Preparation method of polysiloxane-polyphenylether segmented copolymer for penetrative vaporization film material

A pervaporation membrane, polysiloxane technology, applied in chemical instruments and methods, semi-permeable membrane separation, membrane technology and other directions, can solve the problems of complex reaction process and high reaction requirements, achieve simple reaction process, wide application fields, The effect of good separation performance

Inactive Publication Date: 2010-06-02
BEIJING UNIV OF TECH
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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 solve the problem of complex reaction process and high reaction requirements in the prior art, to provide a polysiloxane-polyp

Method used

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  • Preparation method of polysiloxane-polyphenylether segmented copolymer for penetrative vaporization film material
  • Preparation method of polysiloxane-polyphenylether segmented copolymer for penetrative vaporization film material
  • Preparation method of polysiloxane-polyphenylether segmented copolymer for penetrative vaporization film material

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0033] Implementation example 1

[0034] Take 15g carboxyl-terminated poly-2,6-dimethylphenyl ether (molecular weight 12000g / mol) and dissolve it in chlorobenzene for later use, take 81.8g hydroxyl-terminated polydimethylsiloxane (molecular weight 10040g / mol) and dissolve in chlorine In benzene, add the polydimethylsiloxane solution to a dry 500ml four-neck flask equipped with a thermometer, condenser and stirring, then add 0.5g of dilute nitric acid (1mol / L), and divide at 120℃. Poly-2,6-dimethylphenyl ether solution was added in 5 batches, once every 90min, for a total reaction of 8h; after the reaction, the solid insoluble matter was removed by filtration, and the product was precipitated from the reaction solution with methanol, filtered, washed with water and methanol After washing and suction filtration, 95.8 g of polydimethylsiloxane-poly-2,6-dimethylphenyl ether block copolymer was obtained.

[0035] The structure of the polyphenylene ether and polysiloxane is as follows

...

Example Embodiment

[0041] Implementation example 2

[0042] Dissolve 20g of hydroxyl-terminated poly-2-methyl, 6-propyl phenyl ether (molecular weight 16000g / mol) in chlorobenzene for later use, and take 18.25g of aminopropyl-terminated polymethylphenylsiloxane (molecular weight 11200g / mol) mol) dissolved in chlorobenzene, add the polymethylphenylsiloxane solution to a dry 500ml four-neck flask equipped with a thermometer, condenser and stirring, and then add 0.24g dilute nitric acid (1mol / L), Add the poly-2-methyl, 6-propyl phenyl ether solution in 10 batches at 80°C, add once every 110 minutes, and react for a total of 24 hours; after the reaction, filter to remove the solid insolubles, and remove the product from the reaction solution with methanol Precipitate, filtered, washed with water, washed with methanol, and filtered with suction to obtain 34 g of polymethylphenylsiloxane-poly-2-methyl,6-propylphenyl ether block copolymer.

[0043] The structure of the polyphenylene ether and polysiloxane ...

Example Embodiment

[0047] Implementation example 3

[0048] Dissolve 20g of aminopropyl-terminated poly-2,6-diphenylphenyl ether (molecular weight 16000g / mol) in chlorobenzene for later use, and take 30.75g of carboxyl-terminated polydiphenylsiloxane (molecular weight 9200g / mol) to dissolve In toluene, add the polydiphenylsiloxane solution to a dry 500ml four-necked flask equipped with a thermometer, condenser and stirring, and then add 0.1g trifluoroacetic acid (1mol / L) at 100℃. The poly-2,6-diphenylphenyl ether solution was added in 8 batches, and added once every 100min for a total of 16h; after the reaction, the solid insoluble matter was removed by filtration, and the product was precipitated from the reaction solution with methanol, filtered and washed with water , Washed with methanol, and filtered with suction to obtain 45.3 g of polydiphenylsiloxane-poly2,6-diphenylphenyl ether block copolymer.

[0049] The structure of the polyphenylene ether and polysiloxane is as follows

[0050]

[0051]...

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Abstract

The invention belongs to the technical field of a preparation method of a polysiloxane-polyphenylether segmented copolymer. The preparation method is characterized by comprising the following steps of: throwing polysiloxane and polyphenylether which have reactive end groups in the molar ratio of 5-1:1, as well as an acid catalyst accounting for 0.1-5 percent of the gross mass of reactants into a reactor, and reacting for 8-24 hours at the temperature of 80-120 DEG C, wherein the reactants are respectively dissolved in a certain solvent, and a polyphenylether solution is added in batches; filtering mixture obtained after reaction, precipitating with a precipitator, suction filtrating, washing with water and removing the solvent, the catalyst and the precipitator through reduced pressure distillation to obtain the polysiloxane-polyphenylether segmented copolymer in a predicted structure. The invention provides a method which has no strict requirements on the polymerization degree size of the reactants and mild reaction conditions and can synthesize the polysiloxane-polyphenylether segmented copolymer in one step, well solving the problems of severe synthetic conditions and multiple and multifarious reaction steps.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of polysiloxane-polyphenylene ether block copolymers. Specifically, the present invention relates to a method for preparing a block copolymer by performing terminal group reaction between polysiloxane with hydrophobicity and polyphenylene ether with excellent mechanical properties. Background technique [0002] In the field of membrane application, pervaporation (PV) is an emerging membrane separation technology. PV uses the chemical potential difference of a certain component upstream and downstream of the feed liquid membrane as the driving force to achieve mass transfer, and uses the membrane to effect different components in the feed liquid. Selectivity is achieved through differences in affinity and mass transfer resistance. At present, the application of PV includes three aspects: dehydration of organic matter, recovery of valuable organic matter in water, and separation of orga...

Claims

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Application Information

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IPC IPC(8): C08G81/00B01D71/80B01D61/36
Inventor 纪树兰刘威秦振平
Owner BEIJING UNIV OF TECH
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