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Preparation process of mixture ester as foamer

A technology of mixed esters and foaming agents, which is applied in the preparation of organic compounds, carboxylic acid esters, chemical instruments and methods, etc. It can solve the problems that chemical wastes cannot be completely treated, achieve good catalytic effects, reduce production costs, and reduce pollution. little effect

Inactive Publication Date: 2006-02-22
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Since the by-product sodium bisulfate with good catalytic effect is used as a catalyst to directly carry out the esterification reaction to prepare mixed esters and use them as foaming agents, the problem that a large amount of chemical waste cannot be completely processed is solved. The present invention has the following remarkable features and effects :

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: Add 450g of acid oil with acid value of 305mgKOH / g and water content of 11.0% into a 1L esterification reactor, press n(organic acid): n(C 4 ~C 5 Alcohol) = 1.0: 1.1 total molar ratio, add 246g of fusel oil with a boiling range of 105 to 134°C with 90% distillate of 57.0% isoamyl alcohol, 22.3% isobutanol, and 10.7% n-butanol. Add 24g of solid sodium bisulfate which accounts for 3.5% of the total mass of the reactants, react at 110~160℃ for 10h, the acid value of the esterification reaction material drops to 5.72mgKOH / g, cool to 70℃, separate the catalyst, and obtain the carboxylic acid mixed ester liquid 575g.

[0013] The quality index of the mixed ester is: acidity 1.04% (calculated as valeric acid, Wt), ester content 96.0% (Wt), apparent viscosity 2.8×10 -2 pa.s (200°C). Organic acid and C 4 ~C 5 The recovery rate of alcohol reached 99.0%. Taking coal preparation as an example, the measured performance of the ester product (A) and its correlation with 2 # The...

Embodiment 2

[0014] Example 2: Add 300g of acid oil with acid value of 305mgKOH / g and water content of 11.0% into a 1L esterification reactor, press n(organic acid): n(C 4 ~C 5 Alcohol) = 1.0:2.8 total molar ratio, add 416g of fusel oil with a boiling range of 105-134°C, 90% of isoamyl alcohol 57.0%, isobutanol 22.3%, and n-butanol 10.7%, and then Add 10.5g of solid sodium bisulfate, which accounts for 1.5% of the total mass of the reactants, and react at 100~150℃ for 3h. The acid value of the esterification reaction material is reduced to 8.90mgKOH / g, and the temperature is lowered to 40℃ to separate the catalyst to obtain a mixed carboxylic acid ester. Liquid 603g.

[0015] The quality index of mixed ester is: acidity 1.62% (calculated as valeric acid, Wt), ester content 60.8% (Wt), apparent viscosity 9.0×10 -3 pa.s (20°C). Organic acid and C 4 ~C 5 The recovery rate of alcohol was 98.8% and 98.0%, respectively. Taking coal preparation as an example, the measured performance of the ester pro...

Embodiment 3

[0016] Example 3: Add 400g of acid oil with acid value of 305mgKOH / g and water content of 11.0% into an esterification reactor with a capacity of 1L, press n(organic acid): n(C 4 ~C 5Alcohol) = 1.0: 1.1 total molar ratio, adding the separated epoxy cyclohexane containing 41.20% n-pentanol, 15.79% isoamyl alcohol, 17.62% tert-amyl alcohol, 4.71% cyclopentanol, and 7.18% isobutanol Add 22.0g of solid sodium bisulfate, which accounts for 3.5% of the total mass of the reactant, and react at 110~160℃ for 10h. The acid value of the esterification reaction material drops to 7.33mgKOH / g, and the temperature is reduced to 50℃. Catalyst to obtain 520 g of carboxylic acid mixed ester liquid.

[0017] The quality index of the mixed ester is: acidity 1.33% (calculated as valeric acid, Wt), ester content 96.1% (Wt), apparent viscosity 2.7×10 -2 pa.s (20°C). Organic acid and C 4 ~C 5 The recovery rate of alcohol reached 99.0%. Taking coal preparation as an example, the measured performance of th...

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Abstract

The invention discloses a method of preparing carboxylic acid mixed ester as foaming agent by making direct esterification reaction on organic waste acid and alcohol oil under the catalyste action: a. adding organic waste acid in a reaction kettle, adding in alcohol oil in molar ratio of organic acid to alcohol contained, and then adding in catalyst to make esterification reaction; b. carrying the water during water by a water-carrying agent and azeotropism, making stratification in an oil-water separator, and returning the oil layer; c. lowering temperature and separating the catalyst to obtain mixed ester liquid. Because the project of adopting by-product sodium bisulfate as catalyst for making direct esterification, it solves the difficulty in thoroughly treating large numbers of chemical wastes. It completely adopts chemical wastes or by-product as raw material, obviously reducing the production cost, reducing environmental pollution. The product can integrate foaming and catching functions in one during coal separation and can completely replace widely used 2# oil at present.

Description

Technical field [0001] The invention relates to a method for preparing a mixed ester used as a foaming agent, in particular to a method for preparing a mixed ester by directly carrying out an esterification reaction of organic waste acid and alcohol oil under the action of a catalyst. Background technique [0002] In the existing industry, in the oxidation of cyclohexane to produce cyclohexanone or cyclohexanol, a large amount of acidic oil or acidic wastes will be produced, which accounts for about 10% of the corresponding product output. The acid value of these organic waste acids is generally above 280mgKOH / g, of which: 25%~50%C 4 ~C 6 Monobasic acid, 10%~20%C 4 ~C 6 Dibasic acid, 5%-10% hydroxycaproic acid, 5%-10% other acids and 8%-20% moisture. Aiming at the utilization of acidic oil or acidic waste, the "Preparation and Application of New Composite Flotation Agent ME" written by Zhang Jinglai et al. (〖J〗. Coal, 2001, 10(1): 28-29) discloses the use of carboxylic acid For a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08B03D1/02
CPCY02P20/582
Inventor 石顺存
Owner HUNAN UNIV OF SCI & TECH