- A dog (d) for the preparation of hexamethyl disilane
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The invention relates to a preparation method for hydroxypropyl (butyl) disiloxane. The preparation method comprises the following steps: (1) mixing an allyl alcohol salt-allyl alcohol mixed solution or an alkenyl butyl alcohol salt-alkenyl butyl alcohol mixed solution and hydrogen chlorosilane in an organic solvent, introducing inert gas, stirring the mixture to react, distilling the mixture and collecting a fraction to obtain an alcoholysis product; (2) adding a hydrosilylation catalyst and a co-catalyst into the alcoholysis product, stirring the mixture to react for 4-10 hours, and after reaction, naturally cooling the mixture to room temperature; and (3) adding a hydrochloric acid solution into the product obtained in the step (2), stirring the mixture and carrying out reflux reaction for 5-12 hours, after reaction, naturally cooling the mixture to room temperature, adjusting the pH to neutral, separating liquids to remove a lower solution, washing an organic phase by water to neutral, extracting the organic phase by an extraction agent, removing the extraction agent and drying the mixture to obtain the hydroxypropyl (butyl) disiloxane. The method provided by the invention is high in yield of target product, the highest yield of the alcoholysis product can reach 94.32%, and the highest yield of an addition-hydrolysate can reach 89.58%.
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Paragraph 0069-0071; 0075; 0076
(2018/05/30)
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- Method for preparing hydroxyalkyl disiloxane
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The invention relates to a method for preparing hydroxyalkyl disiloxane. The method includes the following steps: (1) mixing carboxylic acid unsaturated ester with dimethylchlorosilane in an organic solvent, introducing inert gas, adding hydrosilyation catalyst and stirring for 2 to 12 hours; (2) dropwising a mixed liquid of acidic aqueous solution and the organic solvent to the hydrosilylation reaction product and hydrolyzing for 1 to 6 hours; (3) regulating the hydrolysis product pH to be neutral, extracting organic layers three times with extraction agent, washing three times, drying for 24 hours and removing the extraction agent by rotary evaporating to obtain the finished product. The method has the advantages of simple operation, simple steps, mild reaction conditions, pure product and high yield, and the yield of the hydrosilylation reaction product can reach 83.2% and the yield of the hydrolysis product can reach 89.5%.
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Paragraph 0064; 0065; 0066; 0067; 0069; 0070
(2017/07/22)
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- Synthesis of disiloxanes containing hydroxyalkyl groups
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Four 1,3-bis(ω-hydroxyalkyl)tetramethyldisiloxanes 2O (I; n = 3-6) were synthsized by methanolysis of the correspondig trimethylsilylterminated disiloxanes (III).The latter were obtained from 1,1,3,3-tetramethyldisiloxane (II) and the appropriate (ω-alkenyloxy)trimethylsilanes (IV).Under acidic conditions III formed in addition to I, the corresponding (ω-hydroxyalkyl)pentamethyldisiloxanes HO(CH2)nSiMe2OSiMe3 (V; n = 3-6).
- Braun, F.,Willner, L.,Hess, M.,Kosfeld, R.
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