CN115521331A - Continuous efficient hydrolysis method and device for dimethylchlorosilane - Google Patents
Continuous efficient hydrolysis method and device for dimethylchlorosilane Download PDFInfo
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- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 89
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 52
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 172
- 238000011010 flushing procedure Methods 0.000 claims abstract description 114
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 104
- 239000002253 acid Substances 0.000 claims abstract description 63
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 239000000126 substance Substances 0.000 claims abstract description 19
- 239000000047 product Substances 0.000 claims abstract description 9
- -1 dimethylchlorosilane hydride Chemical compound 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 6
- 239000012071 phase Substances 0.000 claims description 109
- 239000003921 oil Substances 0.000 claims description 26
- 238000002360 preparation method Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 230000001502 supplementing effect Effects 0.000 claims description 11
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 10
- 239000008346 aqueous phase Substances 0.000 claims description 9
- 238000004581 coalescence Methods 0.000 claims description 8
- 150000001804 chlorine Chemical class 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- 230000001476 alcoholic effect Effects 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000005191 phase separation Methods 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 5
- 230000003068 static effect Effects 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 239000003507 refrigerant Substances 0.000 claims description 4
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 239000005049 silicon tetrachloride Substances 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 150000001340 alkali metals Chemical group 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims description 2
- 239000000413 hydrolysate Substances 0.000 claims description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 2
- 150000004692 metal hydroxides Chemical class 0.000 claims description 2
- 229920005862 polyol Polymers 0.000 claims description 2
- 150000003077 polyols Chemical class 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000002699 waste material Substances 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 108010009736 Protein Hydrolysates Proteins 0.000 abstract description 2
- 238000012423 maintenance Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 40
- 239000007789 gas Substances 0.000 description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 239000005046 Chlorosilane Substances 0.000 description 3
- 239000002826 coolant Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000006459 hydrosilylation reaction Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001345 alkine derivatives Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 125000004103 aminoalkyl group Chemical group 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KTQYJQFGNYHXMB-UHFFFAOYSA-N dichloro(methyl)silicon Chemical compound C[Si](Cl)Cl KTQYJQFGNYHXMB-UHFFFAOYSA-N 0.000 description 1
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0896—Compounds with a Si-H linkage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/60—Pump mixers, i.e. mixing within a pump
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention provides a method and a device for continuously and efficiently hydrolyzing dimethylchlorosilane, belonging to the technical field of hydrolysis of hydrogen-containing halosilane, wherein the method comprises the steps of preparing an acid removing liquid by taking insoluble alkaline solid or soluble weakly alkaline substances, mixing the acid removing liquid with the dimethylchlorosilane serving as a raw material, carrying out hydrolysis reaction, separating the hydrolysate, and returning a water phase to be used as the acid removing liquid or partially extracting; the oil phase enters a flushing unit, is flushed and cleaned by flushing liquid, and is separated again to obtain a hydrolysis product; the device is used for the continuous efficient hydrolysis method of the dimethylchlorosilane hydride. The method has the advantages of short process flow, high production efficiency, low water consumption and no three-waste discharge in the whole production process; the device of the invention has the advantages of less used equipment and facilities, less investment, stable and reliable operation and lower maintenance cost.
Description
Technical Field
The invention relates to a hydrogen-containing halosilane hydrolysis technology, in particular to a method and a device for continuously and efficiently hydrolyzing dimethylhydrogen-chlorosilane.
Background
The dimethylhydrogen monochlorosilane is used as an active monomer, organic groups such as amino alkyl, epoxy group, hydroxyl group, sulfydryl group, methacryloxy group and the like can be introduced at two ends of a polysiloxane molecular chain by utilizing Si-H bonds at the end part of the dimethylhydrogen monochlorosilane through a hydrosilylation reaction, is a hydrosilation agent for organic synthesis and alkene and alkyne, can be used as a blocking agent when being used as an alpha and omega-hydrogen silicon-terminated organic silicon polymer, is used as a starting material for preparing an organic silicon surfactant, and has very high economic value.
The invention patent with publication number CN102757458A discloses that dimethyl hydrogen chlorosilane is hydrolyzed in 5 to 20wt% of dilute hydrochloric acid to obtain a crude product, and then the crude product is rectified to obtain tetramethyl dihydrogen disilane, the product quality is good, but the purity of the raw material dimethyl hydrogen chlorosilane is required to be more than 95%, and the method also has the defects of low concentration of generated wastewater, wastewater neutralization treatment, high wastewater generation rate, reaction liquid filtration and the like, so that the method wastes water resources and affects the production efficiency.
The invention patent with publication number CN111909191A discloses a method for loop hydrolysis after purifying tetramethyl dihydrodisilane from low-boiling residues and mixing the purified tetramethyl dihydrodisilane by a static mixer, but the generation efficiency is low due to poor mixing effect of the static mixer, the temperature control requirement of the whole reaction system is high, and the industrial operation is complex; in addition, hydrochloric acid produced as a by-product in the method needs to be neutralized separately, which increases the production cost.
As the technology needs to control lower hydrochloric acid concentration to avoid the fracture loss of the active Si-H bond, the process control difficulty is higher, the resource utilization difficulty of waste acid is high, and the waste water generation rate is high.
Disclosure of Invention
Aiming at the problems, the invention provides a method and a device for continuously and efficiently hydrolyzing dimethylchlorosilane.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for continuously and efficiently hydrolyzing dimethylchlorosilane is characterized in that insoluble alkaline solids or soluble weakly alkaline substances are taken as alkaline substances and added into an acid removing solution unit to prepare an acid removing solution, the obtained acid removing solution is mixed with dimethylchlorosilane serving as a raw material and then enters a hydrolysis reaction unit for hydrolysis reaction, and the obtained hydrolysis solution is separated to obtain a water phase and an oil phase; the water phase is returned to be used as acid removal liquid or is partially extracted, and the extracted water phase is used for recovering chloride; the oil phase enters a flushing unit, is flushed and cleaned by flushing liquid, is separated again, the flushed water phase returns to the flushing unit again to be used as the flushing liquid or used for preparing acid removing liquid, and the flushed oil phase is subjected to coalescence, impurity removal and water removal to obtain a hydrolysis product;
the coalesced water phase generated in the coalescence process is intermittently returned to the flushing unit to be used as flushing liquid or returned to the acid removing liquid unit to prepare the acid removing liquid.
Further, the insoluble basic solid is alkaline earth metal carbonate (such as barium carbonate, calcium carbonate, etc.) or insoluble metal hydroxide (such as magnesium hydroxide, aluminum hydroxide);
the soluble weakly basic substance is alkali metal bicarbonate (such as sodium bicarbonate, etc.), alkali metal dihydrogen phosphate (such as sodium dihydrogen phosphate), or weakly basic organic ammonia (such as pyridine, aniline, etc.).
Further, when gas is generated in the hydrolysis reaction process, gas phase is recycled when the hydrolysate is separated and washed and then separated;
the concentration of the alkaline substance in the acid solution is 2 to 15wt%, preferably 5 to 9wt%;
the volume ratio of the raw material dimethylchlorosilane to the acid removing liquid is 1:3 to 15, preferably 1:5 to 10;
the time of the hydrolysis reaction is 10 to 40min;
the temperature at the outlet of the hydrolysis reaction unit is 5 to 40 ℃;
the flushing liquid entering the flushing unit comprises a supplemented water/water alcohol solution and a flushed water phase;
the weight of the supplemented water/water alcohol solution is 20 to 50 percent of the weight of the raw material dimethylchlorosilane, preferably 25 to 30 percent;
the supplemented water is regenerated water, desalted water, deoxidized water or clean secondary water, and preferably regenerated water or desalted water;
the mass fraction of alcoholic solution of water is 2-10% of alcoholic hydroxyl group, and the used alcohol is a unit alcohol or a polyol with a carbon chain less than 5;
the volume ratio of the oil phase entering the flushing unit to the flushing liquid is 1 to 10 to 30, preferably 1;
the index requirements of the raw material of the dimethylchlorosilane are as follows: the content of dimethylhydrogen monochlorosilane is more than or equal to 90wt%, the content of silicon tetrachloride is less than or equal to 0.1wt%, and the content of monomethylhydrogen dichlorosilane is less than or equal to 5wt%;
when the coalesced aqueous phase is returned to the washout unit for use as a washout liquid, the washout liquid also includes the coalesced aqueous phase.
A continuous efficient hydrolysis device of dimethylchlorosilane is used for the continuous efficient hydrolysis method of dimethylchlorosilane, and comprises an acid liquid removing unit, a hydrolysis reaction unit, a first separator for three-phase separation, a flushing unit, a second separator for three-phase separation and a coalescer;
the acid removing liquid unit is connected with the hydrolysis reaction unit through a first pipeline, and a dimethylchlorosilane pipeline is communicated with the first pipeline between the acid removing liquid unit and the hydrolysis reaction unit;
the hydrolysis reaction unit is connected with the first separator through a second pipeline; the top end of the first separator is provided with a gas phase overflow outlet;
the bottom end of the first separator is provided with a water phase return pipe; a chlorine salt extraction outlet is arranged on the water phase return pipe; the water phase return pipe is also communicated with the first pipeline;
an overflow pipe for overflowing the oil phase is arranged at the side surface of the first separator close to the top end;
the overflow pipe is connected with the front end of the flushing unit, and the rear end of the flushing unit is connected with the second separator; the top end of the second separator is provided with a flushed second gas phase overflow outlet;
the bottom end of the second separator is provided with an oscillation liquid return pipeline for returning the oscillation liquid; the flushing liquid return pipeline is connected with the front end of the flushing unit; a flushing liquid return pipeline between the second separator and the flushing unit is communicated with a liquid supplementing pipe;
a second overflow pipe for overflowing the flushed oil phase is arranged at the side surface of the second separator close to the top end; the second overflow pipe is connected with the coalescer, and the bottom end of the coalescer is communicated with the flushing liquid return pipeline through a third pipeline.
Further, a first pump is arranged on a first pipeline between the connection part of the dimethylchlorosilane pipeline and the first pipeline and the hydrolysis reaction unit; the first pump adopts a semi-open impeller pump;
the distance between the communication position of the dimethylchlorosilane pipeline and the first pump is 200-2000 mm.
Further, a second pump is arranged on the first pipeline between the communicating part of the dimethylchlorosilane and the first pipeline and the deacidification liquid unit; and an acid removal liquid circulating pipeline communicated with the acid removal liquid unit is also arranged on the first pipeline between the first pump and the second pump.
Furthermore, a liquid distribution pipeline is also communicated with the flushing liquid return pipeline between the communicated part of the liquid supplementing pipe and the flushing liquid return pipeline and the second separator; one end of the liquid preparation pipeline, which is far away from the flushing liquid return pipeline, is connected with the acid liquid removal unit;
the deacidification liquid unit comprises a deacidification liquid preparation container and a conveying part for conveying alkaline substances, and the conveying part is connected with the top end of the deacidification liquid preparation container;
when the alkaline substance is solid, the conveying component adopts a screw conveyor.
Furthermore, a third pump is arranged on the flushing liquid return pipeline between the communicating part of the liquid distribution pipeline and the flushing liquid return pipeline and the second separator.
Further, the gas phase overflow outlet and the second gas phase overflow outlet are both connected with a heat exchanger through a gas phase pipeline, the top of the heat exchanger is provided with a demister, and the bottom end of the heat exchanger is connected with the first separator through a liquid reflux pipeline; the heat exchanger adopts a refrigerant with the temperature of minus 30 to minus 10 ℃ for temperature control.
Furthermore, a control unit is arranged on the third pipeline, and the control unit can adopt a control valve;
the hydrolysis reaction unit adopts a heat exchanger E1, and the temperature of the heat exchanger E1 is controlled by adopting a cooling medium at 0 to 15 ℃;
the first separator and the second separator both adopt cavity type free separators;
the flushing unit adopts a static mixer.
The continuous efficient hydrolysis method and the device for the dimethylchlorosilane have the beneficial effects that:
according to the invention, insoluble alkaline solid or soluble weakly alkaline substance is used for preparing acid removing liquid, and the acid removing liquid is mixed with the raw material of the dimethylchlorosilane and then subjected to hydrolysis reaction, so that hydrochloric acid is not required to be added in the whole hydrolysis process, the breakage loss of active Si-H bonds is effectively avoided, the process control difficulty is reduced, and the production efficiency is improved;
hydrochloric acid is not required to be added, so that the resource utilization difficulty of waste acid is effectively reduced;
the invention can weaken the thermal effect of HCl generated by hydrolysis reaction besides alkaline substances contained in the acid liquor, and is convenient for controlling the temperature of the hydrolysis reaction;
according to the invention, the alkaline substances in the acid liquor can neutralize HCl generated in the hydrolysis reaction process, chloride salt formed in the neutralization reaction can be recycled for resource treatment, and no waste liquid is discharged in the whole process;
the concentration of the deacidification solution is set according to the concentration of a chloride solution (namely a water phase separated by a first separator) formed after the hydrolysis reaction is finished, so that the chloride solution is close to saturation and can be completely dissolved, the volume of the chloride solution can be reduced, the subsequent recycling treatment difficulty can be reduced, and the crystallization on the inner wall of a pipeline in the circulation process of the chloride solution can be avoided;
when gas is generated in the hydrolysis reaction, the high-purity gas is obtained by utilizing the separation devices (namely the first separator and the second separator) and then cooling, demisting and purifying, can be comprehensively utilized, and has no waste gas emission in the whole process;
the method recycles the water phase separated from the hydrolysate, the water phase separated after scouring and the water phase after coalescence, can reduce the consumption of water for production and reduce the production cost;
the method has the advantages of short process flow, high production efficiency, low water consumption and no three-waste discharge in the whole production process;
the device of the invention has the advantages of less equipment and facilities, less investment, stable and reliable operation and lower maintenance cost;
the invention utilizes the pump to efficiently and powerfully mix the raw material of the dimethylchlorosilane and the deacidification solution, thereby greatly improving the production efficiency.
Drawings
FIG. 1 is a schematic structural diagram of a continuous efficient hydrolysis apparatus for dimethylchlorosilane in example 1 of the present invention;
wherein, 1, an acid removing liquid unit; 11. a first pipe; 12. a dimethylmonohydrochlorosilane conduit; 13. a first pump; 14. a second pump; 15. an acid liquid removing circulation pipeline; 16. a liquid preparation pipeline; 17. a conveying member; 2. a hydrolysis reaction unit; 21. a second conduit; 3. a first separator; 31. an overflow pipe; 32. a water phase return pipe; 33. a chlorine salt production outlet; 34. a gas phase conduit; 35. a heat exchanger; 36. a liquid return conduit; 4. a flushing unit; 5. a second separator; 51. a second overflow tube; 52. a flushing liquid return pipeline; 53. a liquid supplementing pipe; 54. a third pump; 6. a coalescer; 61. a third conduit.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Example 1 continuous high-efficiency hydrolysis method of dimethylchlorosilane
The embodiment is a method for continuously and efficiently hydrolyzing dimethylchlorosilane, which aims at the indexes of the raw material dimethylchlorosilane as follows:
the content of dimethylchlorosilane is 95wt%, the content of silicon tetrachloride is 0.1wt%, the content of monomethyldichlorosilane is 2wt%, the content of tetramethylsilicon is 1.9wt%, and the content of alkane impurities is 1wt%.
The method comprises the following steps:
calcium carbonate is taken as an alkaline substance and added into the acid removing liquid unit 1 to prepare acid removing liquid with the concentration of 6wt%, and the acid removing liquid is calcium carbonate suspension;
the volume ratio of the raw material dimethylchlorosilane to the acid removing liquid is 1:8 (wherein the volume ratio of the raw material dimethylchlorosilane to the deacidification solution is marked as V1, that is, V1=1 in this embodiment;
after the oil phase enters the flushing unit 4 and is flushed and cleaned by the flushing liquid, the oil phase is separated again, the flushed water phase returns to the flushing unit 4 again to be used as the flushing liquid or used for preparing acid removing liquid, and the flushed oil phase is subjected to coalescence impurity removal and water removal to obtain a hydrolysis product, wherein the chlorine content and the water content of the hydrolysis product are 26ppm and 1635ppm respectively, and the pH value of the hydrolysis product is 5.0.
The coalesced water phase generated in the coalescence process is intermittently returned to the flushing unit 4 to be used as flushing liquid or returned to the acid removing liquid unit 1 to prepare the acid removing liquid;
when gas is generated in the hydrolysis reaction process, the gas phase is recovered when the hydrolysis liquid is separated and washed, and the carbon dioxide gas is generated in the hydrolysis reaction process and is separated to obtain clean carbon dioxide which can be used for preparing calcium carbonate;
the flushing liquid entering the flushing unit 4 comprises supplemented desalted water and flushed water phase;
when the coalesced water phase is returned to the flushing unit 4 to be used as flushing liquid, the flushing liquid also comprises the coalesced water phase; when the coalesced water phase is temporarily stopped and returned to the flushing unit 4 to be used as flushing liquid, the flushing liquid only comprises supplemented desalted water and the flushed water phase;
the weight of the additional desalted water was 25% of the weight of the starting dimethylmonohydrochlorosilane (the ratio of the weight of the additional water/aqueous alcoholic solution to the weight of the starting dimethylmonohydrochlorosilane was labeled as M1, i.e., M1= 25%).
The volume ratio of the oil phase to the flushing liquid entering the flushing unit 4 (marked M2) is 1.
Examples 2 to 8 continuous efficient hydrolysis method of dimethylchlorosilane
Examples 2 to 8 are continuous efficient hydrolysis methods of dimethylchlorosilane, which have the same steps as example 1 except for different process parameters, and are specifically shown in table 1:
TABLE 1 summary of the process parameters of examples 2 to 8
The process parameters and procedures of the other parts of examples 2 to 8 are the same as those of example 1.
Example 9 continuous high-efficiency hydrolysis method and apparatus for dimethylchlorosilane
The continuous efficient hydrolysis method of dimethylchlorosilane in examples 1 to 8 can be used for actual industrial production by adopting the device in the example, and the specific device is as follows:
as shown in fig. 1, the continuous efficient hydrolysis device of dimethylchlorosilane comprises an acid removing liquid unit 1, a hydrolysis reaction unit 2, a first separator 3 for three-phase separation, a flushing unit 4, a second separator 5 for three-phase separation and a coalescer 6.
The acid removing liquid unit 1 comprises an acid removing liquid preparation container and a conveying part 17 for conveying alkaline substances, and the conveying part 17 is connected with the top end of the acid removing liquid preparation container; the conveying means 17 employs a screw conveyor when the alkaline substance is solid. The deacidification solution preparation container generally adopts a preparation kettle, and indissolvable alkaline suspension/soluble alkalescent solution is formed by stirring, dispersing and dissolving in the deacidification solution preparation process. The hydrolysis reaction unit 2 adopts a heat exchanger E1, the temperature in the hydrolysis reaction process is controlled through the heat exchanger E1, the temperature of the heat exchanger E1 is controlled by a cooling medium at 0 to 15 ℃, and the hydrolysis reaction temperature is controlled at 5 to 40 ℃. The first separator 3 and the second separator 5 are typically hollow free separators. The flushing unit 4 generally adopts a static mixer to contact and mix the oil phase separated by the first separator 3 with the flushing liquid, so as to fully flush and clean the oil phase.
The acid liquid removing unit 1 is connected with the hydrolysis reaction unit 2 through a first pipeline 11, and a dimethylchlorosilane pipeline 12 is communicated with the first pipeline 11 between the acid liquid removing unit 1 and the hydrolysis reaction unit 2; a first pump 13 is further arranged on the first pipeline 11 between the part where the dimethylchlorosilane pipeline 12 is communicated with the first pipeline 11 and the hydrolysis reaction unit 2, a semi-open impeller pump is generally adopted as the first pump 13, the acid removing liquid and the raw material dimethylchlorosilane are strongly mixed by utilizing the high-speed rotation of pump blades, and the circulation volume of the first pump 13 is controlled (generally controlled within 10 to 50m) 3 H), adjusting the retention time of the raw material dimethylchlorosilane in the hydrolysis reaction unit 2; the distance between the connection part of the dimethylchlorosilane pipeline 12 and the first pipeline 11 and the first pump 13 is 200-2000 mm, and the distance in the embodiment is 1000mm.
A second pump 14 is also arranged on the first pipeline 11 between the communication part of the dimethylchlorosilane pipeline 12 and the first pipeline 11 and the acid removal liquid unit 1; and an acid-removing liquid circulating pipeline 15 communicated with the acid-removing liquid unit 1 is also arranged on the first pipeline 11 between the first pump 13 and the second pump 14. In the process of preparing the deacidification solution, the deacidification solution is circularly pumped into the deacidification solution unit 1 by the second pump 14 through the first pipeline 11 and the deacidification solution circulating pipeline 15 except for being stirred by the deacidification solution unit 1, so that the deacidification solution is mixed more uniformly. When the deacidification solution enters the hydrolysis reaction unit 2, the deacidification solution directly passes through the first pipeline 11 and the second pump 14 on the first pipeline 11, contacts with the raw material dimethylchlorosilane, enters the first pump 13, is strongly mixed by the first pump 13, and then enters the hydrolysis reaction unit 2.
The hydrolysis reaction unit 2 is connected with the first separator 3 through a second pipeline 21; the top end of the first separator 3 is provided with a gas phase overflow outlet; the gas phase overflow outlet is connected with a heat exchanger 35 through a gas phase pipeline 34, the top of the heat exchanger 35 is provided with a demisting component (namely a demisting section), and the bottom end of the heat exchanger 35 is connected with the first separator 3 through a liquid return pipe 36; the heat exchanger 35 is generally controlled by a refrigerant at-30 to-10 ℃. The gas phase overflowing from the first separator 3 is cooled and demisted by the heat exchanger 35 to obtain clean gas, which is then used as a production raw material of related industries for comprehensive utilization, and no waste gas is discharged in the whole process. The liquid condensed and demisted by the heat exchanger 35 flows back to the first separator 3 again through the liquid return pipe 36 by gravity.
The bottom end of the first separator 3 is provided with a water phase return pipe 32; the water phase return pipe 32 is provided with a chlorine salt extraction port 33, and the extracted high-concentration chlorine salt solution has stable components and high concentration, can be comprehensively utilized as production raw materials of related industries, and has no waste liquid output in the whole process; the aqueous phase return pipe 32 is also communicated with the first pipeline 11; the water phase separated by the first separator 3 flows into the first pipeline 11 again to be mixed with the raw material dimethylchlorosilane for hydrolysis reaction.
An overflow pipe 31 for overflow of the oil phase is arranged at the side surface of the first separator 3 close to the top end; the overflow pipe 31 is connected with the front end of the flushing unit 4; the oil phase overflowing from the first separator 3 enters the flushing unit 4 to be mixed with the flushing liquid, and the oil phase is flushed and cleaned by the flushing liquid in the flushing unit 4.
The rear end of the flushing unit 4 is connected with the second separator 5; the top end of the second separator 5 is provided with a flushed second gas phase overflow outlet; the second gas phase overflow outlet is connected with a heat exchanger 35 through a gas phase pipeline 34; the gas overflowing from the second gas phase overflow outlet and the gas overflowing from the gas phase overflow outlet can be mixed and simultaneously cooled and demisted by the heat exchanger 35; the gas overflowing from the second gas-phase overflow outlet can also be unmixed with the gas overflowing from the gas-phase overflow outlet, and the gas are cooled and demisted by using different heat exchangers 35 respectively; in this embodiment, the gas overflowing from the second gas phase overflow outlet is mixed with the gas overflowing from the gas phase overflow outlet, and then cooled and demisted.
The bottom end of the second separator 5 is provided with an flushing liquid return pipeline 52 for returning flushing liquid; the flushing liquid return pipeline 52 is connected with the front end of the flushing unit 4; the flushed water phase separated by the second separator 5 is reused as flushing liquid or used for preparing acid removing liquid, and no waste liquid is discharged in the whole process.
A flushing liquid return pipeline 52 between the second separator 5 and the flushing unit 4 is communicated with a liquid supplementing pipe 53, the liquid supplementing pipe 53 is supplemented with a water/water alcohol solution, and the supplemented water/water alcohol solution is mixed with the flushed water phase and the coalesced water phase which is intermittently returned to the flushing unit 4 to form flushing liquid; when the coalesced water phase stops returning to the flushing unit 4, the flushing liquid consists of the supplemented water/water alcohol solution and the flushed water phase; when the coalesced aqueous phase is returned to the flushing unit 4, the flushing liquid consists of additional water/water alcoholic solution together with the flushed aqueous phase and the coalesced aqueous phase. In general, the weight of the added water/water alcohol solution is 20 to 50 percent, preferably 25 to 30 percent of the weight of the raw material dimethylchlorosilane.
The flushing liquid return pipeline 52 positioned between the communication part of the liquid supplementing pipe 53 and the flushing liquid return pipeline 52 and the second separator 5 is also communicated with a liquid distribution pipeline 16; the end of the liquid preparation pipe 16 far from the flushing liquid return pipe 52 is connected to the deacidification liquid unit 1, the liquid preparation pipe 16 is generally connected to a deacidification liquid preparation container, and the flushed water phase and/or the coalesced water phase can be flowed into the deacidification liquid preparation container through the liquid preparation pipe 16 to prepare the deacidification liquid.
A third pump 54 is further arranged on the flushing liquid return pipeline 52 between the communicating part of the liquid distribution pipeline 16 and the flushing liquid return pipeline 52 and the second separator 5; namely, the flushing liquid return pipeline 52 from the second separator 5 to the flushing unit 4 is connected with the third pump 54, the liquid distribution pipeline 16 and the liquid supplementing pipe 53 in sequence.
A second overflow pipe 51 for overflowing the flushed oil phase is arranged at the side surface of the second separator 5 close to the top end; the second overflow pipe 51 is connected with the coalescer 6, the flushed oil phase separated by the second separator 5 enters the coalescer 6 through the second overflow pipe 51 for coalescing, impurity removing and water removing, and a hydrolysis product is obtained.
The bottom end of the coalescer 6 is communicated with the flushing liquid return pipe 52 through a third pipe 61, and the communication part of the third pipe 61 and the flushing liquid return pipe is positioned between the flushing unit 4 and the third pump 54; the third pipeline 61 is also provided with a control unit which can adopt a control valve; the coalesced water phase can intermittently flow into the flushing liquid return pipeline 52 to be mixed with the flushed water phase through the control of the control valve, and the coalesced water phase and the flushed water phase are jointly used as flushing liquid or used for preparing acid removing liquid, and no waste liquid is discharged in the whole process. In general, the control valve is opened once at an interval of 4 hours and for 15 to 30min once, and the water phase after coalescence flows into the flushing liquid return pipeline 52 again when the control valve is opened.
The specific working principle of the continuous efficient hydrolysis device for the dimethylchlorosilane is as follows:
the raw material dimethylchlorosilane and the deacidification liquid are contacted before the first pump 13 and jointly enter the pump body of the first pump 13, the mixed liquid is strongly mixed by utilizing the high-speed rotation of a pump impeller, the outlet of the first pump 13 is connected with the hydrolysis reaction unit 2, the mixed deacidification liquid and the raw material dimethylchlorosilane enter the hydrolysis reaction unit 2 for hydrolysis reaction, and the retention time of the raw material dimethylchlorosilane in the hydrolysis reaction unit 2 is adjusted for 10-40min by controlling the circulation amount of the first pump 13; and controlling the temperature at an outlet of the hydrolysis reaction unit 2 to be 5 to 40 ℃ by adopting a cooling medium at 0 to 15 ℃. The material flowing out of the hydrolysis reaction unit 2 enters a first separator 3, the separated lower-layer water phase returns to the first pump 13 through a water phase return pipe 32 and a first pipeline 11 for recycling, and a small part of water phase is used for extracting a chlorine salt solution through a chlorine salt extraction outlet 33 for recycling; a gas phase overflow outlet at the top end of the first separator 3 is connected with a side port at the bottom of the heat exchanger 35, a demisting section is arranged at the top end of the heat exchanger 35, and the gas phase is cooled and demisted by the heat exchanger 35 to obtain clean gas for recycling; the liquid condensed and demisted by the heat exchanger 35 falls by gravity to the first separator 3. After separation in the first separator 3, the upper oil phase overflows to the flushing unit 4 and is flushed and mixed with the flushing liquid, and the obtained mixed liquid enters the second separator 5. The water phase after the lower layer of flushing after the separation by the second separator 5 is recycled as flushing liquid again through a third pump 54 or is partially extracted and sent to the acid removing liquid unit 1 for preparing acid removing liquid, the flushed water phase and/or the coalesced water phase recycled by the third pump 54 are contacted with the water/water alcohol solution supplemented through a liquid supplementing pipe 53 to form flushing liquid mixed with the oil phase in a flushing manner, and water or water alcohol solution with the weight of 20 to 50 percent of that of the raw material dimethylhydrogen monochlorosilane is supplemented through the liquid supplementing pipe 53 before the flushing unit 4 under a general condition. The second gas phase overflow outlet at the top end of the second separator 5 is also connected with the side port at the bottom of the heat exchanger 35 for recovering clean gas. The oil phase which is separated by the second separator 5 and washed in the upper layer overflows to a coalescer 6, and is coalesced by the coalescer 6 to remove impurities and water, so that a hydrolysis product is obtained and extracted; the aqueous phase coalesced by the coalescer 6 is intermittently returned to the flushing unit 4. The flushed water phase and/or the coalesced water phase from the outlet of the third pump 54 enter the deacidification solution preparation container through the solution preparation pipeline 16, and form deacidification solution with the alkaline substance from the conveying part 17 under the stirring action of the deacidification solution preparation container and the circulation action of the second pump 14, and the deacidification solution is supplemented to the front of the inlet of the first pump 13 through the outlet of the second pump 14.
It should be apparent that the described embodiments are only some of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Claims (10)
1. A method for continuously and efficiently hydrolyzing dimethylchlorosilane is characterized in that insoluble alkaline solids or soluble weakly alkaline substances are taken as alkaline substances and added into an acid removing solution unit to prepare an acid removing solution, the obtained acid removing solution is mixed with dimethylchlorosilane, and then enters a hydrolysis reaction unit for hydrolysis reaction, and the obtained hydrolysis solution is separated to obtain a water phase and an oil phase; the water phase is returned to be used as acid removal liquid or partially extracted, and the extracted water phase is used for recovering chloride; the oil phase enters the flushing unit, is flushed and cleaned by flushing liquid, is separated again, the flushed water phase returns to the flushing unit again to be used as the flushing liquid or used for preparing acid removing liquid, and the flushed oil phase is subjected to coalescence, impurity removal and water removal to obtain a hydrolysis product;
the coalesced water phase generated in the coalescence process is intermittently returned to the flushing unit to be used as flushing liquid or returned to the acid removing liquid unit to prepare the acid removing liquid.
2. The continuous high-efficiency hydrolysis method of dimethylchlorosilane as claimed in claim 1, wherein the insoluble alkaline solid is alkaline earth metal carbonate or insoluble metal hydroxide;
the soluble weakly basic substance is alkali metal bicarbonate, alkali metal dihydrogen phosphate or weakly basic organic ammonia.
3. The continuous high-efficiency hydrolysis method of dimethylchlorosilane according to claim 1 or 2,
when gas is generated in the hydrolysis reaction process, gas phase is recycled when the hydrolysate is separated and washed and then separated;
the concentration of alkaline substances in the acid removing liquid is 2 to 15wt%;
the volume ratio of the raw material dimethylchlorosilane to the acid removing liquid is 1:3 to 15;
the hydrolysis reaction time is 10 to 40min;
the temperature at an outlet of the hydrolysis reaction unit is 5 to 40 ℃;
the flushing liquid entering the flushing unit comprises a supplemented water/water alcohol solution and a flushed water phase;
the weight of the supplemented water/water alcohol solution is 20 to 50 percent of the weight of the raw material dimethylchlorosilane;
the supplemented water is regenerated water, desalted water, deoxygenated water or clean secondary water;
the mass fraction of alcoholic solution of water is 2-20% of alcoholic hydroxyl group, and the used alcohol is a single alcohol or a polyol with a carbon chain less than 5;
the volume ratio of the oil phase entering the flushing unit to the flushing liquid is 1 to 10 to 30;
the index requirements of the raw material of the dimethylchlorosilane are as follows: the content of dimethylhydrogen monochlorosilane is more than or equal to 90wt%, the content of silicon tetrachloride is less than or equal to 0.1wt%, and the content of monomethylhydrogen dichlorosilane is less than or equal to 5wt%;
when the coalesced aqueous phase is returned to the flushing unit for use as a flushing liquid, the flushing liquid also includes the coalesced aqueous phase.
4. A continuous efficient hydrolysis device of dimethylchlorosilane, which is used for the continuous efficient hydrolysis method of dimethylchlorosilane according to any one of claims 1 to 3, and is characterized by comprising an acid liquid removing unit, a hydrolysis reaction unit, a first separator for three-phase separation, a flushing unit, a second separator for three-phase separation and a coalescer;
the acid removing liquid unit is connected with the hydrolysis reaction unit through a first pipeline, and a dimethylchlorosilane pipeline is communicated with the first pipeline between the acid removing liquid unit and the hydrolysis reaction unit;
the hydrolysis reaction unit is connected with the first separator through a second pipeline; the top end of the first separator is provided with a gas phase overflow outlet;
the bottom end of the first separator is provided with a water phase return pipe; a chlorine salt extraction outlet is arranged on the water phase return pipe; the water phase return pipe is also communicated with the first pipeline;
an overflow pipe for overflowing the oil phase is arranged at the side surface of the first separator close to the top end;
the overflow pipe is connected with the front end of the flushing unit, and the rear end of the flushing unit is connected with the second separator; the top end of the second separator is provided with a flushed second gas phase overflow outlet;
the bottom end of the second separator is provided with an oscillating liquid return pipeline for returning the oscillating liquid; the flushing liquid return pipeline is connected with the front end of the flushing unit; a flushing liquid return pipeline between the second separator and the flushing unit is communicated with a liquid supplementing pipe;
a second overflow pipe for overflowing the flushed oil phase is arranged at the side surface of the second separator close to the top end; the second overflow pipe is connected with the coalescer, and the bottom end of the coalescer is communicated with the flushing liquid return pipeline through a third pipeline.
5. The continuous efficient hydrolysis device of dimethylhydrogen monochlorosilane according to claim 4, wherein a first pump is further arranged on a first pipeline between the connection position of the dimethylhydrogen monochlorosilane pipeline and the first pipeline and the hydrolysis reaction unit;
the distance between the communication position of the dimethylchlorosilane pipeline and the first pump is 200-2000 mm.
6. The continuous efficient hydrolysis device for the dimethylmonohydrochlorosilane as claimed in claim 5, wherein a second pump is further arranged on the first pipeline between the part where the dimethylmonohydrochlorosilane pipeline is communicated with the first pipeline and the deacidification solution unit; and an acid removal liquid circulating pipeline communicated with the acid removal liquid unit is also arranged on the first pipeline between the first pump and the second pump.
7. The continuous efficient hydrolysis device for dimethylhydrogen monochlorosilane according to any one of claims 4 to 6, wherein a liquid distribution pipeline is further communicated with the flushing liquid return pipeline between the connection between the liquid supplementing pipe and the flushing liquid return pipeline and the second separator; one end of the liquid preparation pipeline, which is far away from the flushing liquid return pipeline, is connected with the acid removing liquid unit;
the acid removing liquid unit comprises an acid removing liquid preparation container and a conveying part for conveying alkaline substances, and the conveying part is connected with the top end of the acid removing liquid preparation container.
8. The continuous efficient hydrolysis device for dimethylchlorosilane as claimed in claim 7, wherein a third pump is further arranged on the flushing liquid return pipeline between the communicating part of the liquid preparation pipeline and the flushing liquid return pipeline and the second separator.
9. The continuous efficient hydrolysis device for dimethylchlorosilane according to any one of claims 4 to 6 and 8, wherein the gas phase overflow outlet and the second gas phase overflow outlet are both connected with a heat exchanger through a gas phase pipeline, the top of the heat exchanger is provided with a demister, and the bottom end of the heat exchanger is connected with a first separator through a liquid reflux pipeline; the heat exchanger adopts a refrigerant with the temperature of minus 30 to minus 10 ℃ for temperature control.
10. The continuous efficient hydrolysis device for dimethylchlorosilane according to any one of claims 4 to 6 and 8, wherein a control unit is arranged on the third pipeline;
the hydrolysis reaction unit adopts a heat exchanger E1, and the heat exchanger E1 adopts a refrigerant with the temperature of 0 to 15 ℃ for temperature control;
the first separator and the second separator both adopt cavity type free separators;
the flushing unit adopts a static mixer.
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