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Production method for preparing high-purity solid malonic acid from calcium malonate

A technology of calcium malonate and a production method, which are applied in the directions of carboxylate preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problem of restricting downstream applications, high cost of high-purity malonate products, and malonate diacids. The problem of high price of ethyl ester can achieve the effect of low material consumption and energy consumption, avoiding cumbersome extraction operation and low production cost.

Inactive Publication Date: 2020-08-18
龙智
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the price of the raw material diethyl malonate is relatively high, and the high-purity malonate produced by this method is expensive, which greatly limits its downstream application.

Method used

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  • Production method for preparing high-purity solid malonic acid from calcium malonate

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Example 1: Put 519.1 g of calcium malonate and 3.5 times the quality of calcium malonate into an acidification reaction kettle to stir and make a slurry, add 1197.24 g of 35% sulfuric acid dropwise at 52 ° C, filter after the reaction is completed and wash the calcium sulfate filter with water Combine the washing water and the filtrate to obtain the acidified liquid, measure the free sulfate content in it, add barium hydroxide according to 1.8 times of the theoretical amount, and add a certain amount of activated carbon fiber for desulfurization and decolorization, filter out activated carbon residue and barium sulfate precipitation and refine After filtration, enter the cation exchange resin column for purification to obtain Ca 2+ An aqueous solution of malonic acid with a content of 0.02 wt%. The cation exchange resin is regenerated by electric regeneration technology. The malonic acid aqueous solution was evaporated and concentrated under negative pressure, cooled a...

Embodiment 2

[0046] Example 2: Put 572.53 g of calcium malonate and 2.1 times the quality of calcium malonate into an acidification reaction kettle to stir and make a slurry, add 1024.2 g of 30% phosphoric acid dropwise at 60 ° C, filter and wash the calcium phosphate filter after the reaction is completed Cake, combined washing water and filtrate to obtain acidified liquid, measure free phosphate content in it, add barium hydroxide according to 2.1 times of theoretical amount, add a certain amount of modified zeolite molecular sieve adsorbent at the same time to dephosphorize and decolorize, filter out adsorbent residue After precipitation with barium phosphate and fine filtration, enter the cation exchange resin column for purification to obtain Ca 2+ An aqueous solution of malonic acid with a content of 0.01 wt%. The cation exchange resin is regenerated by electric regeneration technology. The malonic acid aqueous solution was evaporated and concentrated under negative pressure, cooled...

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Abstract

The invention discloses a production method for preparing high-purity solid malonic acid from calcium malonate. Calcium malonate is acidified by sulfuric acid or phosphoric acid to obtain a salt-containing malonic acid solution, then high-purity solid malonic acid is prepared by refining and purifying means such as solid-liquid separation, barium hydroxide desulfurization or dephosphorization, decoloration and ion exchange; the main content of the produced solid malonic acid product is greater than or equal to 99.5%, and the produced solid malonic acid product does not contain an organic solvent and is low in production cost.

Description

technical field [0001] The invention relates to a production method of calcium malonate for preparing high-purity solid malonate, especially a production method for producing low-cost high-purity solid malonate with a main content ≥ 99.5% and no organic solvent. The field of chemical intermediates. Background technique [0002] Malonate CH 2 (COOH) 2 , also known as carrot acid, beet acid, and malic acid, are widely used in spices, adhesives, resin additives, pharmaceutical intermediates, food additives, electroplating polishing agents, explosion control agents, etc., and are important fine chemical intermediates . [0003] There is no national standard for malonic acid products in our country, only enterprise standards, and general manufacturers can only achieve the main content of the product ≥ 99.0%, and cannot produce products with higher purity. Malonic acid products with a main content of ≥99.5% are generally called high-purity products. According to the enterpris...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/02C07C51/42C07C51/47C07C51/487C07C55/08
CPCC07C51/02C07C51/42C07C51/47C07C51/487C07C55/08
Inventor 龙智高春燕李宽义
Owner 龙智
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