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Preparation method and application of acetamidine hydrochloride

A technology of acetamidine hydrochloride and acetamidine hydrochloride, which is applied in the field of preparation of acetamidine hydrochloride, can solve the problems of pipeline blockage and high energy consumption, and achieve the effects of high cooling efficiency, large specific surface area, and avoiding side reactions

Active Publication Date: 2021-04-20
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process has high energy consumption, and calcium chloride is likely to cause pipeline blockage during the transfer of concentrated and recycled materials, and there is a certain risk of operational safety.

Method used

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  • Preparation method and application of acetamidine hydrochloride
  • Preparation method and application of acetamidine hydrochloride
  • Preparation method and application of acetamidine hydrochloride

Examples

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preparation example Construction

[0046] According to a first aspect of the present invention, a kind of preparation method of acetamidine hydrochloride comprises the following steps:

[0047] a) After acetonitrile is mixed with methanol, it is passed into the first microchannel reactor together with hydrogen chloride for addition reaction to obtain acetamidine;

[0048] B) ammonia and methanol are passed into the second microchannel reactor to react to obtain ammonia methanol;

[0049] c) The acetamidine obtained at the outlet of the first microchannel reactor and the ammonia methanol obtained at the outlet of the second microchannel reactor are simultaneously added to the reactor for ammoniation reaction to obtain acetamidine hydrochloride.

[0050] Step a)

[0051] In a preferred embodiment, the mass ratio of acetonitrile and methanol is 1:1.3-1.4, and its typical but non-limiting mass ratios are, for example, 1:1.30, 1:1.35, and 1:1.40.

[0052] In a preferred embodiment, the mixing of acetonitrile and...

Embodiment 1

[0098] A preparation method of acetamidine hydrochloride, comprising the following steps:

[0099] (1) acetonitrile, methyl alcohol are passed in the first microchannel reactor after static device mixing by the material proportion of table 1, control its residence time 2 hours in the microchannel reactor;

[0100](2) 31% concentrated hydrochloric acid is added dropwise in the vitriol oil of 70%, hydrogen chloride is resolved by the concentrated sulfuric acid dissolution heat, and the hydrogen chloride that resolves is lyophilized and dehydrated, then passes into step ( 1) in the first microchannel reactor, its residence time is consistent with the residence time of acetonitrile and methanol in the first microchannel reactor, and the reaction temperature in the first microchannel reaction is 15~20 ℃, the addition reaction Finally, ethyleneamidine is obtained, wherein the diluted sulfuric acid is concentrated to about 70% by distillation, and hydrogen chloride can be recycled fo...

Embodiment 2

[0108] The difference between this embodiment and Example 1 is that the temperature of the addition reaction in step (2) of the present embodiment is 20-30°C, and the time of the addition reaction is 1-1.5 hours, and all the other operating steps are the same as those in the implementation Example 1 is the same, and the yield of the acetamidine hydrochloride that the present embodiment obtains is 80%.

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Abstract

The invention provides a preparation method and application of acetamidine hydrochloride, and relates to the technical field of chemical engineering, and the preparation method comprises the following steps: a) mixing acetonitrile and methanol, and introducing the mixture and hydrogen chloride into a first micro-channel reactor for addition reaction to obtain acetamidine; b) introducing ammonia gas and methanol into a second micro-channel reactor for reaction to obtain aminomethanol; and c) simultaneously adding the acetamidine at the outlet of the first micro-channel reactor and the aminomethanol at the outlet of the second micro-channel reactor into the reaction kettle for ammoniation reaction to obtain the acetamidine hydrochloride. According to the method, the ethylidene amidine and the aminomethanol are obtained through the micro-channel reaction, then the acetamidine hydrochloride is obtained through ammonification, continuous operation is achieved, the cooling effect of the reaction is good, the cooling efficiency is high, the standing time is uniform and controllable, and side reactions caused by different reaction states can be avoided.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method and application of acetamidine hydrochloride. Background technique [0002] At present, the general process for the synthesis of acetamidine hydrochloride in the prior art is due to the large heat release of hydrogen chloride during the preparation process, and the heat of addition reaction of acetamidine hydrochloride is also relatively large. However, the reaction vessel in the general process is a reactor, and the heat exchange area of ​​the reactor is limited and the heat exchange efficiency is low, which leads to the fact that the process must first prepare acid methanol and then add acetonitrile dropwise to the acid methanol, so that the hydrogen chloride The heat of dissolution and the heat of addition reaction are dispersed. Based on the above reasons, the process of acetamidine hydrochloride cannot realize continuous production at present, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C257/14C07C249/02C07C251/08C07C213/02C07C215/08
Inventor 王诚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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