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Method of preparing polycarbonate dihydric alcohol

A technology of polycarbonate diol and polycarbonate diol, which is applied in the field of preparation of polycarbonate diol, and can solve problems such as difficult removal and difficult control of the process

Inactive Publication Date: 2007-08-08
JIANGSU CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • 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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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 making method of polycarbonate dihydroxy alcohol, which comprises the following steps: A) synthesizing polycarbonate dihydroxy alcohol through ester exchange of dialcohol and carbonate under catalyst; B) adding inactive material to inactivate ester change 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 Applications(China)
IPC IPC(8): C08G64/42
Inventor 刘晓燕戚全辉
Owner JIANGSU CHEM RES INST
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