Method for increasing yield of dimethyl malonate

A technology of dimethyl malonate and methyl cyanoacetate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, purification/separation of carboxylic acid nitriles, etc., and can solve the problems of cyanoacetic acid decomposition, easy decomposition of cyanoacetic acid, and consumption of sulfuric acid Acidic waste water and other problems, to avoid reaction, improve dispersion performance and mass transfer heat transfer, reduce the amount of use and the effect of waste water production

Inactive Publication Date: 2017-03-15
内蒙古紫光化工有限责任公司
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Problems solved by technology

[0006] The shortcoming that this method exists is: the reaction process of synthesizing cyanoacetic acid produces a large amount of inorganic salt sodium chloride, and the mixture of cyanoacetic acid and salt carries out esterification reaction after being concentrated, but cyanoacetic acid is easy to decompose after being concentrated, and because ther

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  • Method for increasing yield of dimethyl malonate
  • Method for increasing yield of dimethyl malonate
  • Method for increasing yield of dimethyl malonate

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Embodiment 1

[0037] A preparation method for dimethyl malonate, comprising the steps of:

[0038] 1) Neutralization reaction: Add 620kg of water to 445kg of chloroacetic acid (98% by mass, 4.62kmol) and stir to dissolve, then neutralize with saturated aqueous sodium carbonate to pH=6.5-7.0 to generate sodium chloroacetate.

[0039] 2) Cyanide reaction: the sodium chloroacetate that step 1) obtains is transferred to the cyanide reaction kettle, is warming up to 50 ℃, then drips the sodium cyanide aqueous solution 765kg that mass concentration is 30% (containing 4.68kmol sodium cyanide in the aqueous solution ), when the reaction temperature reaches 85-90°C, stop heating and start cooling, when the reaction temperature reaches 105°C (the later stage is a strong exothermic reaction), the reaction ends, and it is cooled to room temperature to obtain an aqueous solution containing sodium cyanoacetate.

[0040] 3) Acidification reaction: transfer the sodium cyanoacetate aqueous solution obtained...

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Abstract

The invention provides a method for increasing the yield of dimethyl malonate. The method includes the steps of: 1) acidification reaction: adding acid or hydrogen chloride gas into sodium cyanoacetate to carry out reaction to obtain a cyanoacetic acid aqueous solution; 2) distillation and concentration: adding methyl cyanoacetate into the cyanoacetic acid aqueous solution, conducting distillation and concentration until no water flows out, and removing inorganic salt solid; 3) first esterification reaction: adding methanol and a catalyst into the desalted solution of step 2) to carry out esterification reaction, thus obtaining a solution containing methyl cyanoacetate; 4) desalting: removing inorganic salt solid from the solution; and 5) second esterification reaction: dividing a part of the desalted solution in step 3) and reusing it to step 2), adding methanol to the other part of solution, and carrying out esterification reaction under an acidic condition, thus obtaining dimethyl malonate. The method provided by the invention reduces the consumption of sulfuric acid and generation of wastewater, avoids the decomposition of cyanoacetic acid in the process of concentration and dehydration, and effectively improves the yield of dimethyl malonate.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for improving the yield of dimethyl malonate. Background technique [0002] Dimethyl malonate is an intermediate of medicines, pesticides and dyes. At present, there are many production methods at home and abroad. In China, cyanation esterification is mainly used, that is, chloroacetic acid, sodium cyanide and methanol are used as raw materials, and after neutralization , Cyanide, acidification and esterification processes to obtain dimethyl malonate. [0003] Common synthetic methods are as follows: [0004] 1. Direct esterification of cyanoacetic acid [0005] [0006] The shortcoming that this method exists is: the reaction process of synthesizing cyanoacetic acid produces a large amount of inorganic salt sodium chloride, and the mixture of cyanoacetic acid and salt carries out esterification reaction after being concentrated, but cyanoacetic acid is easily decom...

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Application Information

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IPC IPC(8): C07C67/22C07C69/38C07C253/34C07C255/23
CPCC07C67/22C07C253/14C07C253/34C07C69/38C07C255/23
Inventor 丁永良刘佳唐大家邓建伟刘兵刘文枚
Owner 内蒙古紫光化工有限责任公司
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