Preparation method and application of porous material with surface grafted beta-cyclodextrin

A porous material, cyclodextrin technology, applied in chemical instruments and methods, other chemical processes, adsorption water/sewage treatment, etc., can solve problems such as particle surface reduction, increase specific surface area, and good environmental compatibility , good adsorption effect

Active Publication Date: 2014-02-12
BEIJING UNIV OF CHEM TECH
3 Cites 20 Cited by

AI-Extracted Technical Summary

Problems solved by technology

However, the adsorbent particles after adsorbing phenol will stick together, resulting in a rapid decrease in the surfa...
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Abstract

The invention discloses a preparation method and application of porous material with surface grafted beta-cyclodextrin, and belongs to the technical field of adsorbents. The preparation method comprises the following steps: preparing a polystyrene porous material by polymerizing concentrated emulsion, and then performing chloromethylation and amination reaction, feeding amino group into the surface of the polystyrene porous material, chemically modifying beta-cyclodextrin, feeding carboxyl group into the beta-cyclodextrin molecule, immersing the surface aminated polystyrene porous material in water solution of the carboxylated beta-cyclodextrin, reacting for 12-72 hours at 20-60 DEG.C under vacuum pumping condition to obtain the porous material with surface chemically grated beta-cyclodextrin. The porous material not only maintains the specific supermolecule performance of parent molecule, but also has unique macromolecule effect; since the cyclodextrin is starch fermentation product and good in environment compatibility, the cyclodextrin can be used for treating wastewater containing organic pollutant after being modified, the organic pollutant in the wastewater can be effectively removed, and the cyclodextrin is an ideal environment-friendly adsorbent.

Application Domain

Other chemical processesWater/sewage treatment by sorption

Technology Topic

EmulsionPolystyrene +15

Image

  • Preparation method and application of porous material with surface grafted beta-cyclodextrin
  • Preparation method and application of porous material with surface grafted beta-cyclodextrin

Examples

  • Experimental program(5)

Example Embodiment

[0017] Example 1:
[0018] (1) Preparation of polystyrene porous material by concentrated emulsion polymerization: firstly, in a flask, 6 g of continuous phase styrene, 1.5 g of crosslinking agent p-vinylbenzene, and 802.02 g of emulsifier Span were mixed uniformly under high-speed stirring. Then configure the dispersed phase, dissolve 0.15g of water-soluble initiator potassium persulfate and 0.375g of electrolyte potassium sulfate in 90g of deionized water, mix well, and slowly add it dropwise to the continuous phase with a syringe under stirring state to disperse in the emulsion system The latex particles are uniform in size, forming a thick emulsion. Finally, it was reacted in a water bath at 70°C for 36 hours, and the product was taken out. Washing several times with ethanol and water, drying in a vacuum oven to constant weight, the polystyrene porous material can be obtained.
[0019] (2) Amination treatment of polystyrene porous material: swell 3 g of polystyrene porous material prepared in step (1) in chloroform for 2 h, then add 3 g of paraformaldehyde and 12 ml of trimethylchlorosilane to continue soaking and swelling for 1 h, Afterwards, 2 ml of tin tetrachloride catalyst was added under ice bath, and after stirring for 30 min, the mixture was condensed and refluxed at 50°C for 60 h. After the reaction, the product was filtered and washed three times with absolute ethanol, and dried in a vacuum oven at 40°C to constant weight. Then add 1.25 g of the dried chloromethylated polystyrene porous material to 10 ml of an ethanol solution in which 3 g of polyethylene polyamine is dissolved, and conduct a vacuum reaction at room temperature for 20 hours, filter after the reaction and wash with absolute ethanol for 3 times, and dry After drying, the aminated polystyrene porous material was obtained.
[0020] (3) Synthesis of carboxylated β-cyclodextrin: First, add 5.06g of β-cyclodextrin, 5.5g of sodium hydroxide and 32.5mL of distilled water to the flask. After 5 minutes, the β-CD is completely dissolved. Add 6g of chloroacetic acid and heat at 80°C. Under the condition of reaction 3h. After the reaction is over, pour the reaction solution into a 250mL beaker, adjust the pH to 2 with HCl, then add a large amount of acetone as a precipitant to produce white floc, let it stand for 30min, filter it with a cellulose acetate filter, and vacuum at 40°C Dry to constant weight.
[0021] (4) Weigh 5 g of the carboxylated β-cyclodextrin prepared in step (3) and dissolve it in 20 ml of deionized water, add 1.5 g of the aminated polystyrene porous material prepared in step (2), and stir the reaction at room temperature 12h. After the reaction, it was washed three times with deionized water and dried to constant weight.

Example Embodiment

[0022] Example 2:
[0023] (1) Preparation of polystyrene porous material by concentrated emulsion polymerization: firstly, in a flask, 6 g of continuous phase styrene, 1.5 g of crosslinking agent p-vinylbenzene, and 802.02 g of emulsifier Span were mixed uniformly under high-speed stirring. Then configure the dispersed phase, dissolve 0.15g of water-soluble initiator potassium persulfate and 0.375g of electrolyte potassium sulfate in 90g of deionized water, mix well, and slowly add it dropwise to the continuous phase with a syringe under stirring state to disperse in the emulsion system The latex particles are uniform in size, forming a thick emulsion. Finally, it was reacted in a water bath at 70°C for 36 hours, and the product was taken out. Washing several times with ethanol and water, drying in a vacuum oven to constant weight, the polystyrene porous material can be obtained.
[0024] (2) Amination treatment of polystyrene porous material: swell 3 g of polystyrene porous material prepared in step (1) in chloroform for 2 h, then add 3 g of paraformaldehyde and 12 ml of trimethylchlorosilane to continue soaking and swelling for 1 h, Afterwards, 2 ml of tin tetrachloride catalyst was added under ice bath, and after stirring for 30 min, the mixture was condensed and refluxed at 60°C for 48 h. After the reaction, the product was filtered and washed three times with absolute ethanol, and dried in a vacuum oven at 40°C to constant weight. Then add 1.25 g of the dried chloromethylated polystyrene porous material to 12 ml of an ethanol solution in which 3 g of polyethyleneimine is dissolved, and conduct a vacuum reaction at room temperature for 24 hours. After the reaction, filter and wash 3 times with absolute ethanol, and dry After drying, the aminated polystyrene porous material was obtained.
[0025] (3) Synthesis of carboxylated β-cyclodextrin: first add 5.06g of β-cyclodextrin, 5.5g of sodium hydroxide and 32.5mL of distilled water into the flask, after 5min all β-CD is dissolved, add 6g of chloroacetic acid, 50℃ Under the condition of reaction 3h. After the reaction is over, pour the reaction solution into a 250mL beaker, adjust the pH to 3 with HCl, then add a large amount of acetone as a precipitant to produce white flocs, let stand for 30min, filter with a cellulose acetate filter, and vacuum at 40°C Dry to constant weight.
[0026] (4) Weigh 5 g of the carboxylated β-cyclodextrin prepared in step (3) and dissolve it in 15 ml of deionized water, add 1.5 g of the aminated polystyrene porous material prepared in step (2), and stir the reaction at room temperature 36h. After the reaction, it was washed three times with deionized water and dried to constant weight.

Example Embodiment

[0027] Example 3:
[0028](1) Preparation of polystyrene porous material by concentrated emulsion polymerization: first, in a flask, mix 6.85 g of continuous phase styrene, 1.72 g of crosslinking agent p-vinylbenzene and 800.89 g of emulsifier Span under high-speed stirring. . Then configure the dispersed phase, dissolve 0.17g of water-soluble initiator potassium persulfate and 0.42g of electrolyte potassium sulfate in 40g of deionized water, mix well, and slowly add it dropwise to the continuous phase with a syringe under stirring state to disperse in the emulsion system The latex particles are uniform in size, forming a thick emulsion. Finally, it was reacted in a water bath at 50°C for 24 hours, and the product was taken out. Washing several times with ethanol and water, drying in a vacuum oven to constant weight, the polystyrene porous material can be obtained.
[0029] (2) Amination treatment of polystyrene porous material: swell 3 g of polystyrene porous material prepared in step (1) in chloroform for 2 h, then add 4 g of paraformaldehyde and 8 ml of trimethylchlorosilane to continue soaking and swelling for 1 h, After that, 1 ml of tin tetrachloride catalyst was added under ice bath, and after stirring for 30 min, the reaction was condensed and refluxed at 40° C. for 48 h. After the reaction, the product was filtered and washed three times with absolute ethanol, and dried in a vacuum oven at 40°C to constant weight. Then add 1.25 g of the dried chloromethylated polystyrene porous material to 10 ml of an ethanol solution in which 3 g of triethylenetetramine is dissolved, and conduct a vacuum reaction at room temperature for 24 hours. After the reaction, filter and wash 3 times with absolute ethanol, and dry After drying, the aminated polystyrene porous material was obtained.
[0030] (3) Synthesis of carboxylated β-cyclodextrin: First, add 5.06g of β-cyclodextrin, 5.5g of sodium hydroxide and 32.5mL of distilled water to the flask. After 5 minutes, the β-CD is completely dissolved. Add 6g of chloroacetic acid and heat at 80°C. Under the condition of reaction 3h. After the reaction is over, pour the reaction solution into a 250mL beaker, adjust the pH to 2 with HCl, then add a large amount of acetone as a precipitant to produce white floc, let it stand for 30min, filter it with a cellulose acetate filter, and vacuum at 40°C Dry to constant weight.
[0031] (4) Weigh 5 g of the carboxylated β-cyclodextrin prepared in step (3) and dissolve it in 20 ml of deionized water, add 1.5 g of the aminated polystyrene porous material prepared in step (2), and stir the reaction at room temperature 24h. After the reaction, it was washed three times with deionized water and dried to constant weight.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

no PUM

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Similar technology patents

Cast-in-situ X-shaped concrete pile construction method

InactiveCN101021070ALarge specific surface areaReduce the amount of concreteBulkheads/pilesRebarReinforced concrete
Owner:史本良

Graphene/titanate nanometer composite visible-light activated photocatalyst and preparation method thereof

InactiveCN102847529AGood surface morphologyLarge specific surface areaMetal/metal-oxides/metal-hydroxide catalystsPhotocatalytic degradationCvd graphene
Owner:JIANGSU UNIV

Preparation method of diatomite-based porous ceramic microspheres

InactiveCN102391011ALarge specific surface areaHigh strengthCeramicwareMetallurgyMicrosphere
Owner:SOUTH CHINA UNIV OF TECH

Composite aerogel photocatalyst for recovering titanium dioxide/silicon dioxide

InactiveCN101306359ALarge specific surface areaHigh porosityPhysical/chemical process catalystsWater/sewage treatment by irradiationPore distributionSol-gel
Owner:PLA SECOND ARTILLERY ENGINEERING UNIVERSITY

Metallic catalyst for synthesizing dimethoxym ethane and methyl formate and production method thereof and use

InactiveCN101327444ALarge specific surface areaSmall particlesMolecular sieve catalystsOrganic compound preparationFormate EstersTitanium
Owner:SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI

Classification and recommendation of technical efficacy words

  • Large specific surface area
  • Good adsorption effect
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2023 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap