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Crystallization method of stearoylbenzoylmethane

A stearoylbenzoylmethane and crystallization technology, applied in the chemical field, can solve problems such as difficult separation and reuse, great impact on the environment, and large energy consumption, so as to reduce the separation and recovery process of toluene methanol and improve labor productivity , the effect of reducing production costs

Inactive Publication Date: 2009-09-16
ANHUI JIAXIAN FUNCTIONAL AUXILIARY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the distillate methanol toluene mixture of the condensation reaction in the existing process, it is difficult to effectively separate and reuse methanol and toluene due to the azeotropy, and the separation process is long, energy consumption is large, and because of its volatility, the impact on the environment Big
Generally, acetone or ethanol is used as the crystallization solvent, and the crystallization yields are 65% and 73% respectively, and the yield is relatively low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1. Condensation: Add 1600KG toluene to a 3000L reaction kettle equipped with a condenser and agitator and connected to a nitrogen source, then add 120KG sodium methoxide under a nitrogen atmosphere, raise the temperature of the above medium to 110°C, and The temperature is controlled at 110°C during the process. Add 600KG methyl stearate (98%), then add 200KG acetophenone in 3 hours. After the addition of acetophenone was complete, the reaction mixture was kept at temperature (110°C) for 1 hour. A total of 174L of methanol-toluene mixture was collected in the reaction.

[0015] 2. Acidification: Then add the thermally condensed solution into 20% hydrochloric acid solution, so that the pH of the water layer after settling is 1.

[0016] 3. Concentration: After the dilute acid layer is separated, it is washed with water. After washing 3 times, the acidified solution was distilled to remove toluene to obtain a solid crude product.

[0017] 4. Crystallization: The 174L ...

Embodiment 2

[0019] 1. Condensation: Add 1700KG toluene to a 3000L reaction kettle equipped with a condenser and agitator and connected to a nitrogen source, then add 120KG sodium methoxide under a nitrogen atmosphere, raise the temperature of the above medium to 110°C, and The temperature is controlled at 110°C during the process. Add 600KG methyl stearate (98%), then add 200KG acetophenone in 3 hours. After the addition of acetophenone was complete, the reaction mixture was kept at temperature (110°C) for 1 hour. A total of 207L of methanol-toluene mixture was collected during the reaction.

[0020] 2. Acidification: Then add the thermally condensed solution into 20% hydrochloric acid solution, so that the pH of the water layer after settling is 1.

[0021] 3. Concentration: After the dilute acid layer is separated, it is washed with water. After washing 3 times, the acidified solution was distilled to remove toluene to obtain a solid crude product.

[0022] 4. Crystallization: The 2...

Embodiment 3

[0024] 1. Condensation: Add 1800KG toluene to a 3000L reaction kettle equipped with a condenser and agitator and connected to a nitrogen source, then add 120KG sodium methoxide under a nitrogen atmosphere, raise the temperature of the above medium to 105°C, and The temperature is controlled at 105°C during the process. Add 600KG methyl stearate (98%), then add 200KG acetophenone in 3 hours. After the addition of acetophenone was complete, the reaction mixture was kept at temperature (105°C) for 1 hour. A total of 200 L of methanol-toluene mixture was collected during the reaction.

[0025] 2. Acidification: Then add the thermally condensed solution into 20% hydrochloric acid solution, so that the pH of the water layer after settling is 1.

[0026] 3. Concentration: After the dilute acid layer is separated, it is washed with water. After washing 3 times, the acidified solution was distilled to remove toluene to obtain a solid crude product.

[0027] 4. Crystallization: The ...

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PUM

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Abstract

The invention relates to a crystallization method of stearoylbenzoylmethane, comprising the following steps: condensating, acidifying, concentrating acetophenone, methyl stearate and sodium methoxide; dissolving the obtained solid crude product in crystallization solvent to crystallize; drying the filtered crystallized product to obtain stearoylbenzoylmethane product. Toluene as diluent is added into the reactant of the condensation reaction and the reaction temperature of the condensation reaction is kept 80-110 DEG C and the methanol toluene mixture liquid as distillate of the condensation reaction is collected, and the toluene mass ratio in the mixture liquid is adjusted to 10-50%; the concentrated solid crude product is dissolved in the methanol toluene mixture liquid to crystallize. The crystallization method has features of lily-white product, higher crystallization yield, reduced production cost and increased labor capacity.

Description

technical field [0001] The invention relates to a method for the industrial production of stearoylbenzoylmethane, and relates to the field of chemistry. Background technique [0002] The synthesis of stearoylbenzoylmethane started relatively late in China, and only a few academic chapters reported that the synthesis methods are basically the same, all of which use esters and ketones to undergo Claisen condensation reaction under strong alkaline conditions and in an appropriate solvent. , to prepare its sodium salt, and then get the product through acidification, concentration, crystallization and other processes. In the distillate methanol toluene mixture of the condensation reaction in the existing process, it is difficult to effectively separate and reuse methanol and toluene due to the azeotrope, and the separation process is long, energy consumption is large, and because of its volatility, the impact on the environment big. Generally, acetone or ethanol is used as the ...

Claims

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Application Information

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IPC IPC(8): C07C49/76C07C45/81C07C45/45
Inventor 赵信诚黄先胜李平周新源韩操陈启军
Owner ANHUI JIAXIAN FUNCTIONAL AUXILIARY