Ternary iron-based catalyst and application thereof to catalyzing epoxy chloropropane and butadiene to prepare novel polymer through copolymerization

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

Active Publication Date: 2017-01-04
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

[0023] In a two-necked flask with a thermometer and a stirring rotor, add 20ml of hexane that has been treated with anhydrous and oxygen-free oxygen, turn on the stirring, and then successively pass in 1.5ml of butadiene and 6.0ml of epichlorohydrin. After heating in a 70℃ water bath 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 flask into a 70°C water bath and react for 2 hours. After the reaction is over, add 5% hydrochloric acid ethanol solution to terminate the polymerization, pour out the supernatant, wash the obtained polymer with a large amount of ethanol, add antioxidant (1010 and 2,6-di-tert-butyl-4-methylphenol Mix at a weight ratio of 1:1), weighed after drying, and the polymer yield was 45.0%. GPC test was performed on the polymer sample, and the number average molecular weight of the poly...

Embodiment 2

[0025] In a two-necked flask with a thermometer and a stirring rotor, add 20 ml of hexane treated with anhydrous and oxygen-free according to the meter, and start stirring, and then pass in 6 ml of butadiene and 1.5 ml of epichlorohydrin in sequence. After heating in a 60℃ water bath for 15 minutes, add 0.6mL iron acetylacetonate solution (0.1mol / L hexane solution), 1.2mL sesqui aluminum solution (1mol / L hexane solution), 0.6mL three O-Methylphenyl phosphite solution (0.2mol / L hexane solution), put the polymerization flask into a 60℃ water bath, and react for 4 hours. After the reaction is over, add 5% hydrochloric acid ethanol solution to terminate the polymerization, pour out the supernatant, wash the obtained polymer with a large amount of ethanol, add antioxidant (1010 and 2,6-di-tert-butyl-4-methyl Phenol was mixed at a weight ratio of 1:1), weighed after drying treatment, and the polymer yield was 65.0%. GPC test was performed on the polymer sample, and the number averag...

Embodiment 3

[0027] In a two-necked flask with a thermometer and a stirring rotor, add 20 ml of hexane treated with anhydrous and oxygen-free according to the meter, and start stirring, and then pass in 6 ml of butadiene and 1.5 ml of epichlorohydrin in sequence. After heating in a 70℃ water bath 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 diethyl phosphite solution (0.2mol / L hexane solution), put the polymerization flask into a 70℃ water bath, and react for 2 hours. After the reaction is over, add 5% hydrochloric acid ethanol solution to terminate the polymerization, pour out the supernatant, wash the obtained polymer with a large amount of ethanol, add antioxidant (1010 and 2,6-di-tert-butyl-4-methyl Phenol was mixed at a weight ratio of 1:1), and weighed after drying treatment. The polymer yield was 70.0%. GPC test was performed on the polymer sample, and the number average molecul...

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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

[0001] (1) Technical field [0002] The invention relates to the field of polymer synthesis, in particular to a ternary iron-based catalyst and its application to catalyze the copolymerization of epichlorohydrin and butadiene to prepare novel polymers. [0003] (2) Background technology [0004] The new polymer is prepared by copolymerization of epichlorohydrin and butadiene. The main chain contains -COC-ether bond and the side chain contains chloromethyl. Therefore, it has good oil resistance, solvent resistance, acid resistance, Alkali resistance, weather resistance, gas permeability resistance, ozone resistance, etc., and outstanding shock absorption performance. It has excellent low temperature resistance and excellent adhesion and processability. [0005] The prior art has disclosed a variety of methods for the catalytic polymerization of epichlorohydrin. For example, JP04198319 proposes to use SbCl 5 As a catalyst, ethylene glycol is an initiator to prepare hydroxyl-terminated po...

Claims

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Application Information

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Patent Type & Authority Applications(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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