CN110818735B - Method for preparing 1,1,3, 3-tetramethyldisiloxane - Google Patents
Method for preparing 1,1,3, 3-tetramethyldisiloxane Download PDFInfo
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- KWEKXPWNFQBJAY-UHFFFAOYSA-N (dimethyl-$l^{3}-silanyl)oxy-dimethylsilicon Chemical compound C[Si](C)O[Si](C)C KWEKXPWNFQBJAY-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 82
- 239000000126 substance Substances 0.000 claims abstract description 59
- 238000009835 boiling Methods 0.000 claims abstract description 32
- -1 methyl hydrogen Chemical class 0.000 claims abstract description 21
- 238000006136 alcoholysis reaction Methods 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 13
- 230000007062 hydrolysis Effects 0.000 claims abstract description 9
- 239000000413 hydrolysate Substances 0.000 claims abstract 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 28
- 239000005046 Chlorosilane Substances 0.000 claims description 27
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 27
- 230000003472 neutralizing effect Effects 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000003921 oil Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 15
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 14
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 9
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 claims description 3
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005052 trichlorosilane Substances 0.000 claims description 3
- KTQYJQFGNYHXMB-UHFFFAOYSA-N dichloro(methyl)silicon Chemical compound C[Si](Cl)Cl KTQYJQFGNYHXMB-UHFFFAOYSA-N 0.000 claims description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims 1
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims 1
- 125000002723 alicyclic group Chemical group 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 29
- 239000002253 acid Substances 0.000 abstract description 25
- 239000000047 product Substances 0.000 abstract description 6
- 150000001298 alcohols Chemical class 0.000 abstract description 4
- 229920001296 polysiloxane Polymers 0.000 abstract description 4
- 229920002545 silicone oil Polymers 0.000 abstract description 3
- 150000001367 organochlorosilanes Chemical class 0.000 abstract description 2
- 229920002379 silicone rubber Polymers 0.000 abstract description 2
- 239000000654 additive Substances 0.000 abstract 1
- 239000004945 silicone rubber Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 28
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 26
- 239000007789 gas Substances 0.000 description 17
- 238000010521 absorption reaction Methods 0.000 description 12
- 238000007599 discharging Methods 0.000 description 12
- 239000011521 glass Substances 0.000 description 12
- 238000005303 weighing Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 5
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect 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
- 238000007323 disproportionation reaction Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 2
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000012280 lithium aluminium hydride Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 1
- 230000027311 M phase Effects 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000000412 dendrimer Substances 0.000 description 1
- 229920000736 dendritic polymer Polymers 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- QFLLWLFOOHGSBE-UHFFFAOYSA-N dichloro-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(Cl)Cl QFLLWLFOOHGSBE-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- CCERQOYLJJULMD-UHFFFAOYSA-M magnesium;carbanide;chloride Chemical compound [CH3-].[Mg+2].[Cl-] CCERQOYLJJULMD-UHFFFAOYSA-M 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 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
- 238000006386 neutralization reaction Methods 0.000 description 1
- 125000000962 organic group Chemical group 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
- 238000007670 refining Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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Classifications
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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
- C07F7/0896—Compounds with a Si-H linkage
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention relates to a preparation method of high-purity 1,1,3, 3-tetramethyldisiloxane. The method adopts organochlorosilane low-boiling-point substances with the boiling point of less than 40 ℃ and alcohol compounds as raw materials, the low-boiling-point substances and the alcohol compounds are fed according to a specific ratio, subjected to alcoholysis and hydrolysis, kept stand to remove acid water, dried and filtered, the filtered hydrolysate is rectified, distillate at the temperature of 70-71 ℃ at the top of a tower is extracted, and the product 1,1,3, 3-tetramethyldisiloxane with the purity of more than or equal to 98.5 percent is obtained. The 1,1,3, 3-tetramethyl disiloxane can be used as raw materials for the production of addition type silicone rubber, silicone gel, methyl hydrogen silicone oil (SiH bond is more than 3) and other special additives.
Description
Technical Field
The invention relates to the technical field of chemical industry, belongs to the technical field of organic silicon materials, and particularly relates to a preparation method for synthesizing 1,1,3, 3-tetramethyldisiloxane from low-boiling-point organic chlorosilane.
Background
1,1,3, 3-tetramethyl disiloxane, also known as hydrogen-containing double-end socket, can introduce various organic groups on a polysiloxane molecular chain by utilizing SiH bonds on the end group of the 1,1,3, 3-tetramethyl disiloxane through hydrosilation reaction, so that the hydrogen-end polysiloxane has important application in synthesis of plastics, resin modification, silicone oil modification, cross-linking agents of liquid silicone rubber, special organic silicon surfactants and dendritic polymers.
At present, there are few reports on the Synthesis of 1,1,3, 3-tetramethyldisiloxane at home and 3 major Synthesis methods at abroad (1) direct method EP348902B (Cameron R A, Lewis K M, Kanner B, et al direct Synthesis Process for Organohalohydrosilanes:1990-01-03.) discloses a direct Synthesis method for producing Organohalohydrosilanes, in which a mixture of active silicon, organohalides and hydrogen is subjected to a catalytic reaction under the condition that the concentration of a selected metal atom is controlled, thereby selectively producing Organohalohydrosilanes at a high rate, a high selectivity and a high conversion rate. (2) A Grignard method: JPH0656852(Kubota T, Endo M, Yamamoto A, et al.production of dimethyl chlorosilane:1994-03-01) discloses a process for the production of dimethylsilane gas from dimethylsilane and dimethyldichlorosilane by injecting the dichlorosilane into a solution of methyl magnesium chloride prepared from methyl chloride and magnesium in a Grignard reactor. In a disproportionation reactor, continuously carrying out disproportionation reaction on dimethyl silane gas and dimethyl dichlorosilane to obtain a target compound. (3) A reduction method: EP0476597B (Takago T, Kishita H, Fujii H. Process for Preparing 1,1,3, 3-tetramethyl 1,3 Disiloxanes: 1992-03-25.) discloses a process for Preparing 1,1,3, 3-tetramethyl 1, 3-Disiloxane comprising the step of reducing 1,1,3, 3-tetramethyl, 3-dichloro, 3-Disiloxane by using a metal hydride such as lithium aluminum hydride, sodium aluminum hydride, etc.; the process described is very economically advantageous and in significantly high yields.
In the above synthesis method, the direct process reaction tail gas contains excessive hydrogen and chloromethane, which are difficult to compress and separate; the main raw material adopted by the Grignard method is dihydrodichlorosilane, so that the raw material is not easy to purchase and the synthesis cost is high; the reduction method adopts dimethyldichlorosilane and cyclic or linear polydimethylsiloxane as raw materials, and mainly obtains products of dimethyl siloxane tripolymer of chlorine end capping by means of Lewis acid telomerization or hydrolysis, while the yield of intermediate dichlorotetramethyldisiloxane 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 by-product obtained by synthesizing methyl chlorosilane by a direct method contains 1-2% of a series of compounds with boiling points lower than 40 ℃. With the rapid increase in the production capacity and yield of methylchlorosilanes, the absolute amount of low boilers is also rapidly increasing. The organosilicon low-boiling mainly contains methyl-rich tetramethylsilane (the content is more than 30 percent) and dimethylchlorosilane (the content is about 20 percent), is not easy to store, and low-boiling residues can not be recycled, and the treatment method mainly comprises the step of treating the low-boiling residues by burning or selling at low price and subsiding to qualified units. At present, the capacity of an incineration device is limited, and more organosilicon low-boiling-point substances are easily produced to block a warehouse and face production stoppage, so that the low-boiling-point utilization is imperatively sought.
In order to effectively solve the problem of low-cost sale of byproducts, remove the worries about expanding the production scale of monomers and simultaneously be the indispensable trend of sustainable development, the 1,1,3, 3-tetramethyldisiloxane is prepared by hydrolyzing low-boiling-point substances to generate new economic benefits, and the method has certain significance for the technical progress of organic silicon, leading industry, safe production and environmental protection.
In view of the above-mentioned disadvantages of the prior art, there is also a need for a better method for treating low boiling components in the production of organosilicon monomers, and a safer, environmentally friendly and low-cost method for producing 1,1,3, 3-tetramethyldisiloxane is desired.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing 1,1,3, 3-tetramethyldisiloxane, which has mild reaction conditions and simple reaction process, and the method synthesizes the 1,1,3, 3-tetramethyldisiloxane by using low-boiling-point substances generated in the production process of organosilicon monomers and through steps of alcoholysis, hydrolysis and rectification.
According to the invention, the low-boiling substances are a mixture of low-boiling substances removed during the production of the organosilicon monomers, the boiling range of the collected low-boiling substances is less than 40 ℃, and the low-boiling substances mainly contain SiM 4 30-50%,HSiCl 3 Less than 2%, M 2 15-45% of H, less than 10% of MH, less than 20% of hydrocarbon and the like.
The organosilicon monomer low-boiling-point substance can be obtained from any known organosilicon monomer production process, and the specific composition of the obtained organosilicon low-boiling-point substance can be changed due to the change of reaction conditions, raw materials and the like in different production processes, but the organosilicon low-boiling-point substance contains organosilicon chlorosilane low-boiling-point substances with higher proportion in general and can be used in the synthesis method of the invention. In contrast, the higher the content of dimethylhydrochlorosilane in the organosilicon chlorosilane low-boiling components, the higher the yield of 1,1,3, 3-tetramethyldisiloxane produced by the method is. In one embodiment of the invention, typical components and percentages of the low boilers of the organosilicon chlorosilanes can be as follows, for example:
in the above table: SiM 4 Is tetramethylsilicon, HSiCl 3 Is trichlorosilane, M 2 H is dimethyl hydrogen chlorosilane, and MH is methyl hydrogen dichlorosilane.
In the method for preparing 1,1,3, 3-tetramethyl disiloxane by using organosilicon monomer low-boiling residues, because the difference of the boiling points of all substances in the low-boiling residues is less than 10 ℃, the compounds are difficult to separate by direct normal-pressure rectification, in addition, the direct low-boiling residues contain more trifunctional group substances, more cross-linked substances are generated during hydrolysis, equipment is easy to block, and the yield is generally less than 50%; the inventor finds that trifunctional materials such as trichlorosilane and methylhydrodichlorosilane in low-boiling substances can be removed through alcoholysis, the purity of dimethylhydrochlorosilane is improved, the yield is more than 85 percent, and the preparation for 1,1,3, 3-tetramethyldisiloxane is provided.
Further, the invention provides a method for preparing 1,1,3, 3-tetramethyldisiloxane by taking organosilicon chlorosilane low-boiling-point substances as raw materials, which comprises the following steps:
(1) alcoholysis step: dropwise adding an alcohol compound into the organosilicon chlorosilane low-boiling-point substance for alcoholysis reaction, rapidly heating, and rectifying to extract a fraction with the temperature of less than 40 ℃;
(2) a hydrolysis step: dropwise adding the fractions into water for hydrolysis, balancing after dropwise adding, layering oil and water after standing, collecting an upper oil phase, drying, neutralizing and filtering;
(3) a rectification step: rectifying the hydrolysate, and receiving distillate at the temperature of 70-71 ℃ at the top of the tower, namely 1,1,3, 3-tetramethyldisiloxane;
according to the invention, the preferable dropping flow rate in the step (1) is 250 g/h-300 g/h, and the alcoholysis reaction temperature is 10-20 ℃;
according to the invention, preferably, in the step (2), the dropping flow rate is 450-530 g/min, the hydrolysis reaction temperature is 6-8 ℃, the dropping is completed and balanced for 0.5h, and the standing time is 5 min; drying with anhydrous sodium sulfate, and neutralizing and stirring with a neutralizing agent for 0.5-2 h;
according to the invention, the preferable weight ratio of the raw materials is as follows: low-boiling-point substances: the alcohol compound is (8-13: 1), preferably (8-12: 1); in a preferred embodiment of the present invention, the low boilers: the weight ratio of the alcohol compounds is as follows: (9 to 12: 1)
According to the invention, the preferred weight ratio of alcoholysis overhead is: fraction (c): the water is (1: 1.3-2.2), preferably (1: 1.3-2.0); in a preferred embodiment of the invention, the fraction: the weight ratio of water is as follows: (1: 1.3 to 1.9)
The reaction kettle and the reaction tower used according to the invention can be reaction kettles and reaction towers commonly used in the field, and the materials and the specifications can be materials and specifications which are conventional in the field.
According to the invention, the purification and refining method comprises vacuum rectification and optional atmospheric rectification.
In one embodiment of the present invention, the purification and purification method is: rectifying under normal pressure, and separating 1,1,3, 3-tetramethyldisiloxane in a fraction at 70-71 ℃.
Preferably, when the distillation is carried out under normal pressure, the distillation top temperature is controlled to be 70-71 ℃. According to the invention, M is distilled off 2 H can be used as a method for synthesizing 1,1,3, 3-tetramethyldisiloxane used in the present invention; can also be used as raw materials in other processes for synthesizing 1,1,3, 3-tetramethyldisiloxane.
Preferably, in the above method for preparing 1,1,3, 3-tetramethyldisiloxane, the raw materials are organochlorosilane low-boiling components and alcohols with boiling points less than 40 ℃.
Preferably, in the preparation method of 1,1,3, 3-tetramethyldisiloxane, the alcoholysis reaction temperature is 10-25 ℃, and preferably 10-20 ℃.
Preferably, in the above method for preparing 1,1,3, 3-tetramethyldisiloxane, the alcohol compound used in the alcoholysis reaction is selected from aliphatic alcohols, aromatic alcohols and alicyclic alcohols, preferably from aliphatic alcohols, and more preferably from one or a mixture of two of methanol, ethanol, propanol, ethylene glycol, propylene glycol and glycerol.
Preferably, in the preparation method of the 1,1,3, 3-tetramethyldisiloxane, the hydrolysis reaction temperature is 5-12 ℃, and the most preferred temperature is 6-8 ℃.
Preferably, in the preparation method of the 1,1,3, 3-tetramethyldisiloxane, the alcoholysis dropping flow rate is 250-400 g/h, and preferably 250-350 g/h.
Preferably, in the preparation method of 1,1,3, 3-tetramethyldisiloxane, the reaction equilibrium time is 0.5-1 h, and the equilibrium time is 0.5 h.
Preferably, in the preparation method of the 1,1,3, 3-tetramethyldisiloxane, the neutralization time is 0.5-2 h, and more preferably 1-2 h.
Preferably, in the preparation method of the 1,1,3, 3-tetramethyldisiloxane, the purity range of the rectification extraction reaction product 1,1,3, 3-tetramethyldisiloxane can be controlled to be more than or equal to 98.5%.
Preferably, in the preparation method of 1,1,3, 3-tetramethyldisiloxane, the viscosity of the reaction product 1,1,3, 3-tetramethyldisiloxane can be controlled within the range of 2-2.5 cs.
Preferably, in the preparation method of the 1,1,3, 3-tetramethyldisiloxane, the reaction product 1,1,3, 3-tetramethyldisiloxane has a storage temperature of less than 20 DEG C
The preparation process comprises the following steps: feeding materials according to a certain proportion, adding the weighed organosilicon chlorosilane low-boiling material into a four-neck flask with a stirring device, a thermometer, a rectifying tower and a condensing device, fixing the flask in a constant-temperature cooling device, adding the weighed alcohol compound into a dropping bottle when the temperature of an ice maker is reduced to 0 ℃, controlling the dropping speed to be 250-350 g/h, controlling the reaction temperature to be 10-20 ℃, discharging tail gas into an acid water tank for absorption, balancing for 30min after dropping, starting a heating device, and starting heating for rapid rectification and extraction of fractions less than 40 ℃.
Feeding a fraction extracted by rectification and less than 40 ℃ and water according to a certain ratio, firstly adding the water into a four-neck flask with a stirring device, a thermometer, a condensing device and a constant-pressure dropping funnel, fixing the flask in a constant-temperature cooling device, when the temperature of an ice maker is reduced to 3 ℃, beginning to drop the fraction, controlling the dropping flow rate to be 450-530 g/h, simultaneously controlling the reaction temperature to be 6-8 ℃, balancing for 0.5h after dropping, standing for 5min to remove lower-layer acid water, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate for drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying a filtered hydrolysate, extracting a distillate at the temperature of 70-71 ℃ at the top of the tower for chromatographic analysis, wherein the purity of 1,1,3, 3-tetramethyldisiloxane is more than or equal to 98.5%.
ADVANTAGEOUS EFFECTS OF INVENTION
The novel method for synthesizing 1,1,3, 3-tetramethyldisiloxane by using the organosilicon chlorosilane low-boiling-point substance has the following excellent effects:
(1) the invention uses organosilicon chlorosilane low-boiling residue as raw material, M 2 The conversion per pass of H is more than 85 percent, the synthesis cost of 1,1,3, 3-tetramethyldisiloxane is reduced in the actual production, the process is simple, the technical problem that the byproduct low-boiling-point substances produced by the organosilicon monomer are converted into products with high added values is solved, the method belongs to waste utilization, increases the high-value economic benefits of the byproduct, and is environment-friendly and low in comprehensive cost.
(2) In the preparation method of the invention, the useful substance in the low-boiling raw material is M 2 H, becomes 1,1,3, 3-tetramethyl disiloxane after reaction, and all M is contained in the rest low-boiling substances 4 And a CH compound, M4 can be used for disproportionation reaction, the rest CH material enters an incineration device, and the kettle liquid can be used for preparing hydrogen-containing silicone oil.
(3) The organosilicon chlorosilane low-boiling-point substance is fully utilized, and the danger of the organosilicon chlorosilane low-boiling-point substance as liquid waste is reduced; the low-boiling component contains relatively more chain hydrocarbon, has low flash point, is extremely easy to burn and is more dangerous. The low-boiling-point substances are converted into products with higher secondary value, and a new idea for treating the low-boiling-point waste is provided.
(4) The purity of the 1,1,3, 3-tetramethyldisiloxane prepared by the method is more than or equal to 98.5 percent, the viscosity range is 2-2.5cs, and the yield is more than 80 percent.
Drawings
FIG. 1: a process flow diagram for preparing 1,1,3, 3-tetramethyldisiloxane from organosilicon monomer low-boiling-point substances;
FIG. 2: the gas chromatogram of the low boiling substance as the raw material used in example 1 and the contents of the main components;
FIG. 3: example 1 gas chromatogram and main component content of 1,1,3, 3-tetramethyldisiloxane obtained after rectification.
Detailed Description
Hereinafter, a mode for carrying out the present invention will be described in detail.
The present invention is further described below with reference to examples. It should be noted that the examples are not intended to limit the scope of the present invention, and those skilled in the art will appreciate that any modifications and variations based on the present invention are within the scope of the present invention.
Conventional chemicals used in the following examples are commercially available.
The low-boiling-point substances used in the following examples are derived from the by-products of the synthesis of organosilicon monomers, and the typical components and percentages of the low-boiling-point substances are as follows:
boiling point of low-boiling component
In the above table are the boiling points and compositions of the major components in the low boiling point material.
Sources and purities of the raw materials used in the following examples:
organosilicon chlorosilane low-boiling-point substances: ekensin Silicones Ltd
Methanol, ethanol, propanol: analytical purity
Water: deionized water
Anhydrous sodium sulfate: analytical purity
Sodium bicarbonate: analytical purity
Diatomite: 60-80 mesh Guangzhou Yikang New Material science and technology Co., Ltd
Example 1:
adding 500g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, controlling the temperature of an ice maker to be reduced to 0 ℃, adding 55g of methanol into a dropping bottle, dropping when the temperature in the flask is cooled to 10 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 300g/h, starting a heating device to heat up, performing fast rectification to extract fractions with the temperature of less than 40 ℃, and M 2 The H utilization was 92.3%. . Weighing 300g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 3 ℃, pouring 168g of fraction which is extracted by rectification and is less than 40 ℃ into a dropping bottle, starting dropping the fraction, controlling the dropping flow rate at 472g/h, controlling the reaction temperature at 8 ℃, balancing the dropping for 0.5h, standing for 5min, and separatingCollecting the layered acid water and the oil phase by using a glass bottle, adding anhydrous sodium sulfate for drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and obtaining distillate with the purity of 98.97 percent by using a hydrogen-containing double-end socket at the temperature of 70-71 ℃ at the receiving tower top. The viscosity is 2.1cs, and the yield of the hydrogen-containing double-end socket is 83.7%.
TABLE 1 gas chromatography for measuring the content of the main component of the low boiling substance of the raw material
TABLE 2 gas chromatography measurement of the content of the main component of the rectified product
Note: retention time min: the time from the introduction of the separated component to the time when the maximum concentration of the component appears after the column
The percentage content is as follows: mass fraction of a certain component
Example 2:
adding 500g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, controlling the temperature of an ice maker to be reduced to 0 ℃, adding 55g of methanol into a dropping bottle, dropping when the temperature in the flask is cooled to 10 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 300g/h, starting a heating device to heat up, performing fast rectification to extract fractions with the temperature of less than 40 ℃, and M 2 The H utilization was 93.9%. . Weighing 300g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 3 ℃, pouring 168g of fraction which is extracted by rectification and is less than 40 ℃ into a dropping bottle, starting dropping the fraction, controlling the dropping flow rate at 472g/h, controlling the reaction temperature at 8 ℃, balancing the dropping for 0.5h, standing for 5min, removing lower-layer acid water, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate for drying, and using sodium bicarbonate to dry the oil phaseNeutralizing and stirring for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and obtaining distillate with the purity of 98.97% of a hydrogen-containing double-end socket at the temperature of 70-71 ℃ at the top of the receiving tower. The viscosity is 2.1cs, and the yield of the hydrogen-containing double-end socket is 86.5%.
Example 3:
adding 600g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, controlling the temperature of an ice maker to be reduced to 0 ℃, adding 50g of ethanol into a dropping bottle, dropping when the temperature in the flask is cooled to 10 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 250g/h, starting a heating device to heat up, performing fast rectification to extract fractions with the temperature of less than 40 ℃, and M 2 The H utilization was 95.1%. . Weighing 300g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 3 ℃, pouring 150g of fraction with the temperature less than 40 ℃ obtained by rectification into a dropping bottle, starting dropping the fraction, controlling the dropping flow rate at 490g/h, controlling the reaction temperature at 8 ℃, balancing the dropping for 0.5h, standing for 5min, removing lower-layer acid water, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate for drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and receiving distillate with the purity of 98.57% containing hydrogen and double end enclosures at the top of the tower at 70-71 ℃. The viscosity is 2.0cs, and the yield of the hydrogen-containing double end enclosure is 89.4%.
Example 4:
adding 500g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, controlling the temperature of an ice maker to be reduced to 0 ℃, adding 62.5g of ethanol into a dropping bottle, dropping when the temperature in the flask is cooled to 10 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 300g/h, starting a heating device to start heating up, performing fast rectification and extraction on fractions with the temperature of less than 40 ℃, and performing M-phase rectification on fractions with the temperature of less than 40 DEG C 2 The H utilization was 93.6%. . Weighing 300g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 3 ℃, pouring 187g of fraction with the temperature less than 40 ℃ obtained by rectification extraction into a dropping bottle, starting dropping the fraction, controlling the dropping flow rate at 472g/h, controlling the reaction temperature at 8 ℃, balancing the dropping for 0.5h, standing for 5min, removing lower-layer acid water, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate for drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and receiving the distillate of 70-71 ℃ at the top of a towerThe purity of the product is 98.97 percent of hydrogen-containing double end sockets. The viscosity is 2.1cs, and the yield of the hydrogen-containing double-end socket is 84.9 percent.
Example 5:
adding 500g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, controlling the temperature of an ice maker to be reduced to 0 ℃, adding 55g of propanol into a dropping bottle, dropping when the temperature in the flask is cooled to 10 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 300g/h, starting a heating device to heat up, performing fast rectification to extract fractions with the temperature of less than 40 ℃, and M 2 The H utilization was 93.6%. . Weighing 300g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 3 ℃, pouring 168g of fraction which is extracted by rectification and is less than 40 ℃ into a dropping bottle, starting dropping fraction, controlling the dropping flow rate at 472g/h, controlling the reaction temperature at 8 ℃, balancing the dropping for 0.5h, standing for 5min, removing lower-layer acid water, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate for drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and receiving distillate with the purity of 98.97% of a hydrogen-containing double-end enclosure at the top of a tower at 70-71 ℃. The viscosity is 2.1cs, and the yield of the hydrogen-containing double-end socket is 86.8%.
Example 6:
adding 500g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is controlled to be reduced to 0 ℃, adding 45g of propanol into a dropping bottle, dropping when the temperature in the flask is cooled to 10 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 350g/h, starting a heating device to heat up, performing fast rectification to extract fractions with the temperature of less than 40 ℃, and M 2 The H utilization was 95.1%. . Weighing 350g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 3 ℃, pouring 205g of fraction which is extracted by rectification and is less than 40 ℃ into a dropping bottle, starting dropping the fraction, controlling the dropping flow rate at 450g/h, controlling the reaction temperature at 6 ℃, balancing the dropping for 0.5h, standing for 5min, removing lower-layer acid water, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate for drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and receiving distillate at the tower top of 70-71 ℃ with the purity of a hydrogen-containing double-end enclosure of 99.04%. The viscosity is 2.12cs, and the yield of the hydrogen-containing double-end socket is 88.2%.
Example 7:
adding 500g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, controlling the temperature of an ice maker to be reduced to 0 ℃, adding 52g of a mixture of methanol and ethanol into a dropping bottle, dropping when the temperature in the flask is cooled to 15 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 250g/h, starting a heating device to heat up, performing fast rectification and extracting fractions with the temperature of less than 40 ℃, and performing M 2 The H utilization was 94.1%. . Weighing 350g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 3-10 ℃, pouring 269g of fraction with the distillation extraction temperature being less than 40 ℃ into a dropping bottle, starting dropping the fraction, controlling the dropping flow rate at 530g/min, controlling the reaction temperature at 8 ℃, balancing the dropping for 0.5h, standing for 5min, removing lower-layer acid water, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate for drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and obtaining a distillate with the purity of 98.49 percent of a hydrogen-containing double-end enclosure at the top of a receiving tower, wherein the distillate at the temperature of 70-71 ℃ is hydrogen-containing double-end enclosure. The viscosity is 2.2cs, and the yield of the hydrogen-containing double-end socket is 87.8%. .
Example 8:
adding 500g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, controlling the temperature of an ice maker to be reduced to 0 ℃, adding 53g of methanol and propanol mixture into a dropping bottle, dropping when the temperature in the flask is cooled to 12 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 320g/h, starting a heating device to heat up, performing fast rectification to extract fractions with the temperature of less than 40 ℃, and performing M 2 The H utilization was 92.5%. . Weighing 300g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 5 ℃, pouring 214g of fraction which is extracted by rectification and is less than 40 ℃ into a dropping bottle, beginning dropping the fraction, controlling the dropping flow rate at 450g/min, controlling the reaction temperature at 7 ℃, balancing the dropping for 0.5h, standing for 5min, removing lower-layer acid water, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate for drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and receiving distillate with the purity of 99.23% of a hydrogen-containing double-end enclosure at the top of the tower at 70-71 ℃. The viscosity is 2.07cs, and the yield of the hydrogen-containing double end socket is 85.3%. .
Comparative example 1
Adding 500g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, controlling the temperature of an ice maker to be reduced to 0 ℃, adding 71g of a methanol and propanol mixture into a dropping bottle, dropping when the temperature in the flask is cooled to 12 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 320g/h, starting a heating device to start heating up, performing fast rectification and extraction on fractions with the temperature of less than 40 ℃, and causing part M to be partially due to excessive alcohol at the moment 2 H was alcoholyzed and M2H utilization was 72%. Weighing 300g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 5 ℃, pouring 250g of fraction with the temperature less than 40 ℃ obtained by rectification into a dropping bottle, starting dropping the fraction, controlling the dropping flow rate at 450g/min, controlling the reaction temperature at 7 ℃, balancing the dropping for 0.5h, standing for 5min, removing lower-layer acid water, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate for drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and receiving distillate with the purity of 98.13% of a hydrogen-containing double-end enclosure at the top of the tower at 70-71 ℃. The viscosity is 2.02cs, and the yield of the hydrogen-containing double end socket is 69%.
Comparative example 2
Adding 500g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, controlling the temperature of an ice maker to be reduced to 0 ℃, adding 35.71g of a mixture of methanol and propanol into a dropping bottle, dropping when the temperature in the flask is cooled to 12 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 320g/h, starting a heating device to heat up, performing fast rectification to extract fractions with the temperature of less than 40 ℃, and carrying partial substances MH, M which do not finish alcoholysis into distillate 2 The H utilization was 67%. Weighing 300g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 5 ℃, pouring 291g of fraction with the temperature less than 40 ℃ obtained by rectification into a dropping bottle, starting dropping the fraction, controlling the dropping flow rate at 450g/min, controlling the reaction temperature at 7 ℃, balancing for 0.5h after dropping, allowing part of MH hydrolyzed cross-linked substances in the reaction bottle to stand for 5min, removing acid water and cross-linked substances at the lower layer, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate, drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and receiving distillate at the top of the tower with the temperature of 70-71 ℃ and having the purity of 98.13% of a hydrogen-containing double-end enclosure. Viscosity of 2.02cs, containing hydrogenThe yield of the double heads is 62%.
Comparative example 3
Adding 500g of organic chlorosilane low-boiling-point substances into a dry 1000mL four-mouth bottle, controlling the temperature of an ice maker to be reduced to 0 ℃, adding 35.71g of a mixture of methanol and propanol into a dropping bottle, dropping when the temperature in the flask is cooled to 12 ℃, discharging tail gas into an acid water tank for absorption, controlling the dropping flow rate to be 320g/h, starting a heating device to heat up, performing fast rectification to extract fractions with the temperature of less than 40 ℃, and carrying partial substances MH, M which do not finish alcoholysis into distillate 2 The H utilization was 68%. Weighing 300g of water, adding the water into a dry 1000mL four-mouth bottle, when the temperature of an ice maker is reduced to 5 ℃, pouring 130g of fraction with the temperature of less than 40 ℃ obtained by rectification into a dropping bottle, starting dropping the fraction, controlling the dropping flow rate at 450g/min, controlling the reaction temperature at 7 ℃, balancing for 0.5h after dropping, allowing part of MH hydrolyzed cross-linked substances in the reaction bottle to stand for 5min, removing acid water and cross-linked substances at the lower layer, collecting an oil phase by using a glass bottle, adding anhydrous sodium sulfate, drying, neutralizing and stirring by using sodium bicarbonate for 0.5-2 h, filtering, rectifying the filtered hydrolysate, and receiving distillate with the temperature of 70-71 ℃ at the top of a tower, wherein the purity of a hydrogen-containing double-end enclosure is 98.13%. The viscosity is 2.02cs, and the yield of the hydrogen-containing double-end socket is 63%.
The above embodiments are merely illustrative of the present disclosure and do not represent a limitation of the present disclosure. Other variations of the specific structure of the invention will occur to those skilled in the art.
Claims (5)
1. A preparation method for synthesizing 1,1,3, 3-tetramethyl disiloxane by organosilicon chlorosilane low-boiling-point substances is characterized in that the 1,1,3, 3-tetramethyl disiloxane is synthesized by alcoholysis and hydrolysis of the organosilicon chlorosilane low-boiling-point substances; the low-boiling-point substance is a mixture consisting of low-boiling-point substances removed in the process of producing an organic silicon monomer, the boiling point range of the collected low-boiling-point substance is less than 40 ℃, the low-boiling-point substance mainly contains 30-50 wt% of tetramethylsilane, less than 2 wt% of trichlorosilane, 15-45 wt% of dimethylhydrochlorosilane, less than 10 wt% of methylhydrodichlorosilane and less than 20 wt% of hydrocarbon, and the sum of the components is 100 wt%, and the method comprises the following steps: (1) alcoholysis: dropwise adding an alcohol compound into the organosilicon chlorosilane low-boiling residue for alcoholysis reaction, quickly heating and rectifying, and extracting a fraction with the temperature of less than 40 ℃ from a distillate at the top of an alcoholysis tower;
(2) hydrolysis: dropwise adding the fraction into water for hydrolysis, balancing after dropwise adding, layering oil and water after standing, collecting an upper oil phase, drying, neutralizing, and filtering to obtain a hydrolysate;
(3) and (3) rectification: rectifying the hydrolysate, and receiving distillate at the temperature of 70-71 ℃ at the top of the tower, namely 1,1,3, 3-tetramethyldisiloxane; in the step (1), the dropping flow rate of the alcohol compound is 250-400 g/h, and the alcoholysis reaction temperature is 10-25 ℃; the weight ratio of the raw materials is as follows: low-boiling-point substances: the alcohol compound is 8-13: 1; in the step (2), the dropping flow rate of the distillate is 450-530 g/h, the hydrolysis reaction temperature is 5-12 ℃, the dropping is balanced for 0.5-1 h, and the standing time is 5 min; drying with anhydrous sodium sulfate, and neutralizing and stirring with a neutralizing agent for 0.5-2 h; the weight ratio of the raw materials is as follows: fraction (c): 1 part of water: 1.3-2.2, wherein the alcohol compound is selected from aliphatic alcohol, aromatic alcohol and alicyclic alcohol.
2. The method of claim 1,1,3, 3-tetramethyldisiloxane in which the neutralizing agent is anhydrous sodium bicarbonate.
3. The method for producing 1,1,3, 3-tetramethyldisiloxane in accordance with any one of claims 1 to 2, wherein the alcoholysis reaction temperature is 10 to 20 ℃ and the hydrolysis reaction temperature is 6 to 8 ℃.
4. The process for producing 1,1,3, 3-tetramethyldisiloxane in accordance with claim 3, wherein the alcohol compound is added at a flow rate of 250 to 350g/h in the step (1) and the distillate is added at a flow rate of 480 to 530g/h in the step (2).
5. The method of claim 4, wherein the viscosity of the reaction product 1,1,3, 3-tetramethyldisiloxane is 2 to 2.5 cs.
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