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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
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  • 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 reactors. The production efficiency is low, and the subsequent separation process is cumbersome.

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Dissolve 2000g of sodium metabisulfite in 5450g of deionized water. After it is completely dissolved, add 2g of sodium metabisulfite and 0.2g of tetrabutylammonium bromide to the sodium metabisulfite solution. - The mixed solution enters the metering pump after being filtered through the membrane, and then the mixed solution containing HSO3 - The mixed solution is passed in the 1st microchannel reactor simultaneously with the speed of 100g / min, 1910g epichlorohydrin with the speed of 25.63g / min, the reaction temperature in the 1st microchannel reactor is adjusted to 50 ℃, adjusts After the back pressure valve makes the pressure of the 1st microchannel reactor stabilized at 2MPa, the reaction product in the 1st reaction unit of the microchannel reactor is entered into the 2nd microchannel reactor, simultaneously with the feed rate of 21.76g / min to the 2nd Pass into the mixed solution of 1620g pyridine and 1.62g 1,4,7,13-tetraoxa-10-aza-2,3-benzocyclopentacene-2-ene in II...

Embodiment 2

[0033] Dissolve 2000g of sodium metabisulfite in 5450g of deionized water. After it is completely dissolved, add 5g of sodium metabisulfite and 0.4g of tetrabutylammonium bromide to the sodium metabisulfite solution. - The mixed solution enters the metering pump after being filtered through the membrane, and then the mixed solution containing HSO3 -The mixed solution is passed in the 1st microchannel reactor simultaneously with 100g / min speed, 1910g epichlorohydrin with 25.62g / min speed, the reaction temperature in the 1st microchannel reactor is adjusted to 30 ℃, regulates back pressure Valve makes the pressure of the 1st microchannel reactor stabilized at 2.5MPa, makes the reaction product in the 1st microchannel reactor enter the 2nd microchannel reactor, simultaneously with the feeding speed of 21.77g / min to the 2nd microchannel The mixed solution of 1620g pyridine and 3g1,4,7,13-tetraoxa-10-aza-2,3-benzocyclopenta-2-ene is passed into the reactor, and the microchannel rea...

Embodiment 3

[0036] Dissolve 2000g of sodium metabisulfite in 5450g of deionized water. After it is completely dissolved, add 3g of sodium metabisulfite and 0.4g of tetrabutylammonium bromide to the sodium metabisulfite solution. - The mixed solution enters the metering pump after being filtered through the membrane, and then the mixed solution containing HSO3 - The mixed solution is passed in the 1st microchannel reactor with 90g / min speed, 1948g epichlorohydrin simultaneously with 23g / min speed, the reaction temperature in the 1st microchannel reactor is adjusted to 30 ℃, adjusts the back pressure valve After the pressure of the 1st microchannel reactor is stabilized at 2.5MPa, the reaction product in the 1st microchannel reactor is entered into the 2nd microchannel reactor, and simultaneously with the feed rate of 22g / min to the 2nd microchannel reactor Into the mixed solution of 1665g pyridine and 3g 1,4,7,13-tetraoxa-10-aza-2,3-benzocyclopenta-2-ene, the II microchannel reactor The r...

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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

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Application Information

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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
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