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Method for preparing cellulose acetate butyrate microsphere adsorption material

A technology of cellulose microspheres and acetic acid butyric acid, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve difficult problems, achieve short production process and good thermal stability As well as the effect of acid and alkali resistance and good mechanical properties

Inactive Publication Date: 2014-08-20
中国科技开发院广西分院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is difficult to prepare cellulose microspheres by ionic liquid dissolution method, and some key processes still need to be perfected

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 1.0 g of purified bagasse cellulose, add it to 100 g of ionic liquid, and dissolve it in an oil bath at 50°C. After dissolving, add 1.2 g of butyric anhydride with a pipette, react for 1 hour, and then add 0.5 g of acetic anhydride. g continue to react until the total acylation reaction time is 2h to obtain cellulose acetate butyrate solution. Add 150mL soybean oil and 3mL Span83 into a 500mL three-necked flask, heat it in an oil bath to 60°C, then slowly add the cellulose solution into the three-necked flask under low-speed stirring, and set the stirring speed to 900r / min after the addition is complete. start the timer. After 30 minutes, the heating was stopped and the temperature was slowly lowered to 50°C, and the cellulose acetate butyrate solution was coagulated into balls through reverse suspension and programmed cooling. During the stirring process, slowly add 100 mL of distilled water with a dropper to solidify the cellulose solution droplets to form cell...

Embodiment 2

[0019] Accurately weigh 2g of sawdust cellulose, add it to 200g of ionic liquid, and dissolve it in an oil bath at 60°C. After dissolving, add 3g of butyric anhydride with a pipette, and react for 4 hours, then add 2.4g of acetic anhydride to continue the reaction. Until the total acylation reaction time is 5 hours, a cellulose acetate butyrate solution is obtained. Add 200mL palm oil and 6mL Span65 into a 500mL three-necked flask, heat it in an oil bath to 70°C, then slowly add the cellulose acetate butyrate solution into the three-necked flask under low-speed stirring, and set the stirring speed to 900r / min, start timing. After 15 minutes, the heating was stopped and the temperature was slowly lowered to 40°C, and the cellulose acetate butyrate solution was coagulated into balls through inverse suspension and programmed cooling. During the stirring process, slowly add 500 mL of distilled water with a dropper to solidify the droplets of the cellulose acetate butyrate solutio...

Embodiment 3

[0021] Accurately weigh 2.5g of bamboo cellulose, add it to 200g of ionic liquid, and dissolve it in an oil bath at 80°C. After dissolving, add 3g of butyric anhydride with a pipette and react for 4 hours, then add 2g of acetic anhydride to continue the reaction. Until the total acylation reaction time is 7 hours, a cellulose acetate butyrate solution is obtained. Add 150mL rapeseed oil and 1mL Span20 into a 500mL three-necked flask, heat it in an oil bath to 70°C, then slowly add the cellulose acetate butyrate solution into the three-necked flask under low-speed stirring, and set the stirring speed to 600r / min, start timing. After 40 minutes, the heating was stopped and the temperature was slowly lowered to 40°C, and the cellulose acetate butyrate solution was coagulated into balls through reverse suspension and programmed cooling. During the stirring process, slowly add 500 mL of distilled water with a dropper to solidify the cellulose acetate butyrate solution droplets to ...

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Abstract

The invention relates to a method for preparing a cellulose acetate butyrate microsphere adsorption material by an ionic liquid as a solvent. The method comprises that cellulose is dissolved in an ionic liquid, the cellulose solution reacts respectively with butyric anhydride and acetic anhydride to produce cellulose acetate butyrate products having different substitution degrees, the cellulose acetate butyrate solution is condensed to form liquid drops by reversed phase suspension and programmed cooling, a curing agent is added into the cellulose acetate butyrate liquid drops to cure the liquid drops so that microspheres are formed, and the ionic liquid is removed by distilled water washing so that cellulose acetate butyrate microspheres are obtained. The method has simple processes, realizes recycle of the solvent, utilizes the cellulose raw material having a wide source and a low cost, and realizes high-value utilization of natural plant cellulose. The cellulose acetate butyrate microspheres prepared by the method have acetyl content of 3-20% and butyryl group content of 5-43%, have controllable acyl content and have regular spherical shapes. 95% of the cellulose acetate butyrate microspheres have grain diameters of 50-200 microns. The cellulose acetate butyrate microspheres have good mechanical properties, good thermostability and acid and alkali resistance and are good carriers and adsorption materials.

Description

technical field [0001] The invention relates to a preparation method of a cellulose acetate butyrate microsphere adsorption material, belonging to the field of organic polymer materials. Background technique [0002] Cellulose is the renewable green resource with the largest storage capacity in nature. It mainly comes from the cell wall of plants. It has a wide range of sources and is cheap and easy to get. Cellulose is a polysaccharide compound, which contains a large number of hydroxyl groups in its structure and has strong hydrophilicity. Due to the different positions of hydroxyl groups in cellulose, it has different activities and can absorb heavy metal ions in water. Esterification of cellulose is through the reaction of acid groups with hydroxyl groups on cellulose, which can reduce the number of hydroxyl groups and change the steric hindrance of cellulose, so that cellulose esters with different degrees of substitution have different effects on different substances. ...

Claims

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Application Information

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IPC IPC(8): B01J20/24B01J20/28B01J20/30C08B3/18
CPCY02P20/54
Inventor 林成刚宋洪浪梁涛覃宁波倪海明莫鸿业黄科林蔡广超贾艳桦王则奋柳春蓝丽
Owner 中国科技开发院广西分院
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