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Recovery method of N-methylmorpholine oxide solvent in process of producing regenerated cellulose fibre by solvent method

A technology of regenerated cellulose and methylmorpholine, which is applied in the fields of fiber chemical characteristics, rayon recycling, and final product manufacturing. It can solve the problems of increased production cost of regenerated cellulose fibers, large investment in evaporation and concentration equipment, and difficulty in industrial promotion, etc. problem, to achieve the effect of prolonging life, convenient operation and less production investment

Inactive Publication Date: 2012-05-23
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although vacuum evaporation and concentration can make the mass concentration of recovered NMMO reach about 87%, the condensed water will contain some volatile substances such as amines and solvents during evaporation and concentration, and reverse osmosis or cation exchange resin should be used to effectively separate the residual Amines, amine oxides and other substances, but the recovery of condensed water will easily cause the loss of NMMO solvent
Evaporation and concentration equipment requires a large investment, and the process requires a large amount of water, electricity, steam, etc. In addition, impurities in condensed water must be treated. The cumbersome and complicated process leads to an increase in the production cost of NMMO solvent-based regenerated cellulose fibers, making it difficult to achieve industrial promotion.

Method used

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  • Recovery method of N-methylmorpholine oxide solvent in process of producing regenerated cellulose fibre by solvent method
  • Recovery method of N-methylmorpholine oxide solvent in process of producing regenerated cellulose fibre by solvent method

Examples

Experimental program
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Effect test

Embodiment 1

[0024] See figure 1 .

[0025](1) In the spinning process production of the regenerated reed fiber prepared by the solvent method, the NMMO aqueous solution with a commercially available mass concentration of 50% is used as a solvent to indirectly dissolve the reed pulp (polymer 302, the mass content of α-cellulose is 95.6%) ) preparing regenerated reed fibers; using an NMMO aqueous solution with a mass concentration of 50% as a coagulation bath for the regenerated reed fibers;

[0026] (2) Along with the carrying out of spinning process, add the NMMO aqueous solution that mass concentration is 25% in the coagulation bath of step (1) with the flow velocity of 340kg / h, make containing mass concentration be 50% with the flow velocity of 570kg / h simultaneously The NMMO aqueous solution discharges the container of loading coagulation bath in the receiving tank, under making the NMMO aqueous solution coagulation bath effectively circulates, the mass concentration of the NMMO aqueo...

Embodiment 2

[0033] (1) In the spinning process production of the regenerated bamboo fiber prepared by the solvent method, the NMMO aqueous solution of 50% is the solvent indirect dissolution of the bamboo pulp (the degree of polymerization is 773, the mass content of α-cellulose is 93.2% with the commercially available mass concentration). %) to prepare regenerated bamboo fiber; be the coagulation bath of regenerated bamboo fiber with the NMMO aqueous solution of 50% in mass concentration;

[0034] (2) Along with the carrying out of spinning process, add the NMMO aqueous solution that mass concentration is 10% in the coagulation bath of step (1) with the flow velocity of 0.54kg / h, make containing mass concentration be with the flow velocity of 1.11kg / h simultaneously 50% NMMO aqueous solution discharges the container of loading coagulation bath to receiving tank, under making NMMO aqueous solution coagulation bath effectively circulates, the mass concentration of the NMMO aqueous solution ...

Embodiment 3

[0041] (1) In the spinning process production of the regenerated cotton fiber prepared by the solvent method, the NMMO aqueous solution with a commercially available mass concentration of 50% is used as a solvent to indirectly dissolve the cotton pulp (the degree of polymerization is 1193, and the mass content of α-cellulose is 98.1 %) to prepare regenerated cotton fibers; the NMMO aqueous solution with a mass concentration of 50% is a coagulation bath for regenerated cotton fibers;

[0042] (2) Along with the carrying out of spinning process, add the NMMO aqueous solution that mass concentration is 15% in the coagulation bath of step (1) with the flow velocity of 121kg / h, make containing mass concentration be 50% with the flow velocity of 236kg / h simultaneously The NMMO aqueous solution discharges the container of loading coagulation bath in the receiving tank, under making the NMMO aqueous solution coagulation bath effectively circulates, the mass concentration of the NMMO aq...

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Abstract

The invention relates to a recovery method of an N-methylmorpholine oxide (NMMO) solvent in a process of producing regenerated cellulose fibre by a solvent method in a spinning technology. The technical scheme of the invention is designed as follows: a NMMO aqueous solution with the mass concentration of 50% is taken as a coagulating bath of the regenerated cellulose fibre; the circulation of thecoagulating bath is optimally controlled so that the mass concentration of the coagulating bath of the NMMO aqueous solution in a coagulating bath-loading container is controlled to be 50%; and multiple impurities in recovery liquid, namely a coagulating bath solution, are removed through rough filtration, microporous membrane microfiltration, anion exchange resin treatment, cation exchange resintreatment and hydrogen peroxide oxidization, thereby achieving the recovery of the NMMO solvent.

Description

technical field [0001] The invention relates to a method for recovering N-methylmorpholine oxide (NMMO) solvent in the process of producing regenerated cellulose fiber by solvent method in spinning process. technical background [0002] N-methylmorpholine oxide (NMMO) is a kind of non-toxic solvent, it is made by oxidation of N-methylmorpholine through hydrogen peroxide, take N-methylmorpholine oxide (mass concentration is 50%) as In recent years, more and more attention has been paid to the technology of preparing regenerated cellulose fibers by indirectly dissolving cellulose pulp raw materials with solvents. Due to the high price of NMMO, foreign manufacturers attach great importance to the recycling of NMMO, and have proposed a variety of technical solutions for recycling NMMO in order to find the most practical technical method for production. In theory, the process of NMMO dissolving cellulose pulp to prepare regenerated cellulose fibers is a purely physical process, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F13/02
CPCY02P70/62
Inventor 刘必前汪前东李兰吴杰
Owner INST OF CHEM CHINESE ACAD OF SCI
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