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Preparation method of hydrophilic polycarbonate diol

A technology of polycarbonate diols and diols, which is applied in the field of preparation of hydrophilic polycarbonate diols, can solve problems such as difficult removal, residual polyurethane monomers, and affecting the performance of water-based polyurethanes, so as to improve hydrophilicity High purity, high purity, and controllable product molecular weight

Active Publication Date: 2020-11-10
WEIFANG YUANLI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] (3) The generated polyurethane has monomer residues and is difficult to remove, which affects the performance of water-based polyurethane

Method used

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  • Preparation method of hydrophilic polycarbonate diol
  • Preparation method of hydrophilic polycarbonate diol
  • Preparation method of hydrophilic polycarbonate diol

Examples

Experimental program
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Effect test

Embodiment 1

[0047]Under the protection of nitrogen, 124 g of diethyl carbonate, 82 g of 1,4-butanediol, and 13.4 g of dimethylolpropionic acid (DMPA) were added to a 500 mL four-necked flask, and the catalyst 0.012 Put 57 g of tetrabutyl titanate and 57 g of isooctane entrainer into an oil bath, put a rectification and fractionation device equipped with fillers on the neck of the bottle, and carry out atmospheric rectification at 110 ° C. After reacting for 5 hours, the by-products formed by the reaction and isooctane formed an azeotrope and flowed out. After the fraction was removed to the theoretical value, the temperature continued to rise to 180 °C; the vacuum distillation operation was carried out in stages. Set the vacuum degree to 3 kPa, continue to vacuumize for 1 h; then continue to reduce the pressure, set the vacuum degree to 100 Pa, and react for 1 h; stop the reaction after the product reaches the ideal viscosity (8000~16000 mPa.s), and wait for the system to cool to After ro...

Embodiment 2

[0052] Under the protection of nitrogen, 94.5 g of dimethyl carbonate, 82 g of 1,4-butanediol, and 13.4 g of dimethylolpropionic acid (DMPA) were added to a 500 mL four-necked flask, and the catalyst 0.012 g of tetrabutyl titanate and 57 g of isooctane entrainer were put into an oil bath, and a rectification and fractionation device equipped with fillers was placed on the neck of the bottle, and the atmospheric rectification reaction was carried out at 90°C. After reacting for 6 hours, the by-products formed by the reaction and isooctane formed an azeotrope and flowed out. After the fraction was removed to the theoretical value, the temperature continued to rise to 170 °C, and the vacuum distillation operation was carried out in stages. After replacing the vacuum device, the vacuum degree Set it to 3 kPa, continue vacuuming and reacting for 1 hour, then continue to reduce pressure, set the vacuum degree to 100 Pa, react for 1 hour, stop the reaction after the product reaches th...

Embodiment 3

[0055] Under the protection of nitrogen, 124 g of diethyl carbonate, 82 g of 1,4-butanediol, and 14.8 g of dimethylolbutyric acid (DMBA) were added to a 500 mL four-necked flask, and the catalyst 0.016 g of triethylamine and 100 g of n-heptane entrainer are placed in an oil bath, and a rectification and fractionation device equipped with fillers is placed on the neck of the bottle, and the atmospheric rectification reaction is carried out at 110 ° C. Reaction 6 h, the by-products formed by the reaction and isooctane form an azeotrope and flow out. After the fraction is removed to the theoretical value, continue to heat up to 180 °C, and carry out vacuum distillation operations in stages. After replacing the decompression device, set the vacuum degree to to 3 kPa, continue the vacuum reaction for 1 h, then continue to reduce the pressure, set the vacuum degree to 100 Pa, and react for 1 h. After the product reaches the ideal viscosity (7000~16000mPa.s), the reaction is stopped, ...

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Abstract

The invention provides a preparation method of hydrophilic polycarbonate diol. The method specifically comprises the following steps: adding carbonate, diol and a hydrophilic monomer into a reaction kettle, carrying out ternary polymerization, adding a certain amount of catalyst and entrainer, gradually removing low-boiling-point byproducts generated in the reaction process by a fractionating device, gradually reducing reaction pressure, and carrying out staged reduced pressure distillation operation. According to the present invention, the segmented polymerization process is combined with theintroduction of the azeotropic solvent to promote the forward proceeding of the reaction, reduce the azeotropic temperature, avoid the escape of the azeotrope formed by the carbonic ester and the alcohol compound, and after the product achieves the ideal viscosity, the system is cooled to room temperature to obtain the waterborne polycarbonate diol product; and the technological process is simple, controllability and reproducibility are good, the product is free of micromolecular monomer residues and high in purity, and preparation of waterborne polyurethane with excellent performance is facilitated.

Description

technical field [0001] The invention belongs to the technical field of preparation of polyester diols, in particular to a method for preparing hydrophilic polycarbonate diols. Background technique [0002] Polycarbonate diol is a type of polymer containing multiple carbonate groups and aliphatic methylene groups in the molecule, and hydroxyl groups at both ends of the molecule. Compared with traditional polyether polyurethane and polyester polyurethane, polycarbonate polyurethane synthesized from polycarbonate diol has better properties, including excellent hydrolysis resistance, oxidation resistance, heat resistance, abrasiveness and biocompatibility, etc., and due to the excellent properties of polycarbonate polyurethane, its synthetic raw material polycarbonate diol has been widely used in polyurethane elastomers, leather finishing agents, water-based paints, adhesives, etc. field, with broad application prospects. [0003] The currently known polycarbonate diols are ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/30C08G64/16C08G64/02C08G18/44C08G18/46
CPCC08G64/305C08G64/0208C08G64/025C08G64/165C08G18/44C08G18/4676
Inventor 秦国栋刘修华张建梅钟家春蒲泽军李培花
Owner WEIFANG YUANLI CHEM
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