A kind of prepolymerization-emulsification fully continuous method for preparing waterborne polyurethane

A water-based polyurethane, fully continuous technology, applied in the direction of climate sustainability, sustainable manufacturing/processing, chemical industry, etc., can solve the problems of destroying the ratio of raw materials, affecting product quality, and low degree of automation, so as to improve reactivity, The effect of controllable product structure and high degree of automation

Active Publication Date: 2021-12-14
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This production process mainly has the following disadvantages: (1) long reaction time (6-8 hours), low production efficiency, and high production cost; (2) production is overly dependent on labor, and the degree of automation is low; (3) product quality is unstable, There is a large difference between batches; (4) In order to facilitate emulsification, a low-boiling organic solvent must be added to the prepolymer to reduce the viscosity, and after emulsification, the solvent is removed by vacuum distillation, resulting in increased energy consumption and waste of resources; Low content, resulting in high drying and shipping costs
However, the temperature of the polyurethane reaction is generally in the range of 70-90°C, especially in the late stage of the reaction. If the temperature exceeds 90°C, side reactions such as branching and cross-linking will be triggered, which will destroy the ratio of raw materials and cause the product structure to be out of control. Emulsification also affects product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Formula: (parts by weight)

[0030] 80 parts polymer diol: polyethylene carbonate diol (Mn=3000)

[0031] 50 parts Diisocyanate: Isophorone Diisocyanate

[0032] 2 parts small molecule chain extender: 1,3-propanediol

[0033] 5 parts Hydrophilic Chain Extender: Methyldiethanolamine

[0034] 0.055 parts Catalyst: dibutyltin dilaurate

[0035] 300 parts deionized water

[0036] 1.93 parts neutralizer: formic acid

[0037] 2 parts post-chain extender: Ethylenediamine

[0038] Preparation:

[0039] (1) Mix 50 parts of isophorone diisocyanate, 80 parts of polyethylene carbonate diol (Mn=3000), 2 parts of small molecule chain extender (1,3-propanediol), hydrophilic chain extender (A Diethanolamine) 5 parts, catalyst (dibutyltin dilaurate) 0.055 parts, mixed evenly, and then preheated to 100 ° C, continuously injected into the first stage twin-screw reactor, the reaction temperature was controlled at 120 ° C, and the reaction time was 3 minutes;

[0040] (2) After the ...

Embodiment 2

[0047] Formula: (parts by weight)

[0048] 200 parts polymer diol: polyethylene carbonate diol (Mn=2000)

[0049] 100 parts diisocyanate: toluene diisocyanate

[0050] 6 parts small molecule chain extender: 1,4-butanediol

[0051] 15 parts Hydrophilic Chain Extender: Dimethylolpropionic Acid

[0052] 0.15 parts Catalyst: bismuth isooctanoate

[0053] 400 parts deionized water

[0054] 10 parts Neutralizer: Dimethylethanolamine

[0055] 2.5 parts post-chain extender: hydrazine hydrate

[0056] Preparation:

[0057] (1) 100 parts of toluene diisocyanate, 200 parts of polyethylene carbonate diol (Mn=2000), 6 parts of small molecule chain extender (1,4-butanediol), 6 parts of hydrophilic chain extender (dihydroxy 15 parts of methylpropionic acid) and 0.15 parts of catalyst (bismuth isooctanoate) were mixed evenly, then preheated to 120°C, and continuously injected into the first stage twin-screw reactor, the reaction temperature was controlled at 130°C, and the reaction tim...

Embodiment 3

[0065] Formula: (parts by weight)

[0066] 300 parts polymer diol: polyethylene glycol (Mn=2000)

[0067] 180 parts diisocyanate: hexamethylene diisocyanate

[0068] 8 parts small molecule chain extender: ethylene glycol

[0069] 20 parts Hydrophilic chain extender: sodium 1,4-butanediol-2-sulfonate

[0070] 0.22 parts Catalyst: bismuth laurate

[0071] 400 parts deionized water

[0072] 2 parts post-chain extender: p-phenylenediamine

[0073] (1) Mix 180 parts of hexamethylene diisocyanate, 300 parts of polyethylene glycol (Mn=2000), 8 parts of small molecule chain extender (ethylene glycol), hydrophilic chain extender (1,4-butanedi Alcohol-2-sodium sulfonate) 20 parts, catalyst (bismuth laurate) 0.22 parts, mixed evenly, then preheated to 120 ° C, and continuously injected into the first twin-screw reactor, the reaction temperature was controlled at 140 ° C, and the reaction time was 2 minutes;

[0074] (2) After the first stage of reaction is completed, the material e...

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PUM

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Abstract

The invention discloses a process method for fully continuous preparation of water-based polyurethane by prepolymerization-emulsification. In this method, the sonochemically strengthened twin-screw extruder is used as the water-based polyurethane prepolymerization and neutralization reactor, and the static mixer and tubular emulsifier are used as the prepolymer emulsification device. The prepolymerization and emulsification are fully continuous, and the production efficiency is high. , low cost, stable product quality, especially suitable for the production of high-solid aqueous polyurethane. More importantly, in a specific area of ​​the twin-screw extruder, a special ultrasonic generator is installed to perform sonochemical treatment on the prepolymerization intermediate, which can significantly improve the reactivity of the material, so that the late stage of the prepolymerization reaction can be at 70‑80 It is completed quickly under low temperature conditions, the production process is energy-saving and environmentally friendly, and side reactions such as branching, cross-linking, and degradation caused by high temperatures in the later stage are avoided. The obtained water-based polyurethane has a controllable structure and stable quality. The above process method does not use any organic solvent, has no selectivity to raw materials, and is applicable to the synthesis of any type of water-based polyurethane.

Description

technical field [0001] The invention relates to a prepolymerization-emulsification fully continuous method for preparing water-based polyurethane, which belongs to the field of polymer materials. Background technique [0002] Waterborne polyurethane came out in the 1960s. It is a new type of polyurethane system that uses water instead of organic solvents as the dispersion medium. Compared with traditional solvent-based polyurethane, water-based polyurethane only volatilizes into the atmosphere during use, which is environmentally friendly and meets the requirements of modern green chemical processes; at the same time, because the dispersion medium is water, water-based polyurethane is also non-toxic, non-flammable, and non-toxic It can replace traditional solvent-based polyurethane and is widely used in leather, synthetic leather, biomedicine, furniture, automobiles, aerospace and other fields. It is a new material that is being developed by the country. [0003] At present...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/08C08G18/12C08G18/76C08G18/75C08G18/73C08G18/66C08G18/48C08G18/44C08G18/34C08G18/32
CPCC08G18/08C08G18/0895C08G18/12C08G18/755C08G18/44C08G18/3206C08G18/3275C08G18/6655C08G18/7614C08G18/348C08G18/6659C08G18/3855C08G18/4833C08G18/73C08G18/6674C08G18/3228C08G18/3231C08G18/324Y02P20/10
Inventor 陈意周帅范浩军颜俊李成祥
Owner SICHUAN UNIV
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