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Method for processing cellulose by supercritical carbon dioxide, products and use thereof

A carbon dioxide and cellulose technology, applied in the production of bulk chemicals, etc., can solve the problems of expensive precursor isopropyl titanate, unsuitable ratio and rate control, etc., and achieve simple and easy-to-operate processing methods, uniform and stable properties, The effect of improving the reactivity

Inactive Publication Date: 2009-02-11
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the precursor isopropyl titanate used in this method is relatively expensive, and the ratio and rate of its hydrolysis and condensation reactions with the water adsorbed on the fiber surface are not suitable for control

Method used

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  • Method for processing cellulose by supercritical carbon dioxide, products and use thereof
  • Method for processing cellulose by supercritical carbon dioxide, products and use thereof
  • Method for processing cellulose by supercritical carbon dioxide, products and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] see figure 1 As shown in the schematic diagram of the device structure of the present invention, the device includes a carbon dioxide cylinder 1, valves 2, 3, 4, a stirring device 5, a stainless steel high-pressure reactor 6, a pressure sensor 7, a thermometer 8, a thermocouple 9 and an oil bath 10.

[0054] Preparation of activated fiber material:

[0055] (1) Preprocessing:

[0056] Put 4 grams of cotton linters in the fat extractor, extract with 50 milliliters of acetone for 4 hours, remove waxy and grease components in the cotton linters, then put them into a vacuum oven to dry for later use;

[0057] (2) Activation treatment:

[0058] Add 0.3 gram of cotton linters and 3 milliliters of ethanol into the stainless steel autoclave 6 through extraction and pretreatment, control the temperature of the oil bath in the oil bath tank 10 to be 40 ° C, and feed a small amount of carbon dioxide to exhaust the air in the reaction device , inject carbon dioxide through a hig...

Embodiment 2

[0061] Preparation of activated fiber material:

[0062] Add 1 gram of ash-free filter paper and 10 milliliters of ethanol into the stainless steel high-pressure reaction kettle 6, control the temperature of the oil bath in the oil bath tank 10 to be 50° C., feed a small amount of carbon dioxide to exhaust the air in the reaction device, and inject carbon dioxide through a high-pressure pump , the internal pressure of the control device is 20MPa; close the inlet valve, and place the reactor 6 at a constant temperature in an oil bath for 5 hours. Then remove the oil bath 10, and after the temperature drops to room temperature, the carbon dioxide in the reactor 6 is discharged within 3 minutes. After the pressure is released to normal pressure, the sample is taken out, and after vacuum drying, supercritical carbon dioxide and ethanol are processed. Filter paper activated fiber samples.

Embodiment 3

[0064] Preparation of organic / inorganic composite fiber materials:

[0065] (1) Preprocessing:

[0066] Put 10 grams of cotton in the fat extractor, extract it with 100 milliliters of toluene for 8 hours, remove the impurity components in the cotton, and then put it into a vacuum oven to dry for later use;

[0067] (2) Doping of fiber materials by inorganic sol:

[0068] 3 grams of cotton after the above-mentioned extraction treatment, 10 milliliters of titanium dioxide sol and 3 milliliters of ethanol are added in the stainless steel autoclave 6, and the temperature of the oil bath in the oil bath tank 10 is controlled to be 60° C., and a small amount of carbon dioxide is fed into the reaction device. After the air is exhausted, carbon dioxide is injected through a high-pressure pump, and the internal pressure of the control device is 18MPa; the inlet valve is closed, and the reaction kettle is placed at a constant temperature in an oil bath for 4 hours. Then remove the oil...

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Abstract

The invention relates to a method for utilizing supercritical carbon dioxide to process cellulose; firstly, the cellulose and a cosolvent or an inorganic sol or a former body of the inorganic sol are arranged in a high pressure container; carbon dioxide is pumped by a pumping pressure; the reaction condition is 15 to 200 DEG C; the pressure is 4 to 40MPa; the reaction time is 0.5 to 24 hours; then the activated cellulose is manufactured; the cosolvent relates to carbinol, ethanol, normal butanol, isobutyl alcohol, acetone, tetrahydrofuran, formaldehyde, n-butyl aldehyde and isobutyraldehyde; the cellulose is a natural cellulose and a ramification thereof; the natural cellulose relates to chopped cotton fibers, cotton fabrics, bagasse, straws, paper products, bamboo, flax and wood. The method for utilizing the supercritical carbon dioxide to process the cellulose has the advantages that: the processing method is simply and easily operated; the supercritical carbon dioxide is adopted, thus having no burning, no pollution and no toxic action and being conveniently recycled and being repeatedly used; the content of the mixed inorganic oxide in a compound fiber material is high; the product is easily separated and purified; the characteristic is uniform and stable; the method for utilizing the supercritical carbon dioxide to process the cellulose has broad application prospects in the fields of catalyzing, chemical engineering, packaging, weaving, etc.

Description

technical field [0001] The invention belongs to the field of organic / inorganic composite materials, and in particular relates to a method for treating cellulose with supercritical carbon dioxide and its product and application. Background technique [0002] Cellulose is the most abundant renewable resource on the earth, and the cellulose synthesized by photosynthesis in nature is about 1×10 12 Ton. Cellulose is widely used and has excellent biodegradability, biocompatibility and easy derivatization. In the interior of cellulose, the intramolecular and intermolecular hydrogen bond network formed by a large number of hydroxyl groups endows cellulose with excellent hydrophilic properties, but also makes it insoluble and infusible, which greatly limits the processing and application of cellulose ( Angew. Chem., Int. Ed., 2005, 44, 3358.). For this reason, the research on the regeneration of cellulose and its hybrid modification has been a hot topic of exploration, especially ...

Claims

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Application Information

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IPC IPC(8): C08J3/00C08L1/00C08K3/22C08K3/36
CPCY02P20/54
Inventor 余启斯武培怡徐鹏李磊刘涛赵玲
Owner FUDAN UNIV
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