Method for continuous production of epoxy chloropropane through reaction-separation coupling

A technology of epichlorohydrin and chloropropene, applied in the direction of organic chemistry, etc., can solve the problems of affecting the reaction conversion rate, difficult and unfavorable product separation, etc.

Inactive Publication Date: 2015-06-24
TAICANG HENGYI MEDICINE CHEM MATERIAL FACTORY
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method needs to go through ion exchange resin to remove the metal ions in the end, which increases the post-treatment process and process cost.
But in these reactions, the reaction products epichlorohydrin and benzoic acid are constantly accumulated in the system, which is not conducive to the positive direction of the reaction, affects the conversion rate of the reaction, and also causes difficulties in the separation of the products

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 continuous production of epoxy chloropropane through reaction-separation coupling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The qualitative and quantitative detection method of the reaction substrate and product in this example is: using SE-54 (30 m×0.25 mm×0.5 μm) quartz capillary column, the temperature of the vaporization chamber is 200 °C; the temperature of the column is 130 °C; the temperature of the FID detector is 260 °C ; Carrier gas: high-purity N 2 ; Column flow rate: 0.66 mL / min; Split ratio: 60:1.

[0015] Pump 38.26 g (0.5 mol) of allyl chloride and 69.06 g (0.5 mol) of peroxybenzoic acid into reaction kettle 1, heat to a reaction temperature of 80 °C, and stir vigorously for 2.5 h. In the distillation tower 3, the light components of allyl chloride and peroxybenzoic acid at the top of the rectification tower 3 are refluxed in the reactor 1 after being condensed, and the heavy components at the bottom of the tower are pumped into the secondary rectification tower 5 for secondary rectification , the light component epichlorohydrin at the top of the tower was condensed by the to...

Embodiment 2

[0017] Reaction substrate and product qualitative and quantitative detection method and operation are all the same as in Example 1, and the implementation steps of changing the reactant molar ratio and each operating parameter are as follows:

[0018] Pump 38.26 g (0.5 mol) of allyl chloride and 207.18 g (1.5 mol) of peroxybenzoic acid into reaction kettle 1, heat to the reaction temperature of 60 °C, and stir vigorously for 1 h. In the distillation tower 3, the light components of allyl chloride and peroxybenzoic acid at the top of the rectification tower 3 are refluxed in the reactor 1 after being condensed, and the heavy components at the bottom of the tower are pumped into the secondary rectification tower 5 for secondary rectification , the light component epichlorohydrin at the top of the tower was condensed by the top condenser 4 to collect 42.42 g of high-purity product epichlorohydrin, with a yield of 91.7%. .

Embodiment 3

[0020] Reaction substrate and product qualitative and quantitative detection method and operation are all the same as in Example 1, and the implementation steps of changing the reactant molar ratio and each operating parameter are as follows:

[0021] Pump 38.26 g (0.5 mol) of allyl chloride and 345.30 g (2.5 mol) of peroxybenzoic acid into Reactor 1, heat to a reaction temperature of 45 °C, and stir vigorously for 4 h. In the distillation tower 3, the light components of allyl chloride and peroxybenzoic acid at the top of the rectification tower 3 are refluxed in the reactor 1 after being condensed, and the heavy components at the bottom of the tower are pumped into the secondary rectification tower 5 for secondary rectification , the light component epichlorohydrin at the top of the tower was condensed by the top condenser 4 to collect 44.78 g of high-purity product epichlorohydrin, with a yield of 96.8%.

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 for epoxy chloropropane and mainly aims to overcome the problems of a low conversion rate of chloropropene and difficult separation of the product epoxy chloropropane during production of epoxy chloropropane in the prior art. According to the method, chloropropene and peroxybenzoic acid mixed according to a molar ratio are pumped into a reaction vessel and heated to a reaction temperature, a violent reaction with stirring is carried out, a reaction solution is injected to a primary rectifying tower in the process of reaction, the light components consisting of chloropropene and peroxybenzoic acid at the top of the primary rectifying tower flow back to the reaction vessel after condensation, heavy components at the bottom of the primary rectifying tower are pumped into a secondary rectifying tower for secondary rectification, the light component epoxy chloropropane at the top of the secondary rectifying tower undergoes condensation by a condenser at tower top and collection so as to obtain a high purity product, and the heavy component benzoic acid is collected at the bottom of the secondary rectifying tower. The method provided by the invention increases the conversion rate of chloropropene, realizes low-energy consumption, easy, rapid and continuous production and enables yield of the reaction product epoxy chloropropane to be greater than 90%.

Description

technical field [0001] The invention relates to a method for producing epichlorohydrin by using allyl chloride and peroxybenzoic acid, and relates to the preparation technology of epichlorohydrin in the chemical industry. Background technique [0002] Epichlorohydrin is an important organic chemical raw material and fine chemical product, mainly used in the production of epoxy resin, reinforced resin, water treatment resin, synthetic glycerin (accounting for 10% to 15% of demand) and elastomer, etc. A small amount is used in the preparation of glycidyl ethers and esters. At the same time, it is also used to produce coatings, adhesives, reinforcing materials and casting materials, to produce sealing materials and oil hoses used in the automotive industry and aviation industry, and to produce raw materials for chemical stabilizers, chemical fuels and water treatment agents. [0003] At present, the production process of epichlorohydrin is mainly propylene high-temperature chl...

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): C07D303/08C07D301/14
Inventor 倪明前
Owner TAICANG HENGYI MEDICINE CHEM MATERIAL FACTORY
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