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A kind of preparation method of hydroxyl polyurethane

A technology of hydroxyl polyurethane and prepolymers, which is applied in the field of polymer material synthesis, can solve the problems of large-scale industrial production that is not suitable for PHU, and achieve good practical significance and application prospects, high product yield, and wide application range.

Active Publication Date: 2021-10-26
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reported methods disclosed in the above-mentioned patents all adopt the reaction of cyclocarbonate and a primary amine compound to prepare PHU, which is not suitable for large-scale industrial production of PHU

Method used

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  • A kind of preparation method of hydroxyl polyurethane
  • A kind of preparation method of hydroxyl polyurethane
  • A kind of preparation method of hydroxyl polyurethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] A kind of preparation of linear PHU, preparation route such as figure 1 As shown, the specific steps are as follows:

[0060] (1) Preparation of pentaerythritol monoketal:

[0061] Dissolve 30.00g of pentaerythritol and 0.42g of p-toluenesulfonic acid monohydrate in DMF at 80°C, let it stand and cool to 40°C, add 22.95g of 2,2-dimethoxypropane dropwise, and the mixture is cooled at 25°C Stir for 24 hours, add 0.13g trimethylamine and continue to stir for 2 hours, remove DMF by rotary evaporation, dissolve the crude product in dichloromethane, wash three times with deionized water, collect the organic layer, add anhydrous magnesium sulfate to dry, and remove dichloromethane by rotary evaporation. Chloromethane, dried in a vacuum oven at 40°C for 6 hours to obtain powdered pentaerythritol monoketal.

[0062] image 3 It is the proton nuclear magnetic resonance spectrogram of the pentaerythritol monoketal prepared. Specifically, 4.48ppm is the proton peak on the hydrox...

Embodiment 2

[0074] Preparation of cross-linked M-PHU: The synthetic route is shown in figure 2 As shown, the specific steps are as follows:

[0075] The linear M-PHU that 10.00g embodiment 1 is made and 0.75g MDI are dissolved in DMF, join in the reactor that mechanical stirring and nitrogen device are housed, then add dibutyltin dilaurate (accounting for all The mass ratio of reactants is 0.05%), and after passing nitrogen into the system for 0.5 h, the reaction is carried out at 60° C. until a gel is formed. After the gel was taken out, it was placed in an oven at 60°C for 12 hours to remove most of the solvent, and the remaining small amount of solvent was completely removed in a vacuum oven at 60°C for 48 hours to obtain a cross-linked M-PHU material.

[0076] Figure 7 For the photo of the reprocessing process of the cross-linked M-PHU material, the block sample of the cross-linked M-PHU was selected and cut into pieces. It was found that under certain temperature and pressure con...

Embodiment 3

[0079] (1) Preparation of pentaerythritol monoketal:

[0080] Dissolve 30.00g of pentaerythritol and 0.42g of p-toluenesulfonic acid monohydrate in DMF at 80°C, let it stand and cool to 40°C, add 22.95g of 2,2-dimethoxypropane dropwise, and the mixture is cooled at 25°C Stir for 24 hours, add 0.13g trimethylamine and continue to stir for 2 hours, remove DMF by rotary evaporation, dissolve the crude product in dichloromethane, wash three times with deionized water, collect the organic layer, add anhydrous magnesium sulfate to dry, and remove dichloromethane by rotary evaporation. Chloromethane, dried in a vacuum oven at 40°C for 6 hours to obtain powdered pentaerythritol monoketal.

[0081] (2) Preparation of isocyanate-terminated prepolymer:

[0082]Add 10.00g of diphenylmethane diisocyanate (MDI) and 26.67g of polytetrahydrofuran diol (PTMG, Mn=1,000Da) into a reaction kettle equipped with mechanical stirring and a nitrogen device, and then add dilauric acid di Butyltin (ac...

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Abstract

The invention relates to a preparation method of hydroxyl polyurethane (PHU). The method adopts the isocyanate route of synthesizing traditional polyurethane (PU) to synthesize PHU for the first time. For the preparation of linear PHU, it is divided into two steps of prepolymerization and chain extension. The process is as follows: firstly, an excess diisocyanate monomer is reacted with a macromolecular diol to obtain an isocyanate group-terminated prepolymer. Then, add the diol chain extender of ketal (aldehyde) protection and prepolymer reaction to obtain PU ketal (aldehyde), finally, under acidic condition, ketal (aldehyde) in PU ketal (aldehyde) structure ) protecting group is hydrolyzed into hydroxyl to obtain PHU. For the preparation of crosslinked PHU, the process is: react the above-mentioned linear PHU with diisocyanate monomer, control the ratio of PHU to diisocyanate monomer, so that a part of the hydroxyl group remains on the main chain of PHU, so as to obtain crosslinked PHU. Compared with the prior art, the invention has simple operation, readily available raw materials, low economic cost and high product yield, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and relates to a preparation method of hydroxyl polyurethane. Background technique [0002] Polyurethane (PUs) is an important class of polymer materials, widely used in coatings, adhesives, leather, foam, elastomers, etc., active in basic transportation, electromechanical applications, aerospace, building substrates, food processing and other fields. [0003] At present, the industrial polyurethane is generally prepared through the isocyanate route, that is, it is prepared from polyisocyanate monomers and polyhydroxy monomers through a stepwise polymerization method. In addition, the synthesis of polyurethanes via so-called non-isocyanate routes has also been reported. Among them, in the 1990s, the preparation of polyurethanes by the reaction of cyclic carbonates and primary amines aroused widespread interest. Polyurethanes synthesized by this method have additional hydroxyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/76C08G18/66C08G18/48C08G18/10C08G18/32C08G18/83C08G18/73C08G18/75C08G18/42C08G18/44C08G18/69
CPCC08G18/10C08G18/4277C08G18/44C08G18/4825C08G18/4854C08G18/69C08G18/73C08G18/755C08G18/758C08G18/7614C08G18/7671C08G18/83C08G18/3218
Inventor 郑思珣赵冰洁
Owner SHANGHAI JIAO TONG UNIV
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