CN109650339A - Hydrolyzing chlorosilane prepares the technique and device of hydrogen chloride - Google Patents
Hydrolyzing chlorosilane prepares the technique and device of hydrogen chloride Download PDFInfo
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- 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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- hydrogen chloride
- chlorosilane
- scrubbing tower
- technique
- prepares
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910000041 hydrogen chloride Inorganic materials 0.000 title claims abstract description 72
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000005046 Chlorosilane Substances 0.000 title claims abstract description 23
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 230000003301 hydrolyzing effect Effects 0.000 title claims abstract description 17
- 238000005201 scrubbing Methods 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 21
- 230000007062 hydrolysis Effects 0.000 claims abstract description 17
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 17
- 239000003599 detergent Substances 0.000 claims abstract description 15
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 239000000413 hydrolysate Substances 0.000 claims abstract description 7
- 239000007921 spray Substances 0.000 claims abstract description 5
- 238000004064 recycling Methods 0.000 claims abstract description 3
- -1 siloxanes Chemical class 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 150000001555 benzenes Chemical class 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000012263 liquid product Substances 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- 239000000779 smoke Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 claims 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical group C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- 125000001997 phenyl group Chemical class [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000006276 transfer reaction Methods 0.000 description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 2
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 150000008422 chlorobenzenes Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical group C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 description 1
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/035—Preparation of hydrogen chloride from chlorides
Landscapes
- 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
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.
Priority Applications (1)
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CN201910041456.5A CN109650339A (en) | 2019-01-16 | 2019-01-16 | Hydrolyzing chlorosilane prepares the technique and device of hydrogen chloride |
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CN201910041456.5A CN109650339A (en) | 2019-01-16 | 2019-01-16 | Hydrolyzing chlorosilane prepares the technique and device of hydrogen chloride |
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Cited By (4)
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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Cited By (6)
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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