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Method for preparing flame-retardant waterborne polyurethane containing phosphaphenanthrene and/or phenyl phosphate groups

A phenyl phosphate, water-based polyurethane technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. Base chain, unable to meet the requirements of bonding hardness, heat resistance and mechanical properties, etc., to achieve the effect of lasting flame retardant properties, uniform distribution, and difficult migration

Inactive Publication Date: 2015-05-06
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The use of flame retardant compounds that do not contain rigid structures such as benzene rings will have a negative impact on the toughness, hardness, and mechanical properties of the synthesized polyurethane materials; if compounds containing phosphaphenanthrene or phenylphosphonate groups are used, The phosphorus element in the obtained flame-retardant water-based polyurethane is located alone in the main chain or side chain of the polyurethane molecular chain, and it is difficult to have the common advantages of both main-chain and side-chain flame-retardant polyurethane materials, which cannot meet the requirements for different flame-retardant properties. Or other performance requirements such as mechanics, toughness, bond hardness, heat resistance and mechanical properties, and the lack of a certain length of alkyl chain in the flame-retardant diol, it is difficult to meet or adjust the plasticity of polyurethane materials

Method used

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  • Method for preparing flame-retardant waterborne polyurethane containing phosphaphenanthrene and/or phenyl phosphate groups
  • Method for preparing flame-retardant waterborne polyurethane containing phosphaphenanthrene and/or phenyl phosphate groups
  • Method for preparing flame-retardant waterborne polyurethane containing phosphaphenanthrene and/or phenyl phosphate groups

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Dissolve 15 grams of 1,6-hexanediol in 50 mL of ethyl acetate, add 12.8 grams of triethylamine into a 500 mL three-neck flask, and place the reaction system in an ice-water bath. Dissolve 13.4 grams of phenyl dichlorophosphate in 50 mL of ethyl acetate to form a solution, stir and drop the solution into the three-necked flask within 2 hours; the reaction system continues to react in an ice-water bath for 12 hours; The precipitate was filtered, and the filtrate was distilled under reduced pressure to remove the solvent to obtain a flame-retardant dihydric alcohol dihydroxyhexyl phenyl phosphate (ZR-Diol A) with a symmetric phenyl phosphate group structure, and the yield was 85%. The structural formula of ZR-Diol A is:

[0042]

[0043] 50 grams of PPG (M n =2000) was added to a 500mL three-necked flask, dehydrated at 110°C for 1 hour and then cooled to 50°C; 18.3 grams of TDI was added to the three-necked flask, stirred and reacted at 80°C for 2 hours, then added 5.0...

Embodiment 2

[0045] Add 10g of DOPO, 0.03g of triethylamine and 8.6g of MEDB into a 500mL three-necked flask, then add 100mL of toluene as a solvent, stir and heat up to 110°C for 24 hours; after the reaction system is cooled to room temperature, precipitate and filter , dried to obtain intermediate product A; product A was transferred to a three-necked flask, and a mixed solution of tetrahydrofuran and hydrochloric acid (volume ratio 1:1) with a concentration of 1M was added dropwise, wherein the ratio of the amount of DOPO to hydrochloric acid was 2.3:1 ; Reaction at room temperature for 1 hour, after vacuum distillation to remove tetrahydrofuran and water, flame retardant diol II containing phosphaphenanthrene group was obtained with a yield of 85%.

[0046] 80 grams of PCL (M n =1000) into a 500mL three-necked flask, dehydrated at 110°C for 1 hour and then cooled to 50°C; took 52.5 grams of IPDI and added it to the three-necked flask, stirred and reacted at 80°C for 2 hours, then added...

Embodiment 3

[0051] Add 100 grams of DOPO, 50 grams of diethanolamine and 400 mL of water into the reactor, and raise the temperature to 80°C under nitrogen protection and stirring. After the DOPO is dissolved, add 50 grams of formaldehyde with a concentration of 30-40% dropwise within half an hour. The temperature was raised to 120°C, and the reflux reaction was maintained for 3 hours; part of the water was extracted under 60°C and 0.01MPa vacuum conditions (the remaining volume of the reaction solution was controlled to be 100mL); the remaining liquid was recrystallized at 5°C for 96 hours to obtain white crystals; The white crystals were repeatedly rinsed with 100 mL of water and 100 mL of chloroform three times, then placed in a vacuum oven and dried to constant weight to obtain flame retardant diol I with a yield of 81%.

[0052] 50.00 grams of PTMG (M n =2000) into a 500mL three-necked flask, dehydrated at 115°C for 1 hour and then cooled to 50°C; took 22.00 g of IPDI and added it to...

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Abstract

The invention discloses a method for preparing flame-retardant waterborne polyurethane containing phosphaphenanthrene and / or phenyl phosphate groups. The method is characterized by comprising the following step of reacting dihydric alcohol as a reactant which contains phosphaphenanthrene and / or phenyl phosphate groups and of which the hydroxyl groups are symmetric with diisocyanate, macromolecular dihydric alcohol, anionic or cationic hydrophilic chain extender and the like to synthesize flame-retardant waterborne polyurethane. According to the method, since flame-retardant dihydric alcohol is used as one of chain extenders, flame-retardant dihydric alcohol ca partially or totally substitute other small molecular chain extenders, phosphorus-containing flame-retardant groups are controllable in content and difficult to migrate and are evenly distributed, and the flame-retardant property of waterborne polyurethane can be enduringly retained. According to the structural characteristics of selected flame-retardant dihydric alcohol, by virtue of one and a combination of two or more of flame-retardant groups, phosphorus in the flame-retardant groups can be alone located at a main chain, side chains or simultaneously located at the main chain and the side chains of the polyurethane molecule chain as desired so as to meet the requirements of different flame-retardant properties or other properties such as mechanics, toughness and plasticity.

Description

technical field [0001] The invention belongs to the technical field of water-based polyurethane materials, and specifically relates to a flame-retardant water-based polyurethane formed by partially or completely replacing common small-molecule diols with flame-retardant diols containing phosphaphenanthrene or phenylphosphate groups and a preparation method thereof. Background technique [0002] When the diol reactive organophosphorus flame retardant containing phosphaphenanthrene group or phenyl phosphate group participates in the reaction to form a polymer, it can endow the material with organophosphorus flame retardant properties, so that it not only has good It has excellent flame retardant effect, and can solve the problems of large smoke and release of toxic and corrosive gases when halogen flame retardant polymers are burned. Due to its structural tailorability, outstanding environmental protection advantages and excellent comprehensive properties, waterborne polyureth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/32C08G18/34C07F9/12C07F9/6571
Inventor 张兴元李军配彭腾孙伟贺晨
Owner UNIV OF SCI & TECH OF CHINA
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