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Preparation method of cellulosic fibers

A cellulose fiber and cellulose technology, applied in the field of cellulose, can solve the problems of difficult to achieve high-efficiency and low-consumption industrialized production, unfavorable fiber homogeneity and mechanical properties, large investment in multi-effect evaporation equipment, etc. Preparation, avoid the problem of repeated energy consumption, reduce the effect of recovering the amount of evaporated water

Active Publication Date: 2016-12-14
CHINESE TEXTILE ACAD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Prior art In the process of cellulose fiber preparation, the concentration of NMMO aqueous solution to be recovered is low, as described in CN101089262A and CN1318115A, generally 10%-30%, and the concentration of raw material NMMO aqueous solution required for stock solution preparation is high, as described in CN1468889A and CN1635203A , generally 80%-88%, the amount of evaporated water required for recovery is huge, and energy-saving multi-effect evaporation equipment is usually used; The large investment in equipment makes the production cost too high, making it difficult to achieve high-efficiency and low-consumption industrial production
[0004] In addition, a single low-concentration coagulation method can easily lead to severe coagulation, resulting in the formation of a skin-core structure in the fiber, which is not conducive to the homogeneity and mechanical properties of the fiber; moreover, the high-concentration NMMO aqueous solution required for the preparation of the stock solution exists during evaporation, storage, and transportation. Safety risks, there is repeated energy consumption in the preparation of stock solution, and the equipment and process of stock solution preparation are too cumbersome

Method used

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  • Preparation method of cellulosic fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] The NMMO aqueous solution with a mass concentration of 72% and the cellulose pulp without any treatment are directly and uniformly mixed, and mechanically stirred in the mixer 1 to obtain a uniform mixture. Among them, the pulp is mixed with high and low polymerization degrees of cellulose wood pulp, DP:800 and DP:450 wood pulp are mixed according to the mass ratio of 8:92, and the cellulose concentration is 12%.

[0051] The obtained homogeneous mixture is fully swollen, dissolved and defoamed through continuous two-step evaporation dehydration in the dehydration device 2 to obtain the cellulose spinning stock solution, such as image 3 shown. The first step of evaporative dehydration process is mainly a process of full swelling and mixing, and the residence time is 20 minutes; the second step of evaporative dehydration process mainly removes excess water to dissolve cellulose into a homogeneous solution, which is the spinning stock solution. The refraction of the spi...

Embodiment 2

[0057] Cellulose fiber is prepared according to the same conditions as in Example 1, except that:

[0058] The NMMO aqueous solution with a mass concentration of 76% is fed; the pulp is mixed with cellulose wood pulp DP:400 and bamboo pulp DP:300, the mixing ratio is 52:48, and the cellulose concentration is 16%. Gained homogeneous mixture obtains cellulose spinning dope through continuous three-step evaporation dehydration in dehydration device 2, such as image 3 As shown, the residence time of the first two steps is 9min, the refraction of the spinning dope is 1.48623, and the viscosity is 2849Pa·S.

[0059] The prepared spinning dope heat exchange equipment 4 is heat exchanged to 95°C, and after being extruded through the spinneret assembly, it enters the coagulation system 6, and the coagulation system is a three-stage coagulation system, such as Figure 4 shown. The concentration of NMMO in the primary coagulation bath is 70%, and the temperature is 35 °C; the concentr...

Embodiment 3

[0064] Cellulose fiber is prepared according to the same conditions as in Example 1, except that:

[0065] The NMMO aqueous solution with a mass concentration of 74% is used for feeding; the pulp is cellulose wood pulp, DP: 300, and the cellulose concentration is 18%. Gained homogeneous mixture obtains cellulose spinning dope through continuous two-step evaporation dehydration in dehydration device 2, such as image 3 As shown, the residence time of the first step is 25min, the refraction of the spinning dope is 1.48714, and the viscosity is 2415Pa·S.

[0066] The prepared spinning stock solution is heat-exchanged to 90°C through the heat exchanger 4, and after being extruded through the spinneret assembly, it enters the coagulation system 6, and the coagulation system 6 is a three-stage coagulation system, such as Figure 4 shown. The concentration of NMMO in the primary coagulation bath is 65%, and the temperature is 30°C; the concentration of NMMO in the secondary coagula...

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Abstract

The invention discloses a preparation method of cellulosic fibers. The preparation method includes the following steps that 1, cellulose pulp is mixed with an NMMO water solution with the mass concentration of 60%-85%, preferably 70%-76% to obtain a uniform mixture; 2, the obtained uniform mixture is subjected to dehydration swelling and dissolution defoaming to obtain a cellulose spinning solution; 3, the obtained cellulose spinning solution is filtered and subjected to heat exchange and then enters a spinning machine, after the cellulose spinning solution is extruded through a spinning assembly and air-cooled, the cellulose spinning solution enters a solidification system and is solidified in an NMMO solidification bath with the mass concentration larger than 50% and smaller than 72%, and nascent fibers are obtained; 4, the obtained nascent fibers are washed to obtain cellosilk bundles, and then the cellulosic fibers are obtained through subsequent section treatment. Equipment investment can be greatly reduced, the process is simplified, energy consumption and industrialization cost are reduced, safety production is promoted, the homogeneity and mechanical performance of the fibers are improved, and therefore the preparation method is more suitable for efficient low-consumption industrial production.

Description

technical field [0001] The invention belongs to the technical field of cellulose, and in particular relates to a preparation method of cellulose fibers. Background technique [0002] In the process of dissolving cellulose with N-methylmorpholine-N-oxide (NMMO) aqueous solution to prepare cellulose fibers, the swelling, dissolving process and effect of NMMO on cellulose are directly related to the stability of spinning and the performance of the final product ; And the concentration of the spinning dope and whether the process is energy-saving are directly related to the economic benefits and industrialization of the process technology. In view of this, in industrial production, an energy-saving and efficient method for preparing cellulose fibers is particularly important. [0003] Prior art In the process of cellulose fiber preparation, the concentration of NMMO aqueous solution to be recovered is low, as described in CN101089262A and CN1318115A, generally 10%-30%, and the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F2/00D01D1/02D01D5/06D01D10/06
CPCD01F2/00D01D5/06D01D1/02D01D10/06D01F13/02Y02P70/62D01F2/08
Inventor 孙玉山李婷程春祖丁丽兵蔡剑骆强周运安张东徐纪刚
Owner CHINESE TEXTILE ACAD
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