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One-step safety production method of guanidine nitrate

A technology for safe production and guanidine nitrate, which is applied in the chemical industry and can solve problems such as no guidance plan

Inactive Publication Date: 2012-04-11
河北克尔化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above technologies have not given specific guidance on how to make the raw materials of guanidine nitrate cheap and easy to obtain in the production, and the operation steps are simple and safe.

Method used

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  • One-step safety production method of guanidine nitrate
  • One-step safety production method of guanidine nitrate

Examples

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Effect test

Embodiment 1

[0011] Example 1: A safe production method for one-step synthesis of guanidine nitrate, which is made into guanidine nitrate products through the following process steps (the main reaction formula is shown below):

[0012]

[0013] ① Add 1500Kg of raw materials ammonium nitrate and 1000Kg of urea and 150Kg of catalyst silica or inorganic silica gel or alumina (aluminum oxide) into a 5000L reactor. The catalyst selected in this embodiment is silica (or alumina). The weight ratio of urea, ammonium nitrate and catalyst used is 1:1.5:0.15. Heating makes the raw material urea and ammonium nitrate become molten liquid (the liquid temperature is between 170~175℃). ② (Through the heat transfer medium) control the temperature of the reaction liquid in the reactor to 200°C (200±5°C can be selected), and keep this temperature for 3 hours. Set the over-temperature alarm value to 206℃ and the pressure alarm value to 0.1MPa gauge pressure. ③After the reaction, start to cool down and cool to 1...

Embodiment 2

[0015] Example 2: A safe production method for the one-step synthesis of guanidine nitrate, which is made into guanidine nitrate products through the following process steps (the main reaction formula is shown in Example 1): ① Add the raw material ammonium nitrate 1000Kg and Urea 1000Kg and catalyst silica or inorganic silica gel or alumina (aluminum oxide) 150Kg, the catalyst selected in this embodiment is alumina (or silica). The weight ratio of urea, ammonium nitrate and catalyst used is 1:1:0.15. Heating makes the raw material urea and ammonium nitrate become molten liquid (the liquid temperature is between 170~175℃). ② (Through the heat transfer medium) control the temperature of the reaction liquid in the reactor to 190℃ (190±5℃ can be selected), and keep this temperature for 5 hours. Set the over-temperature alarm value to 206℃ and the pressure alarm value to 0.1MPa gauge pressure. ③After the reaction, start to cool down and cool to 160°C. (One-time) add 3000L of distil...

Embodiment 3

[0017] Example 3: A safe production method for the one-step synthesis of guanidine nitrate, which is made into guanidine nitrate products through the following process steps (the main reaction formula is shown in Example 1): ① Add the raw materials ammonium nitrate and urea and The catalyst is silica or inorganic silica gel or alumina, and the catalyst selected in this embodiment is inorganic silica gel (or silica). The weight ratio of urea, ammonium nitrate and catalyst used is 1:2.0: 0.2 (or 1:1.2: 0.1), and the raw materials urea and ammonium nitrate become molten liquid by heating. ② Control the temperature of the reaction liquid in the reactor at 180°C (or 220°C), and keep this temperature for 1 hour (or 6 hours). Set the over-temperature alarm value to 206℃ and the pressure alarm value to 0.1MPa gauge pressure. ③After the reaction, the temperature is reduced to 170°C (or 100°C), and process water is added. The ratio of the weight of urea plus ammonium nitrate to the weig...

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Abstract

The invention discloses a one-step safety production method of guanidine nitrate. The guanidine nitrate product is prepared through the following steps: adding ammonium nitrate, urea and a catalyst which is silicon dioxide or inorganic silica gel or aluminum oxide into a reaction kettle, heating to ensure that urea and ammonium nitrate are molten; controlling the temperature of the reaction liquid in the reaction kettle to maintain a reaction at the temperature; and cooling after the reaction, adding process water, heating the solution, performing hot filtering, recycling the catalyst, cooling the filtrate, filtering out a wet product, and drying the wet product to obtain the finished guanidine nitrate product. Ammonium nitrate is excess, thus urea can be completely reacted, side reactions such as the polymerization or sublimation of urea and decomposition can be reduced, the product yield can be increased and simultaneously the product quality can be increased. The production method has safety; and in order to ensure that the reaction has higher safety, the reaction kettle is connected with a temperature-pressure integrated fire device. The content of the obtained guanidine nitrate can meet the standard of the high-class product. The method has the advantages of simple technology and cheap and common raw material, and is economical and efficient.

Description

Technical field [0001] The invention relates to a production method of guanidine nitrate, in particular to a safe production method of one-step synthesis of guanidine nitrate, belonging to the chemical industry. Background technique [0002] Guanidine nitrate is a widely used chemical raw material. It is used to produce sulfamidine, sulfadiazine and other sulfa drugs and explosive nitroguanidine. It is also used to prepare guanidine carbonate and other guanidine salts, as well as paint industry, photographic materials and disinfection. Agent and other aspects. Since guanidine nitrate emits less light and heat, it has special value as a gunpowder. The preparation method of guanidine nitrate differs from country to country. Japan and the United States use dicyandiamide method to prepare it, and Germany uses direct method to prepare it from cyanamide. Either way, the initial raw material cannot be separated from lime nitrogen. Due to the small scale of lime nitrogen production, t...

Claims

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Application Information

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IPC IPC(8): C07C279/02C07C277/00A62C3/00
CPCY02P20/584
Inventor 王振中王智勇张金星郭仁昭吴述光刘中伟黄诘杨勇李志新
Owner 河北克尔化工有限公司
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