CN102234852A - Solvent recovery method of Lyocell fibers - Google Patents
Solvent recovery method of Lyocell fibers Download PDFInfo
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- CN102234852A CN102234852A CN2010101514413A CN201010151441A CN102234852A CN 102234852 A CN102234852 A CN 102234852A CN 2010101514413 A CN2010101514413 A CN 2010101514413A CN 201010151441 A CN201010151441 A CN 201010151441A CN 102234852 A CN102234852 A CN 102234852A
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Abstract
The invention discloses a solvent recovery method of Lyocell fibers, comprising the following steps: processing collected Lyocell fibers into a washing liquor, introducing the washing liquor to a decolouring groove, using active carbon powder to decolor through suspension, then removing the active carbon and impurities from the decolored washing liquor by a two-stage filtration containing prefiltration and ultrafiltration, removing the water from the washing liquor by one of the following two methods: mechanical vapor recompression condensation method and triple effect evaporation vapor condensation method, so as to obtain a recovered solution with the solvent concentration which coincides with fiber processing. Because the recovery process is simple, the devices used in conjunction with the process are not complicate, easy to access, and suitable for using in the recovery of a large amount of low concentration washing liquor, so that the invention has competitive recovery cost, recovery efficiency and quality of the recovered solution, and has practicability and environmental nature.
Description
Technical field
The present invention relates to a kind of recovery method that is used for the solvent of fiber processing procedure, particularly relate to a kind of method for recovering solvents of Lyocell fiber.
Background technology
The Lyocell fiber is made by native cellulose, therefore, but its discarded object natural degradation and can not cause environmental issue, in addition, the Lyocell fiber also has the physical mechanical strength near synthetic fiber, and have that drapability is good, feel is abundant, sense of touch is comfortable, good hygroscopicity, dyeing easily, easily and characteristics such as the natural fabric of other material or synthetic fiber blending, and texture and processability are all good, are a kind of fibre with high-performance and high additive value.
Consult Fig. 1, existing Lyocell fiber processing procedure mainly be divided into size mixing, step such as dissolving, spinning and washing, wherein, size mixing is just to add in wood pulp-oxidation methyl beautiful jade (N-Methyl Morpholine N-Oxide, abbreviating NMMO as) solvent to be to carry out cellulosic dissolving, through spinning is the renewable Lyocell of obtaining precursor, remains in NMMO solvent in the precursor through the washing operation eccysis again, just can make Lyocell filament finished product.
Because the NMMO solvent has characteristics such as nontoxic, odorless, higher boiling, make with NMMO to be the processing procedure of the Lyocell fiber processing procedure of solvent compared to general synthetic fiber, more meet the demand of safety and environmental protection.Yet; the NMMO solvent costs an arm and a leg; consider the economic benefit of suitability for industrialized production; usually NMMO can be reclaimed circulation re-uses; and its rate of recovery can reach more than 99.5%; whereby, the pollution problem that can effectively avoid outside waste discharge and caused makes the Lyocell fiber become environmental protection fiber worthy of the name.
Though have the technology that in the Lyocell processing procedure, reclaims the NMMO solvent at present, but in order further to reduce the price competitiveness of manufacturing cost and then increase Lyocell fiber again, still have to continue equipment and the program that the exploitation use is more simplified, and can reach the demand of the recovery method of preferable efficient.
Summary of the invention
The object of the present invention is to provide a kind of solvent that can in the water lotion of fiber processing procedure, reclaim for reusing, and the method for recovering solvents of the Lyocell fiber that can improve organic efficiency with the equipment of simplifying and program.
The method for recovering solvents of Lyocell fiber of the present invention comprises the following step:
One, decolouring, the water lotion of collected Lyocell fiber processing procedure is guided to a decolouring groove, and in this water lotion, add activated carbon powder with adsorptivity and suspension, with leaving standstill the mode that the absorption that suspends alternately carries out water lotion is fully mixed with the air blast mixing and absorption with activated carbon again, with the adsorption efficiency of enhancement activated carbon powder;
Two, filter, in regular turn with coarse filtration and hyperfiltration (Ultrafiltration, abbreviate UF as) the water lotion finished of two-stage filter type filtering decolouring in activated carbon and impurity component, the activated carbon powder that is added when handling with coarse filtration filtering decolouring respectively and the impurity of big particle diameter and with the impurity of hyperfiltration filtering small particle diameter;
Three, concentrate, adopt wherein a kind of mode of mechanical steam recompression concentration method and triple effect steam concentration method to remove moisture in this water lotion, with the not solvent-laden condensed water liquid of acquisition respectively and just contain-concentrate of oxidation methyl beautiful jade solvent.
Preferably, this recovery method also comprises a step 4, step 4 is refining, for in the concentrate that concentration obtained, adding an oxidant, so that the methyl beautiful jade (N-MethylMorpholine abbreviates NMM as) of trace just is being oxidized to-the oxidation methyl beautiful jade in this concentrate, and when oxidation reaction is finished, add the oxidisability that remains in the oxidant in this concentrate in the reductant with unreacted, just can obtain to have the recovery liquid of just highly purified-oxidation methyl beautiful jade solvent.
Preferably, in step 1, carry out the air blast mixing and absorption is 1: 3～1: 6 with the time scale that leaves standstill the absorption that suspends at every turn, and the total time of the processing of decolouring was smaller or equal to 8 hours.
Preferably, in step 1, the dosage of the activated carbon powder that is added is the 0.05wt%～0.10wt% of this water lotion total amount.
Preferably, in step 2, carry out coarse filtration with the filer element type filter, and also be coated with filter aid in advance in this cartridge surface, and in the not filtrate that decolouring is finished, also adding the filter aid of scheduled volume, this filter aid comprises diatomite and the cellulose that mixes mutually according to predetermined ratio.
Preferably, in step 2, be added on this not the filter aid content in the filtrate be 0.03wt%～0.05wt%, and the diatomite in this filter aid and cellulosic mixed proportion are 4: 1.
Preferably, in step 2, the filter residue raffinate after the coarse filtration can reclaim use again after centrifugal dehydration.
Preferably, in step 2, the filter opening aperture of the used filter material of coarse filtration is 1 μ m～100 μ m, and the filter opening aperture of the used filter material of hyperfiltration is 0.01 μ m～1 μ m.
Preferably, in step 3, in this concentrate just-concentration of oxidation methyl beautiful jade solvent is 50wt%～55wt%.
Preferably, used oxidant is H when step 4 is carried out refinement treatment
2O
2, used reductant is N
2H
4H
2O.
Preferably, in step 4, the methyl beautiful jade in this concentrate and then just is oxidized to-the oxidation methyl beautiful jade under the environment of 80 ℃ ± 2 ℃ of temperature and oxidant reaction.
Beneficial effect of the present invention is: can utilize decolouring earlier and filter the impurity of removing in the water lotion, remove the moisture in the water lotion so that the solvent strength in the water lotion reaches predetermined concentration standard by concentration again, just can obtain to meet the recovery liquid of user demand, the program of aforementioned recycling is quite simplified effectively, the equipment that is used is also uncomplicated and obtain easily, add that this recovery method is applicable to that also the water lotion of big output fiber processing procedure reclaims, make equipment cost of the present invention, organic efficiency all has competitiveness with recovery liquid quality, and has practical value and can meet the environmental protection demand.
Description of drawings
Fig. 1 is the flow chart of existing Lyocell fiber processing procedure;
Fig. 2 is a flow chart that preferred embodiment matches with Lyocell fiber processing procedure of the method for recovering solvents of Lyocell fiber of the present invention;
Fig. 3 is a schematic diagram, illustrates that interpolation activated carbon powder and correspondence are provided with an air blast in a decolouring groove in a decolouring step of this preferred embodiment.
Among the figure: 101. decolourings; 102. filter; 103. concentrate; 104. it is refining; 21. decolouring groove; 22. air blast; 23. timing switch; 3. water lotion; 4. activated carbon powder.
The specific embodiment
The present invention is described in detail below in conjunction with drawings and Examples.
Consult Fig. 2, a preferred embodiment of the method for recovering solvents of Lyocell fiber of the present invention, be used to reclaim that Lyocell fiber processing procedure produced is a large amount of and contain the water lotion of low concentration NMMO solvent, Lyocell fiber processing procedure mainly comprise size mixing, dissolving, spinning and wash four treatment steps, in the water lotion that this fiber processing procedure produces except containing the NMMO solvent that is useful on the dissolving cellulos raw material, the NMM that also has trace, NMM is that NMMO is in the process of dissolving cellulos, because of heating causes the NMMO cracking formed.The preferred embodiment of this recovery method comprises the following step.
The air blast mixing and absorption is to utilize the blade rotation of an air blast 22, air pressurized is squeezed in this decolouring groove 21, with agitate water washing lotion 3 it is fully mixed with activated carbon powder 4, and startup and time-out by timing switch 23 control air blasts 22, and by repeatedly starting and suspending, reach and alternately carry out air blast mixing and absorption and the purpose that leaves standstill the absorption that suspends, carry out the air blast mixing and absorption is 1: 3～1: 6 with the time scale that leaves standstill the absorption that suspends at every turn, and the total time of the processing of decolouring was smaller or equal to 8 hours, in the present embodiment, the time set of decolouring processing was at 8 hours.Utilize and alternately open and close this air blast 22, can make activated carbon powder 4 and water lotion 3 fully mix the adsorption bleaching speed of quickening by the running of air blast 22 on the one hand, then can save the energy by leaving standstill the absorption that suspends on the other hand, and still can reach the adsorption bleaching effect by the activated carbon powder 4 of abundant dispersion.Wherein, preferably, the dosage of the activated carbon powder 4 that is added is the 0.05wt%～0.10wt% of these water lotion 3 total amounts.
Wherein, carry out coarse filtration with the filer element type filter, preferably, in order to improve and promote the rate of filtration, cartridge surface at this candle filter is coated with filter aid in advance, and in the not filtrate that decolouring is finished, also adding the filter aid of 0.03wt%～0.05wt%, this filter aid comprises diatomite and the cellulose that mixes mutually according to predetermined ratio, and the diatomite in this filter aid and cellulosic mixed proportion are preferably 4: 1.Borrow coating and add filter aid to help to increase filter area, and can effectively avoid the activated carbon powder to be accumulated in the filter core outermost layer and block filter core or slow down the rate of filtration.
What deserves to be explained is, after coarse filtration is finished, can be by the filter residue raffinate of filtering again through centrifugal, processed, the filter aid in the filter residue after the dehydration still helps the filter effect, and can reclaim use more once.Wherein, except containing filter aid, the activated carbon powder is arranged also in the filter residue after the dehydration, therefore, must earlier the more part of appearance activated carbon powder be struck off during use, remaining filter residue is reclaimed use again.
Wherein, triple effect steam concentration method is with the evaporation operation program of three evaporator series operations, is used to make steam heat repeatedly to be utilized, thereby improves the utilization rate of heat energy, is used for the processing of the aqueous solution more.In the operating process of triple effect steam concentration method, first evaporimeter (being called first imitates) is to give birth to steam as heating steam, all the other two (be called second imitate, triple effect) all with the indirect steam of its last effect as heating steam, whereby, can reduce the consumption of living steam significantly.Because the indirect steam temperature of each effect always is lower than its heating steam, therefore, when adopting triple effect or multiple-effect steam concentration method, each operating pressure and solution boiling temperature of imitating can reduce successively along the flow of steam direction during evaporation.According to the practical operation result, triple effect steam concentration method whenever dewaters 1 ton and needs 0.5 ton of steam consumption approximately, the steam consumption height, but power consumption is little, and the recovery that is fit to the water lotion of the less processing procedure of fiber production is used.
The abbreviation of the steam machinery booster-type distillation concentration systems that the MVR concentration method is meant the supercharging principle of utilizing turbogenerator, form through special fluid design.This flow system, the waste steam that electrical heating generates with make in the closed container menarche is recompressed the gases at high pressure that supercharging forms 107 ℃ by turbogenerator the time.This pressurization gas, can be used as regeneration thermal source and cycle applications in the continuation continuous evaporation of water lotion, and pressurization gas itself is cooled rapidly with condensation, until becoming clean condensed water liquid, can also in the condensed water liquid discharge process of this cleaning, utilizes its afterheat that the water lotion that flows into is carried out heat exchange again.The flow system of MVR concentration method, only need to this water lotion electrical heating it to be warming up to more than the vapor (steam) temperature at the distillation initial stage, follow-up distillation concentrates the needed energy, mainly can obtain, and make this water lotion finally be able to the distillation of high multiple and reach and concentrate the decrement purpose by this system exclusive pressurised steam and special fluid design thereof.MVR concentration method only about 0.003 ton～0.03 ton of the 1 ton of required steam consumption that whenever dewaters, steam consumption is low, but power consumption is big slightly, and the recovery that is fit to the big processing procedure water lotion of fiber production is used.
Though triple effect steam concentration method or MVR concentration method are if continue running, can make water lotion be concentrated to the high concentration of 70wt%～80wt%, but the NMMO solvent strength only needs 50wt%～55wt% just can meet the use specification of fiber processing procedure, in order to save the energy, do not need to improve again the concentrated concentration of this water lotion.
Though just contain the NMM of concentration in the originally fresh NMMO solvent less than 0.06wt%, but in Lyocell fiber processing procedure, still have a fraction of NMMO to become NMM because of heating pyrolyze, if this concentrate does not have more NMM through refinement treatment, relatively poor to the dissolubility of cellulosic material when reclaiming use again, in the spinning step of this fiber processing procedure, cause plug net and fracture of wire etc. to hinder the situation of spinning efficiency easily, and the rerum natura of the fiber product of making, for example intensity also can reduce, therefore, for avoiding reclaiming the quality that use has influence on fiber product, except need concentrate the concentration that reaches predetermined, also to pass through purification step again, allow NMM be oxidized to NMMO, with the purity that improves NMMO and reduce loss.In the present embodiment, the NMM content range in the concentrate before refining is 0.1wt%～0.3wt% after concentration.
Used oxidant is H when in the present embodiment, carrying out refinement treatment
2O
2, used reductant then is N
2H
4H
2O (hydrazine hydrate), and NMM is under the environment of 80 ℃ ± 2 ℃ of temperature and oxidant reaction, and then be oxidized to NMMO.If reaction temperature being set in the main consideration of this condition is that temperature is too high, then NMM and the H in this concentrate
2O
2Easily cracking or volatilization, and cause redox reaction too fierce and waste energy easily, if the too low then redox reaction of temperature weak effect causes purification efficiency to reduce.
The chemical equation of oxidant oxidation NMM is as follows:
The chemical equation of reductant and unreacted oxidant reaction is then as follows:
N
2H
4·H
2O+2H
2O
2→5H
2O+N
2
By aforesaid equation, can detect the NMM content in this concentrate earlier, again according to NMM/H
2O
2Reaction mol ratio rough estimate H
2O
2Addition, can both be oxidized in order to ensure nearly all NMM, H
2O
2Addition can be more than actual amount with the NMM reaction, after oxidation reaction is finished, again with reductant N
2H
4H
2The O reduction consumes excessive H
2O
2Can find out by aforementioned two chemical equations, though in this concentrate, add oxidant and reductant respectively, but the product after reaction is finished is except NMMO, also has water and nitrogen, nitrogen can directly spill in the atmosphere, water then becomes the part of the recovery liquid after making with extra care, in this recovery liquid, can not cause recovery liquid other impurity to occur because of adding other chemical reaction product, make concentrate after refinement treatment, can become recovery liquid really, and can when reclaiming use, the quality to fiber product not cause harmful effect with high purity N MMO.
What deserves to be explained is, the checking result of the practical application in manufacture process shows that the recovery proportion of goods damageds of NMMO are only below 0.5% in the recovery liquid that obtains through recovery method of the present invention, the rate of recovery of NMMO is at all not inferior in the existing recovery method of recovering effect, has practical value.
Conclude above-mentionedly, the method for recovering solvents of Lyocell fiber of the present invention can possess following effect and advantage, so can reach purpose of the present invention:
One, the present invention utilizes decolouring and filters the impurity of removing in the water lotion, and remove the moisture in the water lotion so that the solvent strength in the water lotion reaches predetermined concentration standard by concentration, at last, improve NMMO purity in this concentrate by refining program again, just can obtain to meet the recovery liquid of user demand, carry out aforementioned program in proper order, just water lotion can be recovered as again the raw material of fiber processing procedure, and the large quantity of moisture that is removed in the process is also recyclable to be reused to fiber processing procedure water-washing step, therefore, the massive laundering liquid that the fiber processing procedure is discharged by recovery method of the present invention reclaims fully, a large amount of discarded objects that are discharged in the environment that reduce, also can significantly reduce the former material cost of product by the NMMO solvent in the recycle-water washing lotion, the present invention be had to save cost and meet the environmental protection demand characteristics.
Two, impurity and the redundant moisture in the water lotion simplified and can be removed one by one effectively to the program of recovery method of the present invention, the equipment that is used also has the characteristic that obtains easily and conveniently install and use, and be applicable to the processing of the water lotion of big output fiber processing procedure, thereby can reach the result of efficient recycle-water washing lotion, relend by refinement treatment to reclaim highly purified solvent, can avoid effectively reclaiming that the quality to fiber product causes harmful effect when re-using, also make fiber product have more market competitiveness, therefore, the present invention can be to simplify effective program and equipment, high-quality recovery liquid is provided, and cost recovery is low, organic efficiency is good, and has practical value and economic benefit.
Claims (11)
1. the method for recovering solvents of a Lyocell fiber, it is characterized in that: this recovery method comprises the following step:
One, decolouring, the water lotion of collected Lyocell fiber processing procedure is guided to a decolouring groove, and in this water lotion, add activated carbon powder with adsorptivity and suspension, with leaving standstill the mode that the absorption that suspends alternately carries out water lotion is fully mixed with the air blast mixing and absorption with the activated carbon powder again, with the adsorption efficiency of enhancement activated carbon;
Two, filter, activated carbon and impurity component in the water lotion of finishing with the two-stage filter type filtering decolouring of coarse filtration and hyperfiltration in regular turn, the activated carbon powder that is added when handling with coarse filtration filtering decolouring respectively and the impurity of big particle diameter reach the impurity with hyperfiltration filtering small particle diameter;
Three, concentrate, adopt wherein a kind of mode of mechanical steam recompression concentration method and triple effect steam concentration method to remove moisture in this water lotion, with the not solvent-laden condensed water liquid of acquisition respectively and just contain-concentrate of oxidation methyl beautiful jade solvent.
2. the method for recovering solvents of Lyocell fiber according to claim 1, it is characterized in that: this recovery method also comprises a step 4, step 4 is refining, for in the concentrate that concentration obtained, adding an oxidant, so that the methyl beautiful jade of trace just is being oxidized to-the oxidation methyl beautiful jade in this concentrate, and when oxidation reaction is finished, add the oxidisability that remains in the oxidant in this concentrate in the reductant with unreacted, just can obtain to have the recovery liquid of just highly purified-oxidation methyl beautiful jade solvent.
3. the method for recovering solvents of Lyocell fiber according to claim 1, it is characterized in that: in step 1, carry out the air blast mixing and absorption is 1: 3～1: 6 with the time scale that leaves standstill the absorption that suspends at every turn, and the total time of the processing of decolouring was smaller or equal to 8 hours.
4. the method for recovering solvents of Lyocell fiber according to claim 1 is characterized in that: in step 1, the dosage of the activated carbon powder that is added is the 0.05wt%～0.10wt% of this water lotion total amount.
5. the method for recovering solvents of Lyocell fiber according to claim 1, it is characterized in that: in step 2, carry out coarse filtration with the filer element type filter, and also be coated with filter aid in advance in this cartridge surface, and in the not filtrate that decolouring is finished, also adding the filter aid of scheduled volume, this filter aid comprises diatomite and the cellulose that mixes mutually according to predetermined ratio.
6. the method for recovering solvents of Lyocell fiber according to claim 5, it is characterized in that: in step 2, be added on this not the filter aid content in the filtrate be 0.03wt%～0.05wt%, and the diatomite in this filter aid and cellulosic mixed proportion are 4: 1.
7. the method for recovering solvents of Lyocell fiber according to claim 6 is characterized in that: in step 2, the filter residue raffinate after the coarse filtration can reclaim use again after centrifugal dehydration.
8. the method for recovering solvents of Lyocell fiber according to claim 1 is characterized in that: in step 2, the filter opening aperture of the used filter material of coarse filtration is 1 μ m～100 μ m, and the filter opening aperture of the used filter material of hyperfiltration is 0.01 μ m～1 μ m.
9. the method for recovering solvents of Lyocell fiber according to claim 1 is characterized in that: in step 3, in this concentrate just-concentration of oxidation methyl beautiful jade solvent is 50wt%～55wt%.
10. the method for recovering solvents of Lyocell fiber according to claim 2 is characterized in that: used oxidant is H when step 4 is carried out refinement treatment
2O
2, used reductant is N
2H
4H
2O.
11. the method for recovering solvents of Lyocell fiber according to claim 10 is characterized in that: in step 4, the methyl beautiful jade in this concentrate and then just is oxidized to-the oxidation methyl beautiful jade under the environment of 80 ℃ ± 2 ℃ of temperature and oxidant reaction.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101514413A CN102234852B (en) | 2010-04-21 | 2010-04-21 | Solvent recovery method of Lyocell fibers |
| HK12100552.6A HK1160189A1 (en) | 2010-04-21 | 2012-01-17 | A method for recovering solvent of lyocell fiber lyocell |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101514413A CN102234852B (en) | 2010-04-21 | 2010-04-21 | Solvent recovery method of Lyocell fibers |
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| CN102234852B CN102234852B (en) | 2013-04-10 |
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| CN102516406A (en) * | 2011-11-28 | 2012-06-27 | 上海景峰制药有限公司 | Method for pre-treating sodium hyaluronate fermentation broth |
| CN103215753A (en) * | 2013-03-26 | 2013-07-24 | 聚隆纤维股份有限公司 | Method for producing bamboo pulp cellulose non-woven fabric with deodorization function |
| CN103215678A (en) * | 2013-03-26 | 2013-07-24 | 聚隆纤维股份有限公司 | Method for producing bamboo cellulose fiber with natural antibacterial, deodorizing and negative ion functions |
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| CN104711706A (en) * | 2015-03-17 | 2015-06-17 | 中国纺织科学研究院 | Lyocell fiber spinning solution waste recycling device and recycling method thereof |
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| CN105854319A (en) * | 2016-06-06 | 2016-08-17 | 北京浦仁美华节能环保科技有限公司 | MVR evaporation and concentration process of NMMO solvent |
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| CN109183199A (en) * | 2018-11-22 | 2019-01-11 | 淮安天然丝纺织科技有限公司 | A kind of NMMO solvent recovery method for concentration |
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| CN103290502A (en) * | 2012-02-24 | 2013-09-11 | 聚隆纤维股份有限公司 | Manufacture method of native cellulose fiber with flameproof function |
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| CN103290682B (en) * | 2012-03-01 | 2016-02-10 | 聚隆纤维股份有限公司 | The method for making of the native cellulose melt spraying non-woven fabrics of the resistance to combustion function of tool |
| TWI619863B (en) * | 2013-03-26 | 2018-04-01 | Method for preparing bamboo pulp cellulose non-woven fabric with deodorizing function | |
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| CN103215753A (en) * | 2013-03-26 | 2013-07-24 | 聚隆纤维股份有限公司 | Method for producing bamboo pulp cellulose non-woven fabric with deodorization function |
| CN103215678B (en) * | 2013-03-26 | 2016-03-30 | 聚隆纤维股份有限公司 | There is the method for making of natural antibacterial, deodorizing and anion function bamboo cellulose fibre |
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| CN103215678A (en) * | 2013-03-26 | 2013-07-24 | 聚隆纤维股份有限公司 | Method for producing bamboo cellulose fiber with natural antibacterial, deodorizing and negative ion functions |
| CN104711706A (en) * | 2015-03-17 | 2015-06-17 | 中国纺织科学研究院 | Lyocell fiber spinning solution waste recycling device and recycling method thereof |
| CN105607487A (en) * | 2016-03-11 | 2016-05-25 | 湖北新阳特种纤维股份有限公司 | Solvent recovery cost discharge control device, and method thereof |
| CN105854319A (en) * | 2016-06-06 | 2016-08-17 | 北京浦仁美华节能环保科技有限公司 | MVR evaporation and concentration process of NMMO solvent |
| WO2018014510A1 (en) * | 2016-07-22 | 2018-01-25 | 中国纺织科学研究院 | Method for preparing cellulose fibre |
| US11124899B2 (en) | 2016-07-22 | 2021-09-21 | China Textile Academy | Method for preparing cellulose fiber |
| CN109183199A (en) * | 2018-11-22 | 2019-01-11 | 淮安天然丝纺织科技有限公司 | A kind of NMMO solvent recovery method for concentration |
| CN111074384A (en) * | 2019-12-05 | 2020-04-28 | 中国纺织科学研究院有限公司 | Method for recovering N-methylmorpholine oxide solvent in Lyocell fiber regenerated acid and preparation method of solvent |
| CN111074384B (en) * | 2019-12-05 | 2022-07-29 | 中国纺织科学研究院有限公司 | Method for recovering N-methylmorpholine oxide solvent in Lyocell fiber regenerated acid and preparation method of solvent |
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| CN102234852B (en) | 2013-04-10 |
| HK1160189A1 (en) | 2012-08-10 |
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