CN114989435B - Stable control dimethyl dichlorosilane hydrolysis process - Google Patents
Stable control dimethyl dichlorosilane hydrolysis process Download PDFInfo
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- CN114989435B CN114989435B CN202210595300.3A CN202210595300A CN114989435B CN 114989435 B CN114989435 B CN 114989435B CN 202210595300 A CN202210595300 A CN 202210595300A CN 114989435 B CN114989435 B CN 114989435B
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- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 52
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 170
- 238000005406 washing Methods 0.000 claims abstract description 126
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 117
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 39
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000413 hydrolysate Substances 0.000 claims abstract description 37
- 239000007789 gas Substances 0.000 claims abstract description 28
- 238000007872 degassing Methods 0.000 claims abstract description 24
- 238000004064 recycling Methods 0.000 claims abstract description 22
- 239000000178 monomer Substances 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 230000001502 supplementing effect Effects 0.000 claims abstract description 8
- 238000000746 purification Methods 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 238000011084 recovery Methods 0.000 abstract description 15
- 238000006298 dechlorination reaction Methods 0.000 abstract description 14
- 239000002253 acid Substances 0.000 abstract description 13
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 9
- 239000000460 chlorine Substances 0.000 abstract description 9
- 229910052801 chlorine Inorganic materials 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 7
- 238000003795 desorption Methods 0.000 description 8
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 108010009736 Protein Hydrolysates Proteins 0.000 description 5
- 238000005903 acid hydrolysis reaction Methods 0.000 description 5
- -1 dimethylsiloxane Chemical class 0.000 description 5
- 238000004065 wastewater treatment Methods 0.000 description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 description 4
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- IJOOHPMOJXWVHK-UHFFFAOYSA-N trimethylsilyl-trifluoromethansulfonate Natural products C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 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
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- 239000005048 methyldichlorosilane Substances 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention discloses a stable control dimethyl dichlorosilane hydrolysis process, which comprises the steps of carrying out hydrolysis reaction on dimethyl dichlorosilane monomers and hydrochloric acid, carrying out degassing separation on dimethyl dichlorosilane hydrolysate generated by the hydrolysis reaction, washing and separating hydrogen chloride gas obtained by degassing separation by using dilute hydrochloric acid, carrying out primary water washing reaction, secondary water washing reaction and tertiary water washing reaction on the dimethyl dichlorosilane hydrolysate obtained by degassing separation, recycling dilute hydrochloric acid obtained by tertiary water washing separation into the secondary water washing reaction, recycling dilute hydrochloric acid obtained by washing separation into the primary water washing reaction, recycling dilute hydrochloric acid obtained by primary water washing separation into the hydrolysis reaction, and externally supplementing fresh hydrochloric acid with the concentration of 31% wt when carrying out the primary water washing reaction. The method has the advantages of reasonable process route, controllable reaction process, obvious chlorine dechlorination effect, high hydrogen chloride recovery rate and acid water discharge.
Description
Technical Field
The invention belongs to the technical field of reprocessing of organic silicon byproducts, and particularly relates to a dimethyl dichlorosilane hydrolysis process capable of being controlled stably.
Background
Methyl chlorosilane is an important raw material for preparing organic silicon materials, and the monomers mainly comprise monomethyl trichlorosilane, dimethyl dichlorosilane, trimethyl monochlorosilane and tetramethyl silane, wherein the dosage of the methyl chlorosilane is more than 90 percent of that of the whole organic silicon monomers, and the dosage of the dimethyl dichlorosilane is the largest and is about 80 percent. Dimethyl dichlorosilane is not only the most important platform raw material for synthesizing organic silicon materials, but also the most important index for measuring the development degree of the organic silicon industry in one country. At present, a direct method is generally used for preparing methyl chlorosilane monomers, and besides the main product dimethyl dichlorosilane, a few byproducts are generated, wherein the main byproducts include methyl trichlorosilane, methyl dichlorosilane, trimethyl monochlorosilane, high-boiling substances, a small amount of azeotrope and low-boiling substances. In the existing organosilicon production process, in order to obtain dimethylsiloxane with lower chlorine content, the dimethylsiloxane is required to undergo a series of hydrolysis reactions in a reactor, and the advantages and disadvantages of the hydrolysis process level are directly related to the quality of organosilicon products and the recovery efficiency of chlorine in production raw materials, and the excellent hydrolysis scheme can effectively reduce the production cost of organosilicon products.
At present, the hydrolysis mode of the dimethyl dichlorosilane mainly comprises two modes of saturated acid hydrolysis and unsaturated acid hydrolysis, a large amount of hydrogen chloride can be recovered by utilizing the saturated acid hydrolysis, and a large amount of energy consumption is avoided for the dissolution and heat release of the hydrogen chloride, because the primary hydrolysis reaction of the dimethyl dichlorosilane adopts pressurized saturated hydrochloric acid hydrolysis, the hydrochloric acid concentration is generally 40-47% wt, the viscosity of the hydrolysate is stable, the hydrochloric acid concentration of the secondary hydrolysis depends on the chlorine content brought by the primary hydrolysate, the small fluctuation of the primary hydrolysis process can cause the fluctuation of the hydrochloric acid concentration of the secondary hydrolysate, the control of the viscosity of the hydrolysate is further influenced, once the control is poor, the hydrolysate is emulsified, the phenomenon of oil-water indiscriminate appears, the chlorine content in the hydrolysate exceeds standard, and even the system is stopped; by utilizing unsaturated acid hydrolysis, the effect of dechlorination is not ideal due to lower acid concentration, a great amount of energy consumption is needed for the dissolution and heat release of hydrogen chloride, the obtained acid water can not be reused or is difficult to reuse, the phenomenon of acid discharge can exist, and the wastewater treatment cost and difficulty are still increased. Therefore, development of a stable control dimethyl dichlorosilane hydrolysis process with reasonable process route, stable system control, remarkable dechlorination effect, high hydrogen chloride recovery rate and no acid water emission is needed objectively.
Disclosure of Invention
The invention aims to solve the technical problems of large viscosity fluctuation, low hydrogen chloride recovery efficiency, large control difficulty of hydrolysis process and the like in the prior art, and provides a stable control dimethyl dichlorosilane hydrolysis process which has reasonable process route, controllable reaction process, remarkable dechlorination effect, high hydrogen chloride recovery rate and no acid water emission.
The invention relates to a stable control dimethyl dichlorosilane hydrolysis process which is characterized by comprising the following steps of:
s1: carrying out hydrolysis reaction on a dimethyl dichlorosilane monomer and concentrated hydrochloric acid with the concentration of 40-47% by weight in a hydrolysis system, wherein the volume ratio of the dimethyl dichlorosilane monomer to the hydrochloric acid is 1:15-20, and introducing hydrogen chloride gas generated by the hydrolysis reaction into a purification system for purification treatment;
s2: degassing and separating the dimethyl dichlorosilane hydrolysate generated by the hydrolysis reaction in a degassing system;
s3: washing and absorbing the degassed and separated hydrogen chloride gas in an absorption tower by utilizing dilute hydrochloric acid, and neutralizing tail gas obtained by washing and absorbing by an alkaline washing system;
s4: sequentially performing primary water washing and secondary water washing on the degassed and separated dimethyl dichlorosilane hydrolysate by dilute hydrochloric acid, and then performing tertiary water washing by desalted water to obtain the dimethyl dichlorosilane hydrolysate;
s5, recycling the dilute hydrochloric acid separated by the three-stage water washing into a second-stage water washing process, recycling the dilute hydrochloric acid separated by the second-stage water washing into a washing and absorbing process, recycling the concentrated hydrochloric acid with the concentration of 22-31% wt, which is separated after washing and absorbing, into a first-stage water washing process, recycling the dilute hydrochloric acid separated by the first-stage water washing into a hydrolysis reaction, wherein a fresh hydrochloric acid inlet is further arranged in the first-stage water washing process and used for timely supplementing the fresh hydrochloric acid with the concentration of 31% wt so as to maintain the balance of the system.
The invention has the beneficial effects that: firstly, the hydrolysis desorption process is optimized, through hydrolysis reaction, degassing separation and washing absorption, the thorough separation of hydrogen chloride gas can be realized, the hydrogen chloride gas can be efficiently recovered, the recovery rate of the hydrogen chloride gas can reach more than 99%, meanwhile, through controlling the concentration of hydrochloric acid which is recycled in the three-stage washing reaction process, oleic acid or oil-water separation is easier in the washing process, the efficient washing dechlorination of dimethyl dichlorosilane can be carried out, the hydrolysis viscosity of dimethyl polysiloxane can be reasonably controlled, and the better dechlorination effect is realized; on the basis of the efficient dechlorination technology, the fresh hydrochloric acid with the external concentration of 31 percent by weight is supplemented in the process of the primary water washing reaction, the supplemented fresh hydrochloric acid can supplement water to the whole desorption hydrolysis technology, the water consumption is balanced with the water inflow, the whole system balance is maintained, and the concentration of the hydrochloric acid of the primary water washing can be stably controlled after the fresh hydrochloric acid is supplemented, so that the water washing of the dimethyl dichlorosilane hydrolysate can be realized, the efficient dechlorination can be realized, the recovery rate of hydrogen chloride can be further improved after the dechlorinated hydrochloric acid enters the hydrolysis reaction, and the overall recovery rate of the hydrogen chloride can reach more than 102 percent; in the whole dehydration and hydrolysis process, the discharged dilute hydrochloric acid in each process can be recycled efficiently, the phenomenon of acid water discharge does not exist in the whole process, the cost of wastewater treatment is effectively saved, and the method has the advantages of reasonable process route, controllable reaction process, obvious chlorine removal effect and high hydrogen chloride recovery rate, can generate better economic benefit, and is easy to popularize and use.
Drawings
FIG. 1 is a schematic process flow diagram of the method of the present invention.
Detailed Description
The invention is further described below with reference to examples and the accompanying drawings, which are not in any way limiting, but are any changes or substitutions based on the teachings of the invention, all falling within the scope of the invention.
Example 1
The process for the hydrolysis of the dimethyldichlorosilane of this example 1, which is stably controlled, is carried out according to the following steps:
s1: the method comprises the steps of carrying out hydrolysis reaction on a dimethyl dichlorosilane monomer and concentrated hydrochloric acid with the concentration of 40%wt in a hydrolysis system, wherein the volume ratio of the dimethyl dichlorosilane monomer to the hydrochloric acid is 1:15, hydrogen chloride gas generated in the hydrolysis reaction enters a purification system for purification treatment, the working pressure of the hydrolysis reaction is 0.18MPa, the working temperature is 20 ℃, the dimethyl dichlorosilane monomer is hydrolyzed by hydrochloric acid, so that the hydrolysis desorption of the hydrogen chloride gas and the dimethyl dichlorosilane can be realized, and the hydrogen chloride gas is directly used for synthesizing chloromethane after being purified;
s2: degassing and separating the dimethyl dichlorosilane hydrolysate generated by the hydrolysis reaction in a degassing system, wherein the working pressure of the degassing and separating is 0.05MPa, the pressure of the degassing and separating is reduced to micro positive pressure, and the hydrogen chloride gas of the dimethyl dichlorosilane hydrolysate can be completely separated out due to the pressure change of the degassing and separating;
s3: washing and absorbing the degassed and separated hydrogen chloride gas in an absorption tower by utilizing dilute hydrochloric acid, and neutralizing tail gas obtained by washing and absorbing by an alkaline washing system;
s4: sequentially performing primary water washing and secondary water washing on the degassed and separated dimethyl dichlorosilane hydrolysate by using dilute hydrochloric acid, and then performing tertiary water washing by using desalted water to obtain the dimethyl dichlorosilane hydrolysate, wherein the concentration of the dilute hydrochloric acid in the primary water washing process is 29% wt, and the volume ratio of the dimethyl dichlorosilane hydrolysate to the dilute hydrochloric acid is 1:4; the concentration of dilute hydrochloric acid in the secondary water washing process is 3% wt, the volume ratio of the dimethyl dichlorosilane hydrolysate to the dilute hydrochloric acid is 1:4, the concentration of the dilute hydrochloric acid in the tertiary water washing process is 0.02% wt, the volume ratio of the dimethyl dichlorosilane hydrolysate to the desalted water is 1:4, the working temperature of the primary water washing process is controlled at 20 ℃, and the working temperatures of the secondary water washing process and the tertiary water washing process are controlled at 80 ℃;
s5, recycling the dilute hydrochloric acid separated by the three-stage water washing into the two-stage water washing process, recycling the dilute hydrochloric acid separated by the two-stage water washing into the washing and absorbing process, recycling the concentrated hydrochloric acid with the concentration of 22%wt separated by the washing and absorbing process into the first-stage water washing process, condensing the chilled water with the concentration of less than-15 ℃ in the washing and absorbing process when the concentrated hydrochloric acid with the concentration of 22%wt separated by the washing and absorbing process, recycling the dilute hydrochloric acid separated by the first-stage water washing into the hydrolysis reaction, and further arranging a fresh hydrochloric acid inlet for timely supplementing the fresh hydrochloric acid with the concentration of 31%wt in the first-stage water washing process so as to maintain the balance of the system.
The embodiment 1 not only can carry out high-efficiency water washing and dechlorination on the dimethyl dichlorosilane monomer, effectively control the viscosity of the dimethyl polysiloxane and improve the recovery rate of hydrogen chloride, but also has better dechlorination effect, and the recovery rate of the hydrogen chloride can reach more than 102 percent; on the premise of effectively ensuring the concentration of water washing acid, the balance of the water supplementing amount and the water consumption of the system can be maintained, and the water washing and desorption of the dimethyl dichlorosilane hydrolysate can be realized, so that the product quality of the dimethyl dichlorosilane is greatly improved, and the finally obtained dimethyl dichlorosiloxane has the viscosity of 15Cp and the chlorine content of 5ppmwt; in addition, the whole process has no acid water discharge phenomenon, effectively saves the cost of wastewater treatment, and can generate better economic benefit.
Example 2
The process for the hydrolysis of the dimethyldichlorosilane of this example 2, which is stably controlled, is carried out according to the following steps:
s1: the method comprises the steps of carrying out hydrolysis reaction on a dimethyl dichlorosilane monomer and concentrated hydrochloric acid with the concentration of 45%wt in a hydrolysis system, wherein the volume ratio of the dimethyl dichlorosilane monomer to the hydrochloric acid is 1:18, and hydrogen chloride gas generated in the hydrolysis reaction enters a purification system for purification treatment, the working pressure of the hydrolysis reaction is 0.28MPa, the working temperature is 40 ℃, the dimethyl dichlorosilane monomer is hydrolyzed by hydrochloric acid, so that the hydrolytic desorption of the hydrogen chloride gas and the dimethyl dichlorosilane can be realized, and the hydrogen chloride gas is directly used for synthesizing chloromethane after being purified;
s2: degassing and separating the dimethyl dichlorosilane hydrolysate generated by the hydrolysis reaction in a degassing system, wherein the working pressure of the degassing and separating is 0.06MPa, the pressure of the degassing and separating is reduced to micro positive pressure, and the hydrogen chloride gas of the dimethyl dichlorosilane hydrolysate can be completely separated out due to the pressure change of the degassing and separating;
s3: washing and absorbing the degassed and separated hydrogen chloride gas in an absorption tower by utilizing dilute hydrochloric acid, and neutralizing tail gas obtained by washing and absorbing by an alkaline washing system;
s4: sequentially performing primary water washing and secondary water washing on the degassed and separated dimethyl dichlorosilane hydrolysate by using dilute hydrochloric acid, and then performing tertiary water washing by using desalted water to obtain the dimethyl dichlorosilane hydrolysate, wherein the concentration of the dilute hydrochloric acid in the primary water washing process is 30% wt, and the volume ratio of the dimethyl dichlorosilane hydrolysate to the dilute hydrochloric acid is 1:8; the concentration of dilute hydrochloric acid in the secondary water washing process is 6% wt, the volume ratio of the dimethyl dichlorosilane hydrolysate to the dilute hydrochloric acid is 1:8, the concentration of the dilute hydrochloric acid in the tertiary water washing process is 0.1% wt, the volume ratio of the dimethyl dichlorosilane hydrolysate to the desalted water is 1:8, the working temperature of the primary water washing process is controlled at 25 ℃, and the working temperatures of the secondary water washing process and the tertiary water washing process are controlled at 85 ℃;
s5, recycling the dilute hydrochloric acid separated by the three-stage water washing into the two-stage water washing process, recycling the dilute hydrochloric acid separated by the two-stage water washing into the washing and absorbing process, recycling the concentrated hydrochloric acid with the concentration of 25% wt separated by the washing and absorbing process into the first-stage water washing process, condensing the chilled water with the concentration of less than-15 ℃ in the washing and absorbing process when the concentrated hydrochloric acid with the concentration of 25% wt separated by the washing and absorbing process, recycling the dilute hydrochloric acid separated by the first-stage water washing into the hydrolysis reaction, and further arranging a fresh hydrochloric acid inlet for timely supplementing the fresh hydrochloric acid with the concentration of 31% wt in the first-stage water washing process so as to maintain the balance of the system.
The embodiment 2 not only can carry out high-efficiency water washing and dechlorination on the dimethyl dichlorosilane monomer, effectively control the viscosity of the dimethyl polysiloxane and improve the recovery rate of hydrogen chloride, but also has better dechlorination effect, and the recovery rate of the hydrogen chloride can reach more than 102 percent; on the premise of effectively ensuring the concentration of water washing acid, the balance of the water supplementing amount and the water consumption of the system can be maintained, and the water washing and desorption of the dimethyl dichlorosilane hydrolysate can be realized, so that the product quality of the dimethyl dichlorosilane is greatly improved, and the finally obtained dimethyl dichlorosiloxane has the viscosity of 20Cp and the chlorine content of 5ppmwt; in addition, the whole process has no acid water discharge phenomenon, effectively saves the cost of wastewater treatment, and can generate better economic benefit.
Example 3
The process for the hydrolysis of the dimethyldichlorosilane of this example 3, which is stably controlled, is carried out according to the following steps:
s1: the method comprises the steps of carrying out hydrolysis reaction on dimethyl dichlorosilane monomer and concentrated hydrochloric acid with the concentration of 47%wt in a hydrolysis system, wherein the volume ratio of the dimethyl dichlorosilane monomer to the hydrochloric acid is 1:20, hydrogen chloride gas generated in the hydrolysis reaction enters a purification system for purification treatment, the working pressure of the hydrolysis reaction is 0.30MPa, the working temperature is 50 ℃, the dimethyl dichlorosilane monomer is hydrolyzed by hydrochloric acid, so that the hydrolysis desorption of the hydrogen chloride gas and the dimethyl dichlorosilane can be realized, and the hydrogen chloride gas is directly used for synthesizing chloromethane after being purified;
s2: degassing and separating the dimethyl dichlorosilane hydrolysate generated by the hydrolysis reaction in a degassing system, wherein the working pressure of the degassing and separating is 0.08MPa, the pressure of the degassing and separating is reduced to micro positive pressure, and the hydrogen chloride gas of the dimethyl dichlorosilane hydrolysate can be completely separated out due to the pressure change of the degassing and separating;
s3: washing and absorbing the degassed and separated hydrogen chloride gas in an absorption tower by utilizing dilute hydrochloric acid, and neutralizing tail gas obtained by washing and absorbing by an alkaline washing system;
s4: sequentially performing primary water washing and secondary water washing on the degassed and separated dimethyl dichlorosilane hydrolysate by using dilute hydrochloric acid, and then performing tertiary water washing by using desalted water to obtain the dimethyl dichlorosilane hydrolysate, wherein the concentration of the dilute hydrochloric acid in the primary water washing process is 33% wt, and the volume ratio of the dimethyl dichlorosilane hydrolysate to the dilute hydrochloric acid is 1:10; the concentration of dilute hydrochloric acid in the secondary water washing process is 8%wt, the volume ratio of the dimethyl dichlorosilane hydrolysate to the dilute hydrochloric acid is 1:10, the concentration of the dilute hydrochloric acid in the tertiary water washing process is 0.2%wt, the volume ratio of the dimethyl dichlorosilane hydrolysate to the desalted water is 1:10, the working temperature of the primary water washing process is controlled at 30 ℃, and the working temperatures of the secondary water washing process and the tertiary water washing process are controlled at 90 ℃;
s5, recycling the dilute hydrochloric acid separated by the three-stage water washing into the two-stage water washing process, recycling the dilute hydrochloric acid separated by the two-stage water washing into the washing and absorbing process, recycling the concentrated hydrochloric acid with the concentration of 31 percent by weight separated by the washing and absorbing process into the first-stage water washing process, condensing the dilute hydrochloric acid separated by the first-stage water washing into the hydrolysis reaction by using chilled water with the concentration of below-15 ℃ when the concentration of the concentrated hydrochloric acid separated by the washing and absorbing process is 22-31 percent by weight, and recycling the dilute hydrochloric acid separated by the first-stage water washing into the hydrolysis reaction.
The embodiment 3 not only can carry out high-efficiency water washing and dechlorination on the dimethyl dichlorosilane monomer, effectively control the viscosity of the dimethyl polysiloxane and improve the recovery rate of hydrogen chloride, but also has better dechlorination effect, and the recovery rate of the hydrogen chloride can reach more than 102 percent; on the premise of effectively ensuring the concentration of water washing acid, the balance of the water supplementing amount and the water consumption of the system can be maintained, and the water washing and desorption of the dimethyl dichlorosilane hydrolysate can be realized, so that the product quality of the dimethyl dichlorosilane is greatly improved, and the finally obtained dimethyl dichlorosiloxane has the viscosity of 25Cp and the chlorine content of 8ppmwt; in addition, the whole process has no acid water discharge phenomenon, effectively saves the cost of wastewater treatment, and can generate better economic benefit.
Claims (4)
1. A stable control dimethyl dichlorosilane hydrolysis process is characterized by comprising the following steps:
s1: carrying out hydrolysis reaction on a dimethyl dichlorosilane monomer and concentrated hydrochloric acid with the concentration of 40-47% by weight in a hydrolysis system, wherein the volume ratio of the dimethyl dichlorosilane monomer to the hydrochloric acid is 1:15-20, and introducing hydrogen chloride gas generated by the hydrolysis reaction into a purification system for purification treatment;
s2: degassing and separating the dimethyl dichlorosilane hydrolysate generated by the hydrolysis reaction in a degassing system;
s3: washing and absorbing the degassed and separated hydrogen chloride gas in an absorption tower by utilizing dilute hydrochloric acid, and neutralizing tail gas obtained by washing and absorbing by an alkaline washing system;
s4: sequentially performing primary water washing and secondary water washing on the degassed and separated dimethyl dichlorosilane hydrolysate by dilute hydrochloric acid, and then performing tertiary water washing by desalted water to obtain the dimethyl dichlorosilane hydrolysate; in the primary water washing process, the concentration of the dilute hydrochloric acid is 29-33%wt, and the volume ratio of the dimethyl dichlorosilane hydrolysate to the dilute hydrochloric acid is 1:4-10; the concentration of the dilute hydrochloric acid in the secondary water washing process is 3-8%wt, the volume ratio of the dimethyl dichlorosilane hydrolysate to the dilute hydrochloric acid is 1:4-10, the concentration of the dilute hydrochloric acid in the tertiary water washing process is 0.02-0.2%wt, and the volume ratio of the dimethyl dichlorosilane hydrolysate to the desalted water is 1:4-10;
s5, recycling dilute hydrochloric acid separated by three-stage washing into a second-stage washing process, recycling dilute hydrochloric acid separated by the second-stage washing into a washing and absorbing process, recycling concentrated hydrochloric acid with concentration of 22-31% wt separated after washing and absorbing into a first-stage washing process, wherein the washing and absorbing process is required to be condensed by utilizing chilled water with the temperature below-15 ℃; the dilute hydrochloric acid separated by the primary water washing is recycled to the hydrolysis reaction, and a fresh hydrochloric acid inlet is also arranged in the primary water washing procedure and is used for timely supplementing the fresh hydrochloric acid with the concentration of 31%wt so as to maintain the balance of the system.
2. A process for the hydrolysis of a stably controlled dimethyldichlorosilane according to claim 1 wherein: in the step S1, the working pressure of the hydrolysis reaction is 0.18-0.30 MPa, and the working temperature is 20-50 ℃.
3. A process for the hydrolysis of a stably controlled dimethyldichlorosilane according to claim 1 wherein: in the step S2, the working pressure of the degassing separation is 0.05-0.08 MPa.
4. A process for the hydrolysis of a stably controlled dimethyldichlorosilane according to claim 1 wherein: in the step S4, the working temperature of the primary water washing process is controlled to be 20-30 ℃, and the working temperatures of the secondary water washing process and the tertiary water washing process are controlled to be 80-90 ℃.
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| CN202210595300.3A CN114989435B (en) | 2022-05-29 | 2022-05-29 | Stable control dimethyl dichlorosilane hydrolysis process |
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| CN101982485B (en) * | 2010-10-19 | 2012-11-21 | 江苏宏达新材料股份有限公司 | Method for hydrolyzing dimethyldichlorosilane in saturated acid |
| CN103183827B (en) * | 2013-03-28 | 2015-08-19 | 青岛科技大学 | A kind of organochlorosilane continuous print Concentrated acid hydrolysis method |
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