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WO2020098390A1 - Procédé de préparation d'un adsorbant de microsphères de cellulose - Google Patents

Procédé de préparation d'un adsorbant de microsphères de cellulose Download PDF

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WO2020098390A1
WO2020098390A1 PCT/CN2019/107742 CN2019107742W WO2020098390A1 WO 2020098390 A1 WO2020098390 A1 WO 2020098390A1 CN 2019107742 W CN2019107742 W CN 2019107742W WO 2020098390 A1 WO2020098390 A1 WO 2020098390A1
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cellulose
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cotton straw
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管敏富
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
    • B01J20/267—Cross-linked polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents

Definitions

  • the invention relates to the field of chemical industry and environmental protection, in particular to a preparation method of cellulose microsphere adsorbent.
  • Cellulose is the oldest and richest natural polymer on the planet, and the most precious natural renewable resource for human beings. Cellulose has the advantages of reproducibility, biodegradability, good biocompatibility and non-toxicity. Modification of cellulose, introduction of some functional groups, preparation of adsorbents with a certain form, can be widely used in wastewater treatment. China's printing and dyeing textile industry discharges a large amount of dye wastewater every year, causing serious pollution to the environment. The composition of dye wastewater is complex, the color is deep, and the amount of discharge is large. It is extremely difficult to treat and recycle. In addition, many production wastewaters contain heavy metal ions. These wastewaters have a great adverse impact on the environment, water resources and human health. The preparation of effective wastewater treatment substances is the focus of research.
  • the purpose of the present invention is to provide a method for preparing cellulose microsphere adsorbent in order to solve the problems mentioned in the background and the deficiencies of the prior art.
  • the invention provides a method for preparing a cellulose microsphere adsorbent, which includes the following steps:
  • Step 1 Wash cotton straw, mechanically crush it after drying, add a mixed solution of xylene and ethanol to the cotton straw powder, put it in a boiling water bath to react, take out and wash, suction filter, add hydrochloric acid solution, 90 °C Water bath treatment for 1.5h, then add deionized water to the water bath for 3h, filter with suction, dry for use;
  • Step 2 Add solution A to the cotton straw powder pretreated in step 1 for reaction, suction filtration, and after drying, add solution B to the obtained powder for reaction. After the reaction, wash with distilled water until neutral and dry. Get cotton straw cellulose;
  • Step 3 Configure the cotton straw cellulose prepared in Step 2 as an aqueous solution for use;
  • Step 4 Add castor oil and Tween 80 to the flask, turn on the stirring device and heating device, stir for 20min, then add cotton straw cellulose aqueous solution, continue the reaction for 30min, add epichlorohydrin to react for 9h;
  • Step 5 The reaction system was allowed to stand overnight, the surface oil phase was removed, the cellulose microspheres were washed with ethyl acetate and ethanol respectively, and the cellulose microsphere adsorbent was obtained after drying.
  • the volume ratio of xylene and ethanol in the mixed solution in step one is 3: 2.
  • the solution A in the second step is formed by mixing hydrogen peroxide and sodium hydroxide in deionized water.
  • the solution B is formed by mixing trichloroacetic acid and nitric acid dissolved deionized water.
  • the concentration of the cotton straw aqueous solution in step 3 is 8-16 wt%.
  • the rotation speed of the stirring device in step 4 is 540-660 rad / min, and the reaction temperature is 50-80 ° C.
  • the present invention controls the mass fraction of cellulose, and the cellulose molecules can be well dispersed in the solution to perform a sufficient cross-linking reaction, and the prepared cellulose microspheres have a moderate particle size and a large adsorption capacity.
  • the stirring speed of the controlled reaction is 540-660 rad / min, and the reaction temperature is 50-80 ° C, which can make the cross-linking reaction between epichlorohydrin and cellulose molecules sufficient, and the formed microspheres have a Large total surface area, good adsorption performance.
  • Step 1 Rinse the cotton straw with distilled water, dry and mechanically pulverize it to 50 mesh, add a mixed liquid of xylene and ethanol to the cotton straw powder, the material-liquid ratio is 1:10 (g / mL), where The volume ratio of xylene and ethanol is 3: 2, placed in a boiling water bath to react for 6h, taken out and washed with ethanol 3 times, filtered with suction, added 0.1mol / L hydrochloric acid solution, the material-liquid ratio is 1:12 (g / mL) At 90 °C water bath for 1.5h, then add deionized water, the material-liquid ratio is 1:20 (g / mL), 85 °C, 200r / min water bath reaction for 3h, suction filtration, dried at 60 °C for use;
  • Step 2 Add solution A to the cotton straw powder pretreated in step 1, the material-liquid ratio is 1:20 (g / mL), solution A is 0.6mL hydrogen peroxide and 3g sodium hydroxide dissolved in 100mL It is made up by mixing in ionic water, reacting at 90 °C for 4h, filtering with suction, drying at 60 °C, adding solution B to the obtained powder, the material-liquid ratio is 1:25 (g / mL), solution B is 0.8g trichloro Acetic acid and 6mL nitric acid are dissolved in 100mL deionized water and mixed, treated at 60 °C for 3h, washed with distilled water until neutral, and dried at 60 °C to obtain cotton straw cellulose;
  • Step 3 Configure the cotton straw cellulose prepared in Step 2 as a 16wt% aqueous solution for use;
  • Step 4 Add 60mL castor oil and 0.25g Tween 80 to the flask, adjust the rotation speed to 540rad / min, increase the temperature to 80 ° C, stir for 20min, then add 10mL of cotton straw cellulose aqueous solution, continue the reaction for 30min, add 1.45mL ring Oxychloropropane, reaction 9h;
  • Step 5 Allow the reaction system to stand overnight, remove the surface oil phase, wash the cellulose microspheres with ethyl acetate solution 3 times, then with ethanol solution 6 times, and dry in an oven at 80 °C to obtain cellulose Microsphere adsorbent.
  • Step 1 Rinse the cotton straw with distilled water, dry and mechanically pulverize it to 50 mesh, add a mixed liquid of xylene and ethanol to the cotton straw powder, the material-liquid ratio is 1:10 (g / mL), where The volume ratio of xylene and ethanol is 3: 2, placed in a boiling water bath to react for 6h, taken out and washed with ethanol 3 times, filtered with suction, added 0.1mol / L hydrochloric acid solution, the material-liquid ratio is 1:12 (g / mL) At 90 °C water bath for 1.5h, then add deionized water, the material-liquid ratio is 1:20 (g / mL), 85 °C, 200r / min water bath reaction for 3h, suction filtration, dried at 60 °C for use;
  • Step two Add solution A to the cotton straw powder pretreated in step one, the material-liquid ratio is 1:20 (g / mL), solution A is 0.2mL hydrogen peroxide and 8g sodium hydroxide dissolved in 100mL It is made up by mixing in ionic water, reacting at 60 °C for 4h, filtering with suction, drying at 60 °C, adding solution B to the powder obtained, the material-liquid ratio is 1:25 (g / mL), solution B is 1.2g trichloro Acetic acid and 2mL nitric acid are dissolved in 100mL deionized water and mixed, treated at 80 °C for 1h, washed with distilled water until neutral, and dried at 60 °C to obtain cotton straw cellulose;
  • Step 3 Configure the cotton straw cellulose prepared in Step 2 as an 8wt% aqueous solution for use;
  • Step 4 Add 80 mL of castor oil and 0.05 g of Tween 80 to the flask, adjust the rotation speed to 660 rad / min, increase the temperature to 50 ° C, stir for 20 min, then add 10 mL of cotton straw cellulose aqueous solution, continue the reaction for 30 min, add 2.25 mL of ring Oxychloropropane, reaction 9h;
  • Step 5 Allow the reaction system to stand overnight, remove the surface oil phase, wash the cellulose microspheres with ethyl acetate solution 3 times, then with ethanol solution 6 times, and dry in an oven at 80 °C to obtain cellulose Microsphere adsorbent.
  • Step 1 Rinse the cotton straw with distilled water, dry and mechanically pulverize it to 50 mesh, add a mixed liquid of xylene and ethanol to the cotton straw powder, the material-liquid ratio is 1:10 (g / mL), where The volume ratio of xylene and ethanol is 3: 2, placed in a boiling water bath to react for 6h, taken out and washed with ethanol 3 times, filtered with suction, added 0.1mol / L hydrochloric acid solution, the material-liquid ratio is 1:12 (g / mL) At 90 °C water bath for 1.5h, then add deionized water, the material-liquid ratio is 1:20 (g / mL), 85 °C, 200r / min water bath reaction for 3h, suction filtration, dried at 60 °C for use;
  • Step two Add solution A to the cotton straw powder pretreated in step one, the material-liquid ratio is 1:20 (g / mL), solution A is 0.5mL hydrogen peroxide and 4g sodium hydroxide dissolved in 100mL It is made up by mixing in ionic water, reacting at 80 °C for 4h, filtering with suction, drying at 60 °C, adding solution B to the powder obtained, the material-liquid ratio is 1:25 (g / mL), solution B is 0.9g trichloromethane Acetic acid and 5mL nitric acid are dissolved in 100mL deionized water and mixed, treated at 65 °C for 2.5h, washed with distilled water to neutral, and dried at 60 °C to obtain cotton straw cellulose;
  • Step 3 Configure the cotton straw cellulose prepared in Step 2 as a 14wt% aqueous solution for use;
  • Step 4 Add 65mL castor oil and 0.2g Tween 80 to the flask, adjust the rotation speed to 570rad / min, increase the temperature to 70 ° C, stir for 20min, then add 10mL cotton straw aqueous cellulose solution, continue the reaction for 30min, add 1.65mL ring Oxychloropropane, reaction 9h;
  • Step 5 Allow the reaction system to stand overnight, remove the surface oil phase, wash the cellulose microspheres with ethyl acetate solution 3 times, then with ethanol solution 6 times, and dry in an oven at 80 °C to obtain cellulose Microsphere adsorbent.
  • Step 1 Rinse the cotton straw with distilled water, dry and mechanically pulverize it to 50 mesh, add a mixed liquid of xylene and ethanol to the cotton straw powder, the material-liquid ratio is 1:10 (g / mL), where The volume ratio of xylene and ethanol is 3: 2, placed in a boiling water bath to react for 6h, taken out and washed with ethanol 3 times, filtered with suction, added 0.1mol / L hydrochloric acid solution, the material-liquid ratio is 1:12 (g / mL) At 90 °C water bath for 1.5h, then add deionized water, the material-liquid ratio is 1:20 (g / mL), 85 °C, 200r / min water bath reaction for 3h, suction filtration, dried at 60 °C for use;
  • Step two Add solution A to the cotton straw powder pretreated in step one, the material-liquid ratio is 1:20 (g / mL), solution A is 0.3mL hydrogen peroxide and 7g sodium hydroxide dissolved in 100mL It is made up by mixing in ionic water, reacting at 70 °C for 4h, filtering with suction, and drying at 60 °C, adding solution B to the obtained powder, the material-liquid ratio is 1:25 (g / mL), solution B is 1.1g trichloro Acetic acid and 3mL nitric acid are dissolved in 100mL deionized water and mixed, treated at 75 °C for 1.5h, washed with distilled water until neutral, and dried at 60 °C to obtain cotton straw cellulose;
  • Step 3 Configure the cotton straw cellulose prepared in Step 2 as a 10wt% aqueous solution for use;
  • Step 4 Add 75mL castor oil and 0.1g Tween 80 to the flask, adjust the rotation speed to 630rad / min, increase the temperature to 60 °C, stir for 20min, then add 10mL of cotton straw cellulose aqueous solution, and continue the reaction for 30min, add 2.05mL ring Oxychloropropane, reaction 9h;
  • Step 5 Allow the reaction system to stand overnight, remove the surface oil phase, wash the cellulose microspheres with ethyl acetate solution 3 times, then with ethanol solution 6 times, and dry in an oven at 80 °C to obtain cellulose Microsphere adsorbent.
  • Step 1 Rinse the cotton straw with distilled water, dry and mechanically pulverize it to 50 mesh, add a mixed liquid of xylene and ethanol to the cotton straw powder, the material-liquid ratio is 1:10 (g / mL), where The volume ratio of xylene and ethanol is 3: 2, placed in a boiling water bath to react for 6h, taken out and washed with ethanol 3 times, filtered with suction, added 0.1mol / L hydrochloric acid solution, the material-liquid ratio is 1:12 (g / mL) At 90 °C water bath for 1.5h, then add deionized water, the material-liquid ratio is 1:20 (g / mL), 85 °C, 200r / min water bath reaction for 3h, suction filtration, dried at 60 °C for use;
  • Step two Add solution A to the cotton straw powder pretreated in step one, the material-liquid ratio is 1:20 (g / mL), solution A is 0.4mL hydrogen peroxide and 5.5g sodium hydroxide dissolved in 100mL It is mixed with deionized water, reacted at 75 °C for 4h, filtered with suction, and dried at 60 °C. Solution B is added to the obtained powder.
  • the material-liquid ratio is 1:25 (g / mL).
  • Solution B is 1g of trichloromethane Acetic acid and 4mL nitric acid are dissolved in 100mL deionized water and mixed, treated at 70 °C for 2h, washed with distilled water until neutral, and dried at 60 °C to obtain cotton straw cellulose;
  • Step 3 Configure the cotton straw cellulose prepared in Step 2 as a 12wt% aqueous solution for use;
  • Step 4 Add 70mL castor oil and 0.15g Tween 80 to the flask, adjust the rotation speed to 600rad / min, increase the temperature to 65 °C, stir for 20min, then add 10mL of cotton straw cellulose aqueous solution, continue the reaction for 30min, add 1.85mL ring Oxychloropropane, reaction 9h;
  • Step 5 Allow the reaction system to stand overnight, remove the surface oil phase, wash the cellulose microspheres with ethyl acetate solution 3 times, then with ethanol solution 6 times, and dry in an oven at 80 °C to obtain cellulose Microsphere adsorbent.
  • Example 1 The difference between this comparative example and Example 1 is that the concentration of the cotton straw aqueous solution in step 3 is 5 wt%.
  • Step 1 Rinse the cotton straw with distilled water, dry and mechanically pulverize it to 50 mesh, add a mixed liquid of xylene and ethanol to the cotton straw powder, the material-liquid ratio is 1:10 (g / mL), where The volume ratio of xylene and ethanol is 3: 2, placed in a boiling water bath to react for 6h, taken out and washed with ethanol 3 times, filtered with suction, added 0.1mol / L hydrochloric acid solution, the material-liquid ratio is 1:12 (g / mL) At 90 °C water bath for 1.5h, then add deionized water, the material-liquid ratio is 1:20 (g / mL), 85 °C, 200r / min water bath reaction for 3h, suction filtration, dried at 60 °C for use;
  • Step 2 Add solution A to the cotton straw powder pretreated in step 1, the material-liquid ratio is 1:20 (g / mL), solution A is 0.6mL hydrogen peroxide and 3g sodium hydroxide dissolved in 100mL It is made up by mixing in ionic water, reacting at 90 °C for 4h, filtering with suction, drying at 60 °C, adding solution B to the obtained powder, the material-liquid ratio is 1:25 (g / mL), solution B is 0.8g trichloro Acetic acid and 6mL nitric acid are dissolved in 100mL deionized water and mixed, treated at 60 °C for 3h, washed with distilled water until neutral, and dried at 60 °C to obtain cotton straw cellulose;
  • Step 3 Configure the cotton straw cellulose prepared in Step 2 as a 5wt% aqueous solution for use;
  • Step 4 Add 60mL castor oil and 0.25g Tween 80 to the flask, adjust the rotation speed to 540rad / min, increase the temperature to 80 ° C, stir for 20min, then add 10mL of cotton straw cellulose aqueous solution, continue the reaction for 30min, add 1.45mL ring Oxychloropropane, reaction 9h;
  • Step 5 Allow the reaction system to stand overnight, remove the surface oil phase, wash the cellulose microspheres with ethyl acetate solution 3 times, then with ethanol solution 6 times, and dry in an oven at 80 °C to obtain cellulose Microsphere adsorbent.
  • Step 1 Rinse the cotton straw with distilled water, dry and mechanically pulverize it to 50 mesh, add a mixed liquid of xylene and ethanol to the cotton straw powder, the material-liquid ratio is 1:10 (g / mL), where The volume ratio of xylene and ethanol is 3: 2, placed in a boiling water bath to react for 6h, taken out and washed with ethanol 3 times, filtered with suction, added 0.1mol / L hydrochloric acid solution, the material-liquid ratio is 1:12 (g / mL) At 90 °C water bath for 1.5h, then add deionized water, the material-liquid ratio is 1:20 (g / mL), 85 °C, 200r / min water bath reaction for 3h, suction filtration, dried at 60 °C for use;
  • Step 2 Add solution A to the cotton straw powder pretreated in step 1, the material-liquid ratio is 1:20 (g / mL), solution A is 0.6mL hydrogen peroxide and 3g sodium hydroxide dissolved in 100mL It is made up by mixing in ionic water, reacting at 90 °C for 4h, filtering with suction, drying at 60 °C, adding solution B to the obtained powder, the material-liquid ratio is 1:25 (g / mL), solution B is 0.8g trichloro Acetic acid and 6mL nitric acid are dissolved in 100mL deionized water and mixed, treated at 60 °C for 3h, washed with distilled water until neutral, and dried at 60 °C to obtain cotton straw cellulose;
  • Step 3 Configure the cotton straw cellulose prepared in Step 2 as a 16wt% aqueous solution for use;
  • Step 4 Add 60mL of castor oil and 0.25g of Tween 80 to the flask, adjust the speed to 400rad / min, heat to 80 ° C, stir for 20min, then add 10mL of cotton straw cellulose aqueous solution, continue the reaction for 30min, add 1.45mL Oxychloropropane, reaction 9h;
  • Step 5 Allow the reaction system to stand overnight, remove the surface oil phase, wash the cellulose microspheres with ethyl acetate solution 3 times, then with ethanol solution 6 times, and dry in an oven at 80 °C to obtain cellulose Microsphere adsorbent.
  • cellulose microsphere adsorbent was added to 100mL of 5 ⁇ g / mL active blue M solution, 100mL0.08g / mL Cr 6+ solution and 100mL 0.08g / mL Cu 2+ solution for adsorption, measured by spectrophotometry The absorption value of the filtrate after adsorption, the adsorption rate is calculated, the test results are shown in the table below:
  • the cellulose microsphere adsorbent prepared by the present invention has a very good adsorption effect on dye wastewater, the adsorption rate of reactive blue M reaches 92.66-98.74%, and the metal ions Cr 6+ and Cu 2 in wastewater + Also has a good adsorption effect, the adsorption rate of Cr 6+ reaches 82.55-88.37%, and the adsorption rate of Cu 2+ reaches 88.76-93.46%.
  • the cellulose microsphere adsorbent prepared in Example 5 achieves the best treatment effect, so Example 5 is the optimal solution of the present invention.
  • Comparative Example 1 the concentration of the cotton straw aqueous cellulose solution is 5 wt%, the mass fraction is too low, and the cross-linking reaction between the cellulose molecules cannot be performed well, resulting in the formation of microspheres with a too small particle size and poor adsorption performance.
  • the stirring speed in Comparative Example 2 is 400 rad / min. The stirring speed is too low, which is not conducive to the dispersion of the aqueous phase in the reaction system, the droplets cannot be well dispersed, the total surface area of the formed microspheres is small, and the adsorption performance is poor.

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Abstract

L'invention concerne un procédé de préparation d'un adsorbant de microsphères de cellulose, comprenant les étapes suivantes : le nettoyage, le séchage et le broyage de paille de coton, l'ajout d'un mélange de xylène et d'éthanol, la réalisation d'une réaction dans un bain d'eau bouillante, la réalisation d'une filtration de lavage et d'aspiration, l'ajout d'une solution d'acide chlorhydrique pour le traitement, l'ajout d'eau désionisée pour une réaction dans un bain d'eau, la réalisation d'une filtration par aspiration, et le séchage du produit à utiliser ; l'ajout d'une solution A à la poudre de paille de coton prétraitée pour une réaction, la réalisation d'une filtration par aspiration et d'un séchage, puis l'ajout d'une solution B pour une réaction, le lavage et le séchage de la résultante afin d'obtenir de la cellulose de paille de coton, et la formulation de la cellulose de paille de coton dans une solution aqueuse à utiliser ; l'ajout d'huile de ricin et de Tween 80 dans un flacon, l'agitation pendant 20 min, l'ajout de la solution aqueuse de la cellulose de paille de coton afin de continuer la réaction, puis l'ajout de l'épichlorhydrine pour une réaction ; et l'élimination de la phase huileuse dans le système de réaction, et le nettoyage et le séchage du produit afin d'obtenir un adsorbant de microsphères de cellulose. L'adsorbant de microsphères de cellulose obtenu présente un bon effet d'adsorption sur le bleu actif M et les ions métalliques Cr6+ et Cu2+ dans les eaux usées, et présente de vastes perspectives d'application.
PCT/CN2019/107742 2018-11-17 2019-09-25 Procédé de préparation d'un adsorbant de microsphères de cellulose Ceased WO2020098390A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112023897A (zh) * 2020-09-01 2020-12-04 齐鲁工业大学 一种具有选择吸附性的纳米纤维素微球的制备方法及对染料废水的吸附应用
CN116143227A (zh) * 2023-04-19 2023-05-23 新乡学院 一种吸附-超滤联用处理低浓度重金属污染废水的方法

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109201020A (zh) * 2018-11-17 2019-01-15 管敏富 一种纤维素微球吸附剂的制备方法
CN112169774A (zh) * 2020-10-29 2021-01-05 青岛理工大学 一种秸秆基染料吸附剂及其制备方法和应用
CN114775110A (zh) * 2022-05-09 2022-07-22 江苏师范大学 一种防掉粉杂化碳气凝胶纤维的制备方法
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101342485A (zh) * 2008-07-03 2009-01-14 山东大学 利用高纤维素含量植物制备季胺盐阳离子型吸附剂的方法
CN101733074A (zh) * 2008-11-26 2010-06-16 北京化工大学 膜式生物吸附介质的制备方法
CN101862642A (zh) * 2010-06-24 2010-10-20 山东大学 农业秸秆两性螯合吸附剂的制备方法及应用
CN102553545A (zh) * 2012-03-16 2012-07-11 川渝中烟工业有限责任公司 一种纤维素复合微球及其制备方法
EP3266748A1 (fr) * 2016-07-06 2018-01-10 Clariant International Ltd Matériaux d'adsorption à base de lignine à faible coût pour le traitement de l'eau
CN109201020A (zh) * 2018-11-17 2019-01-15 管敏富 一种纤维素微球吸附剂的制备方法

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4212199B2 (ja) * 1999-09-28 2009-01-21 レンゴー株式会社 ゼオライト複合セルロース球状微粒子、その製造方法およびこれを用いた水処理剤
CN1233716C (zh) * 2003-04-14 2005-12-28 福州大学 交联球形再生纤维素珠体及程序降温反相悬浮技术的清洁化制备方法
CN1233715C (zh) * 2003-04-14 2005-12-28 福州大学 大孔交联球形纤维素珠体及其清洁化喷射法制备工艺
CN100542668C (zh) * 2006-03-29 2009-09-23 华东理工大学 一种超大孔耐中压球形纤维素颗粒和吸附剂的制备方法
CN101036876B (zh) * 2007-01-25 2010-09-01 天津大学 超大孔纤维素微球蛋白质吸附介质的制备方法
CN101250267B (zh) * 2008-04-14 2011-09-14 武汉大学 一种纤维素微球的制备方法
CN102671646B (zh) * 2012-05-11 2014-03-26 北京科技大学 一种制备处理含油污水的吸附材料的方法
CN105396561A (zh) * 2015-12-12 2016-03-16 常州大学 一种综纤维素/壳聚糖微球吸附剂的制备方法
CN106749688A (zh) * 2016-12-28 2017-05-31 广州市楹晟生物科技有限公司 一种微晶纤维素的生产方法
CN106832357A (zh) * 2017-02-20 2017-06-13 商洛学院 一种纤维素微球改性的制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101342485A (zh) * 2008-07-03 2009-01-14 山东大学 利用高纤维素含量植物制备季胺盐阳离子型吸附剂的方法
CN101733074A (zh) * 2008-11-26 2010-06-16 北京化工大学 膜式生物吸附介质的制备方法
CN101862642A (zh) * 2010-06-24 2010-10-20 山东大学 农业秸秆两性螯合吸附剂的制备方法及应用
CN102553545A (zh) * 2012-03-16 2012-07-11 川渝中烟工业有限责任公司 一种纤维素复合微球及其制备方法
EP3266748A1 (fr) * 2016-07-06 2018-01-10 Clariant International Ltd Matériaux d'adsorption à base de lignine à faible coût pour le traitement de l'eau
CN109201020A (zh) * 2018-11-17 2019-01-15 管敏富 一种纤维素微球吸附剂的制备方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LI, CHUNGUANG . ET AL.: "Study on Extraction of Cellulose and Removal of Hemicelluloses and Lignin from Bagasse", CHINESE AGRICULTURAL SCIENCE BULLETIN, vol. 27, no. 4, 20 February 2011 (2011-02-20), pages 317, ISSN: 1000-6850 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112023897A (zh) * 2020-09-01 2020-12-04 齐鲁工业大学 一种具有选择吸附性的纳米纤维素微球的制备方法及对染料废水的吸附应用
CN112023897B (zh) * 2020-09-01 2022-06-21 齐鲁工业大学 一种具有选择吸附性的纳米纤维素微球的制备方法及对染料废水的吸附应用
CN116143227A (zh) * 2023-04-19 2023-05-23 新乡学院 一种吸附-超滤联用处理低浓度重金属污染废水的方法

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