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Method for producing poly(alkylene carbonate)polyol

A technology of alkylene carbonate and polyol, applied in the field of preparation of low-molecular-weight polyol, can solve the problems of tediousness, low solubility in organic solvents, difficult to control catalyst content, etc., and achieve the effect of improving activity

Active Publication Date: 2017-09-05
SK INNOVATION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, as far as the double metal cyanide catalyst prepared by the above reaction is concerned, the solubility of the aqueous solution of the metal salt to the organic solvent is very low, so the use of H 2 After O is prepared, it needs to go through the process of washing with organic solvents many times, which is more cumbersome.
In addition, it is difficult to control the content of water or ethanol contained in the catalyst, resulting in a large difference in the activity of each prepared catalyst, thereby limiting commercial utilization

Method used

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  • Method for producing poly(alkylene carbonate)polyol
  • Method for producing poly(alkylene carbonate)polyol
  • Method for producing poly(alkylene carbonate)polyol

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preparation example Construction

[0027] The invention provides the preparation method of low molecular weight poly(alkylene carbonate) polyol, the preparation method of low molecular weight poly(alkylene carbonate) polyol of the present invention comprises the following steps: in the presence of Salen catalyst and double metal cyanide catalyst Next, the epoxy compound, carbon dioxide, and chain transfer agent are reacted to prepare poly(alkylene carbonate) polyol.

[0028] The preparation method of low-molecular-weight poly(alkylene carbonate) polyol of the present invention uses Salen catalyst and double metal cyanide catalyst simultaneously, thereby can realize the copolymer with the high activity that Salen catalyst has and prepare high yield, and can prepare by Poly(alkylene carbonate) polyols having ether-bonded monomers within copolymers brought about by double metal cyanide catalysts.

[0029] In addition, by adjusting the weight ratio of the Salen catalyst and the double metal cyanide catalyst, the co...

preparation example 1

[0099] [Preparation Example 1] Synthesis of Catalyst (Compound 1)

[0100] Below, the simple and economical catalyst synthesis method of the present invention is listed. Compound 1 was synthesized by a known method (Bull. Korean Chem. Soc. 2009, 30, 745-748).

[0101]

[0102] Synthesis of Compound 1-2

[0103] Compound 1-1 (100mg, 0.054mmol) and AgNO 3 (37.3 mg, 0.219 mmol) was dissolved in ethanol (3 mL) and stirred overnight. The resulting AgI was filtered and removed using celite. The solvent was depressurized and removed in vacuo to obtain compound 1-2 (0.80 g, 94%) in the form of yellow solid powder.

[0104] 1 H NMR (CDCl 3 ): δ13.51 (s, 2H, OH), 8.48 (s, 2H, CH=N), 7.15 (s, 4H, m-H), 3.44 (br, 2H, cyclohexyl-CH), 3.19 (br, 32H , NCH 2 ), 2.24(s, 6H, CH 3 ), 1.57-1.52 (br, 4H, cyclohexyl-CH 2 ), 1.43-1.26 (br, 74H), 0.90-070 (br, 36H, CH 3 )ppm.

[0105] Synthesis of compound 1

[0106] Compound 1-2 (95mg, 0.061mmol) and Co(OAc) 2 (10.7 mg, 0.061 mmo...

preparation example 2

[0113] [Preparation Example 2] DMC catalyst [ZnCl] + 2 [HCo(CN) 6 ] 2- ·[CH 3 OH] (Compound 2) Synthesis

[0114] h 3 Co(CN) 6 preparation of

[0115] 5 g (15 mmol) of Potassium hexacyanocobaltate (III) was dissolved in 15 mL of distilled water, then immersed in 140 g of ion exchange resin (Dowex 5x4-200), and filtered after 3 hours. After the filtrate of the ion exchange resin was immersed in the ion exchange resin 4 times again, it was confirmed that K + Ions and H + The ions are completely exchanged. The filtered ion exchange resin can be reused after being washed with 2N sulfuric acid aqueous solution. H was separated from the filtrate by a rotary evaporator 3 Co(CN) 6 , and at P 2 o 5 The remaining moisture was removed by storing in a vacuum desiccator for 12 hours in the presence of . By titration with standard NaOH solution, it is confirmed that the metal cyanide complex salt that has been dehydrated and passed through the ion exchange resin is H 3 Co...

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Abstract

Provided is a method for producing poly(alkylene carbonate)polyol, and specifically, a method for producing poly(alkylene carbonate)polyol having carbonate, ester, and ether bonds by mixing a Salen-based catalyst and a double metal cyanide catalyst.

Description

technical field [0001] The present invention relates to the preparation method of poly (alkylene carbonate) polyol, more specifically, relate to according to the content of catalyst, carbon dioxide and chain transfer agent, can adjust the content and molecular weight of carbonate and ether bond monomer, as a ring Process for the preparation of low molecular weight poly(alkylene carbonate) polyols of oxygenate / carbon dioxide binary copolymers. Background technique [0002] Poly(alkylene carbonate) polyols are readily biodegradable polymers, for example, which are useful materials as adhesives, packaging materials or coating materials. The method for producing poly(alkylene carbonate) polyols from epoxy compounds and carbon dioxide has high environmental value in terms of not using phosgene, which is a toxic compound, and in that carbon dioxide can be obtained at low cost. [0003] Since the 1960s, many researchers have developed catalysts of various morphologies for the prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/34
CPCC08G64/34C08G65/2663C08G65/2603C08G65/269C08G65/2696
Inventor 苏德文·苏吉托李帝豪
Owner SK INNOVATION CO LTD
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