Unlock instant, AI-driven research and patent intelligence for your innovation.

Halogen-free flame-retardant polyaspartic acid ester as well as preparation method and application thereof

A technology of aspartate and hydroxyphosphate, applied in polyurea/polyurethane coatings, chemical instruments and methods, coatings, etc., can solve the problems of inability to meet the requirements of fire protection standards for building materials, insufficient flame retardant performance, etc. The effect of good elasticity, improved elongation at break, and good thermal insulation performance

Pending Publication Date: 2021-09-07
姜山
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to overcome the problem that the polyaspartic ester polyurea coating in the prior art has insufficient flame retardant performance and cannot meet the fire protection standard requirements of building materials, and provides a halogen-free flame retardant polyaspartic acid ester and its Preparation method and application, modifying polyaspartic acid esters with hydroxy phosphates and amino phosphoric acid esters to obtain polyaspartic acid esters modified with phosphorus-based flame retardant groups, and significantly improve its flame retardant performance ; After compounding it with isocyanate to form a two-component coating, the fire protection level has been significantly improved, and at the same time, the thermal insulation performance and elongation at break of the coating film can also be improved

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Halogen-free flame-retardant polyaspartic acid ester as well as preparation method and application thereof
  • Halogen-free flame-retardant polyaspartic acid ester as well as preparation method and application thereof
  • Halogen-free flame-retardant polyaspartic acid ester as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A halogen-free flame-retardant polyaspartic acid ester, the structural formula is:

[0036]

[0037] Among them, R is ethyl, R 1 and R 2 For methyl.

[0038] Its preparation method comprises the following steps:

[0039] (1) Add maleic anhydride, dimethyl hydroxymethyl phosphate, polymerization inhibitor p-hydroxyanisole (MEHQ), p-toluenesulfonic acid and solvent xylene into a flask with a water separator, maleic anhydride and hydroxyl The molar ratio of dimethyl methyl phosphate is 1:2.1, the amount of MEHQ added is 0.02% of the total mass of maleic anhydride and dimethyl hydroxymethyl phosphate, and the amount of p-toluenesulfonic acid added is maleic anhydride and methylol 0.05% of the total mass of dimethyl phosphate; heated to 150° C. for reflux dehydration esterification reaction for 5 hours, and then removed the xylene solvent under reduced pressure to obtain a slightly yellow dimethyl phosphate dimethyl maleate liquid;

[0040](2) Dissolve ethylenediamine...

Embodiment 2

[0043] A halogen-free flame-retardant polyaspartic acid ester, the structural formula is:

[0044]

[0045] Among them, R is ethyl, R 1 is methyl, R 2 For ethyl.

[0046] A preparation method of halogen-free flame-retardant polyaspartate, comprising the steps of:

[0047] (1) Add maleic anhydride, diethyl hydroxymethyl phosphate, polymerization inhibitor p-hydroxyanisole (MEHQ), p-toluenesulfonic acid and solvent xylene into a flask with a water separator, maleic anhydride and hydroxyl The molar ratio of diethyl methyl phosphate is 1:2, the amount of MEHQ added is 0.005% of the total mass of maleic anhydride and diethyl hydroxymethyl phosphate, and the amount of p-toluenesulfonic acid added is maleic anhydride and methylol 0.01% of the total mass of diethyl phosphate; heated to 140 ° C for reflux dehydration esterification for 10 hours, and then decompressed to remove the xylene solvent to obtain a slightly yellow diethyl dimethyl phosphate maleate liquid;

[0048] (2) ...

Embodiment 3

[0051] A halogen-free flame-retardant polyaspartic acid ester, the structural formula is:

[0052]

[0053] Among them, R is isopropyl, R 1 and R 2 For methyl.

[0054] A preparation method of halogen-free flame-retardant polyaspartate, comprising the steps of:

[0055] (1) Add maleic anhydride, dimethyl hydroxymethyl phosphate, polymerization inhibitor p-hydroxyanisole (MEHQ), p-toluenesulfonic acid and solvent xylene into a flask with a water separator, maleic anhydride and hydroxyl The molar ratio of dimethyl methyl phosphate is 1:2.4, the amount of MEHQ added is 0.1% of the total mass of maleic anhydride and dimethyl hydroxymethyl phosphate, and the amount of p-toluenesulfonic acid added is maleic anhydride and methylol 0.1% of the total mass of dimethyl phosphate; heated to 160 ° C for reflux dehydration esterification reaction for 3 hours, and then decompressed to remove the xylene solvent to obtain a slightly yellow dimethyl phosphate dimethyl maleate liquid;

[...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses halogen-free flame-retardant polyaspartic acid ester as well as a preparation method and application thereof. The preparation method comprises the following steps of: (1) reacting maleic anhydride with hydroxyl-containing phosphate to obtain maleic acid diphosphate; (2) reacting dichloromethylphosphine with diamine to obtain a diamino phosphorus-nitrogen intermediate; and (3) reacting the obtained maleic acid diphosphate with the diamino phosphorus-nitrogen intermediate to obtain the halogen-free flame-retardant polyaspartic acid ester. According to the invention, the polyaspartic acid ester is modified by hydroxyl phosphate and amino phosphate to obtain the phosphorus-based flame retardant modified polyaspartic acid ester, so that the flame retardant property of the phosphorus-based flame retardant modified polyaspartic acid ester is remarkably improved; and after a two-component coating is prepared by compounding the polyaspartic acid ester with phosphating phenyl isocyanate, the fireproof grade is obviously improved, and meanwhile, the thermal insulation property and the elongation at break of a coating film can also be improved.

Description

technical field [0001] The invention relates to the technical field of flame-retardant coatings, in particular to a halogen-free flame-retardant polyaspartic acid ester and a preparation method and application thereof. Background technique [0002] As a new type of coating developed in recent years, the polyaspartate polyurea coating prepared by mixing polyaspartic acid ester and isocyanate curing agent has the characteristics of high weather resistance, high performance, and good environmental performance. Polyaspartate polyurea coatings have high gloss and high adhesion on the substrate surface; in addition, polyaspartate polyurea coatings have a suitable pot life and fast drying time. Aspartic ester polyurea coatings also have excellent acid resistance, alkali resistance and salt spray resistance. Therefore, polyaspartate polyurea coatings are highly praised by people for their excellent performance and convenient construction. [0003] However, the existing polyasparta...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07F9/44C09D175/02C09D5/18
CPCC07F9/4465C07F9/4473C09D175/02C09D5/18
Inventor 姜山徐轶卢鹏飞
Owner 姜山