Method of synchronously preparing DL-tartaric acid and DL-potassium hydrogen tartrate

A technology of potassium hydrogen tartrate and tartaric acid, which is applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation, etc., can solve the problems of waste of resources, low conversion rate, increased production cost, etc., and achieve fewer reaction steps, High conversion and yield, easy to control effect

Active Publication Date: 2013-04-03
ZHEJIANG GONGSHANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the production process of tartaric acid at home and abroad is a chemical synthesis method, that is, maleic anhydride is used as a raw material, tungsten oxyacid or its salt is used as a catalyst, and hydrogen peroxide is used as an oxidant to prepare epoxysuccinic acid, and then hydrolysis and crystallization Prepare tartaric acid, centrifuge tartaric acid, adjust mother liquor pH value with potassium hydroxide to prepare its hydrogen potassium salt, then separate, mother liquor is sent to waste water pool, this is a relatively ideal route, with few by-products, but the process is not The conversion rate is not high; moreover, the mother liquor contains unreacted raw materials and unreacted maleic acid generated by the direct hydrolysis of the raw materials. If the mother liquor is directly discharged, it will cause waste of resources and increase production costs; meanwhile, it contains heavy metal tungsten The discharge of waste water has also caused serious environmental pollution problems.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1, a kind of preparation method of DL-tartaric acid, carries out following steps successively:

[0030] 1) Add 100 g of deionized water, 100 g of maleic anhydride, and 150 g of hydrogen peroxide with a mass concentration of 28% in sequence in the reactor; heat up to 50°C for 3 hours;

[0031] 2) Add 5 g of phosphomolybdenum heteropoly acid as a catalyst to the product obtained in step 1), and then slowly raise the temperature at a rate of 6°C / h; when the temperature rises to 72°C, stop heating;

[0032] 3) Insulate and react at 72°C for 20 hours; then heat up to 110°C, and hydrolyze for 3.5 hours to obtain a solution containing epoxysuccinic acid;

[0033] Cool the solution containing epoxysuccinic acid with cooling water, and use ice brine instead when the temperature drops to about 25°C. When the temperature drops to 6~8°C, it will crystallize naturally, and then filter it with a rotary vacuum pump (vacuum degree 0.08; used Filter paper pore size 15~20 mic...

Embodiment 2

[0037] Embodiment 2,4-aminopyridine chelating resin reclaims the catalyst in the mother liquor

[0038] Put 30mg of 4-aminopyridine resin into 25ml of acetic acid-sodium acetate buffer solution with a pH of 4.1 and soak for 20-24 hours to obtain swollen 4-aminopyridine resin.

[0039] Add 10ml of the secondary mother liquor obtained in the above-mentioned Example 1 (after testing, the molybdenum ion content is 1.7mg / ml) to the above-mentioned swollen 4-aminopyridine resin, and use the pH value of the 4-aminopyridine resin after adsorption equilibrium to be 4.1 After washing with acetic acid-sodium acetate buffer solution (5 times in total, 60ml each time), wash several times with deionized water (5 times in total, 60ml each time), and dry to constant weight After soaking (need to be fully submerged), perform vibration desorption in 25ml of NaOH solution with a concentration of 3mol / L; when the concentration of molybdenum ions in the NaOH solution remains unchanged, the adsorpt...

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PUM

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Abstract

The invention discloses a method of synchronously preparing DL-tartaric acid and DL-potassium hydrogen tartrate. The method comprises the following steps: 1) sequentially adding deionized water, maleic anhydride and hydrogen peroxide in a reactor, heating and raising temperature to take reaction; 2) adding phosphorus-molybdenum heteropoly acid as a catalyst into the product obtained in the step 1), and slowly raising the temperature; 3) preserving heat at 70-74 DEG C and taking reaction for 18-22 hours; raising the temperature to 105-115 DEC C, taking hydrolysis reaction for 3-4 hours to obtain a solution comprising 2,3-epoxysuccinic acid; reducing the temperature of the solution comprising 2,3-epoxysuccinic acid to 6-8 DEG C, and naturally crystallizing; and then, performing suction filtration, wherein the obtained filtrate is primary mother solution, and the obtained crystal is dried to obtain DL-tartaric acid; and 4) regulating the pH value of the primary mother solution to 3.5-3.8 by a potassium hydroxide solution with the mass concentration of 45-55%; reducing the temperature to room temperature, and naturally crystallizing, and then performing suction filtration, wherein the obtained filtrate is secondary mother solution, and the obtained crystal is dried to obtain DL-potassium hydrogen tartrate.

Description

technical field [0001] The invention relates to a method for preparing DL-tartaric acid, in particular to a method for simultaneously preparing DL-tartaric acid and DL-potassium hydrogen tartrate. Background technique [0002] Tartaric acid, namely, 2,3-dihydroxysuccinic acid, is a carboxylic acid that exists in various plants such as grapes and tamarind, sweet horn, and is also one of the main organic acids in wine. There are two asymmetric carbon atoms in the tartaric acid molecule, so there are three optical isomers, namely, L-tartaric acid or L-tartaric acid, D-tartaric acid or D-tartaric acid, and meso-tartaric acid. Equal amounts of L-tartaric acid and D-tartaric acid are mixed to obtain racemic tartaric acid or DL-tartaric acid. DL-tartaric acid is widely used in food, medicine, chemical industry, light industry and other industries, mainly for the manufacture of tartrates, and in the food industry as beer foaming agent, food sour agent, flavoring agent, and sour age...

Claims

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Application Information

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IPC IPC(8): C07C59/255C07C51/367C07C51/41
Inventor 熊春华陈昕怡何若铭
Owner ZHEJIANG GONGSHANG UNIVERSITY
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