Preparation method of amidinourea phosphate

A technology of guanidinourea phosphate and dicyandiamide, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problem that the production process of guaninourea phosphate has not been optimized, and the preparation of guaninourea phosphate has not been mentioned. Process and other issues, to achieve the effect of high product purity, mild reaction conditions, and cost savings

Inactive Publication Date: 2018-02-23
宁夏天成生化科技有限公司
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Problems solved by technology

None of the above patents mentioned the detailed preparation process of guanidinourea...

Method used

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  • Preparation method of amidinourea phosphate
  • Preparation method of amidinourea phosphate

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Effect test

Embodiment 1

[0018] Put 100Kg of dicyandiamide and 200Kg of purified water into the reaction kettle and mix them well, then raise the temperature of the system to 80°C and start adding phosphoric acid aqueous solution dropwise, the dropping rate is controlled at 100L / h, after the dropwise addition, slowly raise the temperature of the reaction kettle to 100 ℃ for 8 hours, after the completion of the insulation, the system was cooled to below 20 ℃ to start centrifugation, the centrifuged solid was rinsed with ethanol, and the target product was dried to 192Kg, the total yield was 80.6%, and the detection purity was 99.4%.

Embodiment 2

[0020] Put 100Kg of dicyandiamide and 400Kg of purified water into the reaction kettle and mix them well, then raise the temperature of the system to 100°C and start adding phosphoric acid aqueous solution dropwise, the dropping rate is controlled at 150L / h, after the dropwise addition is completed, slowly raise the temperature of the reaction kettle to 100°C ℃ for 8 hours, after the completion of the incubation, the temperature of the system was lowered to below 20 ℃ to start centrifugation, the centrifuged solid was rinsed with ethanol, and the target product was dried to 181Kg, the total yield was 76%, and the detection purity was 99.3%.

Embodiment 3

[0022] Put 100Kg of dicyandiamide and 200Kg of guanylurea phosphate centrifugal mother liquor into the reaction kettle instead of purified water and mix well, then raise the temperature of the system to 80°C and start adding phosphoric acid aqueous solution dropwise, the dropping rate is controlled at 100L / h, and the dropping is completed Then slowly raise the temperature of the reaction kettle to 100°C and keep it warm for 8 hours. After the heat preservation is completed, cool the system down to below 20°C and start centrifugation. The purity is 99.5%.

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Abstract

The invention relates to a preparation method of amidinourea phosphate. The preparation method comprises the following steps of: (1) stirring and mixing dicyandiamide and purified water; (2) slowly rising the temperature till the dicyandiamide is completely dissolved and filtered; (3) dripping phosphoric acid into a system; (4) insulating for a period of time, starting cooling, crystallization, centrifugation, drying and packaging. Centrifugal mother liquor in production can be recycled. The preparation method adopts the dicyandiamide, the purified water and the phosphoric acid as main materials to produce the amidinourea phosphate, and has the advantages of simple process, mild reaction, high yield, high product purity, green and environmental-friendly effect and the like.

Description

technical field [0001] The invention belongs to a novel method for synthesizing a flame retardant, in particular to a preparation method for guanylurea phosphate. technical background [0002] Guaninourea Phosphate is a new type of wood organic flame retardant, which has been deeply researched on wood flame retardancy at home and abroad. Inorganic wood flame retardants, organic wood flame retardants, resin-based wood flame retardants, and reactive wood flame retardants have all been developed. Nitrogen, phosphorus and boron flame retardants are currently the mainstream of wood flame retardants. Koppers proposed the wood organic flame retardant guanidinourea phosphate as early as 1961, but there are few reports on the specific synthesis method of guaninourea phosphate . Chinese patent (1007272B) introduces a preparation method and application process of a fabric flame retardant finishing agent and proposes to prepare a methylolated guanylurea phosphate aqueous solution with...

Claims

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Application Information

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IPC IPC(8): C07C277/08C07C279/26
CPCC07C277/08C07C279/26
Inventor 李江
Owner 宁夏天成生化科技有限公司
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