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Method for preparing organic or inorganic composite fiber material with supercritical carbonic anhydride

A carbon dioxide and inorganic composite technology, which is applied in the production of bulk chemicals, etc., can solve the problems of the expensive precursor isopropyl titanate, unsuitable control of the ratio and rate, and achieve simple and easy-to-operate preparation methods, improved reactivity, The effect of high doping content

Inactive Publication Date: 2008-09-24
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 preparing organic or inorganic composite fiber material with supercritical carbonic anhydride
  • Method for preparing organic or inorganic composite fiber material with supercritical carbonic anhydride
  • Method for preparing organic or inorganic composite fiber material with supercritical carbonic anhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Put 4 grams of cotton linters in a fat extractor, extract with 50 milliliters of acetone for 4 hours to remove wax and grease components in the linters, and then put them into a vacuum oven to dry for later use.

[0039] Use the device shown in Figure 1. 0.3 grams of cotton linters and 3 milliliters of ethanol after the above-mentioned extraction treatment were added in a stainless steel autoclave, and the temperature of the oil bath in the thermostatic tank was controlled to be 40 ° C, and a small amount of carbon dioxide was introduced to exhaust the air in the reaction device. Carbon dioxide is injected through a high-pressure pump, and the pressure inside the control device is 15 MPa. Close the inlet valve, and place the reactor at a constant temperature in an oil bath for 2 hours. Then remove the constant temperature tank, and discharge the carbon dioxide in the reaction kettle within 5 minutes after the temperature drops to room temperature. After the pressure is...

Embodiment 2

[0041] Use the device shown in Figure 1. Add 1 gram of ash-free filter paper and 10 milliliters of ethanol into a stainless steel high-pressure reaction kettle, control the temperature of the oil bath in the constant temperature tank to 50°C, and feed a small amount of carbon dioxide to exhaust the air in the reaction device, then inject carbon dioxide through a high-pressure pump to control The pressure inside the device was 20 MPa. Close the inlet valve, and place the reactor at a constant temperature in an oil bath for 5 hours. Then remove the constant temperature tank, discharge the carbon dioxide in the reaction kettle within 3 minutes after the temperature drops to room temperature, take out the sample after the pressure is released to normal pressure, and obtain supercritical carbon dioxide and ethanol-treated ash-free filter paper for activation after vacuum drying Fiber samples.

Embodiment 3

[0043] Put 10 grams of cotton in a fat extractor, extract with 100 milliliters of toluene for 8 hours, remove the impurity components in the cotton, and then put it in a vacuum oven to dry for use.

[0044] Use the device shown in Figure 1. Add 3 grams of cotton after the above-mentioned extraction treatment, 10 milliliters of titanium dioxide sol and 3 milliliters of ethanol into a stainless steel autoclave, control the temperature of the oil bath in the constant temperature tank to be 60 ° C, and feed a small amount of carbon dioxide to exhaust the air in the reaction device. After cleaning, carbon dioxide is injected through a high-pressure pump, and the pressure in the control device is 18 MPa. Close the inlet valve, and place the reactor at a constant temperature in an oil bath for 4 hours. Then remove the constant temperature tank, and discharge the carbon dioxide in the reaction kettle within 5 minutes after the temperature drops to room temperature. After the pressure...

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Abstract

The invention belongs to the technical field of organic and inorganic composite materials, in particular to a preparation method of organic and inorganic composite fibrous materials with supercritical carbon dioxide. The method includes pre-treatment and activation treatment of cellulose, doping of inorganic sol to the cellulose, etc. The invention makes use of the strong permeability of the carbon dioxide under supercritical conditions, can activate the cellulose with cosolvent, or lead nano particles in the inorganic sol to be absorbed and settled on the surface of the cellulose to form an even, continuous and stable coating layer; meanwhile, some sol particles penetrate into the fiber, so as to dope plenty of cellulose. The supercritical carbon dioxide adopted by the invention is safe, reliable, non-toxic, no pollutant and recyclable, and is environment friendly green solvent. The method of the invention is simple and easy to be operated, and the hybrid material has broad application prospect.

Description

technical field [0001] The invention belongs to the technical field of organic-inorganic composite materials, and in particular relates to a method for preparing composite materials based on cellulose and inorganic oxides in a supercritical carbon dioxide environment. 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. Inside 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 o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L1/00C08K3/22C08K3/36C08J3/20
CPCY02P20/54
Inventor 余启斯武培怡
Owner FUDAN UNIV
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