Check patentability & draft patents in minutes with Patsnap Eureka AI!

Method for preparing 10,10'-oxyphenoxarsine of industrial anti midew agent

A technology of antifungal agent and phenoxopyr, which is applied in the field of preparation of organic arsenic compounds, can solve the problems of preventing, affecting the yield and quality of OBPA, and incomplete reaction, etc., and achieves the effect of simple process, easy operation and complete reaction

Inactive Publication Date: 2004-10-06
SHANGHAI NO 4 REAGENT & H V CHEM +1
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The OBPA generated in the reaction between CPA and NaOH covers the surface of CPA particles, which will prevent further reaction, make the reaction incomplete, and affect the yield and quality of OBPA. This problem is especially obvious in large-scale production.

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 10,10'-oxyphenoxarsine of industrial anti midew agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The preparation of embodiment 1 CPA

[0013] 7670 grams of diphenyl ether and 120 grams of aluminum trichloride were heated under stirring, and 1410 grams of arsenic trichloride was added dropwise when the temperature reached 250 ° C. During the dropwise addition, the temperature was maintained at 246-250 ° C until the end of the dropwise addition. Then the solid was precipitated by cooling, and then recrystallized in methanol solution to obtain CPA crystals with a content of 98%.

Embodiment 2

[0014] The preparation of embodiment 2 OBPA

[0015] Add 28.6 grams of CPA prepared in Example 1 into 50 grams of 8% NaOH solution and 250 grams of dichloroethane, stir and heat at a stirring rate of 180 cpm, react at 60°C for 8 hours, separate the water phase, wash with water to remove NaCl, and evaporate The solvent was removed to obtain 50.2 g of OBPA with a content of 99.8% (HPLC), a melting point of 184.4-186°C, and a yield of 99.3%.

[0016] Infrared absorption spectrum characteristic frequency (cm -1 ): 685.1 753.5

[0017] Mass Spectrometry:

[0018] Mass-to-charge ratio (m / z) 243 168 244 139 502 231 214 113

[0019] Absorption rate (%RA) 100 28.3 12.15 11.54 8.30 3.23 2.78 2.51

Embodiment 3

[0020] The preparation of embodiment 3 OBPA

[0021] Add 28.6 grams of CPA prepared in Example 1 into 50 grams of 15% NaOH solution and 500 grams of chloroform, stir and heat at a stirring rate of 80 cpm, react at 80° C. for 4 hours, separate the water phase, wash with water to remove NaCl, and evaporate the solvent. 50.3 g of OBPA was obtained, with a content of 99.6% (HPLC), a melting point of 184.4-186° C., and a yield of 99.5%. The mass spectrometry and infrared analysis were the same as in Example 2.

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

A process for preparing industrial antimildew agent 10,10'-oxybiphenoxarsine (OBPA) features the thermal reaction of 10-chlorophenoxarisin (CPA) and the aqueous solution of sodium hydroxide in solvent. It is possible to add phase-transfer catalyst. Its advantages are high output rate (99.3-99.7%), and high purity (99.5-99.8%).

Description

technical field [0001] The invention relates to a preparation method of an organic arsenic compound, in particular to a preparation method of an industrial antifungal agent 10,10'-oxybisphenoxarsin (OBPA, 10,10'-Oxybisphenoxarsin). Background technique [0002] 10,10′-Oxydiphenoxopyridine is a heterocyclic compound containing arsenic, which has a broad-spectrum bactericidal effect on Gram-negative and Gram-positive bacteria, and is widely used as an industrial bactericidal and anti-mold additive Used in plastic products, wall paint, ship bottom paint, antibacterial fiber masterbatch, antibacterial plastic masterbatch, etc. [0003] Regarding the preparation method of OBPA, it is mentioned in U.S. Patent No. 3,701,794 (1972) that OBPA can be prepared by reacting 10-chlorophenoxapyr (CPA, 10-chloro-phenoxarsine) with sodium hydroxide. A method for preparing CPA by reacting aluminum chloride and diphenyl ether. German patent DE 3914288 (1990) also reported the preparation met...

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
IPC IPC(8): A01N55/00A01N55/02C07F9/74
Inventor 顾榴根荣志忍毛羽全李渝涛陆鸿良
Owner SHANGHAI NO 4 REAGENT & H V CHEM
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com