CN101921287B - Method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by continuous catalysis of solid phase catalyst - Google Patents
Method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by continuous catalysis of solid phase catalyst Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000003054 catalyst Substances 0.000 title claims abstract description 33
- 239000007790 solid phase Substances 0.000 title claims abstract description 33
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 26
- 230000002194 synthesizing effect Effects 0.000 title abstract description 3
- SWGZAKPJNWCPRY-UHFFFAOYSA-N methyl-bis(trimethylsilyloxy)silicon Chemical compound C[Si](C)(C)O[Si](C)O[Si](C)(C)C SWGZAKPJNWCPRY-UHFFFAOYSA-N 0.000 title abstract 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 21
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 15
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 38
- JPQBRSQJGWOTGC-UHFFFAOYSA-N methyl(silyloxysilyloxy)silane Chemical class C[SiH2]O[SiH2]O[SiH3] JPQBRSQJGWOTGC-UHFFFAOYSA-N 0.000 claims description 31
- 239000002253 acid Substances 0.000 claims description 27
- 239000003729 cation exchange resin Substances 0.000 claims description 17
- DHXVGJBLRPWPCS-UHFFFAOYSA-N Tetrahydropyran Chemical compound C1CCOCC1 DHXVGJBLRPWPCS-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 6
- 230000004044 response Effects 0.000 claims description 2
- -1 methyl hydrogen Chemical compound 0.000 abstract description 9
- 230000002378 acidificating effect Effects 0.000 abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 229920001296 polysiloxane Polymers 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 abstract 2
- 238000010924 continuous production Methods 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 description 8
- 238000011067 equilibration Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 230000035484 reaction time Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 238000005304 joining Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229920001429 chelating resin Polymers 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 125000005843 halogen group Chemical group 0.000 description 2
- 239000000413 hydrolysate Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 101100400378 Mus musculus Marveld2 gene Proteins 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000010813 municipal solid waste Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001843 polymethylhydrosiloxane Polymers 0.000 description 1
- 230000001020 rhythmical effect Effects 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Silicon Polymers (AREA)
Abstract
The invention relates to a method for synthesizing 1,1,1,3,5,5,5-heptamethyltrisiloxane by continuous catalysis of a solid phase catalyst. Hexamethyldisiloxane and straight chain methyl hydrogen polysiloxane in a molar ratio of 3:1-2:1 are taken as raw materials, strongly acidic ion exchange resin is taken as the solid phase catalyst, the reaction temperature is 40 to 80 DEG C, a fixed bed reactor is adopted, the raw materials pass through the reactor filled with the ion exchange resin at a certain flow rate, the retention period is 5 to 10 hours, the conversion rate of the raw materials is ensured by the retention period of the reaction through controlling the flow rate of the reaction product, the continuous reaction production is realized, and the reaction product is subjected to low fraction and high fraction removal rectification to form the 1,1,1,3,5,5,5-heptamethyltrisiloxane product with the purity of over 99 percent. The method has the advantages of readily available raw materials, no three-waste emission, simple process, continuous production, high-efficiency and stable reaction, simple separation, recyclable catalyst, conversion per pass of the raw material straight chain methyl hydrogen polysiloxane of over 32 percent, good product quality and low production cost.
Description
Technical field
The present invention relates to a kind of employing continuous catalysis of solid phase catalyst and synthesize 1,1,1,3,5,5, the method and the technology of 5-seven methyl trisiloxanes.
Background technology
1,1,1,3; 5,5,5-seven methyl trisiloxanes (MDHM) are a kind of important silicone intermediates; Because of it contains active si-h bond, be the basic raw material of synthesizing polyether, alkyl-modified trisiloxanes, and can be widely used in inert ingredient, coatings additive(s) and daily-use chemical industry etc.; But traditional synthesis process is shortcoming such as not high, by product complicacy of ubiquity productive rate also, and therefore, the improvement of the synthesis technique of MDHM and the raising of productive rate are significant.
Patent GB0632954 mentions the hydrolysate that adopts SWS-F 221 (MM) and methyl hydrogen dichlorosilane (MeSiHC12) and carries out the method for the MDHM of catalytic equilibration system through the vitriol oil, and carrying out acid catalyzed reaction again behind trimethylchlorosilane (Me3SiC1) and the MeSiHC12 cohydrolysis.Wherein the productive rate of MDHM is not high.
U.S. Pat 2491843 adopts cold concentrated hydrochloric acid to come catalysis Me3SiC1 and the condensation of MeSiHC12 cohydrolysis to obtain methylhydrogenpolysi,oxane, and wherein the productive rate of MDHM is not high.
U.S. Pat 2595890 slowly drips MeSiHC12 after adopting and in the mixed solution of MM and normal hexane, adding trash ice again; And the continuous simultaneously ice cube that adds; Then the method with the sulphuric acid catalysis oil reservoir prepares MDHM, and the quality percentage composition of MDHM is 26.7% in the product that obtains.But this method complicated operation, and separate certain degree of difficulty is arranged, and productive rate is not high.
Mention the method for a kind of synthetic MDHM in the U.S. Pat 2920093; In room temperature and stir and to get with MM to methyl hydrogen ring siloxane mixture (DHn, n＞3) down that the adding massfraction is the vitriol oil of 0.5%-0.1% in the mixed system, catalytically rearranging 4-8h; Remove catalyzer, rectifying gets MDHM.This method need be used expensive methyl hydrogen ring siloxane mixture, and raw material is difficult to obtain.
Japanese Patent JP11236389 then adopts linear halo phosphazene compound as catalyzer; With MM and straight chain methylhydrogenpolysi,oxane (MDHnM) or DHn (n＞3) is that raw material reaction obtains the methyl hydrogen siloxane oligopolymer of (the containing 3-8 Siliciumatom) of specific aggregation degree; But catalyzer is more difficult to get in this method, is unfavorable for large-scale industrial production.
Patent CN101020691 is hydrolyzed to the trimethyl silicane alkanes material with Me3SiX general formula with inorganic weak bases solution; In hydrolyzation system, slowly drip methyl hydrogen silicane material (above two general formula X=C1, Br, I, OMe, Oet) again with MeSiHX2 general formula; Condensation reaction under agitation is hydrolyzed; Me3SiX and MeSiHX2 volume(tric)fraction ratio are 150: 20-150: 110, dropwise, and oil phase gets final product through washing, drying, rectifying.The process of the synthetic MDHM of this method is still complicated, and productive rate is not too high.
Patent DD241606 is 10-50 through controlling MM and MDHnM or its mol ratio of DHn (n＞3): 1; And adopt Zeo-karb to carry out catalytic equilibration to prepare; Use the solid catalyst separate easily, but rhythmic reaction catalytic equilibration long reaction time influences reaction efficiency.
In sum, the synthetic main hydrolysate catalytic equilibration under acidizer catalysis that adopts MM and MeSiHC12 of MDHM, or inorganic weak bases solution is hydrolyzed to the Me3SiX material and adds the condensation reaction that is hydrolyzed of MeSiHX2 class material again.Above method exists that long reaction time or separation difficulty, raw material are chloride to exist problem such as pollution to environment, and productive rate is not too high.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, is solid-phase catalyst with the strong acid ion exchange resin, successive reaction, and catalyst consumption is little and renewable; Pollution-free, cost is low, productive rate high synthetic 1,1,1; 3,5,5, the method and the technology of 5-seven methyl trisiloxanes.
Technical scheme of the present invention has following:
The present invention synthetic 1,1,1,3,5; 5, the method for 5-seven methyl trisiloxanes comprises the following steps: that (n=10-50) raw materials mix is even with SWS-F 221 and straight chain methylhydrogenpolysi,oxane (MDHnM), and its mole proportioning is 3: 1-2: 1;, adopting fixed-bed reactor, temperature of reaction is 40-80 ℃, and the reactor drum of strong acid type amberlite is housed with certain flow velocity process; Through strong acid ion exchange resin solid-phase catalyst catalytic equilibration, reaction time is 5-10h, and the residence time of coming realization response through control reaction product flow velocity is to guarantee conversion of raw material, the production of realization successive reaction; Reaction product is taken off low and is taken off high rectifying, obtain purity greater than 99% 1,1,1; 3,5,5,5-seven methyl trisiloxanes products.
Among the present invention, the raw material that is adopted is SWS-F 221 (A) and straight chain methylhydrogenpolysi,oxane (B), and its mole proportioning is 3: 1-2: 1, and the not chloride essence of raw material, its reaction formula is seen Figure of description 3.
Among the present invention; Said solid-phase catalyst is a strong acid ion exchange resin; Can be gel-type strongly acidic styrene Zeo-karb, strong acid type styrene type cation exchange resin, equal hole strongly acidic styrene type cation exchange resin, large hole strong acid styrene system cation exchange resin, perfluorinated sulfonic resin, preferably large porous strong acid type styrene type cation exchange resin.
Among the present invention, adopt fixed reactor to carry out successive reaction, through reactor drum, its reaction time is 5-10h to raw material with certain flow velocity.
Among the present invention, temperature of reaction is 40-80 ℃, preferably 50-60 ℃.
Among the present invention, said to take off low be that the low molecule of MM is removed in rectifying.
Among the present invention, the said height that takes off is to remove high boiling material.
Beneficial effect of the present invention is: desired raw material is simple and easy to, and halogen atom does not have " three wastes " discharging, and is pollution-free, is successive reaction, can realize serialization production; Technology is simple, and does not have the problem of long reaction time, and the reaction efficient stable adopts strong acid ion exchange resin to make catalyzer, and product separates simple, and suitability for industrialized production is highly advantageous to; Catalyzer is renewable, and cost is low, and 1,1,1; 3,5,5,5-seven methyl trisiloxanes productive rates are high, and per pass conversion is greater than 32%.
Advantage of the present invention: desired raw material is simple and easy to, and halogen atom does not have " three wastes " discharging, and is pollution-free, is successive reaction, can realize serialization production; Technology is simple, and does not have the problem of long reaction time, and the reaction efficient stable adopts strong acid ion exchange resin to make catalyzer, and product separates simple, and suitability for industrialized production is highly advantageous to; Catalyzer is renewable, and cost is low, and 1,1,1; 3,5,5,5-seven methyl trisiloxanes productive rates are high, and per pass conversion is greater than 32%.
Description of drawings
The gas chromatogram of Fig. 1 reaction product (GC content: 32.3%);
Fig. 2 is gas chromatogram (the GC content: 99.6%) of product after the rectifying;
Fig. 3 is the reaction composite diagram of seven methyl trisiloxanes.
Embodiment
Embodiment 1, a kind of employing continuous catalysis of solid phase catalyst synthetic 1,1,1; 3,5,5; The method of 5-seven methyl trisiloxanes, wherein: with 2.5: 1 ratio of mol ratio, flow velocity is that constantly the joining of speed of 50mL/h is connected with constant temperature jacket and the strong acid ion exchange resin fixed-bed reactor are housed with SWS-F 221 and straight chain methylhydrogenpolysi,oxane raw material; The temperature of reaction perseverance is 60 ℃, and through large hole strong acid styrene system cation exchange resin's solid-phase catalyst catalytic equilibration, the residence time is 6h; Successive reaction in reactor drum, control reaction product flow velocity is directly flowed out by fixed reactor, and the product that comes out from reactor drum carries out quantitative analysis with gc; Gas chromatogram is as shown in Figure 1, and the content of MDHM is 32.3%.Again through Tuo Gao with take off low rectifying, the cut of intercepting 141-2 ℃ scope carries out quantitative analysis with gc, the content of MDHM is 99.6%, gas chromatogram is as shown in Figure 2.
Because catalyzer is filled fixed bed and is answered device; Do not have loss in theory so catalyzer is renewable, but pollute breakage because of possibly there are some in real reaction, the loss of its catalyzer is also less than 1 ‰; Much smaller than the consumption of liquid acid 2%-5%, solid-phase catalyst is replaceable after use for some time.
Flow velocity is meant the rate of addition of the mixture of SWS-F 221 (MM) and straight chain methylhydrogenpolysi,oxane (MDHnM).
Embodiment 2, a kind of employing continuous catalysis of solid phase catalyst synthetic 1,1,1,3; 5,5, the method for 5-seven methyl trisiloxanes; Wherein: the mol ratio of SWS-F 221 and straight chain methylhydrogenpolysi,oxane (MDHnM) raw material 3: 1, all the other are with embodiment 1, and the content of MDHM is 29.2%.
Embodiment 3, a kind of employing continuous catalysis of solid phase catalyst synthetic 1,1,1,3; 5,5, the method for 5-seven methyl trisiloxanes; Wherein: the mol ratio of SWS-F 221 and straight chain methylhydrogenpolysi,oxane (MDHnM) raw material 2: 1, all the other are with embodiment 1, and the content of MDHM is 30.1%.
Embodiment 4, a kind of employing continuous catalysis of solid phase catalyst synthesize 1,1,1,3,5,5, the method for 5-seven methyl trisiloxanes, and wherein: temperature of reaction is 40 ℃, and all the other are with embodiment 1, and the content of MDHM is 24.3% in the reaction product.
Embodiment 6, a kind of employing continuous catalysis of solid phase catalyst synthesize 1,1,1,3,5,5, the method for 5-seven methyl trisiloxanes, and wherein: the residence time is 4h, and its flow velocity is 75mL/h, and all the other are with embodiment 1, and the content of MDHM is 24.39% in the reaction product.
Embodiment 7, a kind of employing continuous catalysis of solid phase catalyst synthesize 1,1,1,3,5,5, the method for 5-seven methyl trisiloxanes, and wherein: the residence time is 5h, and its flow velocity is 60mL/h, and all the other are with embodiment 1, and the content of MDHM is 32.95% in the reaction product.
Embodiment 11, a kind of employing continuous catalysis of solid phase catalyst synthetic 1,1,1,3; 5,5, the method for 5-seven methyl trisiloxanes; Wherein: catalyzer changes equal hole strongly acidic styrene type cation exchange resin into, and all the other are with embodiment 1, and the content of MDHM is 25.1% in the reaction product.
Embodiment 12, a kind of employing continuous catalysis of solid phase catalyst synthesize 1,1,1,3,5,5, the method for 5-seven methyl trisiloxanes, and wherein: catalyzer changes perfluorinated sulfonic resin into, and all the other are with embodiment 1, and the content of MDHM is 12.5% in the reaction product.
Embodiment 13, a kind of employing continuous catalysis of solid phase catalyst synthetic 1,1,1; 3,5,5; The method of 5-seven methyl trisiloxanes, wherein: with 3: 1 ratio of mol ratio, flow velocity is that constantly the joining of speed of 55mL/h is connected with constant temperature jacket and the strong acid ion exchange resin fixed-bed reactor are housed with SWS-F 221 and straight chain methylhydrogenpolysi,oxane raw material; The temperature of reaction perseverance is 40 ℃, and through large hole strong acid styrene system cation exchange resin's solid-phase catalyst catalytic equilibration, the residence time is 10h; Successive reaction in reactor drum, control reaction product flow velocity is directly flowed out by fixed reactor, obtains the product that comes out from reactor drum.All the other are with embodiment 7.The content of MDHM is 30.66% in the reaction product.
Embodiment 14, a kind of employing continuous catalysis of solid phase catalyst synthetic 1,1,1; 3,5,5; The method of 5-seven methyl trisiloxanes, wherein: with 2: 1 ratio of mol ratio, flow velocity is that constantly the joining of speed of 45mL/h is connected with constant temperature jacket and the strong acid ion exchange resin fixed-bed reactor are housed with SWS-F 221 and straight chain methylhydrogenpolysi,oxane raw material; The temperature of reaction perseverance is 80 ℃, and through large hole strong acid styrene system cation exchange resin's solid-phase catalyst catalytic equilibration, the residence time is 5h; Successive reaction in reactor drum, control reaction product flow velocity is directly flowed out by fixed reactor, obtains the product that comes out from reactor drum.All the other are with embodiment 7.The content of MDHM is 30.84% in the reaction product.
Embodiment 15, a kind of employing continuous catalysis of solid phase catalyst synthesize 1,1,1,3,5,5, the method for 5-seven methyl trisiloxanes, and wherein: large hole strong acid styrene system cation exchange resin's model is the D001 large hole strong acid styrene system cation exchange resin.All the other are with embodiment 1 or embodiment 13 or embodiment 14.
The D001 large hole strong acid styrene system cation exchange resin can be that resin ltd of Langfang City Nanjing University provides.
Embodiment 16, a kind of employing continuous catalysis of solid phase catalyst synthesize 1,1,1,3,5,5, the method for 5-seven methyl trisiloxanes, and wherein: large hole strong acid styrene system cation exchange resin's model is the D001 large hole strong acid styrene system cation exchange resin.The product technology standard that the D001 large hole strong acid styrene system cation exchange resin adopts can be GB/T 16579-1996DL 519-93SH2605.02-1997.All the other are with embodiment 15.
Embodiment 17, a kind of employing continuous catalysis of solid phase catalyst synthetic 1,1,1,3; 5,5, the method for 5-seven methyl trisiloxanes; Wherein: large hole strong acid styrene system cation exchange resin's model is U.S. Amberlite IRA-200, German Lewatit-sp120, Japanese Diaion PK; Britain ZeroliteS-1104, French Allassion AS, any one among the Ky-2-12P of the FSU.All the other are with embodiment 7.The content of MDHM is about 30% in the external resin gained reaction product that adopts.
Claims (3)
1. one kind is adopted solid phase continuous catalysis synthetic 1,1,1,3,5; 5, the method for 5-seven methyl trisiloxanes is characterized in that: with SWS-F 221 and straight chain methylhydrogenpolysi,oxane MDHnM is raw material, n=10-50 wherein, and its mole proportioning is 3: 1-2: 1; The employing strong acid ion exchange resin is a solid-phase catalyst, and temperature of reaction is 40-80 ℃, adopts fixed-bed reactor, raw material is equipped with the reactor drum of ion exchange resin with certain flow velocity process; Residence time 5-10h obtains 1,1,1; 3,5,5,5-seven methyl trisiloxanes products; Wherein strong acid ion exchange resin is the large hole strong acid styrene system cation exchange resin.
2. a kind of employing solid phase continuous catalysis according to claim 1 synthetic 1,1,1; 3,5,5; The method of 5-seven methyl trisiloxanes is characterized in that: adopt fixed-bed reactor, raw material is equipped with the reactor drum of ion exchange resin with certain flow velocity process; The residence time of coming realization response through control reaction product flow velocity is to guarantee conversion of raw material, the production of realization successive reaction.
3. a kind of employing solid phase continuous catalyst as claimed in claim 1 synthetic 1,1,1; 3; 5,5, the method for 5-seven methyl trisiloxanes; It is characterized in that: the mixture of SWS-F 221 and straight chain methylhydrogenpolysi,oxane MDHnM is passed through the reactor drum that ion exchange resin is housed, wherein n=10-50 with the flow velocity with 60mL/h.
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| CN105503931A (en) * | 2016-01-27 | 2016-04-20 | 江西品汉新材料有限公司 | Method for preparing 1, 1, 1, 3, 5, 5, 5-heptamethyltrisiloxane |
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Non-Patent Citations (1)
| Title |
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| Yi-Ming Pai,et al.Preparation of Oligomeric and Polymeric a,o-Bis(trimethylsiloxy)polymethylchlorosiloxanes and Their Reactions with Alkyllithium Reagents.《organometallics》.1986,683-690. * |
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