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Method for increasing esterification reaction rate of pentaerythritol tetramercaptopropionate in synthesis process

A technology of tetramercaptopropionate and pentaerythritol, which is applied in the chemical industry, can solve the problems of low water separation efficiency and slowness, and achieve the effects of increasing the concentration of hydrogen ions, shortening the reaction time, and increasing the rate of esterification reaction

Active Publication Date: 2021-03-12
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as the reaction progresses, less water will be generated in the later stage, and the reflux solvent will not be able to fully stratify with water in the future. In addition, water will have a certain solubility in the solvent with water, which will greatly reduce the water separation efficiency in the later stage of the reaction. lead to a slower reaction in the latter part of the

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Reaction stage: Add 136g of pentaerythritol, 424g of 3-mercaptopropionic acid, 11.2g of methanesulfonic acid, and 560g of cyclohexane into a three-necked flask with condenser, water separator and stirring respectively, start stirring and condensing circulating water, and heat to The reaction is carried out in the reflux state, and the water generated by the reaction is separated from the reaction system through the water separator and metered. When the water content of the reaction reached 90% of the theoretical value, 36 g of methanesulfonyl chloride was added to the reaction system, and the reflux reaction was continued. HPLC followed the reaction process, and when the content of pentaerythritol tetramercapto propionate reached 70%, the reaction was stopped.

[0035] Aftertreatment stage: reaction is cooled to below 60 ℃, adds sodium hydroxide solution (5wt%) to the system, the pH value is adjusted to 4, after stirring for 30min, separate the lower floor product phase,...

Embodiment 2

[0038] Reaction stage: Add 136g of pentaerythritol, 424g of 3-mercaptopropionic acid, 11.2g of methanesulfonic acid, and 560g of cyclohexane into a three-necked flask with condenser, water separator and stirring respectively, start stirring and condensing circulating water, and heat to The reaction is carried out in the reflux state, and the water generated by the reaction is separated from the reaction system through the water separator and metered. When the reaction water content reached 90% of the theoretical value, 22 g of phosphorus pentoxide was added to the reaction system, and the reflux reaction was continued. HPLC followed the reaction process, and when the content of pentaerythritol tetramercapto propionate reached 70%, the reaction was stopped.

[0039] Post-treatment stage: the reaction is cooled to below 60°C, and sodium carbonate solution (5wt%) is added to the system to adjust the pH value to 5. After stirring for 30min, the lower product phase is separated, and...

Embodiment 3

[0042]Reaction stage: Add 136g of pentaerythritol, 424g of 3-mercaptopropionic acid, 11.2g of methanesulfonic acid, and 560g of cyclohexane into a three-necked flask with condenser, water separator and stirring respectively, start stirring and condensing circulating water, and heat to The reaction is carried out in the reflux state, and the water generated by the reaction is separated from the reaction system through the water separator and metered. When the reaction water content reached 90% of theoretical value, phosphorus pentoxide 11g, p-toluenesulfonyl chloride 24g were added to the reaction system, and the reflux reaction was continued. HPLC followed the reaction process. When the content of pentaerythritol tetramercaptopropionate reached 70%, Stop responding.

[0043] Post-treatment stage: the reaction is cooled to below 60°C, add sodium phosphate solution (5wt%) to the system, adjust the pH value to 6, stir for 30min, separate the lower product phase, and add equal qua...

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Abstract

The invention provides a method for increasing the esterification reaction rate in the pentaerythritol tetramercaptopropionate synthesis process, which comprises the following steps: under the actionof a catalyst, carrying out esterification reaction on pentaerythritol and 3-mercaptopropionic acid until the water distribution amount reaches a theoretical value of 87-92%, adding a water removal agent into the reaction system, continuing the reaction, and stopping the reaction after the requirements are met to obtain the pentaerythritol tetramercaptopropionate, wherein the water removal agent is selected from one or more of phosphorus pentoxide, solid phosgene, methylsulfonyl chloride and p-toluenesulfonyl chloride. According to the method provided by the invention, the water removal agentis added in the later stage of esterification reaction of pentaerythritol and mercaptopropionic acid, so that water generated in the reaction can be removed, corresponding acid is generated, the hydrogen ion concentration of a reaction system is increased, the esterification reaction rate is increased, and the reaction time is shortened. Experimental results show that the method obviously shortensthe reaction time by more than 1 / 3.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for increasing the esterification reaction rate in the synthesis process of pentaerythritol tetramercapto propionate. Background technique [0002] Pentaerythritol tetramercaptopropionate is an important class of mercaptans, which are widely used in thiol-ene photopolymerization systems. It is also used as a high-performance curing agent for epoxy resins due to its high reactivity with epoxy groups at low temperatures. . In addition, the cross-linking polymerization of pentaerythritol tetramercaptopropionate and polyisocyanate is also used to prepare optical elements. For example, Maojiao Kuma et al. disclosed the synthesis and application of high-purity pentaerythritol mercaptocarboxylate in Chinese patent 200780009306.1. [0003] The synthesis of pentaerythritol tetramercaptopropionate is mainly based on pentaerythritol and mercaptopropionic acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/12C07C323/52C08G18/38
CPCC07C319/12C08G18/3876C07C323/52
Inventor 于龙易先君江德阳邢莹莹陈志敏张建林
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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