Preparation method of 3-morpholinopropanesulfonic 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 and the like, achieves improved production capacity and product yield, stable and controllable operation process, and eliminates the need for The effect of the three wastes

Active Publication Date: 2020-04-10
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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  • Preparation method of 3-morpholinopropanesulfonic acid
  • Preparation method of 3-morpholinopropanesulfonic acid
  • Preparation method of 3-morpholinopropanesulfonic acid

Examples

Experimental program
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Effect test

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 preparation method of 3-morpholinopropanesulfonic acid, wherein the preparation method comprises the steps: dissolving 1,3-propanesultone with an organic solvent A to obtain an organic solution containing 1,3-propanesultone, and dissolving morpholine with an organic solvent B to obtain an organic solution containing morpholine, wherein the molar ratio of the 1,3-propanesultone to the morpholine is 1:1; respectively pumping the organic solution containing 1,3-propanesultone and the organic solution containing morpholine into a micro-channel reactor at the same time, andcarrying out a reaction to obtain a reaction solution, wherein the pumping speed of the organic solution containing 1,3-propanesultone is 20-35 kg/h, and the pumping speed of the organic solution containing morpholine is 10-25 kg/h; and separating out a 3-morpholinopropanesulfonic acid crude product from the obtained reaction solution by adopting freezing crystallization, then introducing nitrogen, and carrying out filter pressing to obtain the 3-morpholinopropanesulfonic acid finished product. According to the method, 1,3-propanesultone and morpholine are used as raw materials, the micro-channel reactor is adopted, and reaction conditions are set, so that the yield of the product can be greatly increased.

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 Applications(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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