CN114634525A - Preparation method of tetramethylcyclotetrasiloxane - Google Patents
Preparation method of tetramethylcyclotetrasiloxane Download PDFInfo
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- CN114634525A CN114634525A CN202011489702.2A CN202011489702A CN114634525A CN 114634525 A CN114634525 A CN 114634525A CN 202011489702 A CN202011489702 A CN 202011489702A CN 114634525 A CN114634525 A CN 114634525A
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- tetramethylcyclotetrasiloxane
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- crude fraction
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- WZJUBBHODHNQPW-UHFFFAOYSA-N 2,4,6,8-tetramethyl-1,3,5,7,2$l^{3},4$l^{3},6$l^{3},8$l^{3}-tetraoxatetrasilocane Chemical compound C[Si]1O[Si](C)O[Si](C)O[Si](C)O1 WZJUBBHODHNQPW-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920001843 polymethylhydrosiloxane Polymers 0.000 claims abstract description 17
- 238000005336 cracking Methods 0.000 claims abstract description 14
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims abstract description 10
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 22
- 239000001257 hydrogen Substances 0.000 claims description 22
- 150000002431 hydrogen Chemical class 0.000 claims description 11
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 description 7
- 239000012264 purified product Substances 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- -1 alkyl hydrogen Chemical class 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- BQYPERTZJDZBIR-UHFFFAOYSA-N 2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical group C[SiH]1O[SiH](C)O[SiH](C)O[SiH](C)O1 BQYPERTZJDZBIR-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/21—Cyclic compounds having at least one ring containing silicon, but no carbon in the ring
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention is suitable for the technical field of chemical industry, and provides a preparation method of tetramethylcyclotetrasiloxane, which comprises the following steps: mixing linear polymethylhydrosiloxane and sulfonic acid ammonia catalyst, heating for cracking, and then carrying out reduced pressure treatment to obtain cracked crude fraction; rectifying and purifying the cracking crude fraction, and collecting the fraction to obtain the tetramethylcyclotetrasiloxane. The embodiment of the invention can improve the yield and the purity of the product tetramethylcyclotetrasiloxane by taking the linear polymethylhydrosiloxane as the raw material and the sulfonic acid ammonia substance as the catalyst, does not use a solvent, has no pollution to the environment, and has the advantages of cheap and easily obtained raw materials, low cost, simple process, high economic benefit and the like.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a preparation method of tetramethylcyclotetrasiloxane.
Background
The tetramethylcyclotetrasiloxane plays an important role in the field of organic silicon, is widely applied to preparing various modified silicone oils and high-quality hydrogen-containing silicone oils, can also be used as a cross-linking agent and an anti-yellowing agent of silicone rubber, and is also a good sealing material in the electronic industry and an intermediate for preparing hydrogen-containing siloxane with the function of Si-H bonds.
The preparation of tetramethyl-cyclotetrasiloxane mainly comprises two methods, one is that alkyl hydrogen dihalide silane is taken as raw material and hydrolyzed in organic solvent, and then is kept stand for layering and distilled to prepare the tetramethyl-cyclotetrasiloxane; the other is prepared by cracking and rectifying linear polyalkyl hydrogen siloxane under the action of an alkali catalyst.
The first method has complex process, uses a large amount of methanol and alkane as solvents in the reaction, not only pollutes the environment, but also increases the difficulty of the next step of rectification and purification; meanwhile, the yield of the tetramethylcyclotetrasiloxane ring body in the first step is low.
The catalyst used in the second method is an inorganic metal catalyst, such as anhydrous aluminum trichloride, aluminum sulfate, ferric trichloride and ferric sulfate, wherein the inorganic metal catalyst has poor compatibility with a system, the catalytic efficiency is not high, and the possibility of generating hydrochloric acid in the system is very high, so that the product quality is influenced; in addition, the yield of tetramethylcyclotetrasiloxane in this process is generally not more than 60%.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of tetramethylcyclotetrasiloxane, aiming at solving the problems in the background technology.
The embodiment of the invention is realized in such a way that the preparation method of the tetramethylcyclotetrasiloxane comprises the following steps:
mixing linear polymethylhydrosiloxane and sulfonic acid ammonia catalyst, heating for cracking, and then carrying out reduced pressure treatment to obtain cracked crude fraction;
rectifying and purifying the cracking crude fraction, and collecting the fraction to obtain the tetramethylcyclotetrasiloxane.
Wherein, the thermal cracking can be carried out under normal pressure, which can generate a plurality of hydrogen-containing ring bodies including tetramethylcyclotetrasiloxane and linear bodies of micromolecular siloxane; after decompression treatment, the low molecular ring body and linear body can be extracted to obtain cracked crude fraction.
In a preferable embodiment of the invention, the amount of the sulfonic acid ammonia catalyst is 0.01 to 5 percent of the mass of the linear polymethylhydrosiloxane.
As another preferable scheme of the embodiment of the present invention, the structural formula of the linear polymethylhydrosiloxane is formula I:
in the formula I, R1 and R3 are hydrogen, R2 is methyl, and n is an integer of 30-1000.
As another preferable mode of the embodiment of the present invention, the structural formula of the sulfonic acid ammonia catalyst is any one of formula II to formula VI:
in formulas II-VI, R1 and R2 are independently hydrogen or an alkyl group.
As another preferable scheme of the embodiment of the invention, in the step, the temperature for heating and cracking is 160-170 ℃.
In another preferable embodiment of the present invention, the pressure of the reduced pressure treatment in the step is-95 to-93 kPa.
In another preferable embodiment of the present invention, in the step, the purity of the tetramethylcyclotetrasiloxane in the cracked crude fraction is 75.85% -86.23%.
In another preferable scheme of the embodiment of the invention, in the step, after rectification and purification, fractions at 133.7-134.3 ℃ are collected.
In another preferable embodiment of the present invention, in the step, the purity of the rectified and purified tetramethylcyclotetrasiloxane is 98.02% to 99.85%.
According to the preparation method of the tetramethylcyclotetrasiloxane, provided by the embodiment of the invention, the linear polymethylhydrosiloxane is used as a raw material, the sulfonic acid ammonia substance is used as a catalyst, the yield and the purity of the product tetramethylcyclotetrasiloxane can be improved, no solvent is used, no pollution is caused to the environment, and the preparation method has the advantages of cheap and easily obtained raw materials, low cost, simple process, high economic benefit and the like.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
This embodiment provides a method for preparing tetramethylcyclotetrasiloxane, comprising the steps of:
(1) 1000g of linear polymethylhydrosiloxane having a structural formula I (in the formula I, R1 and R3 are hydrogen, R2 is methyl, and n is 500) and 1g of ammonium sulfonate catalyst having a structural formula II (in the formula II, R1 and R2 are both hydrogen) are added into a 2000mL flask with distillation, heated and cracked at 165 ℃ under normal pressure for 30min, then the negative pressure is opened to-94.5 kPa, and a crude fraction is collected to obtain 820g of cracked crude fraction, wherein the content of tetramethylcyclotetrasiloxane is 86.23%.
(2) Transferring the cracking crude fraction into a flask with a rectifying head and a packing column, and collecting the fraction with the top temperature of 134.0 ℃ under the condition of normal pressure rectification to obtain a purified product with the tetramethylcyclotetrasiloxane content of 99.85 percent.
Example 2
This embodiment provides a method for preparing tetramethylcyclotetrasiloxane, comprising the steps of:
(1) 1000g of linear polymethylhydrosiloxane having a structural formula I (in the formula I, R1 and R3 are hydrogen, R2 is methyl, and n is 300), and 1g of ammonium sulfonate catalyst having a structural formula III (in the formula III, R1 is hydrogen, and R2 is methyl) are added into a 2000mL flask with distillation, heated and cracked at 165 ℃ under normal pressure for 30min, and then the negative pressure is opened to-95.0 kPa, and a crude fraction is collected to obtain 850g of cracked crude fraction, wherein the content of tetramethylcyclotetrasiloxane is 82.37%.
(2) Transferring the cracking crude fraction into a flask with a rectifying head and a packing column, and collecting the fraction with the top temperature of 134.3 ℃ under the condition of normal pressure rectification to obtain a purified product with the tetramethylcyclotetrasiloxane content of 98.56%.
Example 3
This embodiment provides a method for preparing tetramethylcyclotetrasiloxane, comprising the steps of:
(1) 1000g of linear polymethylhydrosiloxane having a structural formula I (in the formula I, R1 and R3 are hydrogen, R2 is methyl, and n is 600), 10g of ammonium sulfonate catalyst having a structural formula IV (in the formula IV, R1 and R2 are both methyl) are added into a 2000mL flask with distillation, heated and cracked at 165 ℃ under normal pressure for 30min, then the negative pressure is opened to-94.5 kPa, and crude fraction is collected to obtain 790g of cracked crude fraction, wherein the content of tetramethylcyclotetrasiloxane is 79.88%.
(2) Transferring the cracked crude fraction into a flask with a rectifying head and a packed column, and collecting the fraction with the top temperature of 134.2 ℃ under the condition of normal pressure rectification to obtain a purified product with the tetramethylcyclotetrasiloxane content of 99.21%.
Example 4
This embodiment provides a method for preparing tetramethylcyclotetrasiloxane, comprising the steps of:
(1) 1000g of linear polymethylhydrosiloxane having a structural formula I (in the formula I, R1 and R3 are hydrogen, R2 is methyl, and n is 200), 10g of ammonium sulfonate catalyst having a structural formula V (in the formula V, R1 is hydrogen, and R2 is ethyl) are added into a 2000mL flask with distillation, heated and cracked at 165 ℃ under normal pressure for 30min, then the negative pressure is opened to-93.0 kPa, and crude fraction is collected to obtain 780g of cracked crude fraction, wherein the content of tetramethylcyclotetrasiloxane is 78.46%.
(2) Transferring the cracked crude fraction into a flask with a rectifying head and a packed column, and collecting the fraction with the top temperature of 133.7 ℃ under the condition of normal pressure rectification to obtain a purified product with the tetramethylcyclotetrasiloxane content of 98.78%.
Example 5
This embodiment provides a method for preparing tetramethylcyclotetrasiloxane, comprising the steps of:
(1) 1000g of linear polymethylhydrosiloxane with the structural formula of formula I (in the formula I, R1 and R3 are hydrogen, R2 is methyl, and n is 100) and 2g of ammonium sulfonate catalyst with the structural formula of formula VI (in the formula VI, R1 and R2 are both hydrogen) are added into a 2000mL flask with distillation, heated and cracked at 165 ℃ under normal pressure for 30min, then the negative pressure is opened to-94.2 kPa, and crude fraction is collected to obtain 810g of cracked crude fraction, wherein the content of tetramethylcyclotetrasiloxane is 75.85%.
(2) Transferring the cracked crude fraction into a flask with a rectifying head and a packed column, and collecting the fraction with the top temperature of 133.8 ℃ under the condition of normal pressure rectification to obtain a purified product with the tetramethylcyclotetrasiloxane content of 98.02 percent.
Example 6
This embodiment provides a method for preparing tetramethylcyclotetrasiloxane, comprising the steps of:
(1) adding 1000g of linear polymethylhydrosiloxane with the structural formula of formula I (in the formula I, R1 and R3 are hydrogen, R2 is methyl, and n is 30) and 1g of ammonium sulfonate catalyst with the structural formula of formula II (in the formula II, R1 and R2 are both hydrogen) into a 2000mL flask with distillation, heating and cracking at 160 ℃ under normal pressure for 30min, opening the negative pressure to-94.5 kPa, and collecting the crude fraction to obtain cracked crude fraction.
(2) Transferring the cracking crude fraction into a flask with a rectifying head and a packing column, and collecting the fraction with the top temperature of 134.0 ℃ under the condition of normal pressure rectification to obtain a purified product of tetramethylcyclotetrasiloxane.
Example 7
This embodiment provides a method for preparing tetramethylcyclotetrasiloxane, comprising the steps of:
(1) adding 1000g of linear polymethylhydrosiloxane with the structural formula of formula I (in the formula I, R1 and R3 are hydrogen, R2 is methyl, and n is 1000) and 1g of ammonium sulfonate catalyst with the structural formula of formula II (in the formula II, R1 and R2 are both hydrogen) into a 2000mL flask with distillation, heating and cracking at 170 ℃ under normal pressure for 30min, opening the negative pressure to-94.5 kPa, and collecting the crude fraction to obtain cracked crude fraction.
(2) Transferring the cracked crude fraction into a flask with a rectifying head and a packed column, and collecting the fraction with the top temperature of 134.0 ℃ under the condition of normal pressure rectification to obtain a purified product of the tetramethylcyclotetrasiloxane.
The purity of the purified tetramethylcyclotetrasiloxane produced in examples 1 to 5 was counted, and the statistical results are shown in table 1.
TABLE 1
| Preparation method | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Purity of | 99.85％ | 98.56％ | 99.21％ | 98.78％ | 98.02％ |
It can be seen from the above examples and table 1 that the preparation method of tetramethylcyclotetrasiloxane provided by the embodiments of the present invention can improve the yield and purity of the product tetramethylcyclotetrasiloxane by using linear polymethylhydrosiloxane as the raw material and sulfonic acid ammonia as the catalyst, and has the advantages of no solvent, no environmental pollution, cheap and easily available raw materials, low cost, simple process, high economic benefit, etc.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (9)
1. The preparation method of tetramethylcyclotetrasiloxane is characterized by comprising the following steps:
mixing linear polymethylhydrosiloxane and sulfonic acid ammonia catalyst, heating for cracking, and then carrying out reduced pressure treatment to obtain cracked crude fraction;
rectifying and purifying the cracking crude fraction, and collecting the fraction to obtain the tetramethylcyclotetrasiloxane.
2. The method for preparing tetramethylcyclotetrasiloxane of claim 1, wherein the amount of said sulfonic acid ammonia catalyst is 0.01% -5% of the linear polymethylhydrosiloxane by mass.
3. The method of claim 1 or 2, wherein the linear polymethylhydrosiloxane has the formula I:
in the formula I, R1 and R3 are hydrogen, R2 is methyl, and n is an integer of 30-1000.
4. The method of claim 1 or 2, wherein the sulfonic acid amide catalyst has a structural formula of any one of formula II to formula VI:
in formulas II-VI, R1 and R2 are independently hydrogen or an alkyl group.
5. The method according to claim 1, wherein the pyrolysis temperature is 160-170 ℃.
6. The method according to claim 1, wherein the reduced pressure treatment is carried out at a pressure of-95 to-93 kPa.
7. The method according to claim 1, wherein the purity of tetramethylcyclotetrasiloxane in the cracking crude fraction is 75.85% -86.23%.
8. The method of claim 1, wherein the distillation purification is followed by collection of a 133.7-134.3 ℃ fraction.
9. The method according to claim 1 or 8, wherein the purity of the rectified and purified tetramethylcyclotetrasiloxane is 98.02-99.85%.
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| CN202011489702.2A CN114634525A (en) | 2020-12-16 | 2020-12-16 | Preparation method of tetramethylcyclotetrasiloxane |
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| CN202011489702.2A CN114634525A (en) | 2020-12-16 | 2020-12-16 | Preparation method of tetramethylcyclotetrasiloxane |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1333127A (en) * | 1971-01-06 | 1973-10-10 | Gen Electric | Method of making cyclopolysiloxanes containing silanic hydrogen |
| US4895967A (en) * | 1988-09-26 | 1990-01-23 | General Electric Company | Method for making cyclic poly(siloxane)s |
| US5075474A (en) * | 1990-04-20 | 1991-12-24 | Shin-Etsu Chemical Co., Ltd. | Method for preparing hexamethyl cyclotrisilazane |
| JPH07242678A (en) * | 1994-03-03 | 1995-09-19 | Shin Etsu Chem Co Ltd | Production of 2,4,6,8-tetramethylcyclotetrasiloxane |
| JP2005139123A (en) * | 2003-11-07 | 2005-06-02 | Kaneka Corp | METHOD FOR PRODUCING CYCLIC SILOXANE SKELETON-CONTAINING COMPOUND HAVING SiH GROUP |
| JP2005255629A (en) * | 2004-03-12 | 2005-09-22 | Kaneka Corp | Method for producing 1,3,5,7-tetramethylcyclosiloxane |
| CN101367832A (en) * | 2008-10-10 | 2009-02-18 | 宁波润禾化学工业有限公司 | Preparation method for tetramethyl-ring tetrasiloxane |
| CN102596970A (en) * | 2009-11-03 | 2012-07-18 | 道康宁公司 | A process for the production of polysilalkylenesiloxanes |
| CN105566379A (en) * | 2016-03-09 | 2016-05-11 | 张玲 | Preparation method of octamethylcyclotetrasiloxane |
| CN109400951A (en) * | 2018-12-29 | 2019-03-01 | 佛山市金银河智能装备股份有限公司 | A kind of production method and device of DMC |
-
2020
- 2020-12-16 CN CN202011489702.2A patent/CN114634525A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1333127A (en) * | 1971-01-06 | 1973-10-10 | Gen Electric | Method of making cyclopolysiloxanes containing silanic hydrogen |
| US4895967A (en) * | 1988-09-26 | 1990-01-23 | General Electric Company | Method for making cyclic poly(siloxane)s |
| US5075474A (en) * | 1990-04-20 | 1991-12-24 | Shin-Etsu Chemical Co., Ltd. | Method for preparing hexamethyl cyclotrisilazane |
| JPH07242678A (en) * | 1994-03-03 | 1995-09-19 | Shin Etsu Chem Co Ltd | Production of 2,4,6,8-tetramethylcyclotetrasiloxane |
| JP2005139123A (en) * | 2003-11-07 | 2005-06-02 | Kaneka Corp | METHOD FOR PRODUCING CYCLIC SILOXANE SKELETON-CONTAINING COMPOUND HAVING SiH GROUP |
| JP2005255629A (en) * | 2004-03-12 | 2005-09-22 | Kaneka Corp | Method for producing 1,3,5,7-tetramethylcyclosiloxane |
| CN101367832A (en) * | 2008-10-10 | 2009-02-18 | 宁波润禾化学工业有限公司 | Preparation method for tetramethyl-ring tetrasiloxane |
| CN102596970A (en) * | 2009-11-03 | 2012-07-18 | 道康宁公司 | A process for the production of polysilalkylenesiloxanes |
| CN105566379A (en) * | 2016-03-09 | 2016-05-11 | 张玲 | Preparation method of octamethylcyclotetrasiloxane |
| CN109400951A (en) * | 2018-12-29 | 2019-03-01 | 佛山市金银河智能装备股份有限公司 | A kind of production method and device of DMC |
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Application publication date: 20220617 |