CN116239629A - High-purity 1, 3-tetramethyl disiloxane and preparation method thereof - Google Patents
High-purity 1, 3-tetramethyl disiloxane and preparation method thereof Download PDFInfo
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- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
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- 238000000998 batch distillation Methods 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims description 4
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- 238000002156 mixing Methods 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
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- 230000008901 benefit Effects 0.000 abstract description 5
- 239000010808 liquid waste Substances 0.000 abstract description 3
- 239000002210 silicon-based material Substances 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 11
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- 239000000047 product Substances 0.000 description 8
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 4
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- 229920002545 silicone oil Polymers 0.000 description 4
- 230000032798 delamination Effects 0.000 description 3
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 3
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 description 3
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- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical class C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 2
- 238000007323 disproportionation reaction Methods 0.000 description 2
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- 239000012280 lithium aluminium hydride Substances 0.000 description 2
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- 239000002841 Lewis acid Substances 0.000 description 1
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- QFLLWLFOOHGSBE-UHFFFAOYSA-N dichloro-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(Cl)Cl QFLLWLFOOHGSBE-UHFFFAOYSA-N 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 150000008282 halocarbons Chemical class 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- CCERQOYLJJULMD-UHFFFAOYSA-M magnesium;carbanide;chloride Chemical compound [CH3-].[Mg+2].[Cl-] CCERQOYLJJULMD-UHFFFAOYSA-M 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 229940050176 methyl chloride Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 150000001367 organochlorosilanes Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003304 ruthenium compounds Chemical class 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
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- 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
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0838—Compounds with one or more Si-O-Si sequences
- C07F7/0872—Preparation and treatment thereof
- C07F7/0874—Reactions involving a bond of the Si-O-Si linkage
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- 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
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0838—Compounds with one or more Si-O-Si sequences
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- 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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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to the technical field of organic silicon materials, in particular to high-purity 1, 3-tetramethyl disiloxane and a preparation method thereof. The invention has simple process, makes full use of the low-boiling-point substances of the organosilicon chlorosilane, reduces the danger of the organosilicon chlorosilane as liquid waste, converts the low-boiling-point substances into products with higher side value, and increases the economic benefit.
Description
Technical Field
The invention relates to the technical field of organic silicon materials, in particular to high-purity 1, 3-tetramethyl disiloxane and a preparation method thereof.
Background
Tetramethyl disiloxane, also called as hydrogen-containing double-end socket, can introduce various organic groups on polysiloxane molecular chain through hydrosilation reaction by utilizing Si-H bond on the end group, so that the hydrogen-containing polysiloxane has important application in synthesis of plastics, resin modification, silicone oil modification, cross-linking agent of liquid silicone rubber, special organic silicon surfactant and dendritic polymer.
At present, there are few reports on the synthesis of 1, 3-tetramethyl disiloxane in China, and 3 main synthesis methods in China exist, (1) a direct method is disclosed in EP348902B (CameronRA, lewisKM, kannerB, etal.DirectSynthesisProcessforOrganohalohydrosilanes: 1990-01-03.) for preparing organohalohydrosilane, and a direct synthesis method for selectively producing organohalohydrosilane at a high rate, high selectivity and high conversion rate by catalytic reaction of a mixture of active silicon with an organohalide and hydrogen under a controlled concentration of selected metal atoms; (2) Grignard method: JPH0656852 (KubotaT, endoM, yamamotoA, etal.ProductionofDimethylchlorosilane:1994-03-01) discloses a process for preparing dimethylsilane gas from dimethylsilane and dimethyldichlorosilane by injecting the dichlorosilane into a methylmagnesium chloride solution prepared from methylchloride and magnesium in a Grignard reactor. In a disproportionation reactor, continuously performing disproportionation reaction on dimethyl silane gas and dimethyl dichlorosilane to obtain a target compound; (3) reduction method: EP0476597B (TakagoT, kishitaH, fujiiH.ProcessforPreparing1,1, 3-tetramethyl 1,3Disiloxane: 1992-03-25.) discloses a process for the preparation of 1, 3-tetramethyl 1, 3-disiloxane comprising the step of reducing 1, 3-tetramethyl, 3-dichloro, 3-disiloxane by using a metal hydride such as lithium aluminum hydride, sodium aluminum hydride or the like. Excessive hydrogen and chloromethane exist in the direct method reaction tail gas, so that the direct method reaction tail gas is difficult to compress and separate; the main raw material adopted by the Grignard method is dichlorosilane, the raw material is not easy to purchase, and the synthesis cost is high; the reduction method adopts dimethyl dichlorosilane and cyclic or linear polydimethylsiloxane as raw materials, and adopts Lewis acid telogenic or hydrolytic means to mainly obtain the product above the chlorine-terminated dimethylsiloxane trimer, and the yield of the intermediate dichloro tetramethyl disiloxane is only 30%. In addition, the expensive lithium aluminum hydride is mainly selected as a reducing agent in the literature, so that the cost is too high, and the industrialization is not facilitated.
The main synthesis method in China is 2, and (1) 1, 3-tetramethyl disiloxane, acetylene and promoter amine compounds are reacted with a reaction system formed by a catalyst ruthenium compound to prepare 1, 3-divinyl-1, 3-tetramethyl disiloxane. The preparation method can realize that 1, 3-tetramethyl disiloxane and acetylene react to generate 1, 3-divinyl-1, 3-tetramethyl disiloxane in one step under mild conditions, and has the advantages of less side reaction, high yield of main products, low cost and high safety, and is suitable for industrial production, but because the use of more control points of the process, the chemical industry of raw materials is high in risk, the safety risk in production is high, and the purity is low; (2) The method adopts organochlorosilane low-boiling-point substances and alcohol compounds with boiling points less than 40 ℃ as raw materials, the low-boiling-point substances and the alcohol compounds are added according to a specific proportion, the materials are subjected to alcoholysis, hydrolysis, standing and acid water removal, drying and filtering, the filtered hydrolysate is rectified, distillate with the temperature of 70 ℃ to 71 ℃ at the top of the tower is extracted, and the product 1, 3-tetramethyl disiloxane is obtained. However, as the technology adopts an alcoholysis process, the cost of raw materials for industrial production is high, the purity of the obtained product is slightly low, hazardous waste is generated, and the process continuity is low.
Thus, in the byproducts of the direct process synthesis of methylchlorosilanes, 1% to 2% of a series of compounds having a boiling point below 40 ℃ are contained. With the rapid increase in the capacity and yield of methylchlorosilanes, the relative amount of low boilers is also rapidly increasing. The organosilicon is low-boiling, not easy to store, and the low-boiling substances can not be recycled, and the treatment method is mainly to treat the organosilicon by burning or selling and subsidizing the organosilicon at low cost to qualified units, so the low-boiling utilization is essential.
In order to effectively solve the problem of low-cost sales of byproducts, the method solves the problem of the expansion of the production scale of the monomers, is also an unavoidable trend of sustainable development, and generates new economic benefits by preparing1, 3-tetramethyl disiloxane through the hydrolysis of low-boiling-point substances, thereby having certain significance for the improvement of organosilicon technology, leading industry, safety production and environmental protection.
Disclosure of Invention
The invention provides high-purity 1, 3-tetramethyl disiloxane and a preparation method thereof, overcomes the defects of the prior art, and can effectively solve the problem that low-boiling-point substances, which are byproducts of organosilicon monomer production, are not easy to be converted into high-added-value products in the conventional preparation of 1, 3-tetramethyl disiloxane by hydrolyzing organosilicon chlorosilane low-boiling-point substances.
One of the technical schemes of the invention is realized by the following measures: the preparation method of the high-purity 1, 3-tetramethyl disiloxane comprises the following steps: firstly, mixing a required amount of organosilicon low-boiling-point substances with main components of dimethyl hydrogen-containing monochlorosilane with water for hydrolysis reaction to obtain hydrolysate crude oil containing 1, 3-tetramethyl disiloxane; step two, oleic acid separation is carried out on hydrolysate crude oil containing 1, 3-tetramethyl disiloxane, and the separated acid-containing crude oil is subjected to primary water washing to obtain 1, 3-tetramethyl disiloxane low boiling water oil decomposition; thirdly, washing the low-boiling hydrolysis oil of the 1, 3-tetramethyl disiloxane by secondary water, performing primary normal pressure batch distillation, and extracting tower top fraction of the primary normal pressure distillation tower; and fourthly, performing tertiary water washing on the extracted tower top fraction of the primary normal pressure rectifying tower, performing secondary normal pressure batch rectification, and extracting the tower top fraction of the secondary normal pressure rectifying tower to obtain the high-purity 1, 3-tetramethyl disiloxane.
The following are further optimizations and/or improvements to one of the above-described inventive solutions:
in the first step, the mass ratio of water to dimethyl hydrogen-containing monochlorosilane is 2:1 during the hydrolysis reaction, and the hydrolysis reaction temperature is 8-10 ℃.
In the first step, the mass content of the dimethyl hydrogen-containing monochlorosilane in the organic silicon low-boiling-point substance with the main component of the dimethyl hydrogen-containing monochlorosilane is higher than 50%, and the mass content of the 1, 3-tetramethyl disiloxane in the hydrolysate crude oil containing the 1, 3-tetramethyl disiloxane is 20-40%.
In the third step, the overhead fraction of the first-stage atmospheric rectification tower is a fraction at 64-80 ℃, and the mass content of 1, 3-tetramethyl disiloxane in the extracted fraction is higher than 85%.
In the fourth step, the overhead fraction of the secondary rectifying tower is a fraction at 70-71 ℃, and the mass content of 1, 3-tetramethyl disiloxane in the extracted fraction is higher than 99.5%.
When the primary water washing, the secondary water washing and the tertiary water washing are carried out, the water-oil ratio is 1:1.
In the first step, the boiling point of the organic silicon low-boiling-point substance is lower than 40 ℃, and in the organic silicon low-boiling-point substance, the mass content of the monomethyl hydrogen-containing monochlorosilane is lower than 3%, and the mass content of hydrocarbons is lower than 30%.
The second technical scheme of the invention is realized by the following measures: a high purity 1, 3-tetramethyldisiloxane obtained according to a process for preparing a high purity 1, 3-tetramethyldisiloxane.
The invention has the following excellent effects:
1. the invention uses the organosilicon chlorosilane low-boiling-point substances as raw materials, reduces the synthesis cost of 1, 3-tetramethyl disiloxane in actual production, has simple process, solves the technical problem that the byproduct low-boiling-point substances produced by organosilicon monomers are converted into high-added-value products, belongs to waste utilization, increases the high-value economic benefit of the byproduct, and is environment-friendly and low in comprehensive cost;
2. in the preparation method, the bottom liquid of the rectifying tower is used for preparing hydrogen-containing silicone oil;
3. the organosilicon chlorosilane low-boiling-point substances are fully utilized, and the danger of the organosilicon chlorosilane low-boiling-point substances serving as liquid wastes is reduced; the low boiling component contains relatively more chain hydrocarbon, has low flash point, is easy to burn and is more dangerous. The low-boiling-point substances are converted into products with higher added values, and a new idea for treating the low-boiling-point wastes is provided.
The purity of the high-purity 1, 3-tetramethyl disiloxane prepared by the method is more than or equal to 99.5%, the viscosity range is 2cs to 2.5cs, and the yield can reach 92%.
Drawings
FIG. 1 is a liquid chromatogram of an organosilicon low-boiling-point substance of dimethyl hydrogen-containing monochlorosilane.
FIG. 2 is a liquid chromatogram of high purity 1, 3-tetramethyldisiloxane of the present invention.
FIG. 3 is a flow chart of the hydrolysis process of the organosilicon low-boiling-point substance with the main component of dimethyl hydrogen-containing monochlorosilane.
FIG. 4 is a flow chart of the primary normal pressure rectification and the secondary normal pressure rectification in the invention.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments can be determined according to the technical scheme and practical situations of the present invention. The various chemical reagents and chemicals mentioned in the present invention are all commonly known in the art unless specifically stated otherwise.
The invention is further described below with reference to examples:
example 1: the preparation method of the high-purity 1, 3-tetramethyl disiloxane comprises the following steps: firstly, mixing a required amount of organosilicon low-boiling-point substances with main components of dimethyl hydrogen-containing monochlorosilane with water for hydrolysis reaction to obtain hydrolysate crude oil containing 1, 3-tetramethyl disiloxane; step two, oleic acid separation is carried out on hydrolysate crude oil containing 1, 3-tetramethyl disiloxane, and the separated acid-containing crude oil is subjected to primary water washing to obtain 1, 3-tetramethyl disiloxane low boiling water oil decomposition; thirdly, washing the low-boiling hydrolysis oil of the 1, 3-tetramethyl disiloxane by secondary water, performing primary normal pressure batch distillation, and extracting tower top fraction of the primary normal pressure distillation tower; and fourthly, performing tertiary water washing on the extracted tower top fraction of the primary normal pressure rectifying tower, performing secondary normal pressure batch rectification, and extracting the tower top fraction of the secondary normal pressure rectifying tower to obtain the high-purity 1, 3-tetramethyl disiloxane.
Example 2: as the optimization of the above examples, in the first step, the mass ratio of water to dimethyl hydrogen-containing monochlorosilane is 2:1, and the hydrolysis reaction temperature is 8-10 ℃.
Example 3: as the optimization of the above examples, in the first step, the mass content of dimethyl hydrogen-containing monochlorosilane in the organosilicon low-boiling residue with the main component of dimethyl hydrogen-containing monochlorosilane is higher than 50%, and the mass content of 1, 3-tetramethyl disiloxane in the hydrolysate crude oil containing 1, 3-tetramethyl disiloxane is 20-40%.
Example 4: as an optimization of the above examples, in the third step, the overhead fraction of the first-stage atmospheric distillation column is a fraction of 64 ℃ to 80 ℃ and the mass content of 1, 3-tetramethyldisiloxane in the extracted fraction is higher than 85%.
Example 5: as an optimization of the above examples, in the fourth step, the overhead fraction of the secondary rectifying column was extracted as a fraction of 70 ℃ to 71 ℃ and the mass content of 1, 3-tetramethyldisiloxane in the extracted fraction was higher than 99.5%.
Example 6: as optimization of the embodiment, the water-oil ratio is 1:1 when the primary water washing, the secondary water washing and the tertiary water washing are carried out.
In the invention, after the low-boiling hydrolysis oil of 1, 3-tetramethyl disiloxane is subjected to secondary water washing, the acid value is reduced to be less than 15ppm.
Example 7: as the optimization of the embodiment, in the first step, the boiling point of the organic silicon low-boiling-point substance is lower than 40 ℃, and the mass content of the monomethyl hydrogen-containing monochlorosilane in the organic silicon low-boiling-point substance is lower than 3%, and the mass content of hydrocarbons is lower than 30%.
Example 8: the high-purity 1, 3-tetramethyl disiloxane obtained according to the method for preparing high-purity 1, 3-tetramethyl disiloxane.
Example 9: the preparation method of the high-purity 1, 3-tetramethyl disiloxane comprises the following steps: firstly, mixing the needed amount of organic silicon low-boiling-point substances with the main component of dimethyl hydrogen-containing monochlorosilane with water for hydrolysis reaction to obtain hydrolysate crude oil containing 1, 3-tetramethyl disiloxane (specifically, the process comprises the steps that the organic silicon low-boiling-point substances and the process water are respectively fed into a hydrolysis loop, the organic silicon low-boiling-point substances and the process water are completely mixed in the hydrolysis loop through a hydrolysis loop static mixer, the loop temperature is controlled to be 8-10 ℃ through a low-boiling circulation cooler, and the hydrolysate crude oil containing the 1, 3-tetramethyl disiloxane is separated from the top of the loop and fed into an acid separation system); secondly, oleic acid separation is carried out on hydrolysate crude oil containing 1, 3-tetramethyl disiloxane, and the separated acid-containing crude oil is subjected to primary water washing to obtain 1, 3-tetramethyl disiloxane low boiling water oil decomposition (the specific process is as follows: separating the crude acid-containing crude oil (light layer) and dilute hydrochloric acid (heavy layer) from the crude 1, 3-tetramethyl disiloxane-containing hydrolysate oil of the reaction loop by a low boiling water decomposition separator, wherein the crude acid-containing oil at the top part contains a small amount of HCl gas, the dilute hydrochloric acid at the bottom part is discharged into a dilute acid tank, the dilute hydrochloric acid is sent out periodically, the crude acid-containing oil at the top part enters a water washing layering system for primary water washing, the oil from the top of the low boiling water decomposition and delamination device enters a low boiling oil water washing kettle, the process water is used for fully washing the oil in the water washing kettle, the low boiling water decomposition oil of the 1, 3-tetramethyl disiloxane overflows from the bottom of the water washing kettle to the low boiling oil water washing and delamination device for delamination again, and the low boiling water decomposition oil of the 1, 3-tetramethyl disiloxane at the top enters a low boiling oil intermediate tank); thirdly, washing the low-boiling hydrolysis oil of the 1, 3-tetramethyl disiloxane by secondary water, performing primary normal pressure batch distillation, and extracting the overhead fraction of the primary normal pressure distillation tower (the specific process is as follows: the low-boiling hydrolysis oil of the 1, 3-tetramethyl disiloxane after the first-stage water washing and layering enters a water washing system of a second-stage water washing kettle, after the self process water circulation and the continuous washing of fresh process water, the hydrolysis oil enters a second-stage water washing and layering device for oil-water separation, the separated hydrolysis oil is quantitatively conveyed to a No. 1 rectifying tower kettle of a first-stage normal pressure rectifying tower through a pump, steam of 0.5MPa is used for heating, preliminary low-temperature distillation is carried out, the fraction at the 64 ℃ to 80 ℃ of the top of an extraction tower enters a third-stage water washing system, the rest temperature sections are that the fraction at the top of the tower is less than 40 ℃ for incineration treatment, the fraction at the top of the tower is more than 80 ℃ is returned to the system for continuously extracting the 1, 3-tetramethyl disiloxane, and the bottom kettle liquid is used for preparing hydrogen-containing silicone oil); and fourthly, performing tertiary water washing on the extracted tower top fraction of the primary normal pressure rectifying tower, performing secondary normal pressure batch rectification, and extracting the tower top fraction of the secondary normal pressure rectifying tower to obtain the high-purity 1, 3-tetramethyl disiloxane. ( The specific process is as follows: the fraction at 64-80 ℃ at the top of the primary normal pressure rectifying tower enters a three-stage water washing system, is continuously washed by self process water circulation and fresh process water, enters a three-stage water washing layering device for oil-water separation, is quantitatively conveyed to a secondary normal pressure batch rectifying tower kettle by a pump from 64-80 ℃ at the top of the primary normal pressure rectifying tower after the completion of three-stage water washing, is heated by using 0.5MPa steam, and is extracted to obtain the fraction at 70-71 ℃ at the top of the tower, namely the 1, 3-tetramethyl disiloxane with the content of 99.5%, wherein the rest temperature sections are as follows: the fraction with the temperature of the top of the tower being less than 70 ℃ is recovered and re-extracted, and the fraction with the temperature of the top of the tower being more than 71 ℃ and the bottom of the tower are partially recovered and re-used, and the fraction is partially used for preparing hydrogen-containing silicone oil. )
In the embodiment 9 of the invention, the flow rate of the organosilicon low-boiling-point substances entering a hydrolysis loop is controlled to be 250Kg/h to 600Kg/h, the hydrolysis process adopts a loop forward hydrolysis process, the primary normal pressure rectification and the secondary normal pressure rectification are both carried out by adopting a normal pressure batch rectification process, and the purity of the obtained high-purity 1, 3-tetramethyl disiloxane is 99.5%.
In the embodiment 9 of the invention, the organosilicon low-boiling-point substance of the raw material dimethyl hydrogen-containing monochlorosilane is a byproduct in the synthesis of organosilicon monomers from organosilicon factories in the silicon industry, and the liquid chromatogram and the main components are shown in figure 1; the liquid chromatogram of the obtained high-purity 1, 3-tetramethyl disiloxane and the main components thereof are shown in figure 2; the flow chart of the hydrolysis process of the organosilicon low-boiling-point substance of the dimethyl hydrogen-containing monochlorosilane is shown in figure 3, wherein M2H in figure 3 is the dimethyl hydrogen-containing monochlorosilane; the flow chart of the primary normal pressure rectification and the secondary normal pressure rectification is shown in figure 4, and the double seal heads in figure 4 are 1, 3-tetramethyl disiloxane.
In summary, the invention has simple process, makes full use of the low-boiling-point substances of the organosilicon chlorosilane, reduces the risk of the low-boiling-point substances as liquid wastes, converts the low-boiling-point substances into products with higher side values, and increases the economic benefit.
The technical characteristics form the embodiment of the invention, have stronger adaptability and implementation effect, and can increase or decrease unnecessary technical characteristics according to actual needs so as to meet the requirements of different situations.
Claims (8)
1. The preparation method of the high-purity 1, 3-tetramethyl disiloxane is characterized by comprising the following steps: firstly, mixing a required amount of organosilicon low-boiling-point substances with main components of dimethyl hydrogen-containing monochlorosilane with water for hydrolysis reaction to obtain hydrolysate crude oil containing 1, 3-tetramethyl disiloxane; step two, oleic acid separation is carried out on hydrolysate crude oil containing 1, 3-tetramethyl disiloxane, and the separated acid-containing crude oil is subjected to primary water washing to obtain 1, 3-tetramethyl disiloxane low boiling water oil decomposition; thirdly, washing the low-boiling hydrolysis oil of the 1, 3-tetramethyl disiloxane by secondary water, performing primary normal pressure batch distillation, and extracting tower top fraction of the primary normal pressure distillation tower; and fourthly, performing tertiary water washing on the extracted tower top fraction of the primary normal pressure rectifying tower, performing secondary normal pressure batch rectification, and extracting the tower top fraction of the secondary normal pressure rectifying tower to obtain the high-purity 1, 3-tetramethyl disiloxane.
2. The process for producing high-purity 1, 3-tetramethyldisiloxane according to claim 1, wherein in the first step, the mass ratio of water to dimethylhydrogen-containing monochlorosilane is 2:1 and the hydrolysis reaction temperature is 8℃to 10 ℃.
3. The process for producing high-purity 1, 3-tetramethyldisiloxane according to claim 1 or 2, wherein in the first step, in the organosilicon low-boiling substance whose main component is dimethylhydrogen-containing monochlorosilane, the mass content of the dimethyl hydrogen-containing monochlorosilane is higher than 50%, and the mass content of the 1, 3-tetramethyl disiloxane in the obtained hydrolysate crude oil containing the 1, 3-tetramethyl disiloxane is 20-40%.
4. A process for the preparation of high purity 1, 3-tetramethyldisiloxane according to claim 1 or 2 or 3, characterized in that in the third step the overhead fraction of the first atmospheric distillation column is extracted as a fraction from 64 ℃ to 80 ℃ and the mass content of 1, 3-tetramethyldisiloxane in the extracted fraction is higher than 85%.
5. The process for producing high purity 1, 3-tetramethyldisiloxane according to any one of claims 1 to 4, characterized in that in the fourth step, the overhead fraction of the secondary rectifying column is extracted as a fraction from 70 ℃ to 71 ℃ and the mass content of 1, 3-tetramethyldisiloxane in the extracted fraction is higher than 99.5%.
6. The method for producing high purity 1, 3-tetramethyldisiloxane according to any one of claims 1 to 5, wherein the water-oil ratio is 1:1 when the primary water washing, the secondary water washing and the tertiary water washing are carried out.
7. The process for producing high-purity 1, 3-tetramethyldisiloxane according to any one of claims 1 to 6, wherein in the first step, the boiling point of the low-boiling point organosilicon compound is less than 40 ℃, and the mass content of the monomethyl hydrogen-containing monochlorosilane in the low-boiling point organosilicon compound is less than 3% and the mass content of the hydrocarbon is less than 30%.
8. A high purity 1, 3-tetramethyldisiloxane obtained by the production process according to any one of claims 1 to 7.
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