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A kind of removal method of alkali catalyst

A base catalyst and removal technology, applied in organic chemistry, ether separation/purification, carboxylate separation/purification, etc., can solve problems such as waste water discharge, unqualified product quality, product loss, etc.

Active Publication Date: 2022-02-11
浙江锦润生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, firstly, there is waste water discharge; secondly, after the product is neutralized and washed, vacuum dehydration is required to remove the moisture in the material; thirdly, during the washing process, a small amount of product will be discharged together with the washing water, resulting in product loss Fourth, it is necessary to strictly control the amount of acid. If the acid is excessive, the product quality of the product will also be unqualified or the product will be lost due to increased washing.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 276g of pure glycerin and 1.4g of catalyst sodium hydroxide into the reaction flask respectively, start stirring at the same time, pass nitrogen gas, and carry out glycerin polymerization to prepare tripolyglycerol. The reaction temperature is 245°C, and the reaction water is about 36g. At 80°C, the pH value of the reaction system was determined to be 9 with a pH meter for sampling, and carbon dioxide gas was introduced, and about 1.5 L of carbon dioxide gas was metered in to terminate the reaction. The pH value of the reaction system was measured with a pH meter for sampling to be 7.2. The reaction feed liquid is press-filtered (or high-speed centrifuged) to obtain the target product.

[0031] Note: Unreacted carbon dioxide from the reaction bottle enters the water-sealed bottle and dissolves in water to generate carbonic acid.

Embodiment 2

[0033] Add 300g of glyceryl tristearate, 60g of pure glycerin and 1.5g of catalyst sodium hydroxide into the reaction flask respectively, start stirring at the same time, feed nitrogen, and carry out the reaction to prepare glyceryl monostearate, the reaction temperature is 215 ± 5 ℃, reaction time 2h. End the reaction, lower the temperature to 90°C, measure the pH value of the reaction system with a pH meter for sampling, and measure the pH value of the reaction system to be 8.5, feed carbon dioxide gas, measure and feed about 1.6L of carbon dioxide gas, end the reaction, and measure the pH value of the reaction system with a pH meter for sampling for 7. The reaction feed liquid was filtered to obtain the target product.

[0034] Note: Unreacted carbon dioxide from the reaction bottle enters the water-sealed bottle and dissolves in water to generate carbonic acid.

Embodiment 3

[0036] 800kg of glyceryl tristearate, 200kg of pentaerythritol, and 4.5kg of sodium hydroxide were added to the reaction kettle respectively, and at the same time, stirring was started, nitrogen gas was introduced, and the transesterification reaction was carried out to prepare pentaerythritol glycerol stearate complex ester. React at 225±5°C for 150 minutes, end the reaction, and lower the temperature to 100°C. The pH value of the reaction system was measured by a pH meter for sampling to 8.5, carbon dioxide gas was introduced for about 60 minutes, and about 4.5 cubic meters of carbon dioxide gas was introduced into the reaction meter, and the reaction was terminated, and the pH value of the reaction system was measured by a pH meter for sampling to be 6.8 . The reaction feed liquid was filtered to obtain the target product.

[0037] Note: Unreacted carbon dioxide from the reactor enters the water-sealed tank, dissolves in water, and generates carbonic acid.

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Abstract

The invention provides a method for removing the alkali catalyst, which comprises the following steps: introducing carbon dioxide into an organic reaction system to generate solids, and then removing the solids to realize the removal of the alkali catalysts. In the present invention, by introducing carbon dioxide into the system, carbon dioxide reacts with an alkali catalyst to generate carbonate and / or bicarbonate, wherein the carbonate and / or bicarbonate cannot be dissolved in the organic reaction system and are separated out in solid form. However, the target product of the organic reaction is still dissolved in the reaction system. The invention realizes the removal of the alkali catalyst by removing the solid in the reaction system. The method provided by the invention can effectively remove the alkali catalyst in the reaction system, and the method provided by the invention has zero discharge and does not cause loss to products.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for removing an alkali catalyst. Background technique [0002] In the esterification reaction and the polymerization reaction, the catalysts used are mostly alkali catalysts, such as transesterification reactions, transesterification reactions, glycerol polymerization to prepare polyglycerol, etc. The catalysts are generally sodium hydroxide or potassium hydroxide. For the above reaction, after the reaction is finished, the catalyst needs to be removed from the reaction system, and then the target product can be separated. [0003] In the prior art, the method for removing the alkali catalyst is generally to add acid to neutralize and then wash with water. In this method, firstly, there is waste water discharge; secondly, after the product is neutralized and washed, vacuum dehydration is required to remove the moisture in the material; thirdly, during the wash...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/34C07C43/13C07C67/48C07C69/30C07C69/33A23D7/02
CPCC07C41/34C07C67/48A23D7/02C07C43/135C07C69/30C07C69/33
Inventor 李熊伟李建成
Owner 浙江锦润生物科技有限公司
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