Silsesquioxane cross-linked silicon nitrogen phosphor synergic anti-flaming water-borne epoxy resin and preparation method thereof

A technology of siloxane epoxy resin and water-based epoxy resin, which is applied in the direction of epoxy resin coating, coating, anti-corrosion coating, etc., can solve the problems of high flame retardancy, thick coating thickness of heat insulation function, etc., and achieve improved resistance Combustibility, low cost, high binding effect

Active Publication Date: 2017-08-18
广东一通科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, flame retardant epoxy resin can be divided into two types: intumescent type and non-intumescent type. The non-intumescent type fireproof coating achieves the purpose of fire prevention through its own high flame retardancy, but its heat insulation function requires a thicker coating thickness to achieve

Method used

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  • Silsesquioxane cross-linked silicon nitrogen phosphor synergic anti-flaming water-borne epoxy resin and preparation method thereof
  • Silsesquioxane cross-linked silicon nitrogen phosphor synergic anti-flaming water-borne epoxy resin and preparation method thereof
  • Silsesquioxane cross-linked silicon nitrogen phosphor synergic anti-flaming water-borne epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1: Preparation of cage silsesquioxane

[0052] In a three-neck flask equipped with stirring, dropping funnel and thermometer, add 200ml of isopropanol (IPA) and 15.6g of 5% tetramethylammonium hydroxide (TMAH) aqueous solution, and add 30ml of isopropanol and 60.38g of 3-glycidyl etheroxypropyltrimethoxysilane, and then drop the mixed solution in the dropping funnel into the reaction vessel under stirring, and complete the dropwise addition within 60min. After the dropwise addition, continue to stir at room temperature for 6 hours, then distill off isopropanol under reduced pressure, then add 200ml of toluene to dissolve, reflux at about 80°C for 4-8 hours, adjust the pH of the solution to neutral, and distill under reduced pressure Remove the toluene, and vacuum-dry at a temperature of 60° C. to obtain a colorless and transparent viscous liquid, which is a cage silsesquioxane whose active group R is glycidyl etheroxypropyl.

Embodiment 2

[0053] Embodiment 2: Preparation of cage silsesquioxane

[0054] In a three-neck flask equipped with stirring, dropping funnel and thermometer, add 100 parts of isopropanol (IPA) and 9 parts of 5% tetramethylammonium hydroxide (TMAH) aqueous solution, and add 15 parts of isopropyl alcohol (IPA) into the dropping funnel. propanol and 28 parts of 3-(2,3-glycidoxy)propyltrimethoxysilane, and then add the mixed solution in the dropping funnel dropwise to the reaction vessel under stirring, and the dropwise addition is completed within 60 minutes. After the dropwise addition, continue to stir at room temperature for 6 hours, then distill off isopropanol under reduced pressure, add 100 parts of chloroform to dissolve, reflux at about 80°C for 4-8 hours, distill out chloroform under reduced pressure, After drying under vacuum, a colorless and transparent viscous liquid is obtained, which is a cage silsesquioxane whose active group R is 3-(2,3-glycidoxy)propyl.

Embodiment 3

[0055] Embodiment 3: the preparation of the silsesquioxane epoxy resin curing agent containing silicon nitrogen phosphorus

[0056] Dissolve 5 parts of the cage silsesquioxane prepared in Example 1 in 100 parts of chloroform, and after refluxing for half an hour, add 5 parts of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene- 10-oxide) and a corresponding amount of catalyst triphenylphosphine, continue to reflux reaction for 3-5h, siloxane and DOPO are connected by ether bond, and generate hydroxyl group; then add 5 parts of diethylenetriamine and the remaining 3-glycidol Propoxy reaction, reflux reaction for about 1h, the product is washed with water and then the solvent is removed in a rotary evaporator, the product is dried for 1-3h, and ground to 100-200 mesh to obtain a silsesquioxane epoxy containing silicon, nitrogen and phosphorus Resin curing agent.

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Abstract

The invention discloses a silsesquioxane cross-linked silicon nitrogen phosphor synergic anti-flaming water-borne epoxy resin and a preparation method thereof. The water-borne epoxy resin is prepared from 40-80wt% of epoxy resin base stock, 2-12wt% of silicon nitrogen phosphor containing silsesquioxane epoxy resin curing agent, 0.5-2wt% of curing accelerator, 5-20wt% of foaming agent, 5-20wt% of charring agent, 3-20% of charring catalyst, 2-12wt% of pigment filler and 0.1-2.5wt% of flatting agent, and the sum of the content of the components is 100%. According to the invention, the silicon nitrogen phosphor containing silsesquioxane epoxy resin curing agent is taken as a curing agent and is synergic with the charring agent, the foaming agent and the charring catalyst so as to obviously improve the flame retardant property of the water-borne epoxy resin; the acquired water-borne epoxy resin has high bonding force with the metal surface, has high heat resistance and has an oxygen index of above 32; the preparation method is simple, safe and low-cost; the water-borne epoxy resin has an excellent application prospect.

Description

technical field [0001] The invention belongs to the technical field of chemical material preparation. More specifically, it relates to a silsesquioxane-crosslinked silicon nitrogen phosphorus synergistic flame-retardant waterborne epoxy resin and a preparation method thereof. Background technique [0002] After the steel pipe is rolled off the assembly line of the steel plant, its surface corrosion resistance is poor, and it is easily corroded during storage, transportation and use, which seriously affects its performance and service life. Once its surface is corroded, its subsequent treatment process is cumbersome and the workload is heavy. At the same time, the mechanical properties of steel pipes will decline rapidly in high temperature environments. For example, the general No. 45 steel begins to soften after 0.5 hours at 600 ° C. Therefore, taking protective measures for these steel pipes to avoid direct burning by high-temperature flames can greatly reduce damage to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09D163/00C09D5/08C09D5/18C09D7/12C08G77/395C08G77/388C08G59/64
CPCC08G59/64C08G77/388C08G77/395C08L2201/02C08L2201/08C08L2205/03C09D5/08C09D5/18C09D7/61C09D7/63C09D163/00C08L29/14C08K5/053C08K2003/265C08L97/005C08K2003/2241
Inventor 吴伟国
Owner 广东一通科技股份有限公司
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