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Preparation method of 3-(cyclohexylamino)-1-propanesulfonic acid

A technology of cyclohexylamine and propanesulfonic acid, which is applied in the preparation of sulfonic acid, chemical instruments and methods, chemical/physical/physical-chemical processes, etc., can solve problems such as unrecorded yield and complex process, and achieve improved production capacity and products. The yield, the process steps are simple, and the operation process is simple.

Inactive Publication Date: 2020-03-17
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

The process of this method is more complicated, and the yield is not recorded

Method used

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  • Preparation method of 3-(cyclohexylamino)-1-propanesulfonic acid
  • Preparation method of 3-(cyclohexylamino)-1-propanesulfonic acid
  • Preparation method of 3-(cyclohexylamino)-1-propanesulfonic acid

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Embodiment 1

[0025] 1, Embodiment 1 of the present invention provides a kind of preparation method of 3-(cyclohexylamine)-1-propanesulfonic acid, comprises the steps:

[0026] 2. Add 300kg of dichloromethane and 108kg of electronic grade 1,3-propane sultone into the 500L enamel reaction kettle A with mechanical stirring, and stir to dissolve at room temperature;

[0027] 3. Add 150kg of dichloromethane and 88kg of cyclohexylamine into the 500L enamel reaction kettle B with mechanical stirring, and stir evenly at room temperature;

[0028] 4. Through the metering pump, pump the liquid in kettle A at 30.8kg / h, and the solution in kettle B at 23.8kg / h, and simultaneously pump them into the microchannel reactor for reaction;

[0029] 5. Collect the reaction solution in a 1000L kettle, freeze and crystallize;

[0030] 6. 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 ...

Embodiment 2

[0032] Embodiment 2 of the present invention provides a kind of preparation method of 3-(cyclohexylamine)-1-propanesulfonic acid, comprises the steps:

[0033] (1) Add 300kg of methanol 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;

[0034] (2) Add 150kg methanol and 81.5kg cyclohexylamine in the 500L enamel reactor B with mechanical stirring, and stir evenly at room temperature;

[0035] (3) by metering pump, the liquid in the A kettle is pumped into the microchannel reactor simultaneously with 30kg / h, and the solution in the B kettle is reacted at 23.15kg / h;

[0036] (4) Collect the reaction solution with a 1000L kettle, freeze and crystallize;

[0037] (5) Nitrogen gas is introduced into the crystallization kettle, and a fully automatic stainless steel filter is pressed into it. After the obtained crystals pass the test, they are dried and packaged, and the methanol mother ...

Embodiment 3

[0039] Embodiment 3 of the present invention provides a kind of preparation method of 3-(cyclohexylamine)-1-propanesulfonic acid, comprises the steps:

[0040] (1) Add 200kg of ethyl acetate and 50kg of electronic grade 1,3-propane sultone to a 500L enamel reactor A with mechanical stirring, and stir to dissolve at room temperature;

[0041] (2) Add 150kg ethyl acetate and 36kg cyclohexylamine in the 500L enamel reaction kettle B with mechanical stirring, stir evenly at room temperature;

[0042] (3) by metering pump, with 20kg / h of liquid in the still of A, with 10.88kg / h of solution in the still of B, pump into microchannel reactor simultaneously and react;

[0043] (4) Collect the reaction solution with a 1000L kettle, freeze and crystallize;

[0044] (5) Feed nitrogen into the crystallizer, press into a full-automatic stainless steel filter, the obtained crystals pass the test, dry and pack, and the ethyl acetate mother liquor is recycled to the next batch of production. ...

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Abstract

A preparation method of 3-(cyclohexylamino)-1-propanesulfonic acid is provided. The method includes dissolving 1,3-propanesultone with an organic solvent A to obtain an organic solution containing the1,3-propanesultone; dissolving cyclohexylamine with an organic solvent B to obtain an organic solution containing the cyclohexylamine; pumping the two organic solutions into a microchannel reactor separately and simultaneously for a reaction to obtain a reaction solution, with the pumping speed of the organic solution containing the 1,3-propanesultone being 20-35 kg / h, and the pumping speed of the organic solution containing the cyclohexylamine being 10-25 kg / h; subjecting the obtained reaction solution to freezing crystallization to precipitate a 3-(cyclohexylamino)-1-propanesulfonic acid crude product; feeding nitrogen gas and performing filter pressing to obtain a finished product of the 3-(cyclohexylamino)-1-propanesulfonic acid. According to the method, the 1,3-propanesultone and thecyclohexylamine are adopted as raw materials, the microchannel reactor is adopted, reaction conditions are set, and the product yield can be greatly improved.

Description

technical field [0001] The invention relates to the technical field of substance synthesis, in particular to a preparation method of 3-cyclohexylamine-1-propanesulfonic acid. Background technique [0002] 3-Cyclohexylamine-1-propanesulfonic acid is a biological buffer, the appearance is white powder, used in biochemical diagnostic kits, DNA / RNA extraction kits and PCR diagnostic kits for enzyme chemistry and HPLC separation The buffer solution of alkaline drugs, and dissolved in deionized water, after adjusting the pH to 11.0, is used for the purification of fibronectin. [0003] Comparative document 1: The application number is "CN201610442348.5", and the name is "a method for preparing 3-cyclohexylamine-1 propanesulfonic acid", which discloses the use of sulfite, bisulfite and propenyl alcohol under the action of a special catalyst Reaction to prepare 1,3-propanesulfonate, 1,3-propanesulfonate reacts with carbonic acid to obtain 1,3-propanesulfonic acid; 1,3-propanesulfon...

Claims

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Application Information

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IPC IPC(8): C07C303/04C07C309/19B01J19/00
CPCB01J19/0093C07C303/04C07C2601/14C07C309/19
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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