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A kind of preparation method of 3-morpholine propanesulfonic acid

A technology of morpholine propanesulfonic acid and morpholine, which is applied in the field of preparation of 3-morpholine propanesulfonic acid, can solve the problem of low yield, achieve the effects of increasing yield, simple operation process, and eliminating three wastes

Active Publication Date: 2022-02-08
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, the yield of conventional methods is not high

Method used

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  • A kind of preparation method of 3-morpholine propanesulfonic acid
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  • A kind of preparation method of 3-morpholine propanesulfonic acid

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Embodiment 1

[0024] Embodiment 1 of the present invention provides a kind of preparation method of 3-morpholine propanesulfonic acid, comprises the steps:

[0025] 1. Add 400kg of dichloromethane and 100kg of electronic grade 1,3-propane sultone into a 500L enamel reactor A with mechanical stirring, and stir to dissolve at room temperature;

[0026] 2. Add 150kg of dichloromethane and 72kg of morpholine into the 500L enamel reaction kettle B with mechanical stirring, and stir evenly at room temperature;

[0027] 3. Through the metering pump, pump the liquid in kettle A at 30kg / h, and the solution in kettle B at 22.2kg / h, and simultaneously pump them into the microchannel reactor for reaction;

[0028] 4. Collect the reaction solution in a 1000L kettle, freeze and crystallize;

[0029] 5. Feed nitrogen gas into the crystallizer and press into a fully automatic stainless steel filter. After passing the test, the obtained crystals are dried and packaged, and the dichloromethane mother liquor...

Embodiment 2

[0031] Embodiment 2 of the present invention provides a kind of preparation method of 3-morpholine propanesulfonic acid, comprises the steps:

[0032] 1. Add 300kg of ethanol and 100kg of electronic grade 1,3-propane sultone into a 500L enamel reaction kettle A with mechanical stirring, and stir to dissolve at room temperature;

[0033] 2. Add 150kg of ethanol and 72kg of morpholine into the 500L enamel reactor B with mechanical stirring, and stir evenly at room temperature;

[0034] 3. Through the metering pump, pump the liquid in kettle A at 30kg / h, and the solution in kettle B at 22.2kg / h, and simultaneously pump them into the microchannel reactor for reaction;

[0035] 4. Collect the reaction solution in a 1000L kettle, freeze and crystallize;

[0036] 5. Feed nitrogen gas into the crystallizer, press into a fully automatic stainless steel filter, and after passing the test, the obtained crystals are dried and packaged, and the ethanol mother liquor is recycled to the nex...

Embodiment 3

[0038] Embodiment 3 of the present invention provides a kind of preparation method of 3-morpholine propanesulfonic acid, comprises the steps:

[0039] 1. Add 250kg of ethyl acetate and 50kg of electronic grade 1,3-propane sultone into a 500L enamel reactor A with mechanical stirring, and stir to dissolve at room temperature;

[0040] 2. Add 100kg of ethyl acetate and 36kg of morpholine to the 500L enamel reactor B with mechanical stirring, and stir evenly at room temperature;

[0041] 3. Through the metering pump, pump the liquid in kettle A at 20kg / h, and the solution in kettle B at 10.88kg / h, and simultaneously pump them into the microchannel reactor for reaction;

[0042] 4. Collect the reaction solution in a 1000L kettle, freeze and crystallize;

[0043] 5. Feed nitrogen gas into the crystallizer and press into a fully automatic stainless steel filter. After the obtained crystals pass the test, they are dried and packaged, and the ethyl acetate mother liquor is recycled t...

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Abstract

The invention provides a method for preparing 3-morpholine propanesulfonic acid, comprising dissolving 1,3-propane sultone with an organic solvent A to obtain an organic solution containing 1,3-propane sultone, and dissolving morpholine with The organic solvent B is dissolved to obtain an organic solution containing morpholine; the molar ratio of 1,3-propane sultone and morpholine is 1:1; the organic solution containing 1,3-propane sultone, and the morpholine-containing The organic solution is simultaneously pumped into the microchannel reactor to react to obtain the reaction liquid; the pumping rate of the organic solution containing 1,3-propane sultone is 20~35kg / h, and the pump of the organic solution containing morpholine The feed rate is 10-25kg / h; the obtained reaction liquid is precipitated by freezing crystallization to separate out the crude product of 3-morpholine propanesulfonic acid, and then passed through nitrogen pressure filtration to obtain the finished product of 3-morpholine propanesulfonic acid. The method uses 1,3-propane sultone and morpholine as raw materials and adopts a microchannel reactor, and setting reaction conditions can greatly improve the yield of products.

Description

technical field [0001] The invention relates to the technical field of substance synthesis, in particular to a preparation method of 3-morpholinepropanesulfonic acid. Background technique [0002] 3-Morpholine propanesulfonic acid is a kind of biological buffer, the appearance is white powder, used in biochemical diagnostic kits, DNA / RNA extraction kits and PCR diagnostic kits, as well as components in Good's buffer for biological research. The current industrial production method of 3-morpholinepropanesulfonic acid mainly uses 1,3-propane sultone and morpholine as raw materials, reacts in an organic solvent or water system, and then obtains the product after recrystallization or washing in an organic solvent. However, the conventional method yields are not high. How to provide a method for preparing 3-morpholinepropanesulfonic acid with a high yield has become a technical problem to be solved urgently. Contents of the invention [0003] The purpose of the present invent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/088
CPCC07D295/088
Inventor 冯庆诚付远波杨威黄开伟宋文华肖忠新
Owner 湖北吉和昌化工科技有限公司
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