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Synthesis method of citrazinic acid

A synthesis method and technology of citrazine acid, applied in directions such as organic chemistry, can solve problems such as high consumption, excessive NaOH amount, and difficulty in obtaining pure final products, and achieve simple operation, high product purity, and high yield. Effect

Active Publication Date: 2018-06-15
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if the amount of NaOH is too large, more H 2 SO 4 neutralize
Simultaneously generated Na 2 SO 4 It is easy to crystallize out during cooling, and it is difficult to obtain a high-purity final product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation of embodiment 1 citric acid

[0015] (1) Dissolve 1.2188 g (0.0058 mol) of citric acid and 1.3932 g (0.0231 mol) of urea in 60 ml of deionized water, sonicate for 10 min, and mix well;

[0016] (2) Put the mixed solution into a 100 ml reaction kettle, set the oven temperature to 185°C, and keep it warm for 2 hours under hydrothermal conditions; cool to room temperature to obtain a dark green solution;

[0017] (3) Place the solution in a 60°C constant temperature water bath, stir it magnetically, and drop 50% sulfuric acid into the solution until the pH of the solution is 2-3. A large amount of yellow solid precipitates are observed, and centrifuged at 12000 r / min for 5 min Remove the supernatant, wash with deionized water several times, and then dry the obtained yellow precipitate in an oven at 60°C to obtain 70.66% citrazinic acid product.

[0018] Characterization of citric acid

[0019] 1. UV and fluorescence analysis

[0020] The compound has two...

Embodiment 2

[0023] The preparation of embodiment 2 citric acid

[0024] (1) Dissolve 1.2188 g (0.0058 mol) of citric acid and 2.0898 g (0.0348 mol) of urea in 60 ml of deionized water, sonicate for 10 min, and mix thoroughly;

[0025] (2) Put the mixed solution into the reaction kettle, set the oven temperature to 185°C, and keep it warm for 2 hours under hydrothermal conditions; cool to room temperature to obtain a dark green solution;

[0026] (3) Place the solution in a 60°C constant temperature water bath, stir it magnetically, and drop 50% sulfuric acid into the solution until the pH of the solution is 2-3. A large amount of yellow solid precipitates are observed, and centrifuged at 12000 r / min for 10 min Remove the supernatant, wash with deionized water for several times, and dry the obtained yellow precipitate in an oven at 60°C to obtain 72.78% of the citrazinic acid product.

Embodiment 3

[0027] Embodiment 3 citric acid preparation

[0028] (1) Dissolve 1.2188 g (0.0058 mol) of citric acid and 1.3932 g (0.0231 mol) of urea in 60 ml of deionized water, sonicate for 10 min, and mix thoroughly;

[0029] (2) Put the mixed solution into the reaction kettle, set the oven temperature to 185°C, and keep it warm for 2 hours under hydrothermal conditions; cool to room temperature to obtain a dark green solution;

[0030] (3) Place the solution in a constant temperature water bath at 60°C, stir it magnetically, and drop 98% sulfuric acid into the solution until the pH of the solution is 2-3. A large amount of yellow solid precipitation is observed, and centrifuged at 12000 r / min for 10 min Remove the supernatant, wash with deionized water for several times, and dry the obtained yellow precipitate in an oven at 60°C to obtain 85.18% of the citrazinic acid product.

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PUM

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Abstract

The invention belongs to the technical field of compound preparation and particularly relates to a synthesis method of citrazinic acid. The method adopts a hydrothermal reaction method of citric acidand urea and particularly comprises the steps of dissolving citric acid and urea in deionized water, performing ultrasound dispersion and intensive mixing, performing a hydrothermal reaction under a certain temperature condition in a reaction kettle, performing high-speed centrifugation on reaction liquid at last, removing a supernate, and drying an obtained yellow precipitate, namely a citrazinicacid product with good color, high yield and high purity. The method is mild in reaction condition, and simple to operate; one-step sulfuric acid hydrolysis is required only, and the product is highin purity (greater than 96%) and productivity (70-85%).

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a synthesis method of citrazinic acid. Background technique [0002] Citrazinic acid (Citrazinic Acid, CA) is a heterocyclic compound containing a hydroxyl group and a pyridine ring structure, which can be used as a raw material for the synthesis of a series of pyridines, pyrimidines and oxazolones. In addition, citrazinic acid can also indirectly detect heavy metal ions through diazonium and coupling reactions, and it can be used as a starting material for TiO on solar cells (DSCs). 2 Fixation of sensitizers. Citric acid is used as a bleaching agent and a fixer in the field of photography, and as an inhibitor and cosolvent in the electroplating industry. Its derivatives have a certain antibacterial effect when combined with amphetamine. In electrochemistry, citrazine can be used as an electrochemical sensor to detect biological small molecules. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/79C07D213/803
CPCC07D213/79C07D213/803
Inventor 翁雪香王嘉君向雪琴陈静茹阮永明
Owner ZHEJIANG NORMAL UNIVERSITY