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Preparation method of terminal hydrogen-containing silicone oil

A technology of terminal hydrogen-containing silicone oil and methyl silicone oil, which is applied in the field of silicone softeners, can solve the problems of difficult treatment, high solid waste, poor stability, etc., achieve low boiling and electrolyte content, simplify the synthesis process, The effect of less catalyst usage

Pending Publication Date: 2021-06-25
JIANDE BAISHA CHEM
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Problems solved by technology

The experimental results prove that: concentrated sulfuric acid has the best catalytic performance in the preparation of hydrogen-containing silicone oil by acid balance catalysis, but it will generate more solid waste and be difficult to handle; acidic resin can simplify the process, but its stability is not good, and catalyst deactivation will occur phenomenon, affecting the performance of the product; activated clay is not conducive to production operations

Method used

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  • Preparation method of terminal hydrogen-containing silicone oil

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Embodiment

[0036] Hydrogen-containing silicone oil prepared by traditional process: add DMC or D4, hydrogen-containing double-head, and concentrated sulfuric acid into the container in turn, start stirring, first heat up to 30-35 ° C, and keep reacting for 6 hours. Then add soda ash to neutralize the reaction for 1 hour, make the PH value of the material 6, make the material pass through the filtration device, and remove the generated solid waste. Then the temperature was raised to 100-130°C, and the low boilers were removed by vacuuming. Finally, the material is cooled and discharged to obtain terminal hydrogen-containing silicone oil with a solid content of about 90%.

[0037] The hydrogen-containing silicone oil at the preparation end of the new process: the measured high-viscosity methyl silicone oil and the hydrogen-containing double-head are used as raw materials, put into the container in turn, fully mixed and stirred evenly, and then the linear catalyst H is added. Incubate the ...

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Abstract

The invention relates to a preparation method of terminal hydrogen-containing silicone oil, which is characterized in that the terminal hydrogen-containing silicone oil is prepared by adopting high-viscosity methyl silicone oil and tetramethyldisiloxane as raw materials, and under the action of a linear phosphonitrile chloride composite catalyst H, the catalyst has a degradation effect on siloxane chain segments in methyl silicone oil chain segments, so that macromolecular polysiloxane is degraded into many micromolecular polysiloxane; meanwhile, the micromolecular polysiloxane is quickly subjected to condensation polymerization, the tetramethyldisiloxane participates in reaction and is terminated in time, the linear polysiloxane is redistributed, and the high-activity terminated hydrogen-containing silicone oil is prepared. According to the method disclosed by the invention, no obvious cyclosiloxane is generated, the content of low-boiling-point substances is extremely low, and only extremely trace short-chain polysiloxane is generated. The problems that in a traditional acid equilibrium catalysis process, the prepared target product is low in activity, low in effective component and excessive in residual low-boiling-point substances and ring bodies are well solved, and particularly, the limitation of international regulations such as reaction on the residual quantity of organic silicon ring body components such as D3, D4 and D5 in the product can be met.

Description

technical field [0001] The invention relates to the field of organic silicon softeners, in particular to a preparation method of terminal hydrogen-containing silicone oil. Background technique [0002] In recent years, silicone softeners have developed extremely rapidly, especially ternary copolymer block silicone oil is a new structure of silicone softeners that has developed the fastest in the past ten years. Terpolymer silicone oil combines polysiloxane segment, polyether segment and amino group on the same macromolecule. The polysiloxane segment mainly plays a smooth role, the polyether segment plays a self-emulsifying and hydrophilic role, and the amino group mainly plays a softening role. Compared with traditional softeners, it has more obvious linearity and excellent self-emulsifying properties. It can self-emulsify in water to form a stable emulsion, and its overall softening and finishing effect is very outstanding. [0003] As the basic raw material for synthesiz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/12C08G77/08
CPCC08G77/12C08G77/08
Inventor 叶骎伟胡俊杰苏华高海江胡骏涛凌伟平徐剑飞余珊
Owner JIANDE BAISHA CHEM
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