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Method for preparing polyepichlorohydrin by catalyzing epichlorohydrin polymerization by using three-element iron catalyst

A polyepichlorohydrin and epichlorohydrin technology, applied in the field of polymer synthesis, can solve the problems of low activity, small molecular weight of the product, wide distribution of PDI, etc., and achieve the effects of high yield, easy reaction control and light color

Active Publication Date: 2015-04-29
山东菏泽玉皇化工有限公司
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  • Abstract
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Problems solved by technology

[0004] In order to solve the problems in the prior art of catalyzing the synthesis of polyepichlorohydrin from epichlorohydrin with low catalyst activity, small molecular weight of the obtained product, and wide PDI distribution, the present invention provides a ternary iron catalyst to catalyze the polymerization of epichlorohydrin to prepare Polyepichlorohydrin method

Method used

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  • Method for preparing polyepichlorohydrin by catalyzing epichlorohydrin polymerization by using three-element iron catalyst
  • Method for preparing polyepichlorohydrin by catalyzing epichlorohydrin polymerization by using three-element iron catalyst

Examples

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Effect test

Embodiment 1

[0020] In a 100 mL Schlenk polymerization bottle, add 20 mL of anhydrous and oxygen-free hexane and 7.8 mL of epichlorohydrin in sequence, heat in a water bath at 70 °C for 15 min, and then add 0.5 mL of ferric isooctanoate solution ( 0.1 mol / L hexane solution), 0.25 mL triethylaluminum solution (1 mol / L hexane solution), 0.5 mL diethyl phosphite solution (0.2 mol / L hexane solution). Put the polymerization bottle into a 70°C water bath and react for 2 hours. After the reaction, 5% hydrochloric acid ethanol solution was added to terminate the polymerization, the supernatant was poured out, and the obtained polymer was washed with a large amount of ethanol, dried and weighed, and the yield of the polymer was 41.0%. The polymer sample was tested by GPC, and the number average molecular weight of the polymer was 12000, and the molecular weight distribution was 1.15.

Embodiment 2

[0022] In a 100 mL Schlenk polymerization bottle, add 20 mL of anhydrous and oxygen-free hexane and 7.8 mL of epichlorohydrin in sequence, heat in a water bath at 70 °C for 15 min, and then add 0.5 mL of ferric isooctanoate solution ( 0.1 mol / L hexane solution), 1.0mL triisobutylaluminum solution (1mol / L hexane solution), 0.5mL diethyl phosphite solution (0.2 mol / L hexane solution), put the polymerization bottle Put it into a 70°C water bath and react for 2 hours. After the reaction, 5% hydrochloric acid ethanol solution was added to terminate the polymerization, the supernatant was poured out, and the obtained polymer was washed with a large amount of ethanol, dried and weighed, and the yield of the polymer was 68.0%. The polymer sample was tested by GPC, and the number average molecular weight of the polymer was 15200, and the molecular weight distribution was 1.31.

Embodiment 3

[0024] Into a 100 mL Schlenk polymerization bottle, add 20 mL of anhydrous and oxygen-free hexane and 7.8 mL of epichlorohydrin in sequence, heat in a water bath at 50 ° C for 15 min, and then add 0.5 mL of iron neodecanoate solution ( 0.1 mol / L hexane solution), 1.2 mL triisobutyl aluminum solution (1 mol / L hexane solution), 0.6 mL tributyl phosphate solution (0.2 mol / L hexane solution), put the polymerization bottle Put it into a 50°C water bath and react for 6 hours. After the reaction, 5% hydrochloric acid ethanol solution was added to terminate the polymerization, and the supernatant was poured out. The obtained polymer was washed with a large amount of ethanol, dried and weighed, and the yield of the polymer was 56.0%. The polymer sample was tested by GPC, and the number average molecular weight of the polymer was 13600, and the molecular weight distribution was 1.21.

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Abstract

The invention discloses a method for preparing polyepichlorohydrin by catalyzing epichlorohydrin polymerization by using a three-element iron catalyst, belonging to the field of polymer preparation and solving the problem of low activity of the catalyst for synthesizing polyepichlorohydrin from polymerization, and small molecular weight and wide PDI distribution of the obtained product in the prior art. The three-element iron catalyst (iron compound, alkyl aluminum compound or electron donor) is adopted to catalyze epichlorohydrin homopolymerization to obtain the polyepichlorohydrin, of which the molecular weight is 10000 above, the polymer color is light and the PDI distribution is 1.2 or so; and the reaction is easy to control. The catalyst is easy to prepare and has the advantage of high polymer yield. The iron compound is iron naphthenate, iron neodecanoate, iron isooctoate or the like; the organic aluminum compound is triisobutylaluminum, triethyl aluminum, sesquialuminum or the like; and the electron donor is tri-ortho-methylphenyl phosphite, diethyl phosphite, tributyl phosphate or the like.

Description

technical field [0001] The invention relates to the field of polymer synthesis, in particular to a method for preparing polyepichlorohydrin by catalyzing epichlorohydrin polymerization with a ternary iron catalyst. Background technique [0002] Polyepichlorohydrin is prepared by ring-opening polymerization of epichlorohydrin. Its main chain contains -C-O-C-ether bonds, and there are chloromethyl groups on the side chains. It has good oil resistance, solvent resistance, acid resistance and weather resistance. resistance to gas permeation. [0003] The prior art has disclosed a variety of methods for catalytic polymerization of epichlorohydrin, such as JP04198319 proposed to use SbCl 5 As a catalyst, ethylene glycol is used as an initiator to prepare hydroxyl-terminated polyepichlorohydrin; the Chinese invention patent with application number 200810187705.3 proposes to use double metal cyanide complexes as catalysts to prepare low-molecular-weight hydroxyl-terminated polyepic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/24
Inventor 朱路群焦俊卿侯红霞苏忠魁陈晓丽胡尊燕王玉强陈双喜王瑛王胜伟
Owner 山东菏泽玉皇化工有限公司
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