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Method for synthesizing powdered nitric acid by using allantoin synthetic waste liquid

A technology of allantoin and nitric acid, applied in chemical instruments and methods, preparation of organic compounds, preparation of urea derivatives, etc., can solve problems such as environmental pollution and complicated recycling process, and achieve the goal of reducing environmental pollution and reducing production costs Effect

Inactive Publication Date: 2013-06-12
李无为
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the domestic production scale of allantoin has reached 2,000 tons, and the production scale continues to expand, but the actual production yield of allantoin production in enterprises is only 40%-55%, and the acidic waste mother liquor containing high concentration of urea is difficult to handle, causing serious environmental pollution , which limits the expansion of the production scale of allantoin
Chinese patent CN102060392 (2011-05-18) discloses a method for synthesizing corrosion and scale inhibitors with allantoin waste liquid, but the recycling process is relatively complicated and special equipment needs to be added

Method used

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  • Method for synthesizing powdered nitric acid by using allantoin synthetic waste liquid

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Experimental program
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Embodiment 1

[0023] In a 500 mL four-necked reaction flask equipped with a mechanical stirrer, a thermometer, a dropping funnel, and a reflux condenser, 120 g (2.0 mol) of urea, 200 mL of deionized water and 183 g of 50% sulfuric acid were added. Heat to 60-70° C. in a water bath, add 92 g (0.5 mol) of 40.2% industrial glyoxylic acid within 0.5 hours, and stir for 4 hours to complete the reaction. Cool the reactant to 20°C, centrifuge and wash to obtain a wet product of allantoin. The allantoin synthesis mother liquor is about 500g, of which urea accounts for about 60g (1.0mol), sulfuric acid 92g, and diuretic acid by-product about 40g.

[0024] Concentrate the mother liquor in vacuum to about half volume, put it into a 500mL four-necked reaction bottle, cool it to below 5°C with ice water, slowly add 97g (1.0mol) of dilute nitric acid with a concentration of 65% by weight under stirring, and constantly have nitric acid Precipitation of white urea crystals, control the reaction temperatur...

Embodiment 2

[0026] In a 500mL four-necked reaction flask equipped with a mechanical stirrer, a thermometer, a dropping funnel, and a reflux condenser, add urea 120g (2.0mol), 31% concentrated hydrochloric acid 200mL and 40.2% industrial glyoxylic acid 92g (0.5mol), Heating in a water bath, stirring at 60-70°C for 4 hours, cooling the condensation reaction liquid to 20°C, centrifuging and washing to obtain the allantoin wet product. The allantoin synthesis mother liquor is about 350g, of which urea accounts for about 61g (1.0mol), hydrochloric acid 62g, and diuretoacetic acid by-product about 35g.

[0027] Concentrate the mother liquor in vacuum to about half volume, put it into a 500mL four-neck reaction bottle, cool it to below 5°C with ice water, slowly add 97g (1.0mol) of dilute nitric acid with a concentration of 65% by weight under stirring, and constantly have nitric acid White urea crystals are precipitated. Control the reaction temperature below 20°C during feeding, keep the tempe...

Embodiment 3

[0029] In a 500mL four-necked reaction flask equipped with a mechanical stirrer, a thermometer, a dropping funnel, and a reflux condenser, add urea 120g (2.0mol), deionized water 200mL, 50% nitric acid 50mL and 40.2% industrial glyoxylic acid 92g ( 0.5mol), heated in a water bath, stirred at 60-70°C for 4 hours, cooled the condensation reaction solution to 20°C, centrifuged, washed to obtain the wet product of allantoin. The allantoin synthesis mother liquor is about 400g, of which urea accounts for about 63g (1.05mol), nitric acid is 32g, and diuretoacetic acid by-product is about 30g.

[0030]Concentrate the mother liquor in vacuum to about half volume, put it into a 500mL four-neck reaction bottle, cool it to below 5°C with ice water, a small amount of white crystals of urea nitrate precipitates, slowly add 48.5% dilute nitric acid with a concentration of 65% by weight under stirring g (0.5mol), control the reaction temperature below 20°C during the feeding, keep the reacti...

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Abstract

The invention discloses a method for synthesizing powdered nitric acid by using allantoin synthetic waste liquid. A preparation process is that 40%-50% of percentage concentration by weight of allantoin synthetic waste liquid is added in a reactor for cooling until the temperature is lower than 5 DEG C, 50%-65% of percentage concentration by weight of dilute nitric acid is added during stirring, a molar ratio of nitric acid to urea in reaction liquid is controlled to be 1:0.9-1.1 during material adding, the temperature of the reaction liquid is controlled to be below 20 DEG C, materials are reacted for 0.5-2.0 hours at the temperature of 15 DEG C after material adding is completed, the reaction liquid is cooled to the temperature below 5 DEG C, centrifugal separation is carried out to separate out crystallization, vacuum drying is carried out on the crystallization at the temperature of 50 DEG C, and powdered nitric acid products are obtained. The nitric acid content in the products is 48%-50%, and the allantoic acid impurity content in the products is 3%-5%.

Description

technical field [0001] The invention relates to a method for synthesizing powdered nitric acid, in particular to a method for synthesizing powdered nitric acid with allantoin synthesis waste liquid, and belongs to the fields of petrochemical industry and environmental protection. Background technique [0002] Currently on the market is a powder nitric acid whose chemical composition is actually urea nitrate, which is obtained by the reaction of nitric acid and urea in an equimolar ratio. Contains about 10% moisture. Urea nitrate is solid at room temperature, and becomes acidic when dissolved in water. Its acidity is slightly lower than that of nitric acid, and its chemical stability is better. The solid product itself is not corrosive. It can be used instead of nitric acid in many occasions and make up for the shortage of liquid nitric acid. [0003] British patent GB1109619 (1966-04-29) first disclosed the preparation method of urea nitrate, which made nitric acid and urea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C275/02C07C273/02
Inventor 李无为李建生
Owner 李无为