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Method of preparing polycarbonate dihydric alcohol

A technology of polycarbonate di- and diethyl carbonate is applied in the field of preparation of polycarbonate diol, and can solve the problems of difficulty in removal and difficult control of technological process, so as to achieve uninhibited reactivity, stable reactivity, and high technological progress. The effect of easy control of the process

Inactive Publication Date: 2009-11-18
JIANGSU CHEM RES INST
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  • Abstract
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  • Application Information

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Problems solved by technology

The carbon dioxide epoxide regulated copolymerization method is characterized by low cost of raw materials, but only polycarbonate diols with specific epoxide structures can be synthesized, and a large amount of catalyst needs to be used in the preparation process. It is also difficult to remove large amounts of catalyst in
When this polycarbonate diol containing transesterification catalyst reacts with isocyanate to prepare polycarbonate type polyurethane material, because these residual transesterification catalysts have adverse effects on this urethanization reaction, so this kind The process of urethanization reaction is difficult to control, so it is necessary to develop a new preparation method of polycarbonate diol to solve the existing problems

Method used

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  • Method of preparing polycarbonate dihydric alcohol

Examples

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Effect test

Embodiment 1

[0020] A) In a 1L glass flask, add 427g of diethyl carbonate, 625g of 1,6-hexanediol and 0.084g of tetraisopropyl phthalate, stir and react at 200°C for 3 hours, then stir at 100mmHg Under the pressure, after continuing to react for 5.5 hours, obtain polycarbonate diol 537g containing transesterification catalyst.

[0021] B) Take 100g of the above product in a 500mL reaction flask, add 3g of water at 120°C, stir for 1 hour to deactivate the catalyst, remove excess water under reduced pressure, and obtain polycarbonate without transesterification catalyst Ester diol.

[0022] Polyurethane reaction:

[0023] Add 100 g of the above-mentioned polycarbonate diol that has undergone deactivation treatment into a 500 mL reaction flask, heat it to 70 ° C, then add MDI, take a sample after reacting for 1 hour, and measure the conversion rate of MDI in the system. The results are shown in Table 1 .

Embodiment 2

[0025] 100 g of polycarbonate diol containing transesterification catalyst synthesized by the method in Example 1, added 8.78 mg of tributyl phosphite, heated to 120° C. under continuous stirring, heated and stirred at this temperature for 3 hours, cooled and discharged . Carry out polyurethane reaction with the method of embodiment 1, take a sample after 1 hour, measure the conversion rate of MDI in the system, the results are shown in Table 1.

Embodiment 3

[0027] A) In a 1L glass flask, add 490 g of 1,5-pentanediol, 410 g of diethyl carbonate, 0.08 g of tetraisopropyl phthalate as a transesterification catalyst, stir and react for 4 hours at 150° C., and then Under the pressure of 100 mmHg, after continuing to react for 5.5 hours, the polycarbonate diol containing the transesterification reaction catalyst was obtained.

[0028] B) Take 100g of the above product in a 500mL reaction flask, add 3g of water at 120°C, stir for 1 hour to deactivate the catalyst, remove excess water under reduced pressure, and obtain polycarbonate without transesterification catalyst Ester diol.

[0029] Polyurethane reaction:

[0030] Add 100 g of the above-mentioned polycarbonate diol that has undergone deactivation treatment into a 500 mL reaction flask, heat it to 70 ° C, then add MDI, take a sample after reacting for 1 hour, and measure the conversion rate of MDI in the system. The results are shown in Table 1 .

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Abstract

The invention discloses a preparation method of polycarbonate diol. The preparation method has simple process, and the reactivity of the prepared polycarbonate diol is not inhibited when it undergoes urethane reaction with isocyanate or the like. The technical scheme of the preparation method of the present invention is A) first diol and carbonic acid ester are synthesized the polycarbonate dihydric alcohol containing transesterification catalyst by transesterification method under the presence of catalyst; Adding a substance that deactivates the transesterification catalyst to the ester diol deactivates the transesterification catalyst.

Description

technical field [0001] The present invention relates to a kind of preparation method of dibasic alcohol, more specifically relate to a kind of preparation method of polycarbonate dibasic alcohol. Background technique [0002] Polycarbonate diol (PCDL) is a polymer with multiple carbonate groups in the molecule and hydroxyl groups at both ends of the molecule. It has the following structure: [0003] [0004] (wherein R in the above formula represents an aliphatic or alicyclic hydrocarbon group and an alkoxy group with 2-10 carbon atoms, R can be the same or different) and can be used to synthesize a new generation of polycarbonate polyurethane. Compared with polyurethane materials synthesized by traditional polyols, polycarbonate polyurethanes have excellent mechanical properties, hydrolysis resistance, heat resistance, oxidation resistance and wear resistance. Therefore, polycarbonate diols and corresponding The development of new polycarbonate polyurethane materials ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/42
Inventor 刘晓燕戚全辉
Owner JIANGSU CHEM RES INST
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