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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-polyphenylene ether block copolymer with controllable structure and its preparation method, and to apply it in osmotic Vaporization preferentially penetrates alcohol membrane field

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

Embodiment 1

[0034] Get 15g carboxy-terminated poly-2,6-dimethylphenylene ether (molecular weight 12000g / mol) and dissolve it in chlorobenzene for subsequent use, get 81.8g hydroxyl-terminated polydimethylsiloxane (molecular weight 10040g / mol) and dissolve it in chlorine In benzene, add polydimethylsiloxane solution into 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°C Add poly-2,6-dimethylphenyl ether solution in 5 batches, add once every 90 minutes, and react for 8 hours in total; Wash and filter with suction to obtain 95.8 g of polydimethylsiloxane-poly-2,6-dimethylphenylene ether block copolymer.

[0035] The polyphenylene ether and polysiloxane structures are as follows

[0036]

[0037]Dissolve polydimethylsiloxane-poly2,6-dimethylphenylene ether block copolymer in chloroform to prepare a casting solution, and evenly coat it on a glass plate, evaporate the solvent at room temperature...

Embodiment 2

[0042] Get 20g hydroxyl-terminated poly 2-methyl, 6-propylphenylene ether (molecular weight 16000g / mol) is dissolved in chlorobenzene for subsequent use, get 18.25g aminopropyl-terminated polymethylphenylsiloxane (molecular weight 11200g / mol) mol) was dissolved in chlorobenzene, and the polymethylphenylsiloxane solution was added to a dry 500ml four-necked flask equipped with a thermometer, a condenser tube and stirring, and then 0.24g of dilute nitric acid (1mol / L) was added, Add poly 2-methyl, 6-propylphenyl ether solution in 10 batches at 80°C, add once every 110min, and react for 24h in total; Precipitated, filtered, washed with water, washed with methanol, and suction filtered to obtain 34 g of polymethylphenylsiloxane-poly2-methyl, 6-propylphenylene ether block copolymer.

[0043] The polyphenylene ether and polysiloxane structures are as follows

[0044]

[0045] Dissolve polymethylphenylsiloxane-poly2-methyl, 6-propylphenylene ether block copolymer in trichlorethyl...

Embodiment 3

[0048] Get 20g aminopropyl-terminated poly-2,6-diphenylphenyl ether (molecular weight 16000g / mol) and dissolve it in chlorobenzene for subsequent use, get 30.75g carboxyl-terminated polydiphenylsiloxane (molecular weight 9200g / mol) to dissolve In toluene, add the polydiphenylsiloxane solution into a dry 500ml four-neck flask equipped with a thermometer, condenser and stirring, then add 0.1g trifluoroacetic acid (1mol / L), at 100°C Add poly-2,6-diphenylphenyl ether solution in 8 batches, add once every 100min, and react for 16h in total; after the reaction, filter to remove solid insoluble matter, precipitate the product from the reaction solution with methanol, filter, and wash with water , washed with methanol, and suction filtered to obtain 45.3 g of polydiphenylsiloxane-poly-2,6-diphenylphenylene ether block copolymer.

[0049] The polyphenylene ether and polysiloxane structures are as follows

[0050]

[0051] Dissolve polydiphenylsiloxane-polyphenylene ether block copo...

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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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