Composite cellulose nano-fibril hydrogel sphere, and preparation method and application thereof

A technology of composite cellulose and nanofibrils, applied in chemical instruments and methods, water pollutants, alkali metal compounds, etc. Good adsorption of heavy metal ions and organic pollutants, uniform particle size distribution, and low cost

Active Publication Date: 2020-05-08
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, cellulose is the organic green material with the most abundant reserves in nature, but due to its crystallinity and inter-chain association, the structure of cellulose is dense, and its swelling property in water is poor, so it cannot be directly applied to the adsorption of water systems.
Generally, carboxyl groups are introduced by graft modification to improve hydrophilicity. It is common to use modified cellulose and acrylic acid graft copolymerization to prepare hydrogel adsorbents, which are used for the adsorption of heavy metal ions in water systems, and the adsorption effect is better. However, this method is cumbersome and the grafting efficiency is not high.
In addition, the traditional gel adsorbent is an irregular particle, which has a large flow resistance in the water environment, which has a significant adverse effect on the rheology of sewage, which is not conducive to practical application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Mix 1g of polyvinyl alcohol, 0.1g of polymethacrylic acid with a molecular weight of 1,500,000 and 10g of distilled water at 15°C, then stir at 80°C for 2h at a stirring speed of 200r / min, then naturally cool to 15°C and add 80g of a 1% aqueous suspension of cellulose nanofibrils, stirred at 15°C for 5min at a stirring speed of 200r / min, and then added a homogeneous mixture composed of 6g Span 80 and 300g liquid paraffin, and continued Stir at 15℃ for 5min at 200r / min, then add 1g of 1.5% adialdehyde aqueous solution, continue to stir at 15℃ for 0.25h, then control temperature at 45℃, stir for 4h, stir at 200r / min, then filter the reaction solution with a 60-mesh fine sieve, soak the filtered hydrogel ball with 50g ethyl acetate for 5min, filter, then soak the filtered hydrogel ball with 50g ethanol for 5min, then filter, and finally soak with 50g distilled water The obtained hydrogel balls are filtered for 5 minutes, and then filtered to finally obtain a composite cell...

Embodiment 2

[0028] Mix 1g of polyvinyl alcohol, 0.5g of polyacrylic acid with a molecular weight of 1,000,000 and 20g of distilled water at 35°C, then stir at 95°C for 5h at a stirring speed of 300r / min, and then naturally cool to 35°C and add 80g mass Aqueous suspension of cellulose nanofibrils with a fraction of 3%, stir at 35°C for 30min at a stirring speed of 300r / min, and then add a homogeneous mixture composed of 10g Span 60 and 500g liquid paraffin, and continue at 35°C Stir for 10min under the conditions, the stirring speed is 300r / min, then add 10g of glutaraldehyde aqueous solution with a mass fraction of 1.5%, continue to stir at 35℃ for 0.25h, stir at 300r / min, then control the temperature at 45℃ and stir for 4h , The stirring speed is 300r / min, then filter the reaction solution with a 100 mesh fine sieve, soak the filtered hydrogel ball with 50g ethyl acetate for 5min, then filter, then soak the filtered hydrogel ball with 50g ethanol for 5min, then filter Finally, the resulti...

Embodiment 3

[0030] Mix 1g polyvinyl alcohol, 0.3g acrylic acid / methacrylic acid copolymer (molar ratio of acrylic acid and methacrylic acid monomer is 3:1) with a molecular weight of 500,000 at 25℃, and 15g distilled water, and then at 80℃ Stir for 2h at a stirring speed of 150r / min, then naturally cool to 25°C, add 80g of a 3% mass fraction of cellulose nanofibril aqueous suspension, stir at 25°C for 5min at a stirring speed of 150r / min, and then Add a homogeneous mixture composed of 6g Span 80 and 300g liquid paraffin, continue to stir at 25℃ for 5min, stirring speed is 150r / min, then add 3g of glyoxal aqueous solution with mass fraction of 1.5%, continue at 25℃ Stir for 1h under the conditions, the stirring speed is 150r / min, then the temperature is controlled at 45℃, and the stirring speed is 150r / min, then the reaction solution is filtered through a 100-mesh fine sieve, and the resulting hydrogel balls are soaked and filtered with 100g ethyl acetate for 10min , Then filter, and then s...

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Abstract

The invention relates to a composite cellulose nano-fibril hydrogel sphere, and a preparation method and an application thereof, and belongs to the field of cellulose nano-fiber composite materials. The composite cellulose nanofibril hydrogel sphere is prepared from cellulose nanofibril, polyvinyl alcohol, a water-soluble polymer, water and mineral oil. A water-in-oil emulsion is formed through the emulsification effect of a surfactant, a cross-linking agent is adopted to initiate a cross-linking reaction to prepare the hydrogel sphere, the morphology is spherical, the particle size is 0.5-4 mm, and the water content is than 90%. The composite cellulose hydrogel sphere has good heavy metal ion adsorption capacity and organic pollutant adsorption capacity, has little influence on the rheological property of sewage, can be recycled in a filtering mode, does not contain free acid, and does not influence the pH value of the treated sewage. The preparation method of the composite cellulosehydrogel sphere is simple and convenient to operate and causes little pollution to the environment.

Description

Technical field [0001] The invention relates to a cellulose composite material, in particular to a composite cellulose nanofibril hydrogel ball, and a preparation method and application thereof. Background technique [0002] In sewage treatment, organic pollutants and heavy metal ions are the two main pollutants. The current removal methods generally include biodegradation, oxidative degradation, chemical precipitation, ion exchange, membrane separation, solvent extraction, and reverse osmosis. These methods are usually expensive or cause secondary pollution, so explore New materials that can effectively remove organic pollutants and heavy metal ions in sewage with low cost and pollution-free are problems to be solved urgently. In recent years, the use of natural adsorbents for the removal of organic pollutants and heavy metal ions has attracted much attention, such as cellulose, starch and chitosan. These materials have abundant sources, low cost, renewable and degradable mater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/075C08L1/02C08L29/04C08L33/02C08K5/07B01J20/26B01J20/28B01J20/30C02F1/28C02F101/20C02F101/30
CPCC08J3/075B01J20/267B01J20/28047B01J20/28004B01J20/28019C02F1/285C08J2329/04C08J2401/02C08J2433/02C08J2301/02C08J2429/04C08K5/07C02F2101/20C02F2101/30
Inventor 解洪祥程绍玲伊晴成德华邬清魏鹏鹏马庆雪尹茂辉王康琪刘伟
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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