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A kind of method for preparing 2-hydroxypropyl trimethyl isooctanoic acid ammonium salt

A hydroxypropyl trimethyl iso, ammonium octanoate technology, applied in the preparation of carboxylate, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of temperature sensitivity, high reaction temperature, affecting product quality, etc. Reduce color number and purity, shorten reaction time, reduce the effect of color number

Active Publication Date: 2021-09-03
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of the above method are: the reaction temperature is too high, which will lead to the formation of impurities with polyether structure and the improvement of product color number; , There is moisture in the target product, which affects product quality

Method used

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  • A kind of method for preparing 2-hydroxypropyl trimethyl isooctanoic acid ammonium salt
  • A kind of method for preparing 2-hydroxypropyl trimethyl isooctanoic acid ammonium salt
  • A kind of method for preparing 2-hydroxypropyl trimethyl isooctanoic acid ammonium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Mix 144.2g of isooctanoic acid and 261.4g of ethylene glycol and add them to the first reaction kettle. The reaction kettle is replaced with 1MPa (gauge pressure) nitrogen for 3 times, then pressurized to 5bar (gauge pressure) with nitrogen, and then poured into the reaction kettle Add trimethylamine gas at the bottom, control the feed flow rate to about 3g / min, and maintain the reaction temperature at 15°C. After the feed amount of trimethylamine reaches 70.9g, stop adding trimethylamine gas, and continue stirring for 2h. At 15°C, use a vacuum pump to depressurize and remove trimethylamine at a pressure of 5KPa (absolute pressure), stop the removal operation until there are no bubbles at the tail gas outlet of the vacuum pump, and obtain the first reaction solution.

[0047] In the second reactor, 2.88 g of pretreated 201×7 strong basic styrene-based anion-exchange resins have been added and placed in a nitrogen environment. Then use nitrogen to pressurize the first re...

Embodiment 2

[0050] Mix 144.2g of isooctanoic acid and 87.1g of ethylene glycol and add them to the first reaction kettle. The reaction kettle is replaced with 1MPa (gauge pressure) nitrogen for 3 times, then pressurized to 3bar (gauge pressure) with nitrogen, and then poured into the reaction kettle Add trimethylamine gas at the bottom, control the feed flow rate to about 3g / min, and maintain the reaction temperature at 20°C. After the feed amount of trimethylamine reaches 62.0g, stop adding trimethylamine gas, and continue stirring for 2h. At 20°C, use a vacuum pump to remove trimethylamine under reduced pressure at a pressure of 10KPa (absolute pressure), stop the removal operation until there is no bubbles at the tail gas outlet of the vacuum pump, and obtain the first reaction solution.

[0051] 2.16 g of pretreated 201×7 strong basic styrene-based anion exchange resins have been added to the second reaction kettle and placed in a nitrogen environment. Then use nitrogen to pressurize ...

Embodiment 3

[0054] Mix 144.2g of isooctanoic acid and 174.1g of ethylene glycol and add them to the first reaction kettle. The reaction kettle is replaced with 1MPa (gauge pressure) nitrogen for 3 times, then pressurized to 4bar (gauge pressure) with nitrogen, and then put into the reaction kettle Add trimethylamine gas at the bottom, control the feed flow rate to about 3g / min, and maintain the reaction temperature at 10°C. After the feed amount of trimethylamine reaches 59.0g, stop adding trimethylamine gas, and continue stirring for 2h. At 10°C, use a vacuum pump to remove trimethylamine under reduced pressure at a pressure of 0.1 KPa (absolute pressure), stop the removal operation until there is no bubbles at the tail gas outlet of the vacuum pump, and obtain the first reaction solution.

[0055] 0.72 g of pretreated 201×7 strong basic styrene-based anion exchange resin has been added to the second reaction kettle and it is in a nitrogen environment. Then use nitrogen to pressurize the...

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Abstract

The invention discloses a method for preparing 2-hydroxypropyl trimethyl isooctanoic acid ammonium salt, comprising: 1) reacting isocaprylic acid and trimethylamine in the presence of a solvent, and then removing trimethylamine in the reaction solution to obtain the first Reaction solution; wherein, the reaction temperature is 5-25°C, preferably 10-20°C; 2) In the presence of a basic anion exchange resin, react the first reaction solution with propylene oxide, filter and remove unreacted Propylene oxide to obtain 2-hydroxypropyl trimethyl isooctanoic acid ammonium salt. The preparation method of the invention has simple process, is suitable for industrial production, and the obtained product has high purity and low color number.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, in particular to a method for preparing 2-hydroxypropyltrimethylisooctanoic acid ammonium salt. Background technique [0002] 2-Hydroxypropyl trimethyl isooctanoic acid ammonium salt is a catalyst for the production of rigid polyurethane foam. It has a mild reaction and can accelerate the final curing of the foam without affecting the milk white time; at the same time, it is also a commonly used catalyst for isocyanate trimerization . [0003] There are not many patent literature reports on such quaternary ammonium salts as 2-hydroxypropyl trimethyl isooctanoic acid ammonium salt. US4040992A (1975) Air Chemical Company of the U.S. first reported the synthesis technique of this class of quaternary ammonium salt of N-hydroxyalkyl carboxylate, wherein, including the preparation method of trimethylamine hydroxypropyl isooctanoate, specifically: in Add 144g (1mol) of isooctanoic acid in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/41C07C53/126C07C213/04C07C215/40
CPCC07C51/412C07C213/04C07C53/126C07C215/40
Inventor 刘振国张聪颖李鑫王丛张兵周亚文
Owner WANHUA CHEM GRP CO LTD