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Safe and continuous production method of sulphaguanidine

A production method and technology of sulfamidine, which is applied in the field of production process of chemical raw materials, can solve problems such as explosion and pressure increase, and achieve the effects of improving safety performance, stable reaction, and reducing online volume

Pending Publication Date: 2022-08-05
湖南吴赣药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned heating reaction process is usually carried out in a closed reactor. Guanidine nitrate as a raw material remains in the reaction system due to incomplete reaction and excess guanidine nitrate in the process ratio. Free guanidine will be produced in the later stage of the reaction. It is easy to decompose at high temperature, releases a large amount of decomposition heat, further promotes the decomposition of guanidine nitrate, increases the pressure in the reactor, and may cause an explosion risk in severe cases

Method used

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  • Safe and continuous production method of sulphaguanidine
  • Safe and continuous production method of sulphaguanidine

Examples

Experimental program
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Effect test

Embodiment 1

[0018] This embodiment provides a kind of safe continuous production method of sulfamidine, which is based on figure 1 and figure 2 Continuous reactor shown. The continuous reactor is a solid-phase melt-connected flow reactor, which mainly includes a premixing zone 1 and a reaction component 2 .

[0019] The premixing zone 1 is used for premixing the reaction raw materials, and includes a premixing pipe 11, a first stirring shaft 15 (ie, a first stirring shaft 15) rotatably installed in the premixing pipe 11 and having a first stirring protrusion 151 on the surface. A number of first stirring protrusions 151 are arranged on the surface of the shaft 15 to achieve full mixing of the reaction raw materials; the premixing pipe 11 is usually provided with a support structure for installing the first stirring shaft 15, and the first stirring shaft 15 is realized by bearings. rotatable, the same below), a first motor 16 installed on the premixing pipe 11 and connected with the fir...

Embodiment 2

[0030] The present embodiment provides a safe continuous production method for sulfamidine, which is basically the same as that in Example 1, except that: in step (d), the reflux ratio is 0.2:1; the purity of the final crude sulfamidine is 48.6%, The yield based on the raw material guanidine nitrate was 91%.

Embodiment 3

[0032] The present embodiment provides a safe continuous production method for sulfamidine, which is basically the same as that in Example 1, except that: in step (d), the reflux ratio is 1:1; the purity of the final crude sulfamidine is 62.3%, The yield based on the raw material guanidine nitrate was 99.5%.

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Abstract

The invention provides a safe and continuous production method of sulphaguanidine. The method comprises the following steps: (a) proportionally mixing industrial sulfanilamide, sodium carbonate and guanidine nitrate at normal temperature to obtain a mixed raw material; (b) heating the mixed raw material to 100 to 145 DEG C under the pressure condition of 0.06 to 0.08 MPa so as to preheat the mixed raw material to obtain a semi-solid mixture; (c) continuously heating the mixture to 150-165 DEG C under the pressure condition of 0.01-0.05 MPa, so that the mixture is subjected to chemical reaction in a slurry state; and (d) introducing nitrogen to cool the product in the step (c) to obtain a sulphaguanidine crude product. According to the continuous reactor, the problems that a reaction vessel is large, the online quantity of materials is large, the online time of the materials is long, the stirring effect is poor, the heat transfer effect is poor and the like due to the fact that a reaction kettle cannot be used for continuously carrying out chemical reaction and cannot effectively control material mixing and reaction procedures can be solved, and the problems can be well solved by using the continuous reactor, so that the safety performance is improved.

Description

technical field [0001] The invention belongs to the field of chemical raw material medicine production process, relates to a production method of sulfamidine, and in particular relates to a safe continuous production method of sulfamidine. Background technique [0002] The Chinese invention patent whose application number is 201210584928.X discloses a production process of medicinal sulfamidine, and sequentially puts in prescribed amounts of sulfonamide, sodium carbonate and guanidine nitrate (the molar ratio of feeding is 1.2-1.5:1.0:1.5-1.8), And add catalyst and co-catalyst, heat, heat up to 120 ° C to open vacuum pumping; continue to heat up to 125 ~ 145 ° C to completely melt the material, seal the reaction system, keep the reaction for 1 ~ 3 hours, add purified water equal to the weight of the raw material, stir , naturally cooled to 50 ℃, add the NaOH aqueous solution that the content is 29% (the solution weight is 0.2~0.4 times of the raw material weight), be cooled ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/36C07C311/64
CPCC07C303/36C07C311/64Y02P20/10
Inventor 赵六弟钱炜雯刘永超
Owner 湖南吴赣药业有限公司
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