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A kind of hydrophilic chain extender monomer containing guanidine hydrochloride, nanoemulsion and preparation method

A technology of hydrophilic chain extender and nanoemulsion, which is applied in the fields of emulsion, hydrophilic chain extender monomer containing guanidine hydrochloride and nanoemulsion and preparation, which can solve the problem of high cost and difficult heavy corrosion of water-based fluorine-containing polyurethane. problems, to achieve excellent stability, low-cost characteristics, and excellent anti-bacterial corrosion effects

Active Publication Date: 2019-10-01
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the above-mentioned technical problems in the prior art, the present invention provides a hydrophilic chain extender monomer containing guanidine hydrochloride and a nanoemulsion and a preparation method thereof, the hydrophilic chain extender monomer containing guanidine hydrochloride The chain agent monomer, nanoemulsion and preparation method should solve the technical problems that the water-based fluorine-containing polyurethane in the prior art has high cost and is difficult to apply in the fields of heavy corrosion protection, high salt spray and high pollution

Method used

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  • A kind of hydrophilic chain extender monomer containing guanidine hydrochloride, nanoemulsion and preparation method
  • A kind of hydrophilic chain extender monomer containing guanidine hydrochloride, nanoemulsion and preparation method
  • A kind of hydrophilic chain extender monomer containing guanidine hydrochloride, nanoemulsion and preparation method

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Experimental program
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Effect test

Embodiment 1

[0047] Step (1): Preparation of chain extender containing guanidine hydrochloride

[0048] Dihydroxyethylpropionic acid and phosphorus pentachloride were dissolved in tetrahydrofuran at a molar ratio of 1:0.5, reacted at 40°C for 130 minutes, and purified to obtain the acid chloride monomer; then the acid chloride monomer and biguanide hydrochloride were Mix 1:1.2, adjust the temperature to 30°C, and react for 40 minutes, and purify to obtain the chain extender containing guanidine hydrochloride.

[0049] Step (2): Synthesis of aqueous polyurethane nanoemulsion containing guanidine hydrochloride

[0050] Dehydrate 42% polyester diol under vacuum for 130min at a temperature of 120°C; after lowering the temperature to 80°C, add 48% diisocyanate and 1% catalyst, and prepolymerize for 40min under the protection of an inert gas (nitrogen) ; Add 7% of the chain extender containing guanidine hydrochloride prepared by step (1), and perform a chain extension reaction at 60°C for 45 mi...

Embodiment 2

[0055] In step (2), the consumption of the chain extender containing guanidine hydrochloride is adjusted from 7% to 3%, the diisocyanate is adjusted from 48% to 52%, the percentage of other materials is constant, other operations are all the same as in Example 1 exactly the same. Gained guanidine hydrochloride aqueous fluorine-containing polyurethane nanoemulsion, through scanning electron microscope observation, its particle diameter is 62nm, and the minimum inhibitory concentration (MIC) to Escherichia coli and Staphylococcus aureus is respectively 56ug / mL and 45ug / mL, to Escherichia coli antibacterial and Staphylococcus aureus antibacterial adhesion were 42CFU / cm 2 and 38CFU / cm 2 ; Tested by salt spray test, after 32 hours of copper-accelerated acetic acid salt spray test (CASS test), the mass loss of the reference sample steel plate is 2.8g / m 2 .

Embodiment 3

[0057] In step (2), the consumption of the guanidine hydrochloride chain extender is adjusted from 7% to 12%, the diisocyanate is adjusted from 48% to 43%, the percentage of other materials is constant, and other operations are all the same as in Example 1 exactly the same. Its particle size is 70nm observed by scanning electron microscope; the minimum inhibitory concentration (MIC) for E. 0CFU / cm 2 and 0CFU / cm 2 ; Tested by salt spray test, after 38 hours with copper-accelerated acetic acid salt spray test (CASS test), the mass loss of the reference sample steel plate is 3.2g / m 2 .

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Abstract

The invention provides a guanidine hydrochloride-containing hydrophilic chain extender monomer, wherein the structural general formula is shown in the specification, where R represents alkyl with 1-15hydrogen atoms or carbon atoms, m is an integer between 0 and 15, n is an integer between 0 and 15, and r is an integer between 1 and 20. The invention also discloses a preparation method of the hydrophilic chain extender monomer. The invention further provides a guanidine hydrochloride-containing waterborne fluorinated polyurethane nano emulsion and a preparation method, wherein the preparationmethod comprises the following steps: preparing an antibacterial hydrophilic chain extender through a reaction between guanidine hydrochloride and dihydroxyl-containing carboxylic acids; introducing the antibacterial hydrophilic chain extender into a waterborne polyurethane preparation system to obtain a waterborne fluorinated polyurethane emulsion; finally, under the action of a water-soluble persulfate catalyst, introducing an acrylic fluorine-containing monomer to obtain a waterborne fluorinated polyurethane nano emulsion with particle size of 25-70nm. The preparation method provided by theinvention is simple and environment-friendly and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to an emulsion, specifically a hydrophilic chain extender monomer containing guanidine hydrochloride, a nanoemulsion and a preparation method. Background technique [0002] Water-based fluorinated polyurethane is an environmentally friendly material with low VOC emissions. Because water-based fluorinated polyurethane has good hydrophobic and oleophobic properties, it can be used in industrial fields such as leather, textiles, coatings, waterproof and moisture-permeable. However, at present, the prepolymer method is generally used in the process of preparing water-based fluorine-containing polyurethane. Due to the increase in viscosity during the reaction, it is difficult to emulsify in the later stage or the particle size is too large after emulsification and the stability is poor; and there is no fungicide in the prepared water-based fluorine-containing polyurethane structure. , its a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/00C08F220/24C08G18/67C08G18/42C08G18/10C08G18/32C07C277/08C07C279/26C09D151/08C09D5/14
Inventor 贾润萍赵玻张元倪锦平刘岩刘若灿代倩蓉刘珂
Owner SHANGHAI INST OF TECH
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