Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing high-purity chloropinacolone through photocatalysis

A high-purity technology for pinatonone, which is applied in the efficient preparation of high-purity monochloropinatone and in the field of safety, can solve the problems of high impurity content of dichloropinatone, affecting the production of downstream products, and difficulty in solvent rectification and recovery. Achieve the effect of reducing the content of by-products, reducing costs and improving purity

Pending Publication Date: 2022-04-29
JIANGSU SWORD AGROCHEM +1
View PDF4 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthesis process is difficult to recover by solvent rectification (chlorination reaction generates a large amount of hydrochloric acid and reacts with methanol), and the content of dichloropinatone impurities produced by side reactions in the product is relatively high, which affects the production of downstream products, and the post-processing energy consumption of products is high. Disadvantages such as unsatisfactory

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing high-purity chloropinacolone through photocatalysis
  • Method for preparing high-purity chloropinacolone through photocatalysis
  • Method for preparing high-purity chloropinacolone through photocatalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: drop into 200g pinatone in clean 500ml gasification kettle. Turn on the stirring, turn on the light source: yellow light, the light intensity is 4000lux; when the system is heated to 105-108°C, open the chlorine valve of the reactor, let the chlorine gas into the reactor, and control the rate of the chlorine gas to be 2.1-3.4 g / min, the feed time is 6h; tail gas feeds into the tail gas treatment system: secondary absorption, the first level uses clear water to absorb, and the second level uses liquid caustic soda to absorb; Sampling detection, raw material peak pinazone is less than 1%, and the reaction ends; The system was cooled to room temperature to obtain 258.3 g of a chloropinatone product.

[0023] figure 2 For the mass spectrogram of the product obtained in this embodiment, wherein: the molecular ion peak of chloropinacolone is 134, and it itself also has a carbonyl group, and both sides of the carbonyl carbon can be split; each peak position is ...

Embodiment 2

[0025] Embodiment 2: drop into 200g pinatone in clean 500ml gasification kettle. Turn on the stirring, turn on the light source: purple light, the light intensity is 5000lux; when the system is heated to 105-108°C, open the chlorine gas valve of the reactor, let the chlorine gas into the reactor, and control the rate of chlorine gas introduction to 2.1-3.4g / min, the feeding time is 5h; tail gas feeds into the tail gas treatment system: secondary absorption, the first level uses clear water absorption, and the second level uses liquid caustic soda absorption; sampling detection, raw material peak pinazone is less than 1%, and the reaction is over; the system Cool down to room temperature to obtain 257.9 g of a chloropinatone product.

[0026] After testing, the yield of chloropinatone is 98.4%, and the tested quality is as follows: 98.3% of chloropinatone, 0.7% of chloropinatone, and 0.8% of dichloropinatone. As shown in Table 1.

Embodiment 3

[0027] Embodiment 3: drop into 200g pinatone in clean 500ml gasification kettle. Turn on the stirring, turn on the light source: red light, the light intensity is 4000lux; when the system is heated to 105-108°C, open the chlorine valve of the reactor, pass the chlorine gas into the reactor, and control the speed of introducing chlorine gas to 2.1-3.4 g / min, the feeding time is 5.5h; the tail gas is passed into the tail gas treatment system: secondary absorption, the primary use of clear water absorption, the secondary use of liquid alkali absorption; sampling detection, raw material peak pinazone is less than 1%, and the reaction is over; The system was lowered to room temperature to obtain 258.7 g of a chloropinatone product.

[0028] After testing, the yield of chloropinatone was 95.1%, and the tested quality was as follows: 95.2% of chloropinatone, 0.6% of chloropinatone, and 2.5% of dichloropinatone. As shown in Table 1.

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

PropertyMeasurementUnit
wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for efficiently preparing high-purity chloropinacolone, which comprises the following steps: adding quantitative pinacolone into a clean gasification kettle, and starting stirring; when the system is heated to 105-108 DEG C, pinacolone is gasified and enters the reactor, illumination is started, and chlorine is introduced into the reactor; the method comprises the following steps: reacting pinacolone with chlorine under an illumination condition to generate chloropinacolone; the outlet temperature of the reactor is ensured to be lower than 100 DEG C, pinacolone and chloropinacolone are liquefied and flow back into the gasification kettle, and hydrogen chloride gas generated by reaction can be discharged in time. According to the method disclosed by the invention, photocatalysis and gasification reaction are jointly applied to synthesis of the monochloropinacolone for the first time, and the obtained monochloropinacolone is high in yield, high in purity and low in byproduct content, and the quality of the monochloropinacolone is far higher than that of a product prepared by an existing process.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a safe and efficient method for preparing high-purity monochloropinatone. Background technique [0002] Chloropinacolone, scientific name is 1-chloro-3,3-dimethyl-2-butanone, English 1-Chloropinacolone is a white or light yellow transparent liquid, molecular weight 134.5, CAS No.13547-70-1 ; Molecular formula: C 6 h 11 OCl. Chloropinadone can undergo condensation reaction with many compounds, so it is widely used in the preparation of pesticides, such as: the production of triadimefon and triadimenol, diniconazolone, diniconazole, paclobutrazol, and benzylchlorotriaconol. [0003] At present, the preparation of chloropinatone mostly takes pinatone as the starting raw material, and realizes through taking methanol as the solvent, chlorinating reaction with chlorine, and rectifying and purifying. This synthesis process is difficult to recover by solvent recti...

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 Applications(China)
IPC IPC(8): C07C45/63C07C49/16B01D53/14
CPCC07C45/63B01D53/1406C07C49/16
Inventor 朱鹏顾晨刘志勇顾成希
Owner JIANGSU SWORD AGROCHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com