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Composite functional super high cross-linked adsorption resin containing quaternary amine group, and its preparation method

A technology with ultra-high cross-linking and composite functions, which can be used in chemical instruments and methods, other chemical processes, etc., and can solve the problems of limited adsorption performance, low specific surface area, and poor organic adsorption performance.

Active Publication Date: 2006-11-22
NANJING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Macroporous or gel-type cation exchange resins containing quaternary amine groups (industrialized product name D201 resin) have been widely used in the removal of metal ions, but these resins usually have a low specific surface area and poor adsorption performance on organic matter.
Literature search shows that Wang Ruifang of Nankai University in Tianjin has synthesized ultra-high cross-linked adsorption resins containing quaternary amino groups, but it is disclosed that polystyrene polymers are synthesized by mixing toluene and liquid wax as a porogen, and N is used for amination. N-dimethylformamide is used as a swelling agent, and the specific surface area of ​​the finally prepared trimethylamine-modified ultra-high cross-linked resin is only 174.1m 2 / g, which limits its adsorption performance for less polar organic substances

Method used

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  • Composite functional super high cross-linked adsorption resin containing quaternary amine group, and its preparation method
  • Composite functional super high cross-linked adsorption resin containing quaternary amine group, and its preparation method
  • Composite functional super high cross-linked adsorption resin containing quaternary amine group, and its preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Suspension polymerization.

[0024] Add a certain amount of dilute sodium hydroxide solution to the styrene monomer or directly filter the monomer through a resin column equipped with a strong base anion exchange resin to remove the polymerization inhibitor.

[0025] In a 1000mL beaker, add 210g styrene, 26g divinylbenzene, and 140g liquid paraffin, stir well and set aside.

[0026] In a 1000mL three-neck flask, add 600g of distilled water and raise the temperature to 40°C, then add 6g of gelatin, stir until completely dissolved, and at the same time raise the temperature to 50°C, add 2mL of methylene blue, stir well, add the above-mentioned styrene, divinylbenzene and liquid Add the initiator benzoyl peroxide 4.0g to the wax mixture; adjust the stirring speed to make the oil droplet size appropriate, gradually raise the temperature to 80°C at a speed of 1°C / 6min, keep it warm for 4 hours, and then gradually raise the temperature to 85°C Keep warm for 3 hours, keep ...

Embodiment 2

[0039]The synthetic steps of another embodiment of the present invention are as follows:

[0040] A) Using styrene as monomer, divinylbenzene as crosslinking agent, liquid wax as porogen, magnesium carbonate as dispersant, benzoyl peroxide as initiator, and suspension polymerization Linked macroporous polystyrene-divinylbenzene copolymer, steam distillation or extraction with ethanol as solvent to remove the residual porogen in the resin channels, and then air-dried to obtain low cross-linked macroporous polystyrene- Divinyl benzene resin, that is, white balls.

[0041] Wherein the dosage of the crosslinking agent is 4% of the total amount of the monomer and the crosslinking agent, the dosage of the porogen is 40% of the weight of the monomer, and the crosslinking degree of the low crosslinking macroporous polystyrene is 2%.

[0042] B) soak the white ball in chloromethyl ether which is 4 times its weight, add 20% zinc chloride of the white ball weight as a catalyst, and carr...

Embodiment 3

[0047] The synthetic steps of another embodiment of the present invention are as follows:

[0048] A) Use styrene as a monomer, divinylbenzene as a crosslinking agent, use No. 200 solvent oil as a porogen, and use gelatin (or polyvinyl alcohol, or a mixture of magnesium carbonate, gelatin, and polyvinyl alcohol) As a dispersant, use benzoyl peroxide as an initiator, and use suspension polymerization method to synthesize macroporous polystyrene-divinylbenzene copolymer with low crosslinking degree, and use ethanol (or acetone, industrial alcohol, low boiling point solvent gasoline) Perform solvent extraction to remove the porogen remaining in the resin channels, and then air-dry to obtain low-crosslinked macroporous polystyrene-divinylbenzene resin, that is, white balls.

[0049] Wherein the dosage of the crosslinking agent is 7% of the total amount of the monomer and the crosslinking agent, the dosage of the porogen is 100% of the weight of the monomer, and the crosslinking de...

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Abstract

The invention discloses a super high cross-linking adsorption resin with quaternary amines base composite function and making method, which comprises the following steps: utilizing phenylethene as monomer, diphenyl ethylene as cross linking agent, liquid wax as hole-sealing agent, magnesium carbonate as disperser, benzoyl peroxide as initiator; adopting nitrobenzene, substituted nitrobenzene, dichloroethanes or orthodichlorobenzene as swelling agent in the cross-linking reaction course of chloromethylation low cross-linking large-hole polyphenylacetylene; using zinc chloride, ferric chloride or tin tetrachloride as catalyst to produce different cross linking composite functional resin priority in the preset time and temperature condition; adding trimethylamine to aminate to produce the product. The resin possesses double functions of adsorption and ion exchanging, which can be applied in drug separation, little polluted water source and organic chemical waste water harnessing.

Description

1. Technical field [0001] The invention relates to an adsorption resin and a synthesis method thereof, in particular to an ultra-high cross-linking adsorption resin with composite functions containing quaternary amine groups and a preparation method thereof. 2. Background technology [0002] The School of Environment of Nanjing University has applied for a patent (Patent No. ZL01134143.2) of "A Synthetic Method of an Ultra-Highly Cross-linked Weak Base Anion Exchange Resin with Dual Functions" in 2001. The main steps are: a) using liquid paraffin, 200# solvent oil is used as a porogen, magnesium carbonate, gelatin, polyvinyl alcohol and other mixtures are used as a dispersant, styrene is used as a monomer, divinylbenzene is used as a crosslinking agent, and benzoyl peroxide is used as an initiator. Using suspension polymerization method to synthesize macroporous polystyrene with low cross-linking degree, then according to the properties of porogen, steam distillation or extr...

Claims

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Application Information

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IPC IPC(8): C08F212/08B01J20/26C08F8/20C08F212/36C08J3/24
Inventor 李爱民蒋珍茂葛俊杰张晓吴春金胡学伟王春杨鑫张全兴
Owner NANJING UNIV
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