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Preparation method of polyhexamethylene guanidine hydrochloride

A technology of polyhexamethylene guanidine hydrochloride and guanidine hydrochloride, which is applied in the field of polymer preparation, can solve the problems of high energy consumption, increased cost and the like, and achieves the effects of high yield, avoiding volatilization, and few raw materials and auxiliary materials.

Active Publication Date: 2020-09-04
深圳市盈界生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, the preparation of polyhexamethylene guanidine hydrochloride needs addition of initiator (choline chloride or azobisisoheptanonitrile) except these two raw materials of guanidine hydrochloride and triethylenediamine. , increasing the cost
In addition, the maximum reaction temperature required in the whole process is required to reach 250°C, which consumes a lot of energy.

Method used

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  • Preparation method of polyhexamethylene guanidine hydrochloride

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preparation example Construction

[0028] The preparation method of polyhexamethyleneguanidine hydrochloride provided by the invention comprises the following steps:

[0029] Step 1, put hexamethylenediamine and guanidine hydrochloride into the reactor in a certain proportion, stir and heat until completely dissolved and fully mixed;

[0030] Step 2, the temperature in the reactor is raised to 155-165° C., and the temperature is kept for 0.5-1.5 hours;

[0031] Step 3, the temperature in the reactor rises to 165-175°C, and after 1.5-2.5 hours of heat preservation, add to the reactor every 0.3-0.7 hours. Add a certain amount of deionized water into the reactor every 0.5 hours, and add 2 to 6 times in total;

[0032] Step 4, the temperature in the reactor is raised to 175-185° C., and the temperature is kept for 0-1 hour;

[0033] Step 5, stop heating the reactor, and add a certain amount of deionized water into the reactor, so that the temperature in the reactor drops to 55-65°C;

[0034] Step 6, transferring...

Embodiment 1

[0052] Put hexamethylenediamine and guanidine hydrochloride in a molar ratio of 1.05:1 into the reactor, stir and heat until completely dissolved and fully mixed; the reactor is heated so that the temperature in the reactor rises to 155°C, and the temperature is kept for 1.5 hours; the reactor Continue heating so that the temperature in the reactor rises to 165° C. After 2.5 hours of heat preservation, add a certain amount of deionized water to the reactor every 0.7 hours for a total of 6 times; the reactor continues to heat so that the temperature in the reactor rises to 175°C, heat preservation for 1 hour; the reactor stopped heating, and deionized water with a mass equivalent to the total mass of hexamethylenediamine and guanidine hydrochloride was added to the reactor, so that the temperature in the reactor dropped to 65°C; Transfer the material to a dilute decolorization kettle for decolorization and filtration; slowly add dilute hydrochloric acid to adjust the pH to 7-8, ...

Embodiment 2

[0054] Put hexamethylenediamine and guanidine hydrochloride in a molar ratio of 1.05:1 into the reactor, stir and heat until completely dissolved and fully mixed; the reactor is heated so that the temperature in the reactor rises to 160°C, and the temperature is kept for 1 hour; the reactor Continue heating so that the temperature in the reactor rises to 170° C. After 2 hours of insulation, add quality to the reactor every 0.5 hour to add 1.2% deionized water that is the total mass of hexamethylenediamine and guanidine hydrochloride added in step 1, Added 4 times in total; the reactor continued to heat, so that the temperature in the reactor rose to 180°C, and was kept warm for 0.5 hours; the reactor was stopped heating, and deionized water with a mass equivalent to the total mass of hexamethylenediamine and guanidine hydrochloride was added to the reactor within the reactor so that the temperature in the reactor drops to 60°C; transfer the material in the reactor to a dilute d...

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Abstract

The invention discloses a preparation method of polyhexamethylene guanidine hydrochloride. The preparation method comprises the following steps: adding hexamethylenediamine and guanidine hydrochlorideinto a reactor, stirring and heating until hexamethylenediamine and guanidine hydrochloride are dissolved, and fully mixing; raising the temperature to 155-165 DEG C, and keeping the temperature for0.5-1.5 hours; raising the temperature to 165-175 DEG C, keeping the temperature for 1.5-2.5 hours, and then adding a certain amount of deionized water into the reactor every 0.3-0.7 hour for 2-6 times; raising the temperature to 175-185 DEG C, and keeping the temperature for 0-1 hour; stopping heating, adding deionized water into a reactor, and reducing the temperature in the reactor to 55-65 DEGC; transferring the material to a diluting and decoloring kettle for decoloring and filtering; slowly adding diluted hydrochloric acid to adjust the pH value to 7-8, and observing the color of the solution; wherein if the obtained solution is clear colorless or faint yellow, the obtained solution is a polyhexamethylene guanidine hydrochloride finished product; if the obtained solution is yellow or suspended solids exist in the solution, adding activated carbon for decoloration and filtration to obtain filtrate, namely a finished product of polyhexamethylene guanidine hydrochloride. The preparation method has the advantages of low cost and low energy consumption.

Description

technical field [0001] The invention relates to the technical field of polymer preparation, in particular to a preparation method of polyhexamethyleneguanidine hydrochloride. Background technique [0002] The rapid development of contemporary industry has led to the continuous subdivision and expansion of the application fields of industrial fungicides from traditional textile, daily chemical, papermaking, petroleum products, coatings and other industries to all aspects of human life and living, such as food, medicine, fruits and vegetables, aquatic products , daily chemical detergent, household care products, swimming pool and water treatment, etc. Statistics show that the global fungicide market consumption reached 1.31 million tons in 2013, an increase of 12.9% from 1.16 million tons in 2010. China is the fastest-growing market for fungicide demand in the world. In 2013, China has grown into the second largest fungicide market in the world, with a consumption of about 34...

Claims

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Application Information

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IPC IPC(8): C08G73/00
CPCC08G73/00
Inventor 黄晓东
Owner 深圳市盈界生物工程有限公司
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