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Method for rapidly preparing cellulose DMAc (Dimethylacetylamide) /LiCl solution

A cellulose solution and cellulose technology, applied in the field of preparing cellulose homogeneous solution, can solve the problems of long preparation process, slow dissolution, reduced process cost and the like

Inactive Publication Date: 2011-05-18
EASTERN LIAONING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical scheme of the rapid preparation method of cellulose DMAc / LiCl solution provided by the patent application of the present invention is mainly aimed at the technical problems of slow dissolution of cellulose and LiCl in the existing cellulose DMAc / LiCl solution preparation process, and the preparation process takes too long Proposed, this method realizes synchronous removal of the moisture that may be carried in cellulose, lithium chloride and dimethylacetamide DMAc during the activation and dissolution process implemented by low-pressure distillation, and accelerates the mutual penetration of cellulose in the solvent, Dissolving speed, to achieve the technical purpose of fast and efficient preparation of cellulose DMAc / LiCl solution, and the process is simplified, the whole process can be completed in only one preparation equipment, and the process cost is significantly reduced

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] The degree of polymerization of cellulose is 235, the dosage is 2 grams, 140 ml of dimethylacetamide DMAc, 9 grams of lithium chloride, and the total preparation takes 3.5 hours;

[0011] In the first step, cellulose and dimethylacetamide DMAc are added to a vacuum kettle equipped with a stirring device, the vacuum kettle is connected to a vacuum distillation device, the relative vacuum degree reaches -0.09MPa, and the oil bath temperature is 145°C. Stirring speed is 100rpm-200rpm, vacuum distillation for 30 minutes, collect fraction 40-50ml; in this step, if the distillation temperature is lower, the distillation decompression time needs to be lengthened, which can be completed within 30-60 minutes, for the following The same goes for the examples;

[0012] In the second step, suspend the vacuum distillation, keep the oil bath temperature, add lithium chloride, add dimethylacetamide DMAc equal to the distillation fraction, and make the relative vacuum to -0.07MPa. Afte...

Embodiment 2

[0015] The degree of polymerization of cellulose is 235, the dosage is 2.5 grams, 100 ml of dimethylacetamide DMAc, 4 grams of lithium chloride, and the total preparation time is about 2.5 hours;

[0016]In the first step, cellulose and dimethylacetamide DMAc are added to a vacuum kettle equipped with a stirring device, the vacuum kettle is connected to a vacuum distillation device, and the relative vacuum degree reaches -0.09~0.07MPa, and the oil bath temperature is 135°C, stirring speed 100rpm-200rpm, vacuum distillation for 30 minutes, collect 40-50ml fraction;

[0017] The second step is to suspend the vacuum distillation, maintain the temperature of the oil bath, add lithium chloride, and add dimethylacetamide DMAc equal to the distillation fraction. After 30 minutes, collect 30 ml of the extracted fraction, then stop heating, start vigorous stirring at a speed of 800-1000 rpm, and forcefully cool to room temperature within 60 minutes. At this time, a viscous opaque cellu...

Embodiment 3

[0020] The degree of polymerization of cellulose is 235, the dosage is 4 grams, 100 ml of dimethylacetamide DMAc, 8 grams of lithium chloride, and the total preparation time is 3 hours;

[0021] In the first step, cellulose and dimethylacetamide DMAc are added to a vacuum kettle equipped with a stirring device, the vacuum kettle is connected to a vacuum distillation device, and the relative vacuum degree reaches -0.09~-0.07MPa, and the oil bath is Temperature is 135°C, stirring speed is 100rpm-200rpm, vacuum distillation is 30 minutes, and 40-50ml of extracted fraction is collected;

[0022] In the second step, suspend vacuum distillation, maintain the temperature of the oil bath, add lithium chloride, add dimethylacetamide DMAc equal to the distilled fraction, under the condition of relative vacuum to -0.09~-0.07MPa Distill for 1 hour, extract 30 ml of fractions, then stop heating, start vigorous stirring at a speed of 800-1000 rpm, and forcefully cool to room temperature wit...

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Abstract

The invention provides a method for rapidly preparing a cellulose DMAc (Dimethylacetylamide) / LiCl solution, which comprises the following steps of: performing decompressing evaporation for mixed cellulose and dimethylacetylamide DMAc during stirring under the conditions of vacuumizing at a temperature of not lower than 100 DEG C and extracting the distillate, then adding LiCl and introducing dimethylacetylamide of equal quantity with the distillate, continuously vacuumizing and stirring at a temperature of 100-155 DEG C till LiCl is completely dissolved, and extracting the distillate, stirring strongly and then deforming to prepare the transparent cellulose solution. The mass fraction of cellulose is 0.8-15% and the mass fraction of the LiCl is 1-12%. The preparation method of the technical scheme can be used for preparing the cellulose solution rapidly and effectively; and the prepared cellulose solution with homogeneous phase has smaller degree of degradation and is more suitable for industrial production.

Description

technical field [0001] The patent application of the present invention relates to a process for preparing a homogeneous cellulose solution, in particular to a method for preparing a cellulose solution with a cellulose polymerization degree not higher than 900. Background technique [0002] With the depletion of petroleum resources, people are trying to find new energy materials that can replace petroleum. Cellulose is the most abundant renewable natural polymer in nature. It is a polysaccharide, and each anhydroglucose unit has three reactive hydroxyl groups, which provides the possibility for chemical modification of cellulose. Its preparation As a cellulose solution, it builds a bridge for the full and extensive use of cellulose and alleviates human dependence on petroleum resources. However, the molecular structure of cellulose also determines its insolubility, which has become a key technical problem in the preparation of cellulose solution. [0003] The current prepara...

Claims

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Application Information

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IPC IPC(8): C08J3/09C08L1/02
Inventor 黄凤远吴哓杰于艳
Owner EASTERN LIAONING UNIV
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