一种格氏法制备苯基单体废渣的处理方法

By using a combination of ketone solvents and methylchlorosilanes in the treatment of waste residue from the Grignard process for phenyl monomer preparation, and controlling pH and temperature during centrifugation and distillation, the problems of magnesium salt complexation and hydrolysis in existing technologies were solved, achieving efficient and pollution-free recovery of magnesium chloride, and improving the yield of phenyl monomer and the recovery rate of raw materials.

CN117902603BActive Publication Date: 2026-07-17HUBEI XINGRUI SILICON MATERIAL CO LTD

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
HUBEI XINGRUI SILICON MATERIAL CO LTD
Filing Date
2023-12-14
Publication Date
2026-07-17

AI Technical Summary

Technical Problem

Existing technologies for treating waste residue from the Grignard process for preparing phenyl monomers have several drawbacks. These include the easy complexation of magnesium salts with phenyl monomers, the ineffective recovery of easily hydrolyzed raw materials and products from magnesium salts, the difficulty in controlling the process due to the disruption of coordination bonds by strong acid dissolution, and the challenge of high-precision distillation purification. Furthermore, improper treatment of the waste residue can easily pollute the environment.

Method used

The waste residue from the preparation of phenylalkoxysilane by the Grignard method was treated with ketone solvents such as acetone and methylchlorosilane. By controlling the pH value and temperature, the magnesium chloride, tetrahydrofuran and methyltrimethoxysilane were separated and recovered by centrifugation and distillation. The mother liquor of crystallization was recycled to achieve magnesium chloride recovery in an anhydrous environment.

Benefits of technology

It improves the yield of phenyl monomers and the recovery rate of raw materials, reduces processing costs, reduces environmental pollution, simplifies the process, and improves the purity and efficiency of magnesium chloride crystallization.

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Abstract

本发明涉及一种格氏法制备苯基单体废渣的处理方法,包括以下步骤:步骤(1),将格氏法制备苯基烷氧基硅烷废渣加入酮类溶剂中溶解,加入甲基氯硅烷,升温50‑80℃反应,反应后离心,收集白色固体氯化镁;步骤(2),离心母液加热精馏,收集三段馏分,降温析晶,收集白色固体氯化镁,结晶母液装桶回用;步骤(3),重复步骤(1)、步骤(2)的操作,将精馏塔负压加热,收集第四段馏分,将步骤(2)中结晶母液倒入精馏塔釜中,降温析晶,收集白色固体氯化镁,结晶母液用于下一次结晶操作。该方法可回收氯化镁、醚类溶剂、酮类溶剂和甲基烷氧基硅烷,降低废渣处理成本;释放被废渣包裹的甲基苯基烷氧基硅烷,提高了苯基单体收率。
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