Polycaprolactone polyol as well as preparation method and application thereof
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A polycaprolactone and polyol technology, which is applied in the field of polycaprolactone polyol and its preparation, can solve the problems of uncontrolled distribution of polymerization, defects in physical and chemical properties of polycaprolactone products, and widening, and achieves stable rate. , mild conditions, low acid value
Inactive Publication Date: 2018-11-30
GUANGDONG BOSSIN NOVEL MATERIALS TECH CO LTD
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These reactions are usually encountered in the late stage of polymerization, which leads to the loss of control of the polymerization and the broadening of the distribution; in addition, due to factors such as reactants and catalysts, a certain amount of water vapor is inevitably introduced into th...
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Embodiment 1
[0029] A preparation method of polycaprolactone polyol, described method is as follows:
[0030] Fill the reaction kettle with 62.0 kg of ethylene glycol, 200.0 ppm of stannous octoate, 1140.0 kg of caprolactone, and 100 ppm of ethyl diphenylphosphine, and fill it with nitrogen, stir and raise the temperature to 190.0 ° C, react for 30 minutes, vacuum defoam for 60 minutes, cool down and discharge , and the test acid value was 0.16 mgKOH / g to obtain polycaprolactone polyol P1.
Embodiment 2
[0032] A preparation method of polycaprolactone polyol, described method is as follows:
[0033] In the reactor, 62.0 kg of ethylene glycol, 50.0 ppm of stannous hexanoate, 1140.0 kg of caprolactone, and 25 ppm of ethyl diphenylphosphine were filled with nitrogen, stirred and heated to 120.0 ° C, reacted for 180 min, vacuum degassed for 60 min, and cooled to The test acid value was 0.19 mgKOH / g to obtain polycaprolactone polyol P2.
Embodiment 3
[0035] A preparation method of polycaprolactone polyol, described method is as follows:
[0036] In the reaction kettle, 50.0 kg of polytetrahydrofuran ether, 50.0 ppm of stannous hexanoate, 50.0 kg of caprolactone, and 25 ppm of ethyl diphenylphosphine were filled with nitrogen, stirred and heated to 230.0 ° C, reacted for 10 minutes, vacuum defoamed for 60 minutes, and cooled After discharging, the test acid value was 0.10 mgKOH / g to obtain polycaprolactone polyol P3.
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Abstract
The invention relates to polycaprolactone polyol as well as a preparation method and application thereof. The method comprises the following steps that S1, under the protection of the water-free and oxygen-free conditions and inert gas, an initiator, a catalyst, an inhibitor and caprolactone are uniformly mixed; and S2, a system obtained in the step S1 is heated to 120-230 DEG C for reaction for 10-180 minutes so as to carry out ring-opening polymerization reaction, vacuum defoamation is carried out, and cooling and discharging are carried out so as to obtain the polycaprolactone polyol, wherein the inhibitor is one or more of organic phosphine, glyphosate-sodium, ethyldiphenylphosphine or tribenzylphosphine. According to the preparation method, the specific side reaction inhibitor is added, so that the polycaprolactone polyol which is controllable in molecular weight, low in acid value, few in metal residues, narrow in polymer molecular weight distribution and capable of keeping the original excellent physicochemical properties is obtained, and the acid value of the polycaprolactone polyol prepared through the preparation method is less than 0.5 mg KOH/g.
Description
technical field [0001] The invention relates to the field of polymer materials, in particular to a polycaprolactone polyol and its preparation method and application. Background technique [0002] Polycaprolactone (PCL) is an important polymer with good mechanical properties and biodegradability, and also has good compatibility with most polymers. CN104592501 discloses an anilinolithium compound and a method for preparing polycaprolactone as a catalyst. The polycaprolactone diol prepared by the method is difficult to be used in polyurethane synthesis due to the amine group, and the polycaprolactone prepared by the method contains a solvent, has a yellower color and a wider molecular weight distribution. CN104629028 discloses polycaprolactone with reactive groups in the side chain and its preparation method. The side chain of the reactive polycaprolactone contains carboxyl groups. Adjusting the side chain content can adjust the hydrophilicity and hydrophobicity of the reacti...
Claims
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