Preparation method of halogen-free intrinsic flame-retardant waterborne polyurethane film

A polyurethane film and an essential technology, applied in the field of preparation of halogen-free intrinsically flame retardant water-based polyurethane film, can solve the problems of large amount of flame retardant filler, poor water washing resistance, uneven coating film, etc., and achieve good flame retardant performance, The effect of high thermal stability

Active Publication Date: 2019-11-22
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the flame retardant modification method is a physical blending method, the waterborne polyurethane body and the flame retardant filler have disadvantages such as poor dispersion and poor mutual solubility.
The additive type usually uses a large amount of flame retardant fillers to carry out flame-retardant finishing on water-based polyurethane, but it will cause problems such as uneven coating, excessive use of flame retardant fillers, easy transfer, and poor washing resistance.

Method used

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  • Preparation method of halogen-free intrinsic flame-retardant waterborne polyurethane film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The preparation method of the halogen-free intrinsic flame-retardant water-based polyurethane film of the present embodiment, the steps are as follows:

[0018] 1. According to the number of parts by mass, add 17 parts of pentaerythritol into a three-necked flask with a reflux device and a tail gas treatment device, weigh 115 parts of phosphorus oxychloride, add it to the three-necked flask, turn on the magnetic stirring and condensing device, and start to heat up. When the temperature of the system reaches 60°C, react for 1 hour and then raise the temperature to 105°C, continue the reaction for 6 hours, then end the reaction, wash repeatedly with dichloromethane and absolute ethanol, filter with suction and dry to obtain a white powder, which is the intermediate product pentaerythritol bis Phosphate diphosphoryl chloride (PDD).

[0019] 2. According to the number of parts by mass, add 15 parts of PDD prepared in step 1 into a three-necked flask, and then add 150 parts ...

Embodiment 2

[0023] The preparation method of the halogen-free intrinsic flame-retardant water-based polyurethane film of the present embodiment, the steps are as follows:

[0024] 1. In parts by mass, add 25.5 parts of pentaerythritol into a three-necked flask with a reflux device and a tail gas treatment device, weigh 170 parts of phosphorus oxychloride, add it to the three-necked flask, turn on the magnetic stirring and condensing device, and start to heat up. When the temperature of the system reaches 60°C, react for 1.5 hours and then raise the temperature to 105°C, continue the reaction for 7 hours, then end the reaction, wash repeatedly with dichloromethane and absolute ethanol, filter with suction and dry to obtain a white powder, which is the intermediate product pentaerythritol Bisphosphonate diphosphoryl chloride (PDD).

[0025] 2. According to the number of parts by mass, add 30 parts of PDD prepared in step 1 into the three-necked flask, and then add 200 parts of chloroform, 2...

Embodiment 3

[0029] The preparation method of the halogen-free intrinsic flame-retardant water-based polyurethane film of the present embodiment, the steps are as follows:

[0030] 1. In parts by mass, add 34 parts of pentaerythritol into a three-necked flask with a reflux device and a tail gas treatment device, weigh 230 parts of phosphorus oxychloride, add it to the three-necked flask, turn on the magnetic stirring and condensing device, and start to heat up. When the temperature of the system reaches 60°C, react for 2 hours and then raise the temperature to 105°C, continue the reaction for 8 hours and end the reaction, wash repeatedly with dichloromethane and absolute ethanol, filter with suction and dry to obtain a white powder, which is the intermediate product pentaerythritol bis Phosphate diphosphoryl chloride (PDD).

[0031] 2. According to the number of parts by mass, add 45 parts of PDD prepared in step 1 into the three-necked flask, then add 250 parts of chloroform, 33 parts of di...

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Abstract

The invention discloses a preparation method of halogen-free intrinsic flame-retardant waterborne polyurethane. The preparation method comprises the following steps: firstly, performing a reaction onphosphorus oxychloride with pentaerythritol to prepare an intermediate product with a diphosphoryl chloride functional group; performing a reaction on the intermediate product with diglycolamine and other substances, thereby preparing a micromolecular flame retardant containing phosphorus and nitrogen flame-retardant elements, and finally performing a reaction on the micromolecular flame retardantserving as a hard segment chain extender with polyether polyol, isophorone diisocyanate, 2,2-dimethylolpropionic acid and other substances to prepare the halogen-free intrinsic flame-retardant waterborne polyurethane. According to the invention, the reactive halogen-free intrinsic flame-retardant waterborne polyurethane is prepared by taking the halogen-free flame retardant as a reaction substance, so that the product is good in flame-retardant effect, simple in synthesis method and relatively low in cost, has very good practicability and economy, and has a good market prospect.

Description

technical field [0001] The invention relates to a preparation method of a halogen-free intrinsically flame-retardant water-based polyurethane film, which has the characteristics of good thermal stability and high flame retardancy, and belongs to the field of functional materials. Background technique [0002] Waterborne polyurethane (WPU) is a binary colloid system that uses water as a dispersing agent. It has many excellent features, such as low pollution, non-toxicity, and high safety. Its comprehensive performance can still be compared with solvent-based polyurethane. With the improvement of environmental requirements for industrial life and production, water-based polyurethane shows better performance in many coating finishing agents because it can significantly improve the coating's hardness, toughness, moisture resistance, and quality characteristics, such as Leather goods, wood, clothing, etc. in industrial life. Compared with solvent-based polyurethane, water-based ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/75C08G18/66C08G18/48C08G18/34C08G18/32C08J5/18C08L75/08C07F9/24
CPCC07F9/2454C08G18/3206C08G18/348C08G18/3889C08G18/48C08G18/6692C08G18/755C08J5/18C08J2375/08
Inventor 喻国敏焦书燕李英华贾旭宋梦何方蔺春蕾梅林杨海燕
Owner ZHONGYUAN ENGINEERING COLLEGE
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