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Process for synthesizing ethylenediamine-N-N'-disodium oxalic acid

A technology of disodium acetate and synthesis process, which is applied in the preparation of carboxylic acid nitrile, the preparation of organic compounds, organic chemistry, etc., can solve the problems of low purity, unsuitability for large-scale industrial production, and environmental protection, and achieve a simple reaction process Effect

Inactive Publication Date: 2016-10-26
HEBEI CHENGXIN
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] The present invention provides a kind of ethylenediamine-N-N'-di- The synthesis process of disodium acetate, the process is clean and environmentally friendly, with high purity, which reduces the difficulty of impurity removal

Method used

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  • Process for synthesizing ethylenediamine-N-N'-disodium oxalic acid

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Experimental program
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Embodiment 1

[0020] The detection method used in embodiment and comparative example:

[0021] Product liquid detection method: refer to GB / T1401-1998.

[0022] The reagent used in embodiment and comparative example:

[0023] Ethylenediamine: analytically pure, with a content greater than 99%; formaldehyde solution: analytically pure, with a mass concentration of 36.5%; hydrocyanic acid: industrial grade, with a content greater than 99%; NaOH: industrial grade, with a mass concentration of 30.5%

[0024] Example 1

[0025] Put 140.59g of formaldehyde into the four-neck bottle, add 47.81g of hydrocyanic acid dropwise at 5-10°C, and keep warm for 1 hour after the dropwise addition to obtain a hydroxyacetonitrile solution; In the ethylenediamine, the dropping temperature is 25-30°C, and after the dropping is completed, the temperature is kept for 3 hours to obtain the intermediate product EDDN aqueous solution with a content of 49.6%.

[0026] After mixing the intermediate product EDDN aque...

Embodiment 2

[0027] Embodiment 2 (ethylenediamine: formaldehyde: HCN=1:2.00:2.00)

[0028] Put 141.18g of formaldehyde into the four-neck bottle, add 46.38g of hydrocyanic acid dropwise at 10-15°C, and keep warm for 2 hours after the dropwise addition to obtain a hydroxyacetonitrile solution; In the ethylenediamine, the dropwise addition temperature is 25-30° C., and after the dropwise addition is completed, the temperature is kept for 4 hours to obtain an intermediate product EDDN aqueous solution with a content of 48.5%.

[0029] After mixing the intermediate product EDDN aqueous solution obtained in the previous step with liquid caustic soda, first raise the temperature to 60°C for 2 hours, then raise the temperature to 110-115°C for alkaline hydrolysis, reflux for 2 hours, and remove the ammonia gas generated by the reaction at the same time to obtain EDDA-2Na liquid products. The liquid product of EDDA-2Na is dehydrated to 100°C under normal pressure, and then dried at 100-150°C to o...

Embodiment 3

[0030] Embodiment 3 (ethylenediamine: formaldehyde: HCN=1:1.95:1.95)

[0031] Put 133.64g of formaldehyde into the four-neck bottle, add 43.91g of hydrocyanic acid dropwise at 10-16°C, and keep warm for 3 hours after the dropwise addition to obtain a hydroxyacetonitrile solution; In the ethylenediamine, the dropwise addition temperature is 20-25°C, and after the dropwise addition is completed, the temperature is kept for 5 hours to obtain an intermediate product EDDN aqueous solution with a content of 47.5%.

[0032] After mixing the intermediate product EDDN aqueous solution obtained in the previous step with liquid caustic soda, first raise the temperature to 60°C for 2 hours, then raise the temperature to 110-115°C for alkaline hydrolysis, reflux for 2 hours, and remove the ammonia gas generated by the reaction at the same time to obtain EDDA-2Na liquid products. The liquid product of EDDA-2Na is dehydrated to 100°C under normal pressure, and then dried at 100-150°C to obt...

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Abstract

The invention discloses a process for synthesizing ethylenediamine-N-N'-disodium oxalic acid, and belongs to the field of technologies for synthesizing chemical compounds. The process includes carrying out reaction on glycolonitrile aqueous solution and ethylenediamine to obtain an intermediate ethylenediamine-N-N'-diacetonitrile; carrying out alkaline hydrolysis on the intermediate and dehydrating and drying the intermediate to obtain the ethylenediamine-N-N'-disodium oxalic acid. The intermediate and liquid caustic soda are mixed with each other to obtain mixtures when alkaline hydrolysis is carried out on the intermediate, the mixtures are heated until the temperature of the mixtures reaches 60-65 DEG C at first, then heat is preserved for 2-2.5 h, the mixtures are further heated until the temperature of the mixtures reaches 110-115 DEG C, and reflex heat preservation is carried out for 2-2.5 h to obtain alkaline hydrolysis liquid. The process has the advantages that the process is environmentally friendly, ammonia gas which is a byproduct can be absorbed by water to obtain ammonia water, and accordingly generation of waste gas, wastewater and industrial residues can be prevented; the alkaline hydrolysis temperatures are controlled, accordingly, generation of impurities such as disodium ethylenediamine nitrilotriacetic acid, ethylenediamine-sodium acetate and ethylenediamine tetraacetic acid disodium salt can be effectively controlled, and the ethylenediamine-N-N'-disodium oxalic acid which is a product is high in purity.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and relates to a synthesis process of ethylenediamine-N-N'-diacetate disodium. The process of the invention is simple to operate, environmentally friendly and pollution-free, and the prepared ethylenediamine-N-N'-diacetate disodium High purity and high yield. Background technique [0002] Ethylenediamine-N-N'-disodium diacetate (EDDA-2Na), is white powder or colorless liquid. This product can be used as a pharmaceutical intermediate to synthesize ethylenediamine-N-N'-diacetic acid (alias: No. 1 hemostatic injection), which plays an important role in medicine; it can be used as a material intermediate to synthesize pesticide auxiliary N-N'-bis Sodium lauroyl ethylenediamine diacetate, N-N'-bisdecanoyl ethylenediamine diacetate; downstream products include 2-oxo-1-piperazine acetic acid, etc.; it can also be used as a chemical reagent in the field of fine chemicals. This product is wid...

Claims

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Application Information

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IPC IPC(8): C07C227/02C07C229/16C07C253/30C07C255/24
CPCC07C227/02C07C253/00C07C253/30C07C229/16C07C255/24C07C255/12
Inventor 李燕贾荣荣陈雨佳杨晓林张艳章张林杰程真真
Owner HEBEI CHENGXIN
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