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Method for extracting bromine-magnesium compound from Grignard reaction wastewater and mother liquor

A technology of Grignard reaction and compound, which is applied in the field of Grignard reaction wastewater and mother liquor treatment, can solve the problems such as the reduction of reaction yield, and achieve the effects of high purity, environmental protection and high yield

Active Publication Date: 2019-03-01
TIANJIN SEA WATER DESALINATION & COMPLEX UTILIZATION INST STATE OCEANOGRAPHI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the yield of most Grignard reactions is greater than 75%. Due to the following factors: after a long induction period, adding haloalkanes, iodine tablets or heating at the same time in advance, the reaction that has actually started slowly is suddenly accelerated, and excessive iodine is added after the reaction stops. The flakes will react violently and exothermic. In addition, the complexity of the reaction of some halogenated benzene and polyhalogenated methylbenzene compounds will produce by-products, which will cause the reaction yield to decrease.

Method used

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  • Method for extracting bromine-magnesium compound from Grignard reaction wastewater and mother liquor
  • Method for extracting bromine-magnesium compound from Grignard reaction wastewater and mother liquor
  • Method for extracting bromine-magnesium compound from Grignard reaction wastewater and mother liquor

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Effect test

Embodiment 1

[0025] Present embodiment provides a kind of method that extracts bromine-magnesium compound from Grignard reaction waste water and mother liquor, and its steps are as follows: see image 3 .

[0026] (1) Add compound alkali (mass fraction: NaOH is 10wt%, MgO is 90wt%) to distill and remove ammonia in Grignard reaction waste water and mother liquor, the pH of compound alkali is 11.0, heating temperature is to 106 ℃, heating time is 3h , During the heating process, ammonia gas is continuously precipitated, and a certain volume of water is used to absorb ammonia gas, and the change of pH value and concentration is dynamically detected. The final pH value was stable at 12.0, indicating that the ammonia gas had completely evolved.

[0027] (2) Suction filtration is carried out to the waste water after the deamination, after solid-liquid separation for the first time, after adopting 10 times of water to wash the solid phase filter cake after separation, carry out solid-liquid sepa...

Embodiment 2

[0030] Present embodiment provides a kind of method that extracts bromine-magnesium compound from Grignard reaction waste water and mother liquor, and its steps are as follows: see image 3 .

[0031] (1) Add composite alkali (mass fraction: NaOH is 20wt%, MgO is 80wt%) in Grignard reaction waste water and mother liquor and carry out distillation and remove ammonia, the pH of composite alkali is 11.5, and heating temperature is to 103 ℃, and heating time is 1.5 h, during the heating process, ammonia gas is continuously precipitated, and a certain volume of water is used to absorb ammonia gas, and the change of pH value and concentration is dynamically detected. The final pH value was stable at 11.8, indicating that the ammonia gas had been completely released.

[0032] (2) Suction filtration is carried out to the waste water after the deamination, after solid-liquid separation for the first time, after adopting 12 times of water to wash the solid phase filter cake after separ...

Embodiment 3

[0035] Present embodiment provides a kind of method that extracts bromine-magnesium compound from Grignard reaction waste water and mother liquor, and its steps are as follows: see image 3 .

[0036] (1) Add compound alkali (mass fraction: NaOH is 35wt%, MgO is 65wt%) to distill and remove ammonia in Grignard reaction waste water and mother liquor, the pH of compound alkali is 12.3, heating temperature is to 105 ℃, heating time is 2h , During the heating process, ammonia gas is continuously precipitated, and a certain volume of water is used to absorb ammonia gas, and the change of pH value and concentration is dynamically detected. The final pH value was stable at 12.1, indicating that the ammonia gas had completely evolved.

[0037] (2) Suction filtration is carried out to the waste water after the deamination, after solid-liquid separation for the first time, after adopting 10 times of water to wash the solid phase filter cake after separation, carry out solid-liquid sepa...

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Abstract

The invention relates to a method for extracting a bromine-magnesium compound from Grignard reaction wastewater and mother liquor, and belongs to the technical field of Grignard reaction wastewater and mother liquor treatment. The method comprises the following steps: adding composite alkali into the Grignard reaction wastewater and mother liquor for distillation and ammonia removal; performing solid-liquid separation on the ammonia-removed wastewater twice, and performing water washing and drying to obtain Mg(OH)2; mixing supernatant obtained after the two times of solid-liquid separation, acidifying, heating for evaporation, and cooling to obtain a bromine-magnesium compound solid product. According to the method, the composite alkali is added for evaporation to remove ammonia, solid-liquid separation is performed twice, the solid phase is washed with water and dried, and the liquid phase is acidified, evaporated and crystalized to obtain high-purity high-value Mg(OH)2, MgBr2.6H2O and MgCl2.6H2O. The method has high yield and high purity, and is suitable for industrial amplification, the problem of wastewater discharge is solved, and the valuable bromine-magnesium compound can beextracted efficiently.

Description

technical field [0001] The invention relates to the technical field of Grignard reaction wastewater and mother liquor treatment, in particular to a method for extracting bromine-magnesium compounds from Grignard reaction wastewater and mother liquor. Background technique [0002] Grignard reaction, as one of the most industrially valuable organic chemical reactions, was invented by French scientist Victor Grignard in 1899 and won the Nobel Prize in Chemistry in 1912. In anhydrous solvents (generally anhydrous ether, tetrahydrofuran), magnesium can react with halogen compounds of many aliphatic hydrocarbons and aromatic hydrocarbons to form magnesium organic compounds, which is called Grignard reaction, generally expressed as follows. Because the reactivity of haloalkyl groups varies, it is generally necessary to use elemental iodine as the initiator. [0003] The Grignard reaction is mainly used to construct the combination of carbon-carbon bonds. The main functional groups...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/22C01F5/36C01F5/30C02F9/10C02F101/10C02F101/12C02F103/16
CPCC01F5/22C01F5/30C01F5/36C01P2002/72C01P2006/80C02F1/001C02F1/04C02F1/66C02F9/00C02F2101/10C02F2101/12C02F2103/16C02F2301/08
Inventor 张欣刘伟吴丹张琦黄西平
Owner TIANJIN SEA WATER DESALINATION & COMPLEX UTILIZATION INST STATE OCEANOGRAPHI
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