Polycarbonate diol as well as preparation method and application thereof

A polycarbonate diol technology, applied in the chemical industry, can solve problems such as complex operation, high energy consumption of equipment, large equipment investment, etc., and achieve the effects of stable reaction system, reduced total input, and high efficiency

Active Publication Date: 2021-11-12
佛山市中天融新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the membrane separation method is difficult; the conditions required for the adsorption method are harsh; both the azeotropic distillation method and the extractive distillation method will introduce new solvents, which will bring impurities to dimethyl carbonate, and the recovery of the solvent needs to be considered during subsequent treatment, at least It is also necessary to increase the rectification treatment steps, and the operation is complicated; the operation pressure of the pressurized rectification method is high, resulting in large equipment investment and high energy consumption of the device

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The preparation method of polycarbonate diol in this example comprises the following steps:

[0048] S1: Set the initial temperature of the reactor to 90°C, and the pressure in the reactor to normal pressure, and then put 1,6-hexanediol, dimethyl carbonate and catalyst sodium methoxide into the reactor after the above preset temperature, to The amounts of substances were: 100 parts of 1,6-hexanediol, 96 parts of dimethyl carbonate, and 1.5 parts of catalyst sodium methoxide. By weight: the weight of 1,6-hexanediol is 7.090kg, the weight of dimethyl carbonate is 5.246kg, and the weight of sodium methoxide is 0.049kg. The purpose of this example is to produce polycarbonate binary with a molecular weight of 2000 alcohol. Then gradually increase the temperature in the reactor, and carry out the atmospheric distillation reaction (i.e. the first stage reaction) when the temperature is raised to 150° C.;

[0049] S2: In the process of the atmospheric distillation reaction (i...

Embodiment 2

[0054] The preparation method of polycarbonate diol in this example comprises the following steps:

[0055] S1: Set the initial temperature of the reactor to 90°C, and the pressure in the reactor to normal pressure, and then put 1,6-hexanediol, dimethyl carbonate and catalyst sodium methoxide into the reactor after the above preset temperature, to The amounts of substances are: 100 parts of 1,6-hexanediol, 90 parts of dimethyl carbonate, and 1.5 parts of catalyst sodium methoxide. By weight: the weight of 1,6-hexanediol is 7.090kg, the weight of dimethyl carbonate is 4.918kg, and the weight of sodium methoxide is 0.049kg. The purpose of this example is to produce polycarbonate binary with a molecular weight of 1000 alcohol. Then gradually increase the temperature in the reactor, and carry out the atmospheric distillation reaction (i.e. the first stage reaction) when the temperature is raised to 150° C.;

[0056] S2: In the process of the atmospheric distillation reaction (i....

Embodiment 3

[0061] In this example, polyether diol (PPG) and polycarbonate diol with a molecular weight of 2105 prepared in Example 1 were used as soft chains to synthesize thermoplastic polyurethane. The molecular weight of the polycarbonate diol in this example is 2105, and the hydroxyl value is 53.3mgKOH / g, which is represented by PCDL-2 below; the hydroxyl value of the polyether glycol (PPG) is 55.6mgKOH / g;

[0062] The preparation method of thermoplastic polyurethane in this example is as follows:

[0063] Add 8.95g PCDL-2, 6.5gPPG, 5.6g diphenylmethane-4,4'-diisocyanate (MDI) and react at 70°C until the content of isocyanate group (-NCO) reaches the theoretical value, then add dimethylacetamide (DMAC) as a solvent to disperse the prepolymer, then add the catalyst stannous octoate and 1.28g 1,4-butanediol (BDO), react at 75°C for 2.5h, precipitate with methanol / water mixture, and dry After that, polyurethane 1 was obtained.

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Abstract

The invention discloses polycarbonate diol as well as a preparation method and application thereof. The preparation method comprises the following steps: S1, mixing diol and dimethyl carbonate for reaction, and conducting distilling to obtain a blend of dimethyl carbonate and methanol; S2, cooling the blend, separating out dimethyl carbonate crystals, and adding the dimethyl carbonate crystals into the mixture obtained in the step S1; and S3, repeating the steps, and conducting distilling to obtain the polycarbonate diol. According to the invention, after the distilled dimethyl carbonate and methanol blend is purified and separated, the purified dimethyl carbonate is put into a reaction kettle in the form of a raw material, and the molecular weight and the hydroxyl value of the prepared polycarbonate diol can be accurately controlled by controlling the feeding ratio of the raw material. Compared with a traditional preparation process, the method can reduce the total input amount of the raw material dimethyl carbonate, the reaction system is stable, the cost is low, and the efficiency is high.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to polycarbonate diol and its preparation method and application. Background technique [0002] Polycarbonate diol is a kind of polyester polyol with excellent comprehensive properties. It has both the performance advantages of polyester polyol and polyether polyol. It is a high-end raw material for the synthesis of polyurethane materials and is widely used in elastomers, adhesives and coatings and other fields. [0003] The route for preparing polycarbonate diols by transesterification is based on the transesterification reaction of small molecule carbonates and small molecule diols. The carbonyl group of the small molecule carbonate enters the product, and the groups on both sides are converted into by-products, which are removed from the reaction system. Taking dimethyl carbonate as an example, two molecules of methanol will be removed. The transesterification reacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/30C08G18/44
CPCC08G64/305C08G18/44
Inventor 许阳宾杨武彬黄绍源陈永强
Owner 佛山市中天融新材料科技有限公司
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