A kind of ternary iron catalyst and its application to prepare polymer by catalyzing the copolymerization of epichlorohydrin and butadiene

A technology of epichlorohydrin and catalyst, which is applied in the field of polymer synthesis to achieve the effect of high yield

Active Publication Date: 2018-05-11
SHANDONG YUHUANG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the coordination copolymerization of catalyzed diolefins and epichlorohydrin in the prior art has rarely been reported so far.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a two-necked flask equipped with a thermometer and a stirring rotor, add 20 ml of hexane treated with anhydrous and anaerobic treatment, and start stirring, and then sequentially introduce 1.5 ml of butadiene and 6.0 ml of epichlorohydrin. After heating in a water bath at 70°C for 15 minutes, add 0.5mL iron isooctanoate solution (0.1mol / L hexane solution), 0.25mL triethylaluminum solution (1mol / L hexane solution), 0.5mL Diethyl phosphite solution (0.2mol / L hexane solution). Put the polymerization bottle into a 70°C water bath and react for 2 hours. After the reaction finishes, add 5% hydrochloric acid ethanol solution to terminate the polymerization, pour out the supernatant, and the obtained polymer is washed with a large amount of ethanol, and anti-aging agent (1010 and 2,6-di-tert-butyl-4-methylphenol Mixed at a weight ratio of 1:1), weighed after drying, the polymer yield was 45.0%. The polymer sample was tested by GPC, and the number average molecular weight o...

Embodiment 2

[0021] In a two-necked flask equipped with a thermometer and a stirring rotor, 20 ml of hexane treated with anhydrous and anaerobic treatment was metered in, and the stirring was started, and then 6 ml of butadiene and 1.5 ml of epichlorohydrin were sequentially introduced. After heating in a water bath at 60°C for 15 minutes, add 0.6 mL of iron acetylacetonate solution (0.1 mol / L hexane solution), 1.2 mL of sesquialuminum solution (1 mol / L hexane solution), and 0.6 mL of three o-methylphenyl phosphite solution (0.2mol / L hexane solution), put the polymerization bottle into a water bath at 60°C, and react for 4 hours. After the reaction, add 5% ethanol solution of hydrochloric acid to terminate the polymerization, pour out the supernatant, and the obtained polymer is washed with a large amount of ethanol, and anti-aging agent (1010 and 2,6-di-tert-butyl-4-methyl Phenol was mixed at a weight ratio of 1:1), weighed after drying, and the polymer yield was 65.0%. The polymer sampl...

Embodiment 3

[0023] In a two-necked flask equipped with a thermometer and a stirring rotor, 20 ml of hexane treated with anhydrous and anaerobic treatment was metered in, and the stirring was started, and then 6 ml of butadiene and 1.5 ml of epichlorohydrin were sequentially introduced. After heating in a water bath at 70°C for 15 minutes, add 0.5ml iron isooctanoate solution (0.1mol / L hexane solution), 1.0mL triisobutylaluminum solution (1mol / L hexane solution), 0.5ml mL of diethyl phosphite solution (0.2mol / L hexane solution), put the polymerization bottle into a water bath at 70°C, and react for 2 hours. After the reaction, add 5% ethanol solution of hydrochloric acid to terminate the polymerization, pour out the supernatant, and the obtained polymer is washed with a large amount of ethanol, and anti-aging agent (1010 and 2,6-di-tert-butyl-4-methyl Phenol was mixed at a weight ratio of 1:1), weighed after drying, and the polymer yield was 70.0%. The polymer sample was tested by GPC, an...

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Abstract

The invention relates to the field of polymer synthesis, and in particular discloses a ternary iron-based catalyst and application thereof to catalyzing epoxy chloropropane and butadiene to prepare a novel polymer through copolymerization. The application to preparing the novel polymer is characterized by comprising the following steps: enabling the ternary iron-based catalyst to react in a hydrocarbon solvent, wherein epoxy chloropropane and butadiene are adopted as reaction substrates; performing a reaction for 1-24 hours at 0-100 DEG C, terminating the reaction after polymerization is completed, washing for multiple times with ethanol, adding an anti-aging agent, and drying to obtain a target product. As the ternary iron-based catalyst (an iron compound, an organic aluminum compound and an electron donor) is adopted to catalyze copolymerization of epoxy chloropropane and butadiene, the molecular weight of an obtained polymer is 10,000 or above, the polymer is light in color, the PDI is about 1.0-2.0, and the reaction is stable and easy to control.

Description

(1) Technical field [0001] The invention relates to the field of polymer synthesis, in particular to a ternary iron-based catalyst and its application for preparing novel polymers by catalyzing the copolymerization of epichlorohydrin and butadiene. (2) Background technology [0002] The new type of polymer is prepared by copolymerization of epichlorohydrin and butadiene. Its main chain contains -C-O-C-ether bonds, and there are chloromethyl groups on the side chains, so it has good oil resistance, solvent resistance, acid resistance, Alkali resistance, weather resistance, gas permeability resistance, ozone resistance and other properties, and outstanding shock absorption performance, good low temperature resistance and excellent adhesion and processability. [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 hydro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/26
CPCC08G65/266C08G65/2675
Inventor 焦俊卿苏忠魁王玉强陈双喜王胜伟
Owner SHANDONG YUHUANG CHEM CO LTD
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