CN219128871U - Recovery system of NMMO in lyocell fiber coagulating bath effluent - Google Patents

Recovery system of NMMO in lyocell fiber coagulating bath effluent Download PDF

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CN219128871U
CN219128871U CN202320111627.9U CN202320111627U CN219128871U CN 219128871 U CN219128871 U CN 219128871U CN 202320111627 U CN202320111627 U CN 202320111627U CN 219128871 U CN219128871 U CN 219128871U
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马杰
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Abstract

The utility model discloses a recovery system of NMMO in discharge liquid of a lyocell fiber coagulation bath, wherein a primary ultrafiltration device is introduced into the discharge liquid of the lyocell fiber coagulation bath, an ultrafiltration concentrated liquid outlet is connected with an inlet of a primary flocculation sedimentation device, an ultrafiltration clear liquid outlet is connected with an inlet of a primary nanofiltration device, and a nanofiltration clear liquid outlet is connected with an NMMO purification device; the primary flocculation sedimentation sediment and the nanofiltration concentrated solution outlet are connected with the inlet of the secondary flocculation sedimentation device through a mixing pipeline; the sedimentation liquid outlet of the secondary flocculation sedimentation device is connected with the filtering device, and the clear liquid outlet of the filtering device is connected to the inlet of the primary nanofiltration device. The method adopts the membrane technology and the flocculation sedimentation technology to treat the discharge liquid of the lyocell fiber coagulation bath, so that high COD impurities and salt can be removed step by step, the problem that waste water is difficult to treat in the treatment process of the discharge liquid of the lyocell fiber coagulation bath in the prior art is avoided, and the high-purity NMMO can be efficiently recovered.

Description

Recovery system of NMMO in lyocell fiber coagulating bath effluent
Technical Field
The utility model relates to the technical field of lyocell fiber production, in particular to a recovery system of NMMO in a lyocell fiber coagulation bath effluent.
Background
In the production process of the lyocell fiber, firstly, dissolving lyocell fiber pulp in high-concentration NMMO (N-methylmorpholine-N-oxide) ionic liquid, spinning the obtained mixture into pure water, separating out the lyocell fiber, and then producing the lyocell fiber product through subsequent refining, drying and other treatment processes; the liquid obtained after precipitation of lyocell fibers is called an effluent of a coagulation bath of lyocell fibers, and the concentration of NMMO in the effluent is low due to dilution of pure water. The process for recovering NMMO in the effluent of the lyocell fiber coagulating bath in the prior art mainly comprises the following steps: adding coagulant aid to flocculate and settle, filtering with microporous filter to clarify, adsorbing and purifying impurities in the solution with anion resin column and cation resin column, and concentrating purified NMMO solution to a certain concentration for reuse. When the anion-cation resin is saturated in adsorption, the anion-cation resin needs to be regenerated by sodium hydroxide and hydrochloric acid, so that a large amount of alkaline and acidic wastewater with high COD equivalent is generated. And the wastewater is neutralized to obtain wastewater with high COD equivalent, high salt content and high chromaticity. This wastewater is the most predominant source of wastewater in lyocell fiber production and is difficult to treat due to the high salt content of the wastewater in combination with the high COD equivalent.
Therefore, how to recycle NMMO in the effluent of the lyocell fiber coagulation bath in an environment-friendly way is a technical problem which needs to be solved in the field.
Disclosure of Invention
Therefore, the utility model provides a recovery system of NMMO in the effluent of the lyocell fiber coagulating bath, which aims to solve the problem that the recovery process of NMMO in the effluent of the lyocell fiber coagulating bath in the prior art generates a large amount of wastewater with high COD equivalent and high salt content and causes secondary pollution to the environment.
In order to achieve the above object, the present utility model provides the following technical solutions: a recovery system of NMMO in a lyocell fiber coagulation bath effluent, which comprises a primary ultrafiltration device, a primary flocculation sedimentation device, a primary nanofiltration device and a secondary flocculation sedimentation device;
the method comprises the steps that a raw material inlet of a primary ultrafiltration device is filled with effluent of a lyocell fiber coagulation bath, an ultrafiltration concentrated solution outlet of the primary ultrafiltration device is connected with an inlet of a primary flocculation sedimentation device, an ultrafiltration clear solution outlet of the primary ultrafiltration device is connected with an inlet of a primary nanofiltration device, and a nanofiltration clear solution outlet of the primary nanofiltration device is connected with an NMMO purification device;
the sediment outlet of the primary flocculation sedimentation device and the nanofiltration concentrated solution outlet of the primary nanofiltration device are connected with the inlet of the secondary flocculation sedimentation device through a mixing pipeline; the sedimentation liquid outlet of the secondary flocculation sedimentation device is connected with the filtering device, and the clear liquid outlet of the filtering device is connected to the inlet of the primary nanofiltration device through a circulating pipeline.
Further, NMMO purification device includes the positive and negative electrode, is provided with multiunit anion membrane group in parallel between the positive and negative electrode, and every group anion membrane group is including anion membrane and the cation membrane of relative setting, is filled with organic adsorbent between anion membrane and the cation membrane, is provided with impurity collection liquid pipeline between the adjacent anion membrane group, and positive and negative electrode one side is provided with the electrode and washes the pipeline.
Further, the organic adsorbent is an organic porous material and has a surface with a charge active group of strong polarity.
Further, the filtering precision of the primary ultrafiltration device is 1000-100000 molecular weight.
Further, the filtering precision of the first-stage nanofiltration device is 150-1000 molecular weight.
Further, polyacrylamide is added into the primary flocculation sedimentation device.
Further, the secondary flocculation sedimentation device is added with an aluminum salt flocculant and polyacrylamide.
Further, the filter device comprises a plate frame.
The utility model has the following advantages:
the utility model provides a recovery system of NMMO in a discharge liquid of a lyocell fiber coagulation bath, which comprises a primary ultrafiltration device, a primary flocculation sedimentation device, a primary nanofiltration device and a secondary flocculation sedimentation device, wherein a raw material inlet of the primary ultrafiltration device is communicated with the discharge liquid of the lyocell fiber coagulation bath, an ultrafiltration concentrated liquid outlet of the primary ultrafiltration device is connected with an inlet of the primary flocculation sedimentation device, an ultrafiltration clear liquid outlet of the primary ultrafiltration device is connected with an inlet of the primary nanofiltration device, and a nanofiltration clear liquid outlet of the primary nanofiltration device is connected with an NMMO purification device; the sediment outlet of the primary flocculation sedimentation device and the nanofiltration concentrated solution outlet of the primary nanofiltration device are connected with the inlet of the secondary flocculation sedimentation device through a mixing pipeline; the sedimentation liquid outlet of the secondary flocculation sedimentation device is connected with the filtering device, and the clear liquid outlet of the filtering device is connected to the inlet of the primary nanofiltration device through a circulating pipeline. The method has the advantages that the membrane technology is adopted to treat the discharge liquid of the lyocell fiber coagulating bath, so that high COD impurities can be removed step by step under the condition of not introducing high salt, the problem that waste water is difficult to treat in the treatment process of the discharge liquid of the lyocell fiber coagulating bath in the prior art is avoided, and high-efficiency recovery of high-purity NMMO can be realized; the membrane technology is adopted to treat the effluent of the lyocell fiber coagulating bath, so that the use of acid and alkali which pollute the environment is reduced or even avoided; the concentration of the whole process is not changed, the concentration of the used medicament is low, and the utilization rate of the medicament which is circulated in the system and not discharged is 100%; low cost, low corrosion to equipment, high COD removal rate and less secondary pollution.
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In order to more clearly illustrate the embodiments of the present utility model or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It will be apparent to those of ordinary skill in the art that the drawings in the following description are exemplary only and that other implementations can be obtained from the extensions of the drawings provided without inventive effort.
The structures, proportions, sizes, etc. shown in the present specification are shown only for the purposes of illustration and description, and are not intended to limit the scope of the utility model, which is defined by the claims, so that any structural modifications, changes in proportions, or adjustments of sizes, which do not affect the efficacy or the achievement of the present utility model, should fall within the ambit of the technical disclosure.
Fig. 1 is a schematic structural diagram of a recovery system of NMMO in a lyocell fiber coagulation bath effluent according to embodiment 1 of the present utility model;
fig. 2 is a schematic structural diagram of an NMMO purification device in a recovery system of NMMO in a lyocell fiber coagulation bath effluent according to embodiment 1 of the present utility model.
In the figure: a primary ultrafiltration device 100, a primary flocculation sedimentation device 200, a primary nanofiltration device 300, a secondary flocculation sedimentation device 400, an NMMO purification device 500 and a filtration device 600.
Detailed Description
Other advantages and advantages of the present utility model will become apparent to those skilled in the art from the following detailed description, which, by way of illustration, is to be read in connection with certain specific embodiments, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
As shown in fig. 1, an embodiment of the present utility model provides a recovery system of NMMO in a discharge liquid of a lyocell coagulation bath, which includes a primary ultrafiltration device 100, a primary flocculation sedimentation device 200, a primary nanofiltration device 300, and a secondary flocculation sedimentation device 400;
the raw material inlet of the primary ultrafiltration device 100 is filled with the effluent of the lyocell fiber coagulation bath, the ultrafiltration concentrate outlet of the primary ultrafiltration device 100 is connected with the inlet of the primary flocculation sedimentation device 200, the ultrafiltration clear liquid outlet of the primary ultrafiltration device 100 is connected with the inlet of the primary nanofiltration device 300, and the nanofiltration clear liquid outlet of the primary nanofiltration device 300 is connected with the NMMO purification device 500;
the sediment outlet of the primary flocculation sedimentation device 200 and the nanofiltration concentrated solution outlet of the primary nanofiltration device 300 are connected with the inlet of the secondary flocculation sedimentation device 400 through a mixing pipeline; the sedimentation liquid outlet of the secondary flocculation sedimentation device 400 is connected with the filtering device 600. In this embodiment, the filter device 600 includes a plate frame. The clear liquid outlet of the filtering device is connected to the inlet of the first-stage nanofiltration device 300 through a circulating pipeline, and clear liquid obtained by filtering the secondary flocculation sedimentation liquid through a plate frame is purified and then flows back to the first-stage nanofiltration device 300; and discharging solids.
In this embodiment, the filtering accuracy of the primary ultrafiltration device 100 is 1000-100000 molecular weight; the primary nanofiltration device 300 has a filtration accuracy of 150-1000 molecular weight. In this embodiment, the primary flocculation settling device 200 is added with polyacrylamide. The secondary flocculation settling device 400 is added with an aluminum salt flocculant and polyacrylamide.
The effluent of the lyocell fiber coagulation bath comprises NMMO, and further comprises colloid, macromolecular organic matters, multivalent ions, pigments, metal complexes, saccharides, monovalent salts and other impurities. In this embodiment, first stage ultrafiltration treatment is performed on the effluent of the lyocell coagulation bath to flocculate insoluble solids and colloid, then NMMO is trapped by an ultrafiltration membrane to permeate, and solids are separated to obtain clear and transparent ultrafiltrate, and the concentrate enters a first stage flocculation sedimentation device 200.
In the embodiment, the NMMO content in the effluent of the lyocell fiber coagulating bath is 150-250 g/L, the conductivity is 5-10000 us, and the effluent is yellow; the coagulant aid is Polyacrylamide (PAM). Mixing the ultrafiltration concentrated solution of the lyocell fiber coagulating bath with a coagulant aid to obtain mixed solution, flocculating and settling part of impurities in the mixed solution under the action of the coagulant aid, and discharging solid waste residues to the nanofiltration concentrated solution for recycling.
And then, overflowing the supernatant liquid after the mixed liquid obtained by the effluent liquid of the lyocell fiber coagulating bath and the coagulant aid to the primary ultrafiltration device 100 after settling, wherein the settled liquid contains a large amount of solid-phase flocculants, the primary nanofiltration concentrated liquid, an aluminum salt flocculating agent and a polyacrylamide supplementary liquid which enter the secondary flocculation settling device 400 together, and the impurities in the NMMO solution are adsorbed by utilizing the adsorption characteristic of the flocculants while flocculating and settling the primary nanofiltration concentrated liquid.
Then, the ultrafiltration clear liquid is subjected to primary nanofiltration treatment to obtain primary nanofiltration concentrated solution and primary nanofiltration clear liquid, the filtration precision of the primary nanofiltration treatment is 150-1000 molecular weight, so that the primary nanofiltration membrane entraps saccharide substances such as small-volume colloid, macromolecular organic matters, multivalent ions, pigments, metal complexes, polysaccharide and the like in the primary nanofiltration concentrated solution, and target recovery NMMO and monovalent salt enter the primary nanofiltration clear liquid, so that the NMMO is further purified and sent to a subsequent desalting and concentrating unit.
Wherein, the content of NMMO in the first-level nanofiltration concentrated solution and the first-level nanofiltration clear solution is basically consistent, and is 150-250 g/L.
In order to improve the recovery efficiency of NMMO, reduce the waste of NMMO in the treatment process, the primary nanofiltration concentrated solution needs to be subjected to flocculation sedimentation adsorption, and solid matters are removed through a plate frame filter. And the clear solution of the plate frame flows back to the first-stage nanofiltration treatment device after the flocculating agent and the coagulant aid are removed.
Table 1 below shows the NMMO content data at each stage described above.
Table 1 NMMO content in each stage
Figure BDA0004060870390000051
Figure BDA0004060870390000061
In this embodiment, as shown in fig. 2, the NMMO purification device includes positive and negative electrodes, a plurality of groups of anion-cation membrane groups are arranged in parallel between the positive and negative electrodes, each group of anion-cation membrane groups includes an anion membrane and a cation membrane which are arranged oppositely, an organic adsorbent is filled between the anion membrane and the cation membrane, the organic adsorbent is an organic porous material, the surface of the organic adsorbent is provided with a charge active group with strong polarity, an impurity collecting liquid pipeline is arranged between the adjacent anion-cation membrane groups, and an electrode flushing pipeline is arranged on one side of the positive and negative electrodes.
And (3) sending the obtained NMMO filtrate into a purification device to adsorb and desorb impurities, adsorbing the impurities in the NMMO filtrate flowing through by using an organic adsorbent filled between the anion and cation membranes in the purification device, arranging positive and negative electrodes on two sides of the anion and cation membranes, replacing the impurities adsorbed by the adsorbent by a certain amount of water to form hydrogen and hydroxyl under the action of an electric field to realize desorption, and moving the charged impurities to different electric directions through the anion and cation membranes under the action of the electric field and entering the impurity collection liquid to realize purification of NMMO solution. The voltage range of the applied direct current is 0-600V; the current range is 0-6A, the voltage is 300V, and the current is 2A.
While the utility model has been described in detail in the foregoing general description and specific examples, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the utility model and are intended to be within the scope of the utility model as claimed.

Claims (8)

1. A recovery system of NMMO in a lyocell fiber coagulation bath effluent, which is characterized by comprising a primary ultrafiltration device, a primary flocculation sedimentation device, a primary nanofiltration device and a secondary flocculation sedimentation device;
the method comprises the steps that a raw material inlet of a primary ultrafiltration device is filled with effluent of a lyocell fiber coagulation bath, an ultrafiltration concentrated solution outlet of the primary ultrafiltration device is connected with an inlet of a primary flocculation sedimentation device, an ultrafiltration clear solution outlet of the primary ultrafiltration device is connected with an inlet of a primary nanofiltration device, and a nanofiltration clear solution outlet of the primary nanofiltration device is connected with an NMMO purification device;
the sediment outlet of the primary flocculation sedimentation device and the nanofiltration concentrated solution outlet of the primary nanofiltration device are connected with the inlet of the secondary flocculation sedimentation device through a mixing pipeline; the sedimentation liquid outlet of the secondary flocculation sedimentation device is connected with the filtering device, and the clear liquid outlet of the filtering device is connected to the inlet of the primary nanofiltration device through a circulating pipeline.
2. The system for recycling NMMO in the effluent of a coagulating bath of lyocell fiber according to claim 1, wherein the NMMO purifying device comprises positive and negative electrodes, a plurality of groups of anion and cation membrane groups are arranged between the positive and negative electrodes in parallel, each group of anion and cation membrane group comprises an anion membrane and a cation membrane which are arranged oppositely, an organic adsorbent is filled between the anion membrane and the cation membrane, an impurity collecting liquid pipeline is arranged between the adjacent anion and cation membrane groups, and an electrode flushing pipeline is arranged on one side of the positive and negative electrodes.
3. The recovery system of NMMO in the effluent of a coagulation bath of lyocell fibers according to claim 2, wherein said organic adsorbent is an organic porous material and has a surface with charge-active groups of strong polarity.
4. The recovery system of NMMO in the effluent of a coagulation bath of lyocell fibers according to claim 1, wherein said primary ultrafiltration means has a filtration accuracy of 1000-100000 molecular weight.
5. The recovery system of NMMO in the effluent of a coagulation bath of lyocell fibers according to claim 1, wherein said primary nanofiltration device has a filtration accuracy of 150-1000 molecular weight.
6. A recovery system for NMMO in the effluent of a coagulation bath of lyocell fibers according to claim 1, wherein said primary flocculation settling means incorporates polyacrylamide.
7. The recovery system of NMMO in the effluent of a coagulation bath of lyocell fibers according to claim 1, wherein said secondary flocculation settling means incorporates an aluminum salt flocculant and polyacrylamide.
8. The system for recovering NMMO from a coagulating bath discharge of lyocell fibers according to claim 1, wherein the filter means comprises a frame.
CN202320111627.9U 2023-01-16 2023-01-16 Recovery system of NMMO in lyocell fiber coagulating bath effluent Active CN219128871U (en)

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