Synthetic method for methyl cellulose sample
A technology of methyl cellulose and synthesis method, which is applied in the field of chemical synthesis, can solve problems such as difficult control of substitution effect, unfavorable laboratory preparation, and unsatisfactory homogeneity, and achieve low equipment requirements, small preparation amount, methylation The effect of high degree of substitution
Inactive Publication Date: 2015-11-04
昆山京昆油田化学科技有限公司
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Problems solved by technology
[0003] The traditional industrial methyl cellulose synthesis method is to use monochloromethane to react and synthesize in an alkaline, 60-70°C high-pressure environment. This preparation method is generally not conducive to laboratory preparation.
The traditional laboratory preparation method is to use dry DMSO as a solvent, cellulose is dispersed in the solvent, and alkali is added to react with methyl iodide to synthesize it. Because the cellulose prepared by this synthesis method is in a heterogeneous state in DMSO, the substitution effect Difficult to control, low degree of substitution, unsatisfactory uniformity
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[0019] Such as figure 1 The synthetic method of a kind of methyl cellulose sample shown:
[0020] 1. Add 0.81g of microcrystalline cellulose and 16.2g of N,N-dimethylacetamide into a 50ml three-necked flask, and use a motor to stir at a medium speed at 120°C for 2 hours in a closed environment.
[0021] 2. After stirring the mixture of cellulose and N,N-dimethylacetamide for 2 hours, lower the temperature to 100°C, add crushed and dried lithium chloride powder, and stir for 2 hours.
[0022] 3. After the mixture of cellulose, N,N-dimethylacetamide and lithium chloride was stirred at 100°C for 2 hours, the temperature was lowered to room temperature, and stirred at medium speed for 16 hours.
[0023] 4. After the above steps, the cellulose is in a colorless, transparent and viscous state in a three-necked flask, and is dissolved in N,N-dimethylacetamide / LiCl system, such as figure 2 Shown; Add 1.92g of dry sodium hydroxide powder to a three-necked flask, and stir at a medium...
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The invention discloses a synthetic method for a methyl cellulose sample. Dissolved cellulose or other liquid homogeneous-phase cellulose is adopted as a reaction raw material to carry out a reaction on the mechanical stirring condition, separated and purified through multiple kinds of solvent, so that the high-substitution-degree methyl cellulose sample is prepared. According to the synthetic method for the methyl cellulose sample, equipment in a laboratory, preparation scales and substitution uniformity are considered, the methyl iodide methylation cellulose method is adopted for synthesizing methyl cellulose, the preparation quantity of the method is small, the requirement for the equipment is low, sample substitution is uniform, and the methylation substitution degree is high.
Description
technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing a methyl cellulose sample Background technique [0002] As a common chemical substance, methyl cellulose is widely used in chemical industry, construction and other industries, and occupies an important position in the industry. As a method of cellulose research, cellulose methyl derivatization is widely used in analytical and characterization experiments such as HPLC, NMR, and GPC. Therefore, the establishment of the synthetic method of methyl cellulose has positive significance for industry and scientific research. [0003] The traditional industrial methylcellulose synthesis method is to use methylene chloride to react and synthesize in an alkaline, 60-70°C high-pressure environment. This preparation method is generally not conducive to laboratory preparation. The traditional laboratory preparation method is to use dry DMSO as a solvent, cellulose ...
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Inventor 何建平宫大军陈卫平邓明宇叶应庆李博朱明山何俊唐志娟
Owner 昆山京昆油田化学科技有限公司