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Method for shortening induction time during catalysis of ring opening polymerization of epoxide in discontinuous method

A technology of ring-opening polymerization and induction time, which is applied in the field of batch synthesis of polyether polyols, can solve the problems of shortened induction time, accelerated induction, and insufficient induction, and achieves the effects of shortening the induction period and saving dosage

Active Publication Date: 2013-10-23
HUAIAN BUD POLYURETHANE SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to: provide a method for shortening the induction time when catalyzing the ring-opening polymerization of epoxides in a batch method, and solve the problem of the vacuum system or the raw material itself in the initial induction when the DMC catalyst batch method synthesizes polyether polyols The water content is too high or one or more of K, Na ions, alkaline impurities, chloropropane, etc. in the initial induction raw material is high, and the induction is still not fast enough after adding a certain amount of acid. , to ensure a shortened induction time in the presence of the aforementioned unfavorable conditions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: system polyoxypropylene trihydric alcohol (M n =3000)

[0018] Add 42g polyoxypropylene trihydric alcohol (M n =500) Initiator (K, Na ions n =500) and PO, the control pressure is at 600mmHg, and the initiator is added when the PO feed reaches 470 g; continue to feed PO, 460mmHg, a total of 700g PO; after the full reaction is completed, vacuumize to remove residual gas, and close the vacuum valve , stop the vacuum.

[0019] Result analysis: the initiator was added successively at 3:7; the induction was 1 min; the initiator was added before 70% of PO was added; the hydroxyl value (mg KOH / g) was 57.3; the viscosity (25°C, mpa·s) 570; molecular weight distribution D=1.10.

Embodiment 2

[0026] Embodiment 2: system polyoxypropylene trihydric alcohol (M n =3000)

[0027] With embodiment 1 operation, 84g polyoxypropylene trihydric alcohol (M n =500) The initiator is put in first, and 56g of the initiator is added after induction.

[0028] Result analysis: the initiator was added successively at 6︰4; induction was 5 min; the initiator was added before 70% of PO was added; hydroxyl value (mg KOH / g) 56.7; viscosity (25°C, mpa·s) 565; molecular weight distribution D=1.07.

Embodiment 3

[0029] Embodiment 3: system polyoxypropylene trihydric alcohol (M n =3000)

[0030] Operation with embodiment 1, but initiator (K, Na ion 9ppm, mixes 80ppm sulfuric acid in advance).

[0031] Result analysis: the initiator was added successively at 3:7; the induction was 12 min; the initiator was added before 70% of PO was added; the hydroxyl value (mg KOH / g) was 57.4; the viscosity (25°C, mpa·s) 575; molecular weight distribution D=1.11.

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Abstract

The invention discloses a method for shortening induction time during the catalysis of ring opening polymerization of an epoxide in a discontinuous method. The method comprises the following steps of: adding a certain amount of PO (Propylene Oxide) or a mixture of PO and EO (Ethylene Oxide) in the presence of a DMC (Dimethyl Carbonate) catalyst by taking low-molecular weight polyether glycol as an initiator when the polyether glycol is synthesized through the DMC catalyst by adopting the discontinuous method; inducing and activating, and then continuously introducing surplus PO or EO / PO. The method is characterized in that a part of the low-molecular weight polyether glycol initiator is previously added in order to add the surplus part of the low-molecular weight polyether glycol initiator after induction is completed at relatively high catalyst concentration. The method disclosed by the invention can be used for realizing that a user is easier to implement the application of the DMC catalyst by being used for actual production and preventing the helpless measure of catalyst supplement from being often adopted during former adverse reaction condition, thereby reducing the excessive worry of a polyether manufacturer on the raw material quality.

Description

technical field [0001] The invention relates to a batch synthesis method of polyether polyols, in particular to a method for shortening the induction time when synthesizing polyether polyols with a double metal cyanide (DMC) complex catalyst. Background technique [0002] Double metal cyanide (DMC) complex catalysts are used for ring-opening polymerization of epoxides. The polyether polyols produced by this catalyst have lower unsaturation than those produced by basic catalysts (usually KOH), and can produce A higher molecular weight is obtained, and the resulting polyether is usually exempted from post-processing. The composition of DMC catalyst is generally: M a 1 [M 2 (CN) b (A) c ] d ·xM 3 (X) e ·wH 2 O·yT·zL; M 1 is selected from: Zn （Ⅱ） , Fe （Ⅱ） , Fe （Ⅲ） 、Co （Ⅱ） 、Ni （Ⅱ） 、Mo （Ⅳ） , Sn （Ⅱ） 、Cu （Ⅱ） , Pb （Ⅱ） 、Mo （Ⅵ） 、Al （Ⅲ） , V （Ⅳ） , V （Ⅴ） 、Sr （Ⅱ） , W （Ⅳ） , W （Ⅵ） , Mn （Ⅱ） and Cr （Ⅲ） At least one metal ion in; M 2 is selected from: Fe （Ⅱ） , Fe ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
Inventor 戚渭新李刚强胡冰
Owner HUAIAN BUD POLYURETHANE SCI & TECH CO LTD
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