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Refining method of guanidine nitrate

A refining method and technology of guanidine nitrate, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low yield, low purity, less cycle times of mother liquor, high production cost, and high energy consumption, and achieve The effect of high product purity, stable product purity, and increased recycling rate

Inactive Publication Date: 2020-05-01
宁夏贝利特生物科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In view of this, the purpose of the present invention is to provide a high yield, high content and low energy consumption for the existing problems in the prior art, such as production cost, high energy consumption, low yield and purity, and few times of mother liquor recycling. , high utilization rate of mother liquor, more convenient process for refining guanidine nitrate

Method used

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  • Refining method of guanidine nitrate
  • Refining method of guanidine nitrate
  • Refining method of guanidine nitrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The various indexes of raw material crude product guanidine nitrate are as follows table 1:

[0043] Table 1

[0044]

[0045] Add 550g of distilled water and 264.0g of guanidine nitrate into a three-necked flask with mechanical stirring and a thermometer, start stirring and heating to dissolve; when the material is heated to 80°C, keep it warm at this temperature for 30min, at this time the material is white and turbid, and the system Slightly blue, after the heat preservation is over, take out the Buchner funnel that has been insulated in a water bath at 85°C, and filter the material at 80°C to remove water-insoluble matter. Crystallize and measure the pH value of the filtrate at the same time. When the temperature drops to 30°C, suction filter to obtain the filtrate and the product containing some water. The product is then dried in an oven set at 95°C for 2-3 hours to obtain refined guanidine nitrate ; And the mother liquor continues to be recycled in the next b...

Embodiment 2

[0048]Add 605g of mother liquor and 223g of guanidine nitrate obtained in Example 1 into a three-necked flask with mechanical stirring and a thermometer, stir and heat to dissolve; when the material is heated to 80°C, keep it for 30min at this temperature, and the material is white at this time The system is turbid, and the system is slightly blue. After the heat preservation is over, take out the Buchner funnel that has been insulated in a water bath at 85°C, and filter the material at 80°C to remove water-insoluble matter. After filtration, pour the filtrate back into the three-necked flask, and continue Stir slowly to cool down and crystallize, and measure the pH value of the filtrate at the same time. The filtrate cools down and crystallizes. When the temperature drops below 25°C, filter with suction to obtain the filtrate and product crystals. The product crystals are dried in an oven at 95°C for 2-3 hours and finally refined. Guanidine nitrate; and the mother liquor conti...

Embodiment 3

[0051] Add 617g of mother liquor and 223g of guanidine nitrate obtained in Example 2 into a three-necked flask with mechanical stirring and a thermometer, stir and heat to dissolve; when the material is heated to 80°C, it is kept at this temperature for 30min, and now the material is white The system is turbid, and the system is slightly blue. After the heat preservation is over, take out the Buchner funnel that has been insulated in a water bath at 85°C, and filter the material at 80°C to remove water-insoluble matter. After filtration, pour the filtrate back into the three-necked flask, and continue Stir slowly to cool down and crystallize, measure the pH value of the filtrate at the same time, the filtrate cools down and crystallizes, and when the temperature drops below 20°C, filter with suction to obtain the filtrate and product crystals, in which the product crystals are dried in an oven at 95°C for 2-3 hours and finally refined Guanidine nitrate; and the mother liquor co...

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Abstract

The invention discloses a refining method of guanidine nitrate. The method comprises the following steps: mixing crude guanidine nitrate and water according to a certain ratio; heating the material system until guanidine nitrate is completely dissolved; and then removing the water-insoluble substances and the impurities incapable of being thermally dissolved in the crude guanidine nitrate productby hot filtration through a preheated column filter or a plate filter press; carrying out cooling crystallizing on the filtrate after hot filtration in a stirring state; and cooling the material system to about 20 DEG C, and carrying out suction filtration to separate refined guanidine nitrate and mother liquor, and recycling the mother liquor. All indexes of the guanidine nitrate product obtainedby the method can meet the standard of refined guanidine nitrate in the current industry; and the technical scheme is simple, feasible, energy-saving and environment-friendly, solves the problems that the guanidine nitrate is damaged in the refining process so as not to achieve the high yield and so as to achieve low mother liquor circulation rate, and is suitable for popularization and application.

Description

technical field [0001] The invention belongs to the technical field of refining crude products, and relates to a method for refining guanidine nitrate. Background technique [0002] As an important pharmaceutical intermediate, guanidine nitrate is mainly used to prepare nitroguanidine, which is the raw material of dozens of drugs such as sulfamidine, trimethoprim, pyrimethamine, etc. It is also used to make explosives and disinfectants , photographic chemicals, etc. The content purity of synthetic guanidine nitrate product is not high based on the technology at present stage, is generally between 88-94%, can't be used for the synthesis of the downstream product of guanidine nitrate, and the by-product that it mainly produces has ammonium nitrate, free nitric acid and water Insoluble matter, so the crude product guanidine nitrate needs to be refined so as to meet the requirements of subsequent reaction raw material content. [0003] At present, the main process of refining ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/02C07C277/06
CPCC07C277/06C07C279/02
Inventor 赵黎明王辉苏炜夏学鹏安瑞杰包远平赵明泽王中杰
Owner 宁夏贝利特生物科技有限公司
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