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Method for synthesizing nitrilotriacetic acid by raffinate obtained from iminodiacetonitrile by hydrocyanic acid method

A technology of iminodiacetonitrile and nitrilotriacetic acid, applied in chemical instruments and methods, cyanide reaction preparation, organic compound preparation, etc., can solve the problems of high processing cost, rare HCN raw materials, high production cost, etc., and achieve safe operation The effects of low requirements, thorough treatment methods, and few types and quantities

Inactive Publication Date: 2009-08-12
黄代忠
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Problems solved by technology

[0005] The shortcomings of the above methods are: high processing cost, uneconomical, easy to cause secondary pollution, and great damage to the environment
[0006] 2. There are few foreign reports on the treatment of IDAN residual liquid, among which CA1117550 describes a method for recovering IDAN from IDAN waste liquid, that is, using dichloromethane (CH 2 CL 2 ) to extract the waste water containing IDAN, the cost of this method is too high, and the secondary pollution produced needs further treatment
This method involves the highly toxic substance sodium cyanide, which requires high safety protection requirements for transportation, storage and operation, and high production costs.
[0010] ③. Hydrocyanic acid method: Hydrocyanic acid (HCN), formaldehyde, and ammonia water are mixed and reacted to synthesize NTA in one step. This method involves the highly toxic substance HCN, which requires high safety protection for production equipment sealing and operation, and HCN raw materials are rare. And easy to aggregate, generally ready-to-use, the investment is too large

Method used

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  • Method for synthesizing nitrilotriacetic acid by raffinate obtained from iminodiacetonitrile by hydrocyanic acid method

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Measure the raffinate of 500ml IDAN (containing 50.4g / l of hydroxyacetonitrile, 162.1g / l of aminoacetonitrile, 37.3g / l of iminodiacetonitrile, 19.3g / l of nitrilotriacetonitrile, which is thicker in black) and add 863g of 30% NaOH solution, Stir evenly, gradually heat to 115°C for hydrolysis, the ammonia produced by hydrolysis is absorbed with 40% sulfuric acid solution to generate ammonium sulfate. Hydrolyze for 4.5 hours, cool and add appropriate amount of water to dilute to obtain 800ml of hydrolyzate [containing glycine (GLY) 177.1g / l, iminodiacetic acid (IDA) 32.7g / l, nitrilotriacetic acid (NTA) 17.2g / l], in Add 375.6g (100%) chloroacetic acid at 15°C, adjust the pH of the reaction solution to about 11 with 30% liquid alkali, then raise the temperature to 55-60°C, and keep the reaction for 5 hours. During the heat preservation reaction process, use 30% liquid caustic soda to adjust the pH of the reaction solution to 11 to 12. After the reaction is completed, cool an...

Embodiment 2

[0027] Measure 500ml of the hydrolyzed solution after hydrolysis of IDAN residue with KOH (containing GLY210.1g / lIDA50.4g / l NTA26.3g / l pH=9.6), add KOH131.6g and cool to 20°C, add chloroacetic acid 282.5g, stir Heat up to 50-60°C, keep stirring for 1 hour, keep using KOH to keep the pH of the reaction solution greater than 9 during the heat-retaining reaction process, use 195g of KOH, after the reaction is completed, cool at 20-30°C and acidify with 31% hydrochloric acid, the pH of the acidified solution is 1.0 , cooled and crystallized for 2 hours, suction filtered and washed at 23° C. to obtain 465 g of NTA wet product with a content of 62.8%. Based on GLYIDANTA in the hydrolyzate, the yield was 92.1% of the theoretical yield. The filtrate is neutralized with KOH, decolorized, concentrated, crystallized, and dried to obtain potassium chloride solid, which is used as a raw material for potash fertilizer.

[0028] Suspend the above NTA wet product in 1000ml of water, heat to 6...

Embodiment 3

[0030] Inject 282LIDAN raffinate in 1500L enamel reaction kettle with the hydrolyzed solution after NaOH hydrolysis, solution pH=11.3 (containing GLY 119.3g / l IDA 107.6g / l NTA 56.6g / l), then add 30.2% liquid caustic soda 298KG, Slowly add 110kg of chloroacetic acid (96.5%) at 20-25°C under stirring and cooling, after the addition is complete, stir for 20 minutes, then slowly heat to 50-60°C, keep warm for 4 hours, take samples and analyze and calculate, the conversion rate of chloroacetic acid is 101.2% . Cool the reaction solution, add concentrated sulfuric acid for acidification, when the pH=4 or so, NTA solids start to precipitate, after acidification to pH=0.8, stop adding acid, cool and crystallize for 4.5 hours, and centrifuge to get 200.2KG gray-black solid, NTA content 69.3% %, based on the GLY IDA NTA in the hydrolyzate, the wet product yield is 95.5%, the centrifuged mother liquor is black, add acidic activated carbon 12KG, decolorize at room temperature for 12 hours...

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Abstract

The invention provides a method for synthesizing nitrilotriacetic acid by using residual liquid of iminodiacetonitrile produced by a hydrocyanic acid method, comprising: 1) preparation of crude product of the nitrilotriacetic acid: the residual liquid of the iminodiacetonitrile is added with alkali to be hydrolyzed at the temperature of 30-150DEG C, the hydrolysate is added with chloroactic acid, the pH value of the mixed solution is adjusted to be 9-14 by alkali at 10-100 DEG C, the reaction liquid is acidulated by acid after the reaction lasts for 0.5-10h, and the pH value is adjusted to be 0.5-2, finally, the crude product of the nitrilotriacetic acid can be separated out; (2) preparation of finished product of the nitrilotriacetic acid: the crude product of the nitrilotriacetic acid is suspended in the water and added with alkali, ammonia water or ammonium hydrogen carbonate to neutralize the solution under agitation, so as to lead the pH value of the solution to be 3-6; activated carbon is added into the mixed solution for decolourization until the mixed solution is colorless at the temperature of 20-90 DEG C, then the colorless mixed solution is filtered, filtrate is added with acid to be neutralized until the pH value is 0.5-2, and the separated white nitrilotriacetic acid solid is filtered and dried to obtain the finished product of the nitrilotriacetic acid. The method has the advantages of being easy in raw material acquisition as well as low in safety requirement of operation and production cost, changing waste into valuable, and being beneficial to environmental protection.

Description

Technical field: [0001] What the present invention relates to is a kind of " three wastes " treatment method, particularly utilizes the raffinate that produces iminodiacetonitrile (IDAN, is the raw material of producing herbicide glyphosate) by hydrocyanic acid (HCN) method, synthesizes nitrilotriacetic acid ( NTA) method. Background technique: [0002] NTA is mainly used as metal complexing agent, catalyst, stabilizer, detergent, etc., and is widely used in synthetic detergent, textile printing and dyeing, soap making industry, electroplating industry, etc. [0003] At present, there are the following technical methods for the raffinate treatment of the production of iminodiacetonitrile by the HCN method at home and abroad. [0004] ①. At present, the domestic treatment of IDAN raffinate is mainly as follows: a. Directly mixed with rice bran to form solid matter, which is used as fertilizer. b. Send directly to the boiler for incineration. c. Discharge directly after dil...

Claims

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Application Information

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IPC IPC(8): C07C229/16C07C227/08
Inventor 黄代忠
Owner 黄代忠
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