A kind of synthetic method of citric acid

A synthetic method, the technology of citrazinic acid, applied in the direction of organic chemistry, etc., can solve the problems of high consumption, excessive amount of NaOH, difficulty in obtaining the final product with high purity, etc., and achieve simple operation, high product purity and high yield Effect

Active Publication Date: 2021-02-02
ZHEJIANG NORMAL UNIVERSITY
View PDF5 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

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 well;

[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.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention belongs to the technical field of compound preparation, in particular to a method for synthesizing citrazinic acid. The present invention adopts the hydrothermal reaction method of citric acid and urea, and the specific steps include: dissolving citric acid and urea in deionized water, ultrasonically dispersing, and fully mixing; then in the reactor, carry out hydrothermal reaction under certain temperature conditions; Finally, the reaction solution is centrifuged at high speed, the supernatant is removed, and the obtained yellow precipitate is dried to obtain the citrazine acid product with good color, high yield and high purity. The method of the invention has mild reaction conditions, simple operation, only one step of sulfuric acid hydrolysis, high product purity (>96%), and high yield (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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap