1,3- two (3- 3-glycidoxypropyl) - four methyl siloxane synthesis of 1,1,3,3- two-Iota

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Service > 1,3- two (3- 3-glycidoxypropyl) - four methyl siloxane synthesis of 1,1,3,3- two

1,3- two (3- 3-glycidoxypropyl) - four methyl siloxane synthesis of 1,1,3,3- two

With the progress of synthesis and application of silicone, silicone copolymerized with other organic species increased rapidly. The reactive groups as side group or groups into the polysiloxane, make it become the active polysiloxane, and other material to synthesize the block or graft copolymers, will greatly improve the performance of silicone materials. Research on all kinds of capping agent having reactive functional group of [1] has an important significance. 1,3- two (3- 3-glycidoxypropyl) -1,1,3,3- four methyl twosiloxane (i.e. epoxy dual head) is a kind of active capping agent, reaction of the epoxy groups, can be made of epoxy terminated silicone oil, and for all kinds of new structure,excellent performance of silicone modified materials. The recent researches on block polyether silicone oil with epoxy terminated silicone oil as the main raw material for the synthesis of polyether silicone oil, has excellent emulsion stability, hydrophilicity, flexibility and anti yellowing, solve a series of problems existing in the traditional amino silicone oilprocessing used in the process of demulsification, floating oil viscosity and [2], etc., so itbecomes a research hotspot of silicone materials. At present, production process ofepoxy silicone more common are: hydrogen dual head and D4 reaction in the presence of acid, neutralization, dehydration synthesis ends with hydrogen containing silicone oil,allyl glycidyl ether in the catalytic synthesis of chloroplatinic acid epoxy terminatedsilicone oil [3]. The synthesis route, process is more complex, more variable factors, the final product poor controllability, and precious metal platinum use can not be recovered,so the reaction of the epoxy dual head and D4, one step preparation of epoxy terminatedsilicone oil, will become the development trend of. We glycidyl ether (AGE) with allylmethyl hydrogen silicone and two four two (HMM) as raw materials, addition reaction of epoxy dual head was prepared by silicon hydrogen by the catalytic system and reaction conditions were optimized, and the optimal process conditions were determined, highyield, low production cost of the products.

The 1 part of the experiment

Two 1.1 four methyl siloxane reagent and instrument two hydrogen (HMM), industrial grade, Jiang Xiyuan Kang silicon industry limited company of science and technology;allyl glycidyl ether (AGE), the industry level, Japan imports; isopropanol, analytically pure,generous Hangzhou Chemical Reagent Factory; three triethylamine, analytically pure,Wuxi Jingke chemical Limited company; chloroplatinic acid, homemade. Rotary vane vacuum pump, 2XZ-2 type, Linhai Tanshi Vacuum Equipment Co. Ltd; gas chromatography: GC-2014C, Shimadzu Corporation.

The synthesis of 1.2 epoxy dual head

Preparation of 1.2.1 catalyst to a certain amount of chloroplatinic acid dissolved inisopropanol, the preparation of Speier catalyst chloroplatinic acid concentration of 0.1 mol/L, as the main catalyst, and then the analysis of three triethylamine, pure threephenyl phosphine and N two, N- dimethylformamide dissolved in isopropanol solution with 0.1 mol/L as a ligand, reaction time and the volume of main catalyst ligands are added into a reaction kettle according to form complex, hydrosilylation of. 1.2.2 silicon hydrogen addition reaction in a blender, a dropping funnel, reflux condenser and a thermometer 250 mL four necked flask, adding measurement of allyl glycidyl ether andwater reduction catalyst, at a certain temperature, adding HMM, adding time control inabout 1 h, drop after reaction time, then vacuum distillation purification, collecting 180~200 C /-0.098 MPa fraction to fraction, and chromatography of the products were analyzed by gas.

2 results and discussion

2.1 catalytic system for addition reaction of silane derivatives were prepared withtransition metal as a catalyst, the catalyst has high activity of Pt complex, Pt complex catalyst is commonly used with Speier catalyst, but the induction period is too long, so its application is limited. Promote the catalytic activity of three phenyl phosphine and aminecompounds in some conditions of chloroplatinic acid. This experiment using Speiercatalyst as main catalyst, with 3 different ligands, investigated the influence of thereaction. The reaction conditions were as follows: hydrogen dual head feeding amount0.6 mol, allyl glycidyl ether is 1.26 mol, catalyst dosage 2.8 10- * 6 mol at 90 DEG C,adding HMM, and then reaction at a temperature of 90 DEG C for 90 min.

3 conclusion

(1) Pt complexes with different ligands and the formation of Speier catalyst, siliconehydrogen catalytic hydrogen dual head with allyl glycidyl ether is added to the reaction, in which Pt-N (C2H5) 3 complex catalyst has high activity and selectivity of the reaction.

(2) through the investigation of factors influencing the product yield, Pt-N (C2H5) to determine the optimum process conditions of catalytic synthesis of Epoxy 3 complex double head: the amount of catalyst is 2.8 10- * 6 mol, the ratio of raw materials n (AGE): n (HMM) =2.1: 1, reaction temperature 90 C, reaction time 90 min, the yield of the product was 89.3%. (3) the process has high yield, the reaction condition is easy to control and has the advantages of low production cost, the product used for the production of block polyether silicone oil, and has broad market prospects.