Method for preparing cellulose sulfate

A technology of cellulose sulfate and sulfuric acid, which is applied in the field of preparation of cellulose sulfate, can solve the problems that it is difficult to simultaneously control the molecular weight of cellulose sulfate and the degree of substitution of sulfate radicals, cellulose hydrolysis, toxicity, etc. Simple, well-sourced effects

Inactive Publication Date: 2011-09-28
HUAQIAO UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On this basis, Yao Shanjing et al. used n-propanol, isopropanol or butanol, improved the process conditions, prepared cellulose sodium sulfate with a degree of substitution of 0.5-1.0, and applied for a patent "a high degree of substitution of cellulose sulfate Sodium Preparation Method" (200810061583.3), in which the reagents n-propanol, isopropanol and butanol still have certain toxicity, and the water generated during the sulfation of cellulose can easily cause cellulose hydrolysis, so it is difficult to simultaneously control the fiber Molecular Weight and Sulfate Substitution Degree of Sulfate Ester

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Embodiment 1: the preparation method of sodium cellulose sulfate

[0014] Measure 500ml of concentrated sulfuric acid (98% concentration by mass) into a beaker, place the beaker in a low-temperature thermostat at -10°C, add 360ml of absolute ethanol, and configure it as a reaction solution. Weigh 50 g of long-staple cotton and 4 g of anhydrous sodium sulfate and add them to the above-mentioned prepared reaction solution, keep the temperature at -4°C, and react for 8 hours. Remove the reaction solution by suction filtration with a sand core funnel, and wash with ethanol until the effluent no longer shows acidity. Dissolve the residue after suction filtration in 1500 mL of water, keep the temperature at 0°C, stir to make it uniform, and add NaOH to adjust the pH to 9. Suction filtration at room temperature, the filtrate is the cellulose sodium sulfate aqueous solution, add 10 times the volume of ethanol to the above glucose sodium sulfate aqueous solution, filter the pre...

Embodiment 2

[0015] Embodiment 2: the preparation method of cellulose potassium sulfate

[0016] Measure 500ml of concentrated sulfuric acid (mass percent concentration: 98%) and pour it into a beaker, place the beaker in a low-temperature thermostat at -5°C, add 360ml of absolute ethanol, and configure it as a reaction solution. Weigh 50 g of short-staple cotton and 8 g of anhydrous sodium sulfate and add them into the above-mentioned prepared reaction solution, keep the temperature at 0° C., and react for 6 hours. Remove the reaction solution by suction filtration with a sand core funnel, and wash with ethanol until the effluent no longer shows acidity. Dissolve the residue after suction filtration in 1500 mL of water, keep the temperature at 0°C, stir to make it uniform, and add KOH to adjust the pH to 9. Suction filtration at room temperature, the filtrate is cellulose potassium sulfate aqueous solution, add 10 times the volume of ethanol to the above cellulose potassium sulfate aqueo...

Embodiment 3

[0017] Embodiment 3: the preparation method of cellulose ammonium sulfate

[0018] Measure 500ml of concentrated sulfuric acid (mass percent concentration: 98%) and pour it into a beaker, place the beaker in a low-temperature thermostat at -5°C, add 360ml of absolute ethanol, and configure it as a reaction solution. Weigh 50 g of short-staple cotton and 16 g of anhydrous sodium sulfate and add them to the above-mentioned prepared reaction liquid, keep the temperature at -4°C, and react for 5 hours. Remove the reaction solution by suction filtration with a sand core funnel, and wash with ethanol until the effluent no longer shows acidity. Dissolve the residue after suction filtration in 1500 mL of water, keep the temperature at 0°C, stir to make it uniform, and add ammonia water to adjust the pH to 9. Suction filtration at room temperature, the filtrate is the cellulose ammonium sulfate aqueous solution, add 10 times the volume of ethanol to the above cellulose ammonium sulfat...

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Abstract

The invention discloses a method for preparing cellulose sulfate. The method comprises the following steps: placing a container in a constant temperature environment at -10 DEG C to 0 DEG C, configuring a mixed reaction solution according to a mole ratio of 1:1 to 1:2.5 of waterless ethanol to sulfuric acid; adding 50g cellulose and 0 to 8g waterless sal glauberi into a 0.5L to 3L mixed reaction solution to react for 1 to 10 hours with a maintaining temperature of -10 DEG C to 0 DEG C, carrying out pumping filtration to the reaction solution and washing with ethanol until the pH value of washing liquid presents neutral; dissolving the filtrated residue in water with maintaining a temperature of 0 DEG C to 5 DEG C, dripping aqueous alkali until pH value is regulated to 7-9; carrying out pumping filtration at normal temperature wherein the filtrate is a cellulose sulfate aqueous solution with different polymerization degree and replacement degree, adding 1 to 50 times volume of ethanol in the aqueous solution for obtaining cellulose sulfate by centrifuging or filtering. The method of the invention employs cellulose for preparing cellulose sulfate, molecular weight and degree of substitution are controllable, The waterless ethanol is taken as a reagent with a better security, A food grade safety reagent is employed in the whole process, and no other harmful waste is generated in the reaction process which is environmental-friendly.

Description

technical field [0001] The invention relates to a preparation method of cellulose derivatives, in particular to a preparation method of cellulose sulfate. Background technique [0002] Cellulose sulfate is an important water-soluble cellulose derivative, which has antibacterial, antiviral and anticoagulant activities, and has attracted extensive attention of researchers. Cellulose sulfate is an anionic polymer, which can be used for the adsorption and flocculation of heavy metals in environmental engineering. At the same time, cellulose sulfate has good water solubility, and its aqueous solution has a relatively large viscosity. Its molecular structure is very similar to that of carrageenan, and it can be used as a viscosifier and thickener instead of carrageenan. Therefore, cellulose sulfate is a new type of cellulose derivative with potential application value. [0003] Due to the complicated preparation process of cellulose sulfate, cellulose sulfate has not yet been pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B5/14
Inventor 陈国姚善泾
Owner HUAQIAO UNIVERSITY
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