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Ethoxylate ester quaternary ammonium salt and its preparation method

A technology of ethoxylated ester and quaternary ammonium salts, which is applied in the preparation of amino hydroxyl compounds, sulfuric acid esters, chemical instruments and methods, etc., and can solve the problem of reducing the overall use of ester quaternary ammonium salts for triesteramine quaternary ammonium salts There are no reports on the modification of ester group quaternary ammonium salt, and the use effect is poor, so as to improve the difficulty of compounding, improve the overall use effect, and the effect of high content of active substances in the product

Inactive Publication Date: 2012-06-20
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The main components of ester-based quaternary ammonium salts are mono-, di-, and tri-ester amine quaternary ammonium salts. Among them, the best softening effect and antistatic effect are diester amine quaternary ammonium salts, followed by monoester amine quaternary ammonium salts. And triesteramine quaternary ammonium salt because of its poor water solubility, the actual use effect as a softener is poor, so the existence of triesteramine quaternary ammonium salt significantly reduces the overall use effect of ester-based quaternary ammonium salt products
At present, there is no report on the modification of ester quaternary ammonium salts to solve this problem

Method used

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  • Ethoxylate ester quaternary ammonium salt and its preparation method
  • Ethoxylate ester quaternary ammonium salt and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Mix 34.2g of MgO and 14g of diatomaceous earth evenly, add to 200mL of aqueous solution containing 11.5g of aluminum chloride, stir for 1hr, wash, dry, calcinate at 500°C for 1hr, grind, and sieve to obtain a composition of MgO with a composition of 65wt%. , Alumina is 8.4wt%, and diatomaceous earth is 26.6wt% Mg-Al ester-based insertion ethoxylation catalyst.

[0031] Take by weighing 284g stearic acid and join in the four-necked flask of 500mL, under N 2 Stir and heat up to 80°C under protected conditions. After they are completely melted, add 1.8g of phosphorous acid and 75g of triethanolamine, and heat up to 180°C. After 6 hours of reaction, the acid value of the product is measured to be 3mgKOH / g, and the reaction is terminated to obtain ester amine.

[0032] Add 0.4g of the above-mentioned ester group-inserted ethoxylation catalyst to the ester amine, put it into a 1L autoclave under stirring, start stirring, N 2 Replace the air, raise the temperature to 120°C, ...

Embodiment 2

[0035] Add 300mL of an aqueous solution containing 85g of aluminum nitrate and 27g of diatomaceous earth dropwise into 150mL of a dispersion containing 58g of CaO, and stir at room temperature for 1 hr to obtain a mixed catalyst slurry, which is removed by strong basic anion exchange resin. NO 3 - , after the ion exchange is completed, the catalyst is separated from the ion resin, dried, calcined at 500° C. for 1 hr, ground and sieved to obtain a Ca- Al ester-based intercalated ethoxylation catalyst.

[0036] Take by weighing 200g lauric acid and join in the four-neck flask of 500mL, under N 2 Stir and heat up to 90°C under protected conditions. After they are all melted, add 0.3g p-toluenesulfonic acid and 75g triethanolamine, heat up to 160°C, and react for 5 hours. The acid value of the product is 2.5mgKOH / g, stop reaction to give esteramine.

[0037] Add 1.6g of the above-mentioned ester group-inserted ethoxylation catalyst into the ester amine, put it into a 1L autocl...

Embodiment 3

[0040] Mix 20g of MgO powder with 9g of 4A zeolite, add to 500mL aqueous solution containing 1.9% gallium nitrate, stir vigorously for 1hr, dry at 110°C for 2hr, calcinate at 500°C for 1hr, grind and sieve to obtain MgO ester group containing gallium ions Plug-in ethoxylation catalyst. A gallium-ion-containing MgO ester-based insertion ethoxylation catalyst with a composition of 61.6 wt% of magnesium oxide, 10.7 wt% of gallium oxide and 27.7 wt% of 4A zeolite was obtained.

[0041] Take by weighing 256g palmitic acid and join in the four-neck flask of 500mL, under N 2 Stir and heat up to 60°C under protected conditions. After they are all melted, add 0.7g p-toluenesulfonic acid and 75g triethanolamine, heat up to 200°C, and react for 7 hours. The acid value of the product is 2.8mgKOH / g, stop reaction to give esteramine.

[0042] Add 3.8g of the above-mentioned ester group-inserted ethoxylation catalyst into the ester amine, put it into a 1L autoclave under stirring, start st...

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Abstract

An ethoxylate ester quaternary ammonium salt has chemical structural formula as follows, wherein R is C6-C22 saturated or unsaturated straight-chain or branched-chain alkyl; X represents an alkylated anion; n is the number of hydroxyethyl in the ester quaternary ammonium salt, and is 0, 2 or 3; n+b=3; b is 1, 2 or 3; and m is the number of ethoxyl, and is 1-30. The method has advantages of high conversion rate and good selectivity. The product has high content of active matters.

Description

technical field [0001] The invention belongs to an ethoxylated ester quaternary ammonium salt and a preparation method thereof, in particular to an ester quaternary ammonium salt synthesized by using ethylene oxide to ethoxylate an ester amine and then quaternizing it and its synthesis method. Background technique [0002] Ester-based quaternary ammonium salts are a new class of green cationic surfactants, which are easily biodegradable. They not only have excellent biodegradability, compounding properties, antistatic properties, and softness, but also have low raw material costs and will not cause fabric damage. After yellowing, it can produce high-concentration products, which is a typical representative of "green" softeners. In the late 1980s, as people paid more attention to environmental protection, esterquats developed rapidly. At present, esterquats prepared with triethanolamine as raw materials have become the most important products of fabric softeners in the inter...

Claims

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Application Information

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IPC IPC(8): C07C217/08C07C213/00C07C305/06C07C303/24C07F9/11C08G65/332C08G65/334C08G65/26B01F17/46C09K23/46
Inventor 孙永强李文静史修启张勇刘广宇杨卉艳
Owner CHINA RES INST OF DAILY CHEM IND
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