Method for continuously synthesizing PPS-OH

A technology for synthesizing hydroxypropanesulfonic acid pyridinium salt and pyridine, which is applied in organic chemistry and other fields, can solve problems such as difficulty in satisfying high-end electroplating customers, cumbersome separation process, and low production efficiency, so as to achieve suitable industrial production, reduce side reactions, and improve The effect of production efficiency

Active Publication Date: 2019-01-25
湖北吉和昌化工科技有限公司
View PDF9 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, the synthesis of PPS-OH is carried out intermittently in traditional rea

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 continuously synthesizing PPS-OH
  • Method for continuously synthesizing PPS-OH
  • Method for continuously synthesizing PPS-OH

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0029] Example 1:

[0030] Dissolve 2000g of sodium metabisulfite in 5450g of deionized water. After it is completely dissolved, add 2g of sodium sulfite and 0.2g of tetrabutylammonium bromide to the sodium metabisulfite solution. After stirring and mixing uniformly, the HSO3 - The mixed liquid is filtered through the membrane and then enters the metering pump, and then the HSO3 - The mixed solution of 1 was passed into the first microchannel reactor at a speed of 100g / min and 1910g of epichlorohydrin at a speed of 25.63g / min at the same time. The reaction temperature in the first microchannel reactor was adjusted to 50℃, and After the back pressure valve stabilizes the pressure of the first microchannel reactor at 2MPa, the reaction product in the first reaction unit of the microchannel reactor enters the second microchannel reactor, and at the same time the feed rate of 21.76g / min A mixture of 1620g pyridine and 1.62g 1,4,7,13-tetraoxa-10-aza-2,3-benzocyclopentadec-2-ene was pa...

Example Embodiment

[0032] Example 2:

[0033] Dissolve 2000g of sodium metabisulfite in 5450g of deionized water. After it is completely dissolved, add 5g of sodium sulfite and 0.4g of tetrabutylammonium bromide to the sodium metabisulfite solution. After stirring and mixing uniformly, the HSO3 - The mixed liquid is filtered through the membrane and then enters the metering pump, and then the HSO3 - The mixed solution of 1 was introduced into the first microchannel reactor at a rate of 100g / min and 1910g of epichlorohydrin at a rate of 25.62g / min at the same time. The reaction temperature in the first microchannel reactor was adjusted to 30°C, and the back pressure was adjusted. After the valve stabilizes the pressure of the first microchannel reactor at 2.5MPa, the reaction product in the first microchannel reactor enters the second microchannel reactor, and at the same time the feed rate of 21.77g / min to the second microchannel A mixture of 1620g pyridine and 3g 1,4,7,13-tetraoxa-10-aza-2,3-benzo...

Example Embodiment

[0035] Example 3:

[0036] Dissolve 2000g of sodium metabisulfite in 5450g of deionized water. After it is completely dissolved, add 3g of sodium sulfite and 0.4g of tetrabutylammonium bromide to the sodium metabisulfite solution. After stirring and mixing uniformly, the HSO3 - The mixed liquid is filtered through the membrane and then enters the metering pump, and then the HSO3 - The mixed solution of 1948g epichlorohydrin was introduced into the first microchannel reactor at a rate of 90g / min and 1948g epichlorohydrin at a rate of 23g / min. The reaction temperature in the first microchannel reactor was adjusted to 30°C, and the back pressure valve was adjusted. After the pressure of the first microchannel reactor was stabilized at 2.5MPa, the reaction product in the first microchannel reactor was allowed to enter the second microchannel reactor, and at the same time, to the second microchannel reactor at a feed rate of 22g / min Into the mixed solution of 1665g pyridine and 3g 1,4...

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 discloses a method for continuously synthesizing PPS-OH. The method comprises the following steps of adding a phase transfer catalyst and sodium sulfite into a hydrosulfite solution or pyrosulfite solution of alkali metal, so as to obtain a mixed solution containing HSO3<->; simultaneously adding the mixed solution and epichlorohydrin into a first reactor, and generating ring-openingreaction; simultaneously adding a mixed solution of pyridine and a catalyst and a ring-opening reaction product into a second reactor, and reacting to obtain a target product. The method has the advantages that the mixing order and adding order of the raw materials are changed, and the raw materials participating in reaction are simultaneously sent into the corresponding reactor to participate inthe corresponding reaction, so that the generation of side effect is effectively reduced, the selectivity and the conversion rate of reaction are improved, the yield rate and purity of the product are improved, and the requirement of high-end customers in the electroplating industry are met; compared with the intermittent operation of the traditional technology, the reaction time is shortened, the production efficiency is improved, and the method is suitable for industrialized production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for continuously synthesizing pyridinium hydroxypropanesulfonate. Background technique [0002] Hydroxypropanesulfonic acid pyridinium salt (referred to as PPS-OH), it is an electroplating intermediate, the molecular formula is: C 8 h 11 NaO 4 S, molecular weight: 217.24, CAS number: 3918-73-8, pure product is white crystal, most of its commercially available products are colorless to light yellow liquid with content between 40-50% and pH value between 3-5 . PPS-OH has excellent brightening and leveling effects in nickel electroplating, especially in high current density areas. As a basic additive in the nickel plating bath, its dosage is 50-500mg / L, and its consumption is 20-50g / kAH. Due to the demand for anti-corrosion and decorative functions, its market demand is large. [0003] At present, the industrial synthesis method of PPS-OH is the normal-pressu...

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): C07D213/20
CPCC07D213/20
Inventor 冯庆诚杨威付远波肖忠新黄开伟宋文华
Owner 湖北吉和昌化工科技有限公司
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