be recycled, Sufficiently acquisition useful resources.
Washing reclaiming device also has the function of a small amount of siloxanes in separating, washing liquid, recycles siloxanes again, with Technical process 1) generate siloxanes collect together so that the siloxanes rate of recovery further increases, hydrogen chloride gas is more It is pure.
Technical process 3) in, remaining gaseous material is back to use technical process 2 again) in front of, be 38%-45% through over-richness After smoke concentrated hydrochloric acid acid solution is washed again, hydrogen chloride scrubbing tower top is returned to.Guarantee that hydrogen chloride supersaturation is quickly precipitated in this way, It being discharged at the top of from scrubbing tower, obtains purer hydrogen chloride gas, other ingredients are mixed to be returned in scrubbing tower in aqueous solution, then Secondary washing.
Above-mentioned steps 2) in detergent in the chlorinated benzene derivative containing 20-40%d (Benzene Chloride containing this concentration is spread out Hydrogen chloride will not be dissolved substantially in the solution of biology, and can sufficiently dissolve and absorb the dimethyl-silicon of 1000 ~ 2000ppm concentration Alkane, and all crystallization is precipitated under subsequent process conditions, recycles, and does not bring biggish be stranded to the wastewater treatment in later period Difficulty, preferred fat base Benzene Chloride, dissolubility is preferable, further preferred dimethylated chlorobenzene, has similar knot with dimethylsilane Structure, intersolubility are more preferable).
It is used for the hydrogen chloride gas of generation to manufacture chloromethanes, which (has wherein been mixed with a small amount of dimethyl dichloro silicon Alkane, same with the product type in later period, compatibility is fine) a variety of methylic chlorosilanes can be made, it can be obtained by refining spearation Part dimethylchlorosilane is obtained, technical process 1 is back to use) in, fulfilling rate resource makes full use of.
Using technique described in claim 1, by hydrogen chloride flow to successively with hydrolysis device, hydrolysate container, chlorine Change hydrogen scrubbing tower, hydrogen chloride collector.
The top of hydrogen chloride scrubbing tower is exported with hydrogen chloride gas, and bottom has cleaning solution collecting tank.
The middle position of hydrogen chloride scrubbing tower has foam-expelling component, enables to liquefied gas quick separating.
Separately there is the detergent reclaiming device being connected to sink, the power of regeneration with detergent may make chlorination Hydrogen quality reaches reuse requirement.There is reuse entrance on hydrogen chloride scrubbing tower top, detergent reclaiming device is connected to reuse Entrance.
There is the spray equipment being connected with reuse entrance inside scrubbing tower, spray equipment makes the detergent and chlorine of reuse Change hydrogen to come into full contact with, further wash.
The utility model has the advantages that
Raw material involved in present invention production, intermediate product, product are both needed to high pressure-temperature operation, no explosion danger, part of appliance The less investment of permanent assets of less production line.The present invention changes by-product hydrogen chloride and need to absorb into 31% hydrochloric acid to be parsed again At the traditional handicraft of hydrogen chloride gas, concise in technology, hydrogen chloride purity is high is energy saving, alleviates environmental protection pressure.Moreover, washing Agent can be recycled, and consume less.Utility dimethyl siloxane can be recycled.The hydrogen chloride yield of production is higher, pure Degree is higher, is suitble to use in the industrialized productions such as chloromethanes production, is truly realized chlorine resource circulation utilization, is effectively reduced organic Silicon produces environmental protection pressure.
Detailed description of the invention
A kind of of the invention structure and flow diagram when Fig. 1.
In figure, 1- hydrolysis device, 2- hydrolysate container, 3- washing tower inlet, 4- cleaning solution collecting tank, 5- cleaning solution go out Mouth, 6- washing reclaiming device portal, 7- reclaiming device, the outlet of 8- washing reclaiming device, the separation of 15- siloxanes Outlet, 9- scrubbing tower refluxing opening, 10- hydrogen chloride gas outlet, 11- hydrogen chloride collection device, 12- spray equipment, 13- washing Tower, 14- foam-expelling component.
Specific embodiment
Hydrolyzing chlorosilane as shown in Figure 1 prepares the process flow of hydrogen chloride, has following technical process:
1) dimethyldichlorosilane hydrolysis generates siloxanes and hydrogen chloride, and hydrolysate is dimethyl siloxane and hydrogen chloride.
2) pass through hydrogen chloride scrubbing tower washing process process 1) in product, gas collection after washing is pure chlorine Change hydrogen;Contain 20-40% chlorinated benzene derivative in detergent.
3) cleaning solution after washing generates pure detergent by reclaiming device, then is back to use technical process 2) in Hydrogen chloride scrubbing tower in, be recycled.

Claims (10)

1. the technique that a kind of hydrolyzing chlorosilane prepares hydrogen chloride, it is characterised in that: have following technical process:
1) hydrolyzing chlorosilane generates siloxanes and hydrogen chloride;
2) liquid product hydrolyzed is flowed out from hydrolysis device bottom;The gaseous products of hydrolysis are washed by hydrogen chloride scrubbing tower, are washed Gas collection after washing is pure hydrogen chloride;
3) contain siloxanes, hydrogen chloride, cleaning solution in the cleaning solution after washing;It first passes through at the recycling function of reclaiming device Reason generates pure detergent, and remaining gaseous material is back to use technical process 2 again) in hydrogen chloride scrubbing tower in, be recycled.
2. the technique that hydrolyzing chlorosilane as described in claim 1 prepares hydrogen chloride, it is characterised in that: washing reclaiming device Also have the function of a small amount of siloxanes in separating, washing liquid, siloxanes recycled again, with technical process 1) generate siloxanes one It rises and collects.
3. the technique that hydrolyzing chlorosilane as described in claim 1 prepares hydrogen chloride, it is characterised in that: technical process 3) in, it is remaining Lower gaseous material is back to use technical process 2 again) in front of, through over-richness be 38%-45% smoke concentrated hydrochloric acid acid solution wash again Afterwards, hydrogen chloride scrubbing tower top is returned to.
4. the technique that hydrolyzing chlorosilane as described in claim 1 prepares hydrogen chloride, it is characterised in that: chlorosilane is dimethyl two Chlorosilane, hydrolysate are dimethyl siloxane and hydrogen chloride.
5. the technique that hydrolyzing chlorosilane as described in claim 1 prepares hydrogen chloride, it is characterised in that: technical process 2) in wash It washs and contains chlorinated benzene derivative in agent.
6. the technique that hydrolyzing chlorosilane as described in claim 1 prepares hydrogen chloride, it is characterised in that: by technical process 1) in produce Raw hydrogen chloride gas further makes methylic chlorosilane, obtains part two by refining spearation for manufacturing chloromethanes Methylchlorosilane.
7. the device that a kind of hydrolyzing chlorosilane prepares hydrogen chloride, it is characterised in that: technique described in claim 1 is used, by chlorine Changing hydrogen flow direction successively has hydrolysis device, hydrolysate container, hydrogen chloride scrubbing tower, hydrogen chloride collector;
Hydrolysis device has the siloxanes outlet of the water inlet at top, the chlorosilane entrance of side and hydrolysate outlet, bottom;
The top of hydrogen chloride scrubbing tower is exported with hydrogen chloride gas, and bottom has cleaning solution collecting tank.
8. the device that hydrolyzing chlorosilane as claimed in claim 6 prepares hydrogen chloride, it is characterised in that: in hydrogen chloride scrubbing tower Between have and defoam component.
9. the device that hydrolyzing chlorosilane as claimed in claim 6 prepares hydrogen chloride, it is characterised in that: separately have and sink lower part The detergent reclaiming device of connection has reuse entrance on hydrogen chloride scrubbing tower top, on detergent reclaiming device Portion has pipeline connection reuse entrance;Separately there is siloxanes outlet in reclaiming device side.
10. the device that hydrolyzing chlorosilane as claimed in claim 6 prepares hydrogen chloride, it is characterised in that: have inside scrubbing tower There is the spray equipment being connected with reuse entrance.
CN201910041456.5A 2019-01-16 2019-01-16 Hydrolyzing chlorosilane prepares the technique and device of hydrogen chloride Pending CN109650339A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110467155A (en) * 2019-09-18 2019-11-19 浙江新安化工集团股份有限公司 A kind of system and technique of the hydrogen chloride that processing hydrolyzing chlorosilane generates
CN112441561A (en) * 2020-11-26 2021-03-05 山东东岳有机硅材料股份有限公司 Device and method for efficiently removing siloxane in chlorosilane hydrolysis byproduct hydrogen chloride
CN113512052A (en) * 2021-07-13 2021-10-19 河北津宏化工有限公司 Preparation process of lithium difluoroborate
CN116907953A (en) * 2023-09-11 2023-10-20 是高(北京)智能科技有限公司 Chlorosilane chemical analysis pretreatment system

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JPS59121112A (en) * 1982-12-24 1984-07-13 デイナミ−ト・ノ−ベル・アクチエンゲゼルシヤフト Separation of chlorosilane from gaseous mixture comprising hydrogen chloride, hydrogen and chlorosilane
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CN101423193A (en) * 2008-12-04 2009-05-06 浙江恒业成有机硅有限公司 Technique for reducing impurity content in gas phase hydrogenchloride from hydrolysis of dimethyldichlorosilane
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
CN106629604A (en) * 2016-11-28 2017-05-10 昆明理工大学 Method for preparing gas-phase hydrogen chloride by utilizing chlorosilane residue
CN108569700A (en) * 2018-07-10 2018-09-25 四川绿源聚能环保科技有限责任公司 A kind of technique of recycling chlorosilane dreg slurry

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JPS59121112A (en) * 1982-12-24 1984-07-13 デイナミ−ト・ノ−ベル・アクチエンゲゼルシヤフト Separation of chlorosilane from gaseous mixture comprising hydrogen chloride, hydrogen and chlorosilane
US4490343A (en) * 1982-12-24 1984-12-25 Dynamit Nobel Ag Method for the separation of chlorosilanes from a gaseous mixture containing hydrogen chloride and hydrogen
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110467155A (en) * 2019-09-18 2019-11-19 浙江新安化工集团股份有限公司 A kind of system and technique of the hydrogen chloride that processing hydrolyzing chlorosilane generates
WO2021051549A1 (en) * 2019-09-18 2021-03-25 浙江新安化工集团股份有限公司 System and technology for treating hydrogen chloride generated by hydrolysis of chlorosilane
CN112441561A (en) * 2020-11-26 2021-03-05 山东东岳有机硅材料股份有限公司 Device and method for efficiently removing siloxane in chlorosilane hydrolysis byproduct hydrogen chloride
CN113512052A (en) * 2021-07-13 2021-10-19 河北津宏化工有限公司 Preparation process of lithium difluoroborate
CN116907953A (en) * 2023-09-11 2023-10-20 是高(北京)智能科技有限公司 Chlorosilane chemical analysis pretreatment system
CN116907953B (en) * 2023-09-11 2023-11-14 是高(北京)智能科技有限公司 Chlorosilane chemical analysis pretreatment system

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Application publication date: 20190419