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Polyhexamethylene guanidine phosphate and synthetic method thereof

A technology of polyhexamethylene guanidine phosphate and ammonium dihydrogen phosphate, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of inability to realize the reaction between guanidine and phosphoric acid and the poor solubility of products , Disinfection and sterilization activity limitations, etc., to achieve the effect of good mold killing effect, low cost, and simple preparation method

Active Publication Date: 2013-06-12
上海高聚生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, there is no report about the preparation method of polyhexamethyleneguanidine phosphate, and only South Korea SK Chemicals can produce it in the world. Therefore, domestic polyhexamethyleneguanidine phosphate products basically rely on imports
According to existing data reports, polyhexamethyleneguanidine phosphate is generally a product obtained by electrolyzing polyhexamethyleneguanidine with phosphoric acid. Since phosphoric acid reacts with polymers, the degree of reaction is limited, and it is not possible to achieve each The guanidine of the repeating unit reacts with phosphoric acid, so the product has poor solubility and limited disinfection and sterilization activity

Method used

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  • Polyhexamethylene guanidine phosphate and synthetic method thereof
  • Polyhexamethylene guanidine phosphate and synthetic method thereof
  • Polyhexamethylene guanidine phosphate and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1, synthesis of aminoguanidine dihydrogen phosphate

[0028] Add 200 kg of dicyandiamide and 550 kg of ammonium dihydrogen phosphate into the rotary mixer, mix for 30 minutes, then start heating, stop heating when the temperature rises to 170~180°C, and keep it in this temperature range for 1 hour to obtain 660 kg Aminoguanidine Dihydrogen Phosphate.

[0029] Step 2, dihydrogen phosphate aminoguanidine salt and hexamethylenediamine copolymerization

[0030] Put 400 kg of aminoguanidine dihydrogen phosphate and 330 kg of 1,6-hexamethylenediamine into the reactor, add 0.8 kg of propylene glycol, and follow the predetermined program at 100°C (1h for heat preservation)-150°C (2h for heat preservation)-200°C ( Keep warm for 2 hours) -250°C (keep warm for 0.5 hours) and gradually increase the temperature. After the reaction, a polyhexamethyleneguanidine phosphate polymer melt is obtained.

[0031] Cooling, obtain 670 kilograms of polyhexamethylene guanidine phosphates,...

Embodiment 2

[0033] Step 1, synthesis of aminoguanidine dihydrogen phosphate

[0034] Add 300 kg of dicyandiamide and 820 kg of ammonium dihydrogen phosphate into the rotary mixer, mix for 30 minutes, then start heating, stop heating when the temperature rises to 170~180°C, and keep it in this temperature range for 2 hours to obtain 990 kg Aminoguanidine Dihydrogen Phosphate.

[0035] Step 2, dihydrogen phosphate aminoguanidine salt and hexamethylenediamine copolymerization

[0036] Put 800 kg of aminoguanidine dihydrogen phosphate and 660 kg of 1,6-hexamethylenediamine into the reactor, add 0.8 kg of ethylene glycol, and follow the predetermined procedure at 100°C (1.5h for heat preservation)-150°C (1.5h for heat preservation) -200°C (1.5h of heat preservation) -250°C (1h of heat preservation) gradually increase the temperature, and after the reaction is completed, a polyhexamethylene guanidine phosphate polymer melt is obtained.

[0037] Cooling, obtain 1340 kilograms of polyhexamethyl...

Embodiment 3

[0039] Step 1, synthesis of aminoguanidine dihydrogen phosphate

[0040] Add 320 kg of dicyandiamide and 880 kg of ammonium dihydrogen phosphate into the rotary mixer, mix for 30 minutes, then start heating, stop heating when the temperature rises to 170~180°C, and keep it in this temperature range for 1.5 hours to obtain about 1000 Kilograms of aminoguanidine dihydrogen phosphate.

[0041] Step 2, dihydrogen phosphate aminoguanidine salt and hexamethylenediamine copolymerization

[0042] Put 500 kg of aminoguanidine dihydrogen phosphate and 400 kg of 1,6-hexamethylenediamine into the reactor, add 0.8 kg of PEG200, and follow the predetermined procedure at 100°C (2h for heat preservation)-150°C (2.5h for heat preservation)-200°C (2.5 hours of heat preservation) -250° C. (1.5 hours of heat preservation) gradually increase the temperature, and obtain a polyhexamethylene guanidine phosphate polymer melt after the reaction.

[0043] Cooling, obtain 650 kilograms of polyhexamethy...

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Abstract

The invention provides a synthetic method for polyhexamethylene guanidine phosphate and poly hexamethylene guanidine phosphate synthesized by the method. The polyhexamethylene guanidine phosphate is obtained by the steps of reacting dicyandiamide and ammonium dihydrogen phosphate to synthesize an aminoguanidine dihydrogen phosphate salt, and then reacting the aminoguanidine dihydrogen phosphate salt with 1, 6-hexamethylene diamine. The method for synthesizing the polyhexamethylene guanidine phosphate is proper in selection of raw materials and technical process, simple in preparation method and low in cost, and is suitable for industrialized production. The prepared polyhexamethylene guanidine phosphate has the characteristics of no toxicity, no stimulation and no corrosion, and has very good killing effect for mildew.

Description

technical field [0001] The invention relates to a synthesis method of polyhexamethylene guanidine salt, in particular to a synthesis method of polyhexamethylene guanidine phosphate and the polyhexamethylene guanidine phosphate synthesized by the method. Background technique [0002] Since a series of guanidine polymers were reported to have bactericidal properties in the 1930s, these compounds have been widely used in the sterilization and mildew prevention of medicine, plant protection, industrial products, food and daily necessities, so the research on guanidine polymers It has received very high attention. Among them, ICI America first prepared polyhexamethylene biguanide hydrochloride in the 1970s, which is a famous preservative with broad-spectrum bactericidal activity in the cosmetics and textile industries. Zhang Chunchang etc. also disclosed the toxicity test of polyhexamethylene biguanide compound disinfectant ("Chinese Journal of Disinfection", 2008, Volume 25, No....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/00C07C279/12C07C277/08
Inventor 余刚
Owner 上海高聚生物科技有限公司
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