A kind of preparation method of polylactic acid polyol with low acid value

A technology of polylactic acid polyol and low acid value, which is applied in the field of preparation of low acid value polylactic acid polyol, can solve the problems affecting the reactivity of polylactic acid polyol and high acid value of polylactic acid polyol, and achieve low production cost, The effect of enhancing reactivity and no discharge of three wastes

Active Publication Date: 2019-01-15
SHENZHEN ESUN IND +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to side reactions such as oxidation and cracking in the polymerization process, polylactic acid polyols contain a certain amount of carboxyl-terminated polylactic acid, which makes the acid value of polylactic acid polyols higher, thus affecting the reactivity of polylactic acid polyols

Method used

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  • A kind of preparation method of polylactic acid polyol with low acid value
  • A kind of preparation method of polylactic acid polyol with low acid value

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preparation example Construction

[0017] A preparation method of low acid value polylactic acid polyols, comprising the following steps (the following parts are parts by weight):

[0018] Preparation of polylactic acid: Add 6.63 to 70.32 parts by weight of 1,4-butanediol, 216.02 to 432.67 parts by weight of lactide, and 0.11 to 0.60 parts by weight of catalyst in a round bottom beaker, vacuumize and ventilate with nitrogen , stirred and heated to 135-175°C under nitrogen protection, and reacted at 135-175°C for 4-28 hours to obtain polylactic acid with a theoretical molecular weight of 500-4000 and an acid value of 3.50-14.10. Preferably, the catalyst is ferric chloride, aluminum chloride, butyllithium, sodium alkoxide, potassium alkoxide stannous octoate, tin tetrachloride, stannous chloride, stannous acetate, tin oxide or any combination thereof. The chemical reaction equation of above-mentioned reaction is as follows:

[0019]

[0020] Preparation of polylactic acid polyols with low acid value: add 50.5...

Embodiment 1

[0028] A preparation method of low acid value polylactic acid polyols, comprising the following steps (the following parts are parts by weight):

[0029] The preparation of polylactic acid with a theoretical molecular weight of 500: add 47.20g of 1,4-butanediol, 216.02g of lactide, and 0.11g of stannous octoate in a round-bottomed beaker, vacuumize and replace with nitrogen for 3 times. Stir and heat up to 140°C under protection, and react at 140°C for 24 hours to obtain 261.56 g of polylactic acid with a theoretical molecular weight of 500 and an acid value of 3.50.

[0030] Modification of polylactic acid: Add 70.32g of polylactic acid prepared above, 0.15g of tetraethylammonium bromide, and then add 1.54g of ethylene carbonate in a round bottom flask, vacuumize and replace with nitrogen for 3 times, and protect Stir under the conditions, raise the temperature to 140° C., and react at 140° C. for 1.0 hour to obtain a polylactic acid polyol with an acid value of 2.20.

Embodiment 2

[0032] A preparation method of low acid value polylactic acid polyols, comprising the following steps (the following parts are parts by weight):

[0033] The preparation of polylactic acid with a theoretical molecular weight of 1000: add 28.40g 1,4-butanediol, 288.65g lactide, and 0.14g stannous octoate to a round-bottomed beaker, vacuumize and replace with nitrogen for 3 times. Stir and heat up to 140°C under protection, and react at 140°C for 24 hours to obtain 301.33g of polylactic acid with a theoretical molecular weight of 1000 and an acid value of 4.00.

[0034] Modification of polylactic acid: add 52.20g of polylactic acid prepared above, 0.43g of tetraethylammonium bromide, and then add 1.46g of ethylene carbonate in a round bottom flask, vacuumize and replace with nitrogen for 3 times, under nitrogen protection conditions Stir under low temperature, increase the temperature to 165°C, and react at 165°C for 6.0 hours to obtain polylactic acid polyol with low acid value...

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Abstract

The invention relates to a preparation method for polylactic acid polyol with a low acid value. The polylactic acid polyol is prepared from polylactic acid and cyclic carbonate by a reaction under the action of a catalyst. Compared with the prior art, the prepared polylactic acid polyol with a low acid value has the following advantages: the content of carboxyl end group is low, and the acid value is less than 3, so the reactiveness of polylactic acid polyol is reinforced, and facilitation to participation of polylactic acid polyol in a reaction in subsequent application is obtained. In addition, the preparation method provided by the invention has the characteristics of simple process, low production cost, no need of a solvent in the process of preparation, no discharge of three wastes, capability of large-scale production, etc.

Description

technical field [0001] The invention relates to a preparation method of polylactic acid polyol with low acid value. Background technique [0002] Polyester polyol is the main raw material for preparing polyurethane materials, which can be used to prepare polyurethane rubber, elastomers, adhesives, coatings, foams and other materials. Usually polyester polyols are formed by condensation of dibasic acids and polyols. The raw materials basically come from petroleum products. With the increasing consumption of petroleum resources, it is more and more popular to use renewable resources instead of petroleum resources to produce polyester polyols. Pay attention to. Polylactic acid polyol is chemically synthesized with lactic acid, a product of microbial fermentation, as a monomer. It is non-toxic, non-irritating, and has good biocompatibility and degradability. It is an ideal resin additive, modifier and raw material for preparing biodegradable polyurethane. Traditional polylacti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/91C08G63/08C08G18/42
Inventor 余海斌石朔赵海超郑艳杨义浒
Owner SHENZHEN ESUN IND
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