Synthetic process of herbicide dicamba

A technology for dicamba and herbicides, which is applied in the preparation of organic compounds, the preparation of carboxylates, organic chemistry, etc., can solve the problems of long reaction time, high energy consumption and low yield, etc., and achieves long reaction time and single-pass yield. Low rate and good product quality

Active Publication Date: 2013-02-27
JIANGSU YOUJIA CHEM +2
View PDF6 Cites 51 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process route is that the reaction time is long, the energy consumption is high and the productive rate is not high

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
  • Synthetic process of herbicide dicamba

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) Synthesis of potassium 2,5-dichlorophenate

[0028] 300g of anhydrous toluene and 65g of 2,5-dichlorophenol were added to the 500ml reaction flask, 21.2g of KOH was added under stirring at room temperature, and the reaction was continued for 1hr-2hr. After removing the water, cool down. A toluene solution of potassium 2,5-dichlorophenolate was obtained almost quantitatively.

[0029] 2) Synthesis of 3,6-dichlorosalicylic acid

[0030] 379g of the toluene solution of potassium 2,5-dichlorophenolate obtained in step 1), 96g of powdered anhydrous potassium carbonate, 3g of butanol and 3g of triethylamine were added to a 500ml autoclave. After introducing an appropriate amount of carbon dioxide, start heating and stirring, control the temperature in the kettle to 130 ° C, and slowly introduce CO 2 to a pressure of 5.0MPa. Add CO slowly as the reaction progresses 2 To ensure that the temperature and pressure in the kettle are maintained at 130°C and 5.0MPa. And in t...

Embodiment example 2

[0034] 1) Synthesis of potassium 2,5-dichlorophenate

[0035] 300g of anhydrous xylene and 65g of 2,5-dichlorophenol were added to the 500ml reaction flask, 21.2g of KOH was added under stirring at room temperature, and the reaction was continued for 1hr-2hr. After removing the water, cool down. An almost quantitative xylene solution of potassium 2,5-dichlorophenolate was obtained.

[0036] 2) Synthesis of sodium 3,6-dichlorosalicylate

[0037] 80.1 g of dried and ground potassium 2,5-dichlorophenate, 96 g of powdered anhydrous potassium carbonate, 2.8 g of octanol and 4.2 g of diisopropylamine were added to a 500 ml autoclave. After introducing an appropriate amount of carbon dioxide, start heating and stirring, control the temperature in the kettle to 135 ° C, and slowly introduce CO 2 to a pressure of 6.0MPa. Add CO slowly as the reaction progresses 2 To ensure that the temperature and pressure in the kettle are maintained at 135°C and 6.0MPa. And keep in this state f...

Embodiment 3

[0041] 1) Synthesis of potassium 2,5-dichlorophenate

[0042] 300g of anhydrous toluene and 65g of 2,5-dichlorophenol were added to the 500ml reaction flask, 22.2g of KOH was added under stirring at room temperature, and the reaction was continued for 1hr-2hr. After removing the water, cool down. A toluene solution of potassium 2,5-dichlorophenolate was obtained almost quantitatively.

[0043] 2) Synthesis of sodium 3,6-dichlorosalicylate

[0044] 379g of the toluene solution of potassium 2,5-dichlorophenolate obtained in step (1), 96g of powdered anhydrous potassium carbonate, 4g of butanol and 2g of triethylamine were added to a 500ml autoclave. After introducing an appropriate amount of carbon dioxide, start heating and stirring, control the temperature in the kettle to 140 ° C, and slowly introduce CO 2 to a pressure of 6.0MPa. Add CO slowly as the reaction progresses 2 To ensure that the temperature and pressure in the kettle are maintained at 140°C and 6.0MPa. And ...

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 relates to a preparation method of herbicide dicamba. The preparation method includes: (1) liquid potassium hydroxide and 2, 5-dichlorophenol are reacted according to molar ratio of 0.95:1-1:1 to obtain 2, 5-dichlorophenol potassium; (2) at the presence of anhydrous potassium carbonate and catalyst, the 2, 5-dichlorophenol potassium obtained in the step (1) is reacted with CO2 to generate 3, 6-dichlorosalicylic acid, pressure of CO2 is controlled to be 4-6MPa, reaction temperature ranges from 100 DEG C to 160 DEG C, and molar ratio of anhydrous potassium carbonate and 2, 5-dichlorophenol potassium is 1-2:1; and (3) in alkaline condition, at the temperature of 70-100 DEG C, the 3, 6-dichlorosalicylic acid obtained in the step (2) and chloromethane are reacted under the action of the catalyst through a tube fixed-bed reactor according to molar ratio 1:1-3.5, saponification and acidification are performed to obtain 3, 6-dichloro-2-methoxysalicylic acid, namely the dicamba. The process is high in reaction yield, simple in reaction condition, good in product quality, small in three wastes and low in energy consumption.

Description

technical field [0001] The invention relates to a synthesis process of a herbicide dicamba. Background technique [0002] Dicamba, also known as paraben, is a benzoic acid herbicide, which is an efficient and broad-spectrum herbicide and is widely used. It has the characteristics of strong selectivity, low dosage and low cost. It is mainly used for field control of annual and perennial broad-leaved weeds in wheat and other gramineous crops with remarkable effect. Dicamba is used for post-emergence spraying. The medicament can be quickly absorbed by the leaves, stems and roots of weeds and conduct upward and downward through the phloem and wood. It is mostly concentrated in the meristem and the parts with strong metabolic activities, which hinder the normal activities of plant hormones. , resulting in its death. Generally, broadleaf weeds will appear deformed and curled within 24 hours after application of dicamba, and die within 15-20 days. The grass plants quickly metabo...

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): C07C65/21C07C51/347C07C51/15
Inventor 戚明珠王东朝孔勇汪国庆解邦伟吴越徐骏
Owner JIANGSU YOUJIA CHEM
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