Preparation method of ethyecellulose-based macromonomer

An ethyl cellulose and macromonomer technology is applied in the field of preparation of ethyl cellulose-based macromonomers, which can solve the problems of limiting cellulose modification and processing and utilization, and achieve high polymerization activity and good application prospects. Effect

Inactive Publication Date: 2013-07-24
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it can be dissolved in some unique solvent complex systems, such as urea-sodium hydroxide solution system, lithium chloride (LiCl)-dimethyla

Method used

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  • Preparation method of ethyecellulose-based macromonomer
  • Preparation method of ethyecellulose-based macromonomer
  • Preparation method of ethyecellulose-based macromonomer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In the first step, ethyl cellulose is dissolved in an organic solvent, and the solvent can be selected such as tetrahydrofuran, dimethylformamide, dimethylacetamide, dioxane, dimethyl sulfoxide, and under low temperature conditions, carry out Ultrasonic activation treatment; temperature optional -20°C, -18°C, -16°C, -14°C, -12°C, -14°C, -10°C, -8°C, -6°C, -4°C, -2°C , 0°C, ultrasonic time is 5~60s, optional 5s, 10s, 15s, 20s, 25s, 30s, 35s, 40s, 45s, 50s, 55s, 60s, ultrasonic interval time is 1~10min, ultrasonic interval time is optional 1min, 2min, 3min, 4min, 5min, 50min, 6min, 7min, 8min, 9min, 10min. The duration of the ultrasonic activation process is 10-60min, 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min, 60min are optional.

[0025] In the second step, catalyst and polymerization inhibitor hydroquinone are added for further low-temperature activation and nitrogen deoxygenation treatment. The catalyst can be selected from any one of N, N-...

Embodiment 2

[0028] Synthetic steps:

[0029]

[0030] In the first step, 1.0 g of ethyl cellulose was dissolved in 50 mL of tetrahydrofuran, and ultrasonic activation was performed at 0 ° C. The ultrasonic time was 10 s, the interval time was 2 min, and the ultrasonic duration was 10 min;

[0031] In the second step, add catalyst triethylamine 2.2mL and polymerization inhibitor hydroquinone 0.001g, further low-temperature activation and nitrogen deoxygenation treatment at 0°C for 30min;

[0032] In the third step, at 0°C, add 1.3 mL of acryloyl chloride dropwise (acryloyl chloride / ethyl cellulose hydroxyl molar ratio = 3:1, keep at 0°C for 2 hours, then raise the temperature to room temperature for 15 hours; then the solution drop into water for precipitation, filter, wash with water and freeze-dry to obtain ethyl cellulose-based macromer with a substitution degree of 0.60.

[0033] Using infrared spectroscopy (FTIR) ( figure 1 ), H NMR spectrum ( 1 H NMR) ( figure 2 ) C-13 NMR sp...

Embodiment 3

[0036] In the first step, dissolve 1.0 g of ethyl cellulose in 50 mL of tetrahydrofuran, and perform ultrasonic activation treatment at -10 ° C. The ultrasonic time is 10 s, the interval time is 2 min, and the ultrasonic duration is 10 min;

[0037] In the second step, add catalyst triethylamine 2.2mL and polymerization inhibitor hydroquinone 0.001g, further low-temperature activation and nitrogen deoxygenation treatment at 0°C for 40min;

[0038] The third step is to add 1.3 mL of acryloyl chloride dropwise at 0°C (acryloyl chloride / ethyl cellulose hydroxyl = 3:1, keep the reaction at 0°C for 2 hours, then raise the temperature to room temperature for 15 hours; then drop the solution into Precipitate in water, filter, freeze-dry after washing with water to obtain ethyl cellulose-based macromer. Test result: substitution degree 0.65.

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Abstract

The invention relates to a preparation method of an ethyecellulose-based macromonomer. The preparation method comprises the following steps of: step one, dissolving ethyecellulose in an organic solvent and carrying out ultrasonic wave activation treatment under a low-temperature condition; step two, adding a catalyst and a polymerization inhibitor for carrying out further low-temperature activation, introducing nitrogen for removing oxygen; and step three, dropwise adding acryloyl chloride or methacryloylchloride to the solvent under a low-temperature condition, reacting for 1-4 hours at a low temperature, and heating to room temperature and reacting for 12-48 hours; and then dropwise adding the solution to water, precipitating, filtering, washing with water and carrying out freeze drying to obtain the ethyecellulose-based macromonomer. The ethyecellulose-based macromonomer can be used for carrying out free radial polymerization reaction and has very good application prospects in the fields such as coating, gel, plastics and medicines.

Description

technical field [0001] The invention relates to a preparation method of ethyl cellulose-based macromolecular monomer. Background technique [0002] Cellulose is the most abundant renewable resource in nature, which has the advantages of cheap and easy to obtain, biodegradability, stability and special mechanical properties. Cellulose and cellulose derivatives have been widely used in many fields such as textile, papermaking, food, medicine, biology and construction. There are a large number of hydroxyl functional groups in cellulose molecules, and cellulose can generate a series of cellulose derivatives through reactions such as esterification, etherification, and graft copolymerization. With the increasing depletion of petroleum resources, the modification of cellulose, a renewable resource, into free radical polymerizable macromonomers is an important direction in the research of cellulose modification and utilization. This is of great significance to alleviating the hug...

Claims

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Application Information

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IPC IPC(8): C08B3/08C08B11/02C08J3/28C08F251/02
Inventor 王基夫俞娟刘玉鹏储富祥王春鹏
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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