Method for preparing thiothiamine oxidation liquid and method for preparing thiamine nitrate applying method

A technology of thiamine nitrate and thiothiamine, applied in organic chemistry and other directions, can solve problems such as prolonging production cycle, wasting cold energy, etc., and achieves the effects of ensuring quality and yield, avoiding abnormal situations, and shortening residence time.

Pending Publication Date: 2021-05-28
江苏兄弟维生素有限公司
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

The current cooling adopts frozen brine jacket temperature control, the actual cooling capacity is higher than the theoretical cooling capacity, and at the same time, the intermittent feeding method cannot keep the heat transfer efficiency stable at a high value, wasting a lot of cooling capacity and prolonging the production cycle

Method used

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  • Method for preparing thiothiamine oxidation liquid and method for preparing thiamine nitrate applying method

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preparation example Construction

[0037] According to one aspect of the present invention, a method for preparing a thiothiamine oxidation liquid, the method comprises: passing the thiothiamine beating liquid and hydrogen peroxide into a microchannel reactor for reaction to obtain the thiothiamine oxidation liquid.

[0038] The invention provides a preparation method of thiothiamine oxidizing solution. In the method, thiothiamine beating solution and hydrogen peroxide are passed into a microchannel reactor for reaction to obtain thiothiamine oxidizing solution. Compared with the existing kettle-type batch-feeding reaction, the above method adopts a microchannel reactor to prepare thiothiamine oxidation liquid, which has a large specific surface area in the reaction section and high cooling efficiency, and is aimed at self-promoting oxidation reactions such as strong exotherms. The reaction can precisely control the temperature of the reaction system, which effectively avoids the over-temperature phenomenon and ...

Embodiment 1

[0066] like figure 1 Shown, a kind of preparation method of thiamine nitrate, described preparation method comprises the following steps:

[0067] 1. Thiamine beating: Add 150g of purified water to the three-necked flask, then add 50g of dry thiothiamine to the purified water several times, add the fine product and stir evenly before continuing to feed, and stir for 30 minutes after adding the fine product and cool down.

[0068] 2. Feeding: The feed rate is controlled by the microchannel reactor, and the refined product after beating is passed into the microchannel reactor according to the ratio of mass flow rate 200:49 with 49g (35%) of cooled hydrogen peroxide. The residence time is controlled at 2 minutes, the reaction temperature is controlled at 25°C, and the oxidation solution is obtained after the reaction is completed, and whether the oxidation solution is qualified or not is checked.

[0069] 3. The obtained oxidized solution was decolorized with 3.4 g of activated...

Embodiment 2

[0073] A preparation method of thiamine nitrate, said preparation method comprising the following steps:

[0074] 1. Thiamine beating: Add 150g of purified water to the three-necked flask, then add 50g of dry thiothiamine to the purified water several times, add the fine product and stir evenly before continuing to feed, and stir for 30 minutes after adding the fine product and cool down.

[0075] 2. Feeding: The feed rate is controlled by the microchannel reactor, and the refined product after beating is passed into the microchannel reactor according to the ratio of mass flow rate 200:49 with 49g (35%) of cooled hydrogen peroxide. The residence time is controlled at 3 minutes, and the reaction temperature is controlled at 23°C to obtain an oxidizing solution after the reaction is completed, and whether the oxidizing solution is qualified is checked.

[0076] 3. Take 170.5 g of the obtained oxidation solution, decolorize it with 3.4 g of activated carbon, neutralize it with a...

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Abstract

The invention provides a preparation method of thiothiamine oxidation liquid and a thiamine nitrate preparation method applying the method, and relates to the technical field of organic synthesis. The preparation method of the thiothiamine oxidation liquid comprises the following step of introducing thiothiamine pulping liquid and hydrogen peroxide into a microchannel reactor for reaction to obtain the thiothiamine oxidation liquid. Compared with the existing kettle type intermittent feeding reaction, the method for preparing the thiothiamine oxidation liquid by adopting the micro-channel reactor has the advantages that the specific surface area of a reaction section is large, the cooling efficiency is high, and the temperature of a reaction system can be accurately controlled aiming at the self-promotion reaction with strong heat release, namely the oxidation reaction; the overtemperature phenomenon caused by factors such as manual feeding in kettle type intermittent reaction and side reaction caused by overtemperature are effectively avoided, and the quality and yield of a finished product are ensured.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing thiothiamine oxidation solution and a method for preparing thiamine nitrate using the method. Background technique [0002] In the preparation process of vitamin B1, due to the redundant double bond sulfur in the structure of thiothiamine, it is necessary to oxidize thiothiamine to prepare thiothiamine oxidation solution. At present, the reaction mode of thiothiamine oxidation is mainly It is a batch-type tank reaction, and the method adopted is to intermittently feed the wet product of thiothiamine. Add all the purified water and hydrogen peroxide required for the reaction into the reaction kettle, lower the temperature, then add a small amount of dilute sulfuric acid, put quantitative thiothiamine wet product into the reaction kettle at a process temperature of 15±3°C, stir evenly, and wait for oxidation in the kettle After the liquid is clarif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/06
CPCC07D417/06
Inventor 赵巅沈燕李褦成陈英明严建斌
Owner 江苏兄弟维生素有限公司
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