Method for reducing odor of mercaptocarboxylic acid ester

A technology of polymercapto carboxylate and mercapto carboxylate, which is applied in the chemical industry, can solve problems such as unpleasant odor of products, and achieve the effect of reducing odor

Active Publication Date: 2019-07-23
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the traditional production process of polymercaptocarboxylate, the residue of raw material mercaptocarboxylic acid will cause the product to have a strong unpleasant smell

Method used

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  • Method for reducing odor of mercaptocarboxylic acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] In a 1000ml four-neck flask equipped with a mechanical stirrer, a thermometer, and a reflux water separator, add 68.8g (0.50mol) of pentaerythritol, 214.1g (2.0mol) of 3-mercaptopropionic acid, 2.8g of catalyst methanesulfonic acid, and cyclohexane Alkanes 140.0g, heat reflux water separation, stop reaction after reaching theoretical water yield. Put the reacted mixture in a separatory funnel, divide the lower layer product into a four-necked flask, add 246.0 g of 3% sodium sulfite aqueous solution, stir for 20 minutes at 50-60° C., and transfer it to a separatory funnel for separation. layer for 10 minutes, divide the crude product of the lower layer into a four-neck flask, add 240.0 g of deionized water, stir at 50°C for 10 minutes, transfer to a separatory funnel to separate layers, and then perform a second water wash to obtain a washed crude product. Distilled for 2 hours under the conditions of pressure ≤ 5kPa, nitrogen flow rate of 8.0L / h / h·kg crude product, and ...

Embodiment 2

[0061] In a 1000ml four-necked flask equipped with mechanical stirring, a thermometer, and a negative pressure condensing device, add 68.8g (0.50mol) of pentaerythritol, 186.1g (2.0mol) of mercaptoacetic acid, 2.5g of catalyst methanesulfonic acid, and 127.0g of cyclohexane , heating to reflux to separate water, and stop the reaction after reaching the theoretical water output. Place the reacted mixture in a separatory funnel, divide the lower layer product into a four-necked flask, add 219.0 g of a 3% sodium sulfite aqueous solution configured by recovering water from Example 1, stir at 50-60° C. for 20 minutes, turn to Put into the separatory funnel to carry out layering for 10 minutes, divide the crude product of the lower layer into the four-necked flask, add 219.0g of the recovered water of Example 1, stir at 50°C for 10 minutes, transfer to the separatory funnel for layering, and then carry out the second Washing twice to obtain the washed crude product. Distilled for 2...

Embodiment 3

[0063] In a 1000ml four-necked flask equipped with mechanical stirring, a thermometer, and a negative pressure condensing device, add 67.7g (0.50mol) of trimethylolpropane, 160.7g (1.5mol) of 3-mercaptopropionic acid, and 2.3 g of catalyst methanesulfonic acid. g, cyclohexane 119.0g, heated to reflux to separate water, stop the reaction after reaching the theoretical water yield. Place the reacted mixture in a separatory funnel, divide the lower layer product into a four-necked flask, add 201.4 g of 2% sodium sulfite aqueous solution configured by recovering water in Example 2, stir at 50-60°C for 20 minutes, turn to Put into the separatory funnel to carry out stratification for 10 minutes, divide the crude product in the lower layer into the four-necked flask, add 201.4g of the recovered water of Example 2, stir at 50°C for 10 minutes, transfer to the separatory funnel for layering, and then carry out the second Washing twice to obtain the washed crude product. Distilled for...

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Abstract

The invention provides a method for reducing odor of a polymercaptic carboxylic acid ester, and the method comprises the following steps of: a) esterifying mercaptocarboxylic acid and polyol to obtainpolymercaptic carboxylic acid ester; (b) mixing the polythiol carboxylic ester and a weak alkali aqueous solution, heating, stirring, layering, and washing with water to obtain a washed crude product; C) distilling the washed crude product under a reduced pressure while introducing of nitrogen to obtain low-odor polythiol carboxylic ester. According to the invention, a raw material carboxylic acid is neutralized by a weak alkali, and converted into a carboxylic acid salt, the weak alkali is cleaned by subsequent water washing, and odor components are discharged by matching with specific nitrogen introduction and reduced pressure distillation, so that the odor of the product is greatly reduced, and the requirements of health and environmental protection in most application fields in contact with human bodies can be met.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for reducing the odor of polymercaptocarboxylates. Background technique [0002] Polymercapto carboxylates are important chemical and organic synthesis intermediates, among which pentaerythritol tetrakis (3-mercaptopropionic acid) ester is the esterification product of pentaerythritol and mercaptopropionic acid, mainly used for the synthesis of optical resins, and can be used for UV coatings, Modifiers, crosslinking agents, acidic ion exchange modifiers, etc. in polymerization reactions of inks and adhesives. [0003] In the traditional production process of polymercaptocarboxylate, the residue of raw material mercaptocarboxylic acid will cause the product to have a strong unpleasant smell. With the strengthening of people's awareness of environmental protection, the environmental protection requirements for daily necessities are getting higher and higher, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/12C07C319/28
CPCC07C319/12C07C319/28C07C323/52
Inventor 孙志利崔卫华费潇瑶任永平周芳晶江德阳
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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