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Method for extruding in-situ grafting modified cellulose through twin screws with ionic liquid serving as solvent

A twin-screw extrusion and twin-screw extruder technology, applied in the production of bulk chemicals, etc., can solve the problems of cellulose solubility of only about 5-15%, restricting the application of industrial production, low dissolution efficiency, etc. The effect of processing and forming, promoting energy consumption and low energy consumption

Inactive Publication Date: 2015-05-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the research on the use of ionic liquids to dissolve and process cellulose has attracted more and more attention. Most of these research methods dissolve cellulose by heating, pressurizing or microwave radiation in a beaker or reactor. The intermittent modification method of cellulose limits its application in industrial production, and the dissolution efficiency is low, and the solubility of cellulose is only about 5-15%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dry the cellulose and acrylic acid in vacuum at 50 °C for 12 hours, add 80 g of cellulose, 400 g of acrylic acid, 800 g of [BMIM]Cl, 0.6 g of ammonium persulfate and 0.6 g of N,N'-dimethylformamide into a high-speed mixer well mixed.

[0026] The temperature of the first zone of the twin-screw extruder is 100°C, the temperature of the second zone is 100°C, the temperature of the third zone is 110°C, the temperature of the fourth zone is 120°C, the temperature of the fifth zone is 120°C, the temperature of the sixth zone is 130°C, and the temperature of the seventh zone It is 140°C, the eight-zone temperature is 140°C, and the head temperature is 135°C. The screw speed is 200 rpm, the extrusion pressure is 3 MPa, and the vacuum pump pressure is 0.8 MPa.

[0027] Precipitate the product with distilled water after extrusion, wash away the ionic liquid, and then use ethanol solvent to precipitate and separate the product, dry to obtain the crude graft, and finally use acet...

Embodiment 2

[0029] Dry the cellulose and acrylic acid under vacuum at 70 °C for 24 hours, add 80 g of cellulose, 560 g of acrylic acid, 800 g of [BMIM]Cl, 0.8 g of ceric ammonium nitrate and 0.8 g of N,N'-dimethylformamide into a high-speed mixer Mix well.

[0030] The temperature of the first zone of the twin-screw extruder is 100°C, the temperature of the second zone is 110°C, the temperature of the third zone is 120°C, the temperature of the fourth zone is 120°C, the temperature of the fifth zone is 130°C, the temperature of the sixth zone is 130°C, and the temperature of the seventh zone 140°C, 150°C in the eighth zone, and 145°C at the head. The screw speed is 300 rpm, the extrusion pressure is 4 MPa, and the vacuum pump pressure is 0.8 MPa.

[0031] Precipitate the product with distilled water after extrusion, wash away the ionic liquid, and then use ethanol solvent to precipitate and separate the product, dry to obtain the crude graft, and finally use acetone to extract in a Soxhl...

Embodiment 3

[0033] The cellulose and acrylic acid were dried under vacuum at 90 °C for 36 hours, and 80 g of cellulose, 400 g of acrylonitrile, 800 g of [EMIM]Ac, 0.6 g of potassium persulfate and 0.6 g of N,N'-dimethylformamide were added to the high-speed Mix well in a blender.

[0034] The temperature of the first zone of the twin-screw extruder is 100°C, the temperature of the second zone is 110°C, the temperature of the third zone is 120°C, the temperature of the fourth zone is 120°C, the temperature of the fifth zone is 130°C, the temperature of the sixth zone is 130°C, and the temperature of the seventh zone 140°C, 150°C in the eighth zone, and 145°C at the head. The screw speed is 300 rpm, the extrusion pressure is 5 MPa, and the vacuum pump pressure is 0.8 MPa.

[0035] Precipitate the product with distilled water after extrusion, wash away the ionic liquid, and then use ethanol solvent to precipitate and separate the product, dry to obtain a crude graft, and finally use acetone...

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Abstract

The invention relates to a method for extruding in-situ grafting modified cellulose through twin screws with ionic liquid serving as a solvent. The method comprises the following steps: (1) drying the cellulose and a grafting monomer in vacuum; (2) uniformly mixing the following raw materials by weight percent: 4 to 8% of cellulose, 30 to 40% of grafting monomer, 51.84 to 65.92% of ionic liquid, 0.04 to 0.08% of initiator, and 0.04 to 0.08% of catalyst; and (3) extruding the mixture by a co-rotating twin-screw extruder, so as to obtain the in-situ grafting modified cellulose. By adopting the method, high flowing property is provided on the basis that the original performances of the cellulose are remained; the cellulose grafting copolymer, which is easily processed and formed, and efficient, green and clean, can be obtained; and the development on novel cellulosic fibers, which are low in energy consumption, economic and feasible and environmentally friendly, can be promoted.

Description

technical field [0001] The invention belongs to the method field of modified cellulose, and particularly relates to a method for twin-screw extruding in-situ grafting modified cellulose using ionic liquid as a solvent. Background technique [0002] Cellulose is one of the most abundant natural polymer materials in the world. It has the advantages of biodegradability and good environmental adaptability. It can neither dissolve in common solvents nor melt at high temperature, which seriously affects the processing performance of cellulose. Researchers from all over the world have used various physical or chemical modification methods on cellulose in order to reduce the polarity of cellulose, thereby improving the processing performance of cellulose and expanding the application field of cellulose. [0003] There are three main ways to modify cellulose: cellulose crosslinking, cellulose derivatives and cellulose graft copolymerization. Among them, the graft copolymerization o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F251/02
CPCY02P20/54
Inventor 余木火张玥李海峰李欣达黎欢
Owner DONGHUA UNIV
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