Preparation of cellulose carbamate and low-temperature dissolution spinning method of cellulose carbamate

A carbamate and low-temperature dissolving technology, applied in the direction of artificial filaments in cellulose solution, can solve the problems of low solubility and low solubility of cellulose, and achieve the effects of good filtration performance, improved solubility and good mechanical properties

Inactive Publication Date: 2014-10-01
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a low-temperature solution-spinning engineering and industrial production of cellulose, the preparation of cellulose carbamate with high spinning speed and its low-temperature solution-spinning method, which solves the problem of In industrial production, the solubility of cellulose carbamate in aqueous sodium hydroxide solution is low and the solubility of cellulose in low temperature alkali / urea solution is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0025] A kind of preparation method of cellulose carbamate, it comprises the following steps:

[0026] (1) common cotton fiber (i.e. cellulose) and urea with a degree of polymerization between 300-600 are vacuum-dried at 70° C. for 24 hours;

[0027] (2) configuration concentration is the sodium hydroxide solution of 12-16%, gets a certain amount of cellulose and joins the sodium hydroxide solution, the cellulose addition is 5-10% of the sodium hydroxide solution quality, stirs evenly, at 50 Soak for 30-60 minutes at ℃;

[0028] (3) Take out the cellulose and wash it to neutral, and wash it until the water content is 200% to obtain alkalized cellulose, then add a certain amount of urea, the amount of urea added is 50-100% of the cellulose mass, stir evenly, put Heating in an oven at a reaction temperature of 120-140°C, reacting for 2-3 hours and drying to obtain cellulose carbamate.

[0029] A low-temperature solution-spinning method of cellulose carbamate, comprising the fo...

Embodiment 1

[0036] The cellulose and urea were vacuum dried at 70°C for 24 hours. Wherein, the cellulose is ordinary cotton fiber with a degree of polymerization of 300. Prepare 15kg of 16% sodium hydroxide aqueous solution, add 1.5kg of cellulose into the sodium hydroxide aqueous solution, stir evenly, soak at 50°C for 30 minutes, wash the cellulose to neutral after soaking, and obtain water-containing alkalized cellulose 3kg, then add 1.5kg urea and stir evenly, put it in an oven at 137°C and react for 2 hours, then dry until the quality of the reaction product remains unchanged, then pulverize the reaction product cellulose carbamate to obtain cellulose carbamate Ester powder, the particle size of which is 800 mesh.

[0037] Get 1kg of cellulose urethane powder and 10kg of solvent into the mixing tank through a metering pump (i.e. a cellulose meter) and stir for 15 minutes to mix evenly, then feed into a low-temperature co-rotating twin-screw extruder through a metering pump, extrude ...

Embodiment 2

[0043] The cellulose and urea were vacuum dried at 70°C for 24 hours. Wherein, the cellulose is common cotton fiber with a degree of polymerization of 400. Prepare 15kg of 14% sodium hydroxide aqueous solution, add 0.75kg of cellulose into the sodium hydroxide aqueous solution, stir evenly, soak at 50°C for 45 minutes, wash the cellulose to neutral after soaking, and obtain water-containing alkalized cellulose 1.5kg, then add 0.6kg urea and stir evenly, put it in an oven at 120°C for 3 hours and then dry it until the quality of the reaction product remains unchanged, then pulverize the reaction product cellulose carbamate to obtain cellulose carbamate Ester powder, the powder particle size is 600 mesh.

[0044] Get 1kg of cellulose urethane powder and 10kg of solvent into the mixing tank through a metering pump (i.e. a cellulose meter) and stir for 15 minutes to mix evenly, then feed into a low-temperature co-rotating twin-screw extruder through a metering pump, extrude Afte...

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Abstract

The invention discloses preparation of cellulose carbamate and a low-temperature dissolution spinning method of the cellulose carbamate. The method comprises the following steps: adding cellulose into a sodium hydroxide solution, stirring uniformly, immersing, taking out the cellulose, washing with water to a neutral state to obtain alkalified cellulose, adding urea, stirring uniformly, putting in a drying oven, heating, reacting and drying to obtain the cellulose carbamate; pulverizing the cellulose carbamate into powder, adding the powder into a mixing kettle, adding double solvents of sodium hydroxide, thiocarbamide and deionized water, and stirring uniformly; and carrying out extrusion, deaeration and filtration on the raw material in the mixing kettle, spraying by spinneret orifices of a spinneret, sequentially sending into a first coagulation bath and a second coagulation bath to obtain a solid, washing with water in a water tank, and carrying out stretching and winding by a spinning component to obtain the cellulose carbamate fiber. The method is suitable for preparing the cellulose carbamate by an industrialized large-scale production process route, and has important meanings for implementing low-temperature dissolution spinning engineering and industrialized production of cellulose.

Description

technical field [0001] The invention relates to the preparation of cellulose carbamate and its low-temperature solution spinning method, belonging to the field of green processing and modification of polymer materials. Background technique [0002] Cellulose is widely derived from nature, such as hemp, wheat straw, rice straw, etc. Because there are two secondary hydroxyl groups and one primary hydroxyl group on each glucose unit ring of cellulose, it is easy to form intramolecular and intermolecular hydrogen bonds, and the crystallinity is very high, so cellulose is difficult to dissolve in general inorganic and organic solvents , need to use special solvents or derivatize and modify them to facilitate processing and utilization. Cellulose derivatization mainly includes esterification, etherification and graft copolymerization. Among them, cellulose and urea react to form cellulose carbamate, the process is relatively simple, the spinnability is good, and the environmenta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/06D01F2/02
Inventor 余木火张玥李欣达何小云黎欢
Owner DONGHUA UNIV
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