CN111334869B - A preparation system and method of lyocell spinning solution - Google Patents
A preparation system and method of lyocell spinning solution Download PDFInfo
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- CN111334869B CN111334869B CN202010254693.2A CN202010254693A CN111334869B CN 111334869 B CN111334869 B CN 111334869B CN 202010254693 A CN202010254693 A CN 202010254693A CN 111334869 B CN111334869 B CN 111334869B
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- 238000000034 method Methods 0.000 title claims abstract description 62
- 238000009987 spinning Methods 0.000 title claims abstract description 50
- 229920000433 Lyocell Polymers 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 117
- 230000008961 swelling Effects 0.000 claims abstract description 84
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims abstract description 83
- 238000005507 spraying Methods 0.000 claims description 69
- 239000007921 spray Substances 0.000 claims description 65
- 238000003756 stirring Methods 0.000 claims description 45
- 238000002156 mixing Methods 0.000 claims description 23
- 238000004090 dissolution Methods 0.000 claims description 18
- 238000007599 discharging Methods 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 abstract description 56
- 230000008569 process Effects 0.000 abstract description 39
- 229920002678 cellulose Polymers 0.000 abstract description 31
- 239000001913 cellulose Substances 0.000 abstract description 31
- 238000010009 beating Methods 0.000 abstract description 15
- 230000009286 beneficial effect Effects 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 238000010924 continuous production Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 78
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 230000002522 swelling effect Effects 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 230000005484 gravity Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229920003043 Cellulose fiber Polymers 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000007771 core particle Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241001417523 Plesiopidae Species 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WAZPLXZGZWWXDQ-UHFFFAOYSA-N 4-methyl-4-oxidomorpholin-4-ium;hydrate Chemical compound O.C[N+]1([O-])CCOCC1 WAZPLXZGZWWXDQ-UHFFFAOYSA-N 0.000 description 1
- 240000007643 Phytolacca americana Species 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 235000021395 porridge Nutrition 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Paper (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a preparation system and a preparation method of a lyocell spinning solution, wherein the system comprises a swelling device and a dissolving device, the swelling device is used for swelling dry pulp by NMMO solution, the swelling device is a rotary drum, two ends of the length direction of the rotary drum are respectively provided with a feed inlet and a discharge outlet, and the rotary drum enables materials in the rotary drum to be brought to a position close to the top from the bottom and then to freely fall back to the bottom through a rotating mode, and simultaneously conveys the swelled materials towards the discharge outlet. According to the invention, cellulose dry pulp and NMMO solution are fed into a rotary drum, the mixed materials are repeatedly beaten in the rotary drum to obtain a swelled material, and the swelled material is discharged from the rotary drum and is fed into a dissolving device to be dissolved, so that the lyocell spinning solution is obtained. The invention can treat the mixture of the whole pulp and the solvent, and the pulp and the solvent are more fully mixed in the beating process in the rotary drum. The invention preferably adopts sectional swelling, which is beneficial to reducing the number of white cores. The invention is continuous production and has low energy consumption.
Description
Technical Field
The invention relates to the technical field of lyocell fiber production, in particular to a preparation system and a preparation method of a lyocell spinning solution.
Background
Lyocell (Lyocell) is a regenerated cellulose fibre produced by a tertiary amine oxide (N-methylmorpholine-N-oxide) solvent spinning technique, and is known as green fibre in the 21 st century because of the solvent recovery.
In the process of preparing Lyocell fiber, the mixing and swelling effects of cellulose pulp in NMMO water solution with a certain concentration are key to complete dissolution of cellulose, and uneven mixing and swelling easily cause the problems of uneven cellulose solid content in solution, white core formation and the like, which are not beneficial to the subsequent spinning and other processes and seriously affect the spinning quality. The preparation of the spinning solution mainly comprises two processes of wet process and dry process. The wet method is to mix cellulose pulp with water for pulping, squeeze the obtained pulp solution for removing water, crush the pulp solution, mix the pulp solution with NMMO, and swell the pulp solution in a storage tank to fully combine the NMMO and cellulose to form cellulose pulp porridge. After swelling, the obtained gruel is conveyed into a reaction kettle (such as a thin film evaporator) for evaporation and dissolution, and a spinning solution is formed.
The Chinese patent document with the application publication number of CN 108004611A discloses a method for preparing a solvent-method cellulose fiber spinning stock solution by using dry pulp, which comprises the steps of firstly preparing an NMMO solution containing NaOH, then gradually adding pulp into the NMMO solution, uniformly mixing to obtain a pulp porridge-like mixture, evaporating and dehydrating the pulp porridge-like mixture to swell cellulose, adding a stabilizer and an antioxidant into the swelled cellulose mixture, uniformly mixing to obtain a premix, and finally dehydrating, dissolving and defoaming the premix to obtain the cellulose spinning stock solution.
The prior art belongs to the dry method for preparing the lyocell spinning solution, and is generally characterized in that (1) pulp is directly mixed with NMMO solution in a pulp state without processing such as crushing, and compared with a wet method, the process of hydraulic pulp crushing is omitted. (2) Compared with the wet process, the dry pulp and NMMO solution are mixed and then enter a thin film evaporator, so that the process flow is shortened. (3) The method reduces the energy consumption of the film evaporator, and is beneficial to improving the productivity because the water content of the dry pulp is about 6-7 percent, and compared with the wet process pulp (the water content is 50 percent), the method greatly reduces the water content brought by the dry pulp, can reduce the energy consumption of the film steam and is beneficial to improving the productivity. (4) The NMMO concentration is about 80% -84% when wet pulp is mixed with NMMO solution in wet process, and the concentration of NMMO solution required by dry pulp mixing is 75% -80%. The NMMO solution is recycled in the production process, the low-concentration NMMO solution is evaporated to obtain the high-concentration NMMO solution, and in the process, the evaporation concentration of the final NMMO solution is reduced, so that the steam unit consumption can be reduced. (5) The dry pulp is mixed with the NMMO solution, and the concentration of the NMMO solution is low, so that the pre-dissolution degree can be reduced, and the NMMO and cellulose can be fully contacted and swelled.
However, in the dry preparation technology, the cellulose/NMMO/H 2 O mixture is prepared by adopting the mechanical external force provided by a hydropulper, and in the production, the obvious white core particles can still be observed in the spinning solution prepared by the method, which also shows that the dry pulp is directly mixed with the NMMO solvent to have certain defects, and the swelling and dissolving effects are required to be improved compared with the wet method. In addition, the mixed material has certain viscosity, mechanical stirring produces strong shearing, and the damage to part of fiber morphology can also seriously affect the spinning quality.
Disclosure of Invention
In view of the above, the application provides a preparation system and a preparation method of a lyocell spinning solution, and the preparation system provided by the application can continuously produce the lyocell spinning solution, has the advantages of sufficient swelling, better quality, improved yield, reduced production cost of unit tows and contribution to popularization and application.
The invention provides a preparation system of a lyocell spinning solution, which comprises a swelling device and a dissolving device, wherein the swelling device is used for swelling dry pulp by an NMMO solution, the swelling device is a rotary drum, two ends of the length direction of the rotary drum are respectively provided with a feed inlet and a discharge outlet, and the rotary drum enables materials in the rotary drum to be brought to a position close to the top from the bottom and then to fall back to the bottom freely through a rotating mode, and simultaneously conveys the swelled materials towards the discharge outlet.
In some preferred embodiments, the rotary drum is fixed by rotating the rotary drum, wherein a rotatable material stirring part is arranged in the rotary drum, and the material stirring part drives the material to freely fall back to the bottom from the bottom to a position close to the top of the rotary drum.
In other preferred embodiments, the rotary drum is rotated by a rotary manner, namely, a shell of the rotary drum is rotated, a material stirring part rotating along with the shell of the rotary drum is arranged in the shell of the rotary drum, and the material stirring part drives materials to freely fall back to the bottom from the bottom to a position close to the top of the rotary drum.
Preferably, a spraying belt is arranged at the top of the shell of the rotary drum or near the top of the shell of the rotary drum between the feeding hole and the discharging hole, the spraying belt extends along the axial direction of the shell of the rotary drum, and NMMO solution is sprayed into the rotary drum from the spraying belt.
Preferably, both ends of the spraying belt extend to both ends of the housing of the drum, respectively.
Preferably, the rotary drum has an adjustable inclination angle of 0-10 degrees.
The embodiment of the invention provides a method for preparing a lyocell spinning solution by using the preparation system, which comprises the following steps:
rotating the rotary drum to repeatedly beating a material formed by mixing the dry pulp and the NMMO solution in the rotary drum to obtain a swelled material;
The swollen material is discharged from the drum and fed to a dissolving device for dissolution, for example, evaporation for dissolution, to obtain the lyocell spinning solution.
Preferably, the NMMO solution is added into the rotary drum through a spraying assembly, the spraying assembly forms a spraying belt extending along the axial direction of the rotary drum, the spraying belt comprises at least two spraying sections for spraying NMMO solutions with different concentrations, and the NMMO concentration sprayed by the front spraying section is lower than that of the rear spraying section in the adjacent spraying sections.
Preferably, the spraying belt comprises two spraying sections, namely a first front spraying section and a second rear spraying section, wherein the mass concentration of the first spraying section NMMO is preferably 72-78%, and the spraying temperature is preferably 75-82 ℃.
Furthermore, the mass concentration of NMMO in the second spraying section is preferably 78-84%, and the spraying temperature is preferably 72-77 ℃.
Preferably, the material is sprayed and mixed in the first spraying section for longer than the material is sprayed and mixed in the second spraying section.
The embodiment of the invention also provides the lyocell spinning solution prepared by the method and application of the lyocell spinning solution in the production of lyocell fibers.
Compared with the prior art, the invention adopts the rotary drum as main equipment for mixing and swelling dry pulp and NMMO, the rotary drum drives the materials in the rotary drum to be brought to a position close to the top from the bottom of the rotary drum through a rotating mode, and then the materials fall down freely to be beaten at the bottom of the rotary drum under the action of gravity, and the rotary drum has a certain inclination angle, so that the materials after swelling can be conveyed to a discharge hole in the rotating process. Practice has shown that this natural beating process is beneficial to the swelling effect of the dry pulp compared to the mechanical stirring process of the hydropulper. Because the mixed material is beaten at the bottom of the rotary drum through weightlessness, solvent molecules can be promoted to enter between cellulose molecular chains. The reason for this is that in the weightless state, the molecular chains of cellulose are in a stretched state, and gaps between the molecular chains are relatively uniform, which is advantageous for the solvent molecules to enter between the molecular chains. The instant material impacts the bottom, the opportunity of NMMO molecule to cellulose molecule chain gap infiltration is provided, NMMO solvent molecule smoothly enters between cellulose molecule chains, and NMMO solvent molecule and cellulose are promoted to fully swell. This significantly increases the swelling ratio of the dried pulp, especially after repeated tumbling for a long period of time, sufficient to allow for substantially uniform swelling of the solvent and cellulose. In the embodiment of the invention, the swelled material is directly sent to a dissolving device for dissolution, and the lyocell spinning solution is obtained. The invention can treat the mixture of the whole pulp and the solvent, and the pulp and the solvent are mixed more fully in the beating process, thereby being beneficial to improving the quality of products. Moreover, the invention adopts sectional spray swelling technical means in a subversion way, so that the number of white cores is further reduced.
In addition, the existing hydropulper dry swelling has the obvious defect that the discharging is difficult, and the hydropulper can only discharge through a pipeline. However, after the swelling is finished, the materials are in a viscous state and poor in fluidity, and the materials cannot be gathered together due to stirring, so that the discharging difficulty of the existing swelling implementation mode is high. In contrast, the materials in the rotary drum are gradually gathered together in the beating process due to the viscosity of the materials, and finally, the materials are in a dough-like state when reaching the discharge port, so that the discharging is easy.
Drawings
FIG. 1 is a schematic illustration of the structure of a swelling device according to some embodiments of the invention;
FIG. 2 is a schematic view of A-A of FIG. 1;
FIG. 3 is a schematic view of B-B of FIG. 1;
FIG. 4 is a schematic view showing the structure of a swelling apparatus according to other embodiments of the present invention;
FIG. 5 is a schematic view of A-A of FIG. 4;
FIG. 6 is a graph showing the effect of the swelling process of example 1 of the present invention on obtaining a dope;
FIG. 7 is a graph showing the effect of the swelling process of example 2 of the present invention on obtaining a dope.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a preparation system of a lyocell spinning solution, which comprises a swelling device and a dissolving device, wherein the swelling device is used for swelling dry pulp by an NMMO solution, the swelling device is a rotary drum, two ends of the length direction of the rotary drum are respectively provided with a feed inlet and a discharge outlet, and the rotary drum enables materials in the rotary drum to be brought to a position close to the top from the bottom and then to fall back to the bottom freely through a rotating mode, and simultaneously conveys the swelled materials towards the discharge outlet.
The preparation system provided by the invention can continuously produce the lyocell spinning solution, has better quality and low energy consumption, and is beneficial to popularization and application.
Referring to FIGS. 1-3, FIG. 1 is a schematic view of a swelling apparatus according to some embodiments of the present invention, and FIGS. 2 and 3 are schematic views of A-A and B-B, respectively. Wherein 10 is a rotary drum shell, 101 is a stirring beam, 102 is a beater, 103 is a supporting leg, 20 is a solvent spraying belt, 30 is a transmission shaft, 301 is a spoke, 302 is an inlet runner, 303 is an outlet runner, 40 is an oil cylinder, 50 is a feed inlet, 60 is a discharge outlet, and 70 is a pulse high-pressure gas inlet.
The system for preparing the lyocell spinning solution according to some embodiments of the present invention includes a swelling device shown in fig. 1, where the swelling device is a drum with a stationary casing and an internal rotating structure, and the specific structure includes a stationary drum casing 10 and a rotatable stirring beam 101 disposed therein, and preferably, a plurality of beater arms 102 are further disposed. The shell 10 is outside the rotary drum and can support the bottom through the supporting legs 103 fixed on the ground, the inner space of the rotary drum shell is used for mixing and swelling materials, the material stirring cross beam 101 is used as a material stirring part, and the material stirring cross beam is combined with the beater 102 to drive the materials to fall back to the bottom from the bottom of the rotary drum to a position close to the top.
In an embodiment of the invention, the interior of the housing 10 may define a volume and configuration suitable for spraying NMMO solution into the interior of the drum. The interior of the shell 10 forms a long cylindrical mixing cavity, the length and caliber of the mixing cavity are customized according to the actual process requirement, for example, the length can be 10 meters, the length of the shell can reach tens of meters in practice, even more, and the diameter can be 1m, 2m and the like. One end of the rotary drum in the length direction is a feeding end (one end of a feeding port), and the other end is a discharging end (one end of a discharging port).
And, a plurality of solvent spraying ports are transversely (i.e. lengthwise) arranged at the top or near the top of the drum shell 10, and solvent spraying belts 20 are formed by extending and arranging along the axial direction of the drum shell, and are used for spraying solvent between a feeding end and a discharging end, namely NMMO solvent is sprayed into the drum from the spraying belts. Preferably, both ends of the spraying belt extend to both ends of the drum housing, respectively. When spraying the solvent, the spraying belt can be divided into a plurality of spraying sections according to different concentrations of the spraying solvent, namely, the spraying area for spraying the solvent with the same concentration is regarded as one spraying section. The spray belt of the invention can form at least two spray sections for spraying solvents with different concentrations.
The swelling device is used for swelling the dry pulp by the NMMO solution, the feeding modes of the NMMO solution and the dry pulp are not particularly limited, and the NMMO solution and the dry pulp can enter the swelling device from a feed inlet. Wherein the NMMO solution can be introduced into the drum through a spray assembly. In the embodiment of the invention, the spray assembly is various in form, and the specification, the sectional distance and the like of each solvent spray port are not particularly limited. The top of the rotary drum shell is provided with a row of long and narrow spray holes along the head and the tail of the rotary drum, a first spray section and a second spray section are divided according to the sectional spray of solvents with different concentrations, or a row of spray nozzles are arranged at the top of the rotary drum corresponding to the spray ports, the spray nozzles at the feeding end spray one concentration solvent, and the spray nozzles at the discharging end spray the other concentration solvent.
Furthermore, the outside of the drum may be provided with a temperature regulating jacket or electric tracing equipment (not shown in fig. 1) for independent sectional control of the temperature. Lifting equipment can be arranged below one end of the rotary drum feeding port, one end of the rotary drum feeding port is controlled to lift relative to one end of the rotary drum discharging port, and the mixing and swelling time is controlled by adjusting the conveying speed of materials in the rotary drum through adjusting the inclination angle.
In the above embodiment of the present invention, the drum shell 10 is not moving, the transmission shaft 30 (driven by an external motor) drives the spoke 301 to rotate, the spoke 301 drives the outlet runner 303 to rotate, the runner 303 drives the stirring beam 101 to rotate, the left end of the stirring beam 101 is fixed on the inlet runner 302, so as to ensure that the stirring beam 101 is clung to the inner wall of the drum shell to reliably revolve, the stirring beam 101 drives the material to rise along the inner wall of the shell, the material falls under the action of gravity, and the repeated beating is performed to realize the mixing and swelling of the material, and the material is slowly conveyed backwards. Because the suspended matter materials have certain viscosity, the materials can be gathered together in the rotating process, like a dough, the suspended matter materials are continuously beaten and gathered after being crushed. In this beating process, the pulp and solvent are more thoroughly mixed. If the materials are mixed only by stirring blades and other parts, the uniformity of the materials is poor, and the swelling effect is poor due to a plurality of stirring dead angles. The invention makes pulp and solvent fully mixed and swelled by using a beating mode, has better effect than that of blade stirring, and has no dead angle in the rotary drum, thereby realizing even swelling.
The embodiment of the invention has no special limitation on structural designs of the rotary drum shell, the stirring part and the like, and can realize the stirring and beating functions. Specifically, a plurality of short rod-shaped protruding parts (i.e. a beater 102) are arranged in the rotary drum, the beater 102 is directly fixed on a rotary drum stirring beam 101, and the stirring beam 101 drives the beater 102, so that materials can be smoothly stirred to a higher height, and the beating effect is improved. Further, the oil cylinder 40 drives the housing 10 to be lifted and lowered. The feed inlet 50 and the discharge outlet 60 are respectively arranged at two ends of the length direction of the rotary drum, pulp is fed into the rotary drum from the feed inlet 50, and is discharged from the discharge outlet 60, one end of the discharge outlet is also provided with a pulse high-pressure gas inlet 70, and when the discharge outlet is blocked by materials, the gas inlet 70 sprays high-pressure gas to break up the blocked material mass, so that the materials are smoothly output.
The inclination angle of the rotary drum is adjustable in the embodiment of the invention, and is used for adjusting the material conveying rate, for example, between more than 0 and less than 10 degrees. In the invention, the beater arranged in the rotary drum is not only beneficial to mixing and swelling, but also can enable materials to be conveyed backwards under an inclined condition. The beater is provided with a plurality of short bar-shaped bulges which are spaced from each other, the overall shape is preferably consistent, one end of the beater, which is far away from the rotary drum, can be any shape such as square heads, round heads, pointed heads and the like, and the number of the beater is not particularly limited. Preferably, the wedge-shaped pointed beater is used to reduce the risk of material being squeezed between the projection and the inner wall of the drum housing. In a preferred embodiment of the present invention, the plurality of raised elements (beater 102) are fixed to the respective toggle beam 101. In addition, the transmission structure of the spoke, the rotating wheel and the like is not particularly limited, and a specific structure shown in fig. 3 can be adopted, and other designs can also be adopted.
In the preparation system provided by the embodiment of the invention, the rotary drum of the swelling device rotates at a certain inclination angle, so that the materials in the rotary drum are brought to a position close to the top from the bottom and then fall back to the bottom freely, meanwhile, the solvent is sprayed in sections, the swelling is finished, and the swelled materials are conveyed to the dissolving device. The dissolution device is a reaction kettle communicated with a discharge hole of the swelling device, and the dissolution device is not particularly limited in the invention, for example, a thin film evaporator well known to the person skilled in the art. The swelled material is dissolved in a reaction kettle, and the obtained spinning solution is sent to a spinning machine for spinning, so as to produce Lyocell fibers.
The preparation system provided by the invention can continuously produce the lyocell spinning solution, has sufficient swelling, better quality, improved yield and reduced production cost of unit tows.
In other embodiments of the present invention, the swelling means is schematically shown in FIGS. 4-5. Wherein 11 is a drum shell, 111 is a stirring beam, 112 is a beater, 31 is a driving assembly, 51 is a feed inlet, and 61 is a discharge outlet.
The system for preparing the lyocell spinning solution according to other embodiments of the present invention includes a swelling device shown in fig. 4, where the swelling device is a rotary drum of a shell rotation structure type, and the specific structure includes a rotatable drum shell 11 and a stirring beam 111 disposed therein and rotating therewith, and preferably, a plurality of beater arms 112 are further disposed. The drum shell 11 rotates, and a material stirring beam 111 fixed on the inner wall of the shell drives the material to beat in the cavity, namely, the material is driven to freely fall back to the bottom from the bottom of the drum to a position close to the top and is slowly conveyed backwards.
In the embodiment of the invention, the inner part of the shell 11 is provided with a mixing cavity, the length and caliber of the mixing cavity are customized according to the actual process requirement, for example, the length can be 10 meters, the length of the shell can reach tens of meters in practice, and even longer, the diameter can be 1m, 2m and the like. One end of the rotary drum in the length direction is a feeding end (one end of a feeding port), and the other end is a discharging end (one end of a discharging port). A spray pipe can extend into the mixing cavity of the rotary drum between the feeding port and the discharging port, the spray pipe is provided with a row of spray nozzles, the spray nozzles form a spray belt, and the spray belt extends along the axial direction of the shell of the rotary drum and can extend to two ends; the NMMO solution is sprayed from the spray belt into the drum. Or both solvent and pulp enter the swelling device from the feed inlet (as shown in fig. 4).
In these embodiments of the present invention, the drum housing 11 is driven to rotate by a driving assembly 31 (the driving assembly 31 is a conventional transmission mechanism composed of a motor and a gear), and a stirring beam 111 fixed on the housing drives the material to beat in the cavity, so that the repeated beating realizes the mixing, swelling and slow backward conveying of the material. Preferably, a plurality of short rod-shaped protruding parts (i.e. a beater 112) are arranged in the rotary drum, the beater 112 is directly fixed on the rotary drum stirring beam 111, and the stirring beam 111 and the beater 112 rotate along with the shell, so that the stirring effect is enhanced. The two ends of the length direction of the rotary drum are respectively provided with a feed inlet 51 and a discharge outlet 61, pulp and NMMO solution are fed into the rotary drum from the feed inlet 51, and the swelled materials are discharged from the discharge outlet 61.
The inclination angle of the drum in the above embodiments of the present invention can also be adjusted, for example, between more than 0 and less than 10 °. In the invention, the beater arranged in the rotary drum is not only beneficial to mixing and swelling, but also can enable materials to be conveyed backwards under an inclined condition. The beater is provided with a plurality of short bar-shaped bulges which are spaced from each other, the overall shape is preferably consistent, one end of the beater, which is far away from the rotary drum, can be any shape such as square heads, round heads, pointed heads and the like, and the number of the beater is not particularly limited. In the preferred embodiment of the present invention, the plurality of raised members (punches 112) are fixed to the respective kick-out beams 111, are uniformly distributed along the circumference of the drum, as shown in fig. 5 for 6 sets of punches, and are arranged in longitudinal rows at uniform intervals. Furthermore, the present invention is not particularly limited to the drive assembly.
The dry pulp is swelled by the swelling device and enters the dissolving device, wherein the dissolving device is a reaction kettle communicated with a discharge hole of the swelling device. The present invention is not particularly limited to the dissolution apparatus, such as a thin film evaporator well known to those skilled in the art. The swelled material is dissolved in a reaction kettle, and the obtained spinning solution is sent to a spinning machine for spinning, so as to produce Lyocell fibers.
The invention adopts the rotary drum as main equipment for mixing and swelling dry pulp and NMMO, and the rotary drum drives the internal materials to rotate through the rotating working process, and can be brought to a position close to the top from the bottom, and can fall freely under the action of gravity to strike the bottom. The invention can treat the mixture of the whole pulp and the solvent, and the pulp and the solvent are mixed more fully in the beating process, so that the spinning solution and the fiber with better quality can be obtained.
The embodiment of the invention provides a method for preparing a lyocell spinning solution by using the preparation system, which comprises the following steps:
rotating the rotary drum to repeatedly beating a material formed by mixing the dry pulp and the NMMO solution in the rotary drum to obtain a swelled material;
Discharging the swelled material from the rotary drum, and feeding the swelled material into a dissolving device for dissolution to obtain the lyocell spinning solution.
The invention can continuously produce the lyocell spinning solution, improves the quality, reduces the energy consumption and is suitable for large-scale production.
The embodiment of the invention adopts a dry preparation process, takes cellulose dry pulp as a raw material, and the water content of the dry pulp is about 6-7%. The water quantity brought by the dry pulp is lower, so that the energy consumption of the film steam can be reduced, and the improvement of the productivity is facilitated. According to some embodiments of the invention, the dry pulp is fed from a feed inlet at a feed rate of 1.0-1.5 t/min. In addition, the NMMO solution is preferably added into the rotary drum through the spraying assembly, the spraying assembly forms a spraying belt extending along the axial direction of the rotary drum, namely pulp and the NMMO solution are added into the swelling device to be mixed and swelled, and the swelled material is obtained.
Wherein, the structure and the like of the swelling device are as described above. For example, the inclination angle of the swelling device is adjustable between more than 0 and less than 10 degrees, and the rotation frequency of the rotary drum is determined according to actual process requirements and can be 3-5rpm for example. The pulp feed and the sprayed NMMO solvent should be maintained in a ratio which can be determined according to the actual process requirements. For example, the NMMO/cellulose mass ratio in the resulting swollen material can be determined to be 6.4 (the proportioning relationship can also be changed according to the process requirements), and then the pulp feed rate and the solvent spray rate can be determined according to this ratio.
According to the embodiment of the invention, the poking beam in the rotary drum can poke materials to rise, and when the materials are close to the top of the rotary drum, the materials fall back to the bottom of the rotary drum due to self gravity, so that the state is maintained, and the repeated movement is continued. Preferably, when spraying NMMO solvent, at least two spraying sections for spraying different concentrations are formed on the spraying belt, and the NMMO concentration sprayed by the front spraying section is lower than that sprayed by the rear spraying section in the adjacent spraying sections. The invention preferably adopts a segmented spray solvent, for example, the solvent is divided into two segments, and a spray mode of three segments or more can be adopted, and the control of the mixing time proportion of each segment can be determined by the length proportion of each segment, namely, the spray time of each segment is in proportional relation with the length.
In some embodiments of the invention, the spray zone comprises two spray segments, a first spray segment in front and a second spray segment in back, respectively. The mass concentration of the NMMO in the first spraying section is preferably 72-78%, and the spraying temperature is preferably 75-82 ℃. The mass concentration of NMMO in the second spraying section is preferably 78-84%, and the spraying temperature is preferably 72-77 ℃. In other embodiments of the invention, the spray zone spray concentration is uniform.
NMMO is very soluble in water, is easily soluble in polar organic solvents such as ethanol, methanol and the like, has higher solubility in hot acetone and benzene, is insoluble in common organic solvents, can be combined with 1-4 water molecules, and has stable chemical properties at room temperature. The NMMO aqueous solution is a high-quality solvent for cellulose, but the cellulose has the characteristics of high crystallinity and a plurality of hydrogen bonds, so that the cellulose is difficult to be successfully dissolved in the concentrated NMMO aqueous solution. In the dry process, the mass concentration of NMMO solution required for dry pulp mixing is typically between 75% and 80%. The NMMO solution is recycled in the production process, the low-concentration NMMO solution is evaporated to obtain the high-concentration NMMO solution, and in the process, the evaporation concentration of the final NMMO solution is reduced, so that the steam unit consumption can be reduced.
For the segmented spraying NMMO solution, solvents with different concentrations can be added in sequence in segments, namely, a front-end nozzle sprays one concentration solvent, a rear-end nozzle sprays the other concentration solvent, and the invention preferably has the advantage that the front spraying concentration is lower than the rear spraying concentration, and has positive effect on swelling. The NMMO solution with lower concentration and higher concentration is added firstly, and the advantages are that pulp is in NMMO solution environment after the NMMO solution with lower concentration is added firstly, partial swelling occurs in the pulp, and the high NMMO solution is added under the buffer action condition, so that the degree of gel formed by the NMMO solvent to the pulp by partial dissolution is weakened, and the gel can prevent the sufficient swelling of cellulose and is unexpected.
Preferably, the material is sprayed and mixed in the first spraying section for longer than the material is sprayed and mixed in the second spraying section. In the embodiment of the invention, the time for controlling the conveying process of the pulp in the rotary drum is also a key parameter, and too fast conveying speed means too short a swelling time of the pulp, so that the swelling is difficult to reach a sufficient degree, and too long a conveying time increases the cost and reduces the production efficiency.
For example, some embodiments of the present invention control the swelling time to 150 minutes (i.e., the time from entry of pulp into the drum to exit of pulp from the drum). This time is related to the length, inner diameter, rotational speed and tilt angle of the drum, since length and inner diameter are fixed parameters (of course, the drum can be changed for adjustment), the present invention can control the swelling time by adjusting tilt angle and rotational speed.
After swelling, the swollen materials are directly sent to a dissolving device such as a reaction kettle and the like for dissolving to prepare the Lyocell spinning solution.
The dissolution device, such as a thin film evaporator, process conditions, etc., is not particularly limited, and the evaporation dissolution process commonly used in the art may be adopted. In the embodiment of the invention, the mass ratio of NMMO/cellulose in the obtained cellulose suspension is 6-7, for example 6.4.
The invention also provides application of the Lyocell spinning solution obtained by the preparation method in the production of Lyocell fibers, namely, the obtained Lyocell spinning solution is conveyed to a spinning machine for conventional spinning, and the Lyocell fibers are produced.
The method has good swelling effect and low white core quantity. In addition, the invention has simple process flow and low energy consumption, and is suitable for large-scale production.
In order to further understand the present application, the preparation system and method of lyocell spinning solution provided by the present application will be specifically described with reference to examples. It is to be understood that these examples are provided for the purpose of illustrating the details of the application and the particular process and are not intended to limit the scope of the application, which is defined solely by the claims, but not by the way of limitation.
Example 1
1. Main raw materials
1. NMMO aqueous solution as solvent was 75% and 83% respectively;
2. pulp raw material wood pulp (south Africa Sappi pulp, water content 6%, polymerization degree 520).
2. The main equipment comprises:
1. The rotary drum with the structure shown in fig. 1-3, namely the shell is fixed, and the material stirring parts such as the material stirring cross beam and the like rotate along the inner wall of the shell, so that the aim of scraping materials on the inner wall of the shell is achieved. The length of the drum is 20 m and the diameter is 2 m.
The top of the shell of the rotary drum is provided with a spray belt, the first spray section (namely the front half part) sprays solvent with concentration of 75%, the second spray section (namely the rear half part) sprays solvent with concentration of 83%, and the length ratio of the two spray sections is 1:1.
2. The model of the swelling ratio test equipment is DD5M low-speed centrifuge.
3. Description of the embodiments
Continuously conveying pulp to a feed inlet of the rotary drum, and conveying the pulp entering the rotary drum backwards along the rotary drum under the stirring of a rotary drum stirring part, wherein the coiling speed of a stirring beam is 3-5rpm;
The spraying belt at the top of the rotary drum sprays solvent into the rotary drum according to preset concentration (namely, the front half part sprays solvent with concentration of 75 percent and the rear half part sprays solvent with concentration of 83 percent), and the whole spraying process is not stopped.
In production, the pulp is continuously put into the rotary drum at a feeding speed of 1.06t/min, and the rotary drum keeps normal and stable operation. Thus, the pulp feed rate of 1.06t/min corresponds to a rate of injection of pure NMMO of 6.4t/min (satisfying the NMMO/cellulose=6.4 relationship). In the operation, the front half part of the spraying belt is set to uniformly spray 3.2t/min, and the rear half part of the spraying belt is set to uniformly spray 3.2t/min. According to the spray concentration of each part, the spray speed of the solvent with the spray concentration of 75% in the front half of the spray belt is 4.27t/min, and the spray speed of the solvent with the spray concentration of 83% in the rear half of the spray belt is 3.86t/min. The spraying temperature of the front half part is 75-82 ℃, and the spraying temperature of the rear half part is 72-77 ℃. As mentioned above, the solvent is sprayed in the form of a spray belt, which is necessary to effectively avoid the problem that the solvent is not mixed with the pulp locally due to concentrated spraying. The mixed solvent can flow out backwards quickly when sprayed a little less, so that the swelling process of cellulose cannot be completed.
In this operation, the swelling time was controlled to 150 minutes (i.e., the time from entry of pulp into the drum to exit of pulp from the drum).
Through the operation, the finally swelled material can directly enter a reaction kettle for evaporation and dissolution.
3 Parts of the materials swelled by the operation are taken, each 2kg of materials are taken, and the swelling ratio is tested.
The first centrifuged material weighed 1.93kg, the second centrifuged material weighed 1.92kg, and the third centrifuged material weighed 1.94kg. Thus, the corresponding swelling ratios were 96.5%, 96.0% and 97.0%, respectively, and the average swelling ratio was 96.65%.
The swelling rate of the prior art is generally 88-92%, such as swelling materials (suspension) prepared by a wet method. It can be seen that the cellulose suspensions prepared using the technique of the present application have excellent swelling effects.
In addition, after the materials with poor swelling effect are evaporated and dissolved to prepare spinning stock solution, more white cores still remain in the solution. Based on this, in order to further demonstrate the above-mentioned swelling effect, in the dope obtained in this example, 1 part of the dope was taken out, and placed under an environment excellent in sunlight, and observed with a magnifying glass at a magnification of 5 times, white core particles were hardly found except for a small amount of bubbles (see fig. 6). This is almost impossible with conventional dissolution processes.
Example 2
1. Main raw materials
1. An aqueous NMMO solution at a concentration of 80%;
2. pulp raw material wood pulp (south Africa Sappi pulp, water content 6%, polymerization degree 520).
2. Main equipment
1. The NMMO solvent and pulp are conveyed into the rotary drum from the pulp inlet by adopting the rotary drum (stirring members such as a stirring beam are directly fixed on the inner wall of the shell of the rotary drum, and the shell of the rotary drum is driven by an external bearing and a power assembly to rotate) as shown in fig. 4-5. The length of the drum is 20m and the diameter is 2 m.
2. The model of the swelling ratio test equipment is DD5M low-speed centrifuge.
3. Description of the embodiments
In production, the pulp is continuously put into a rotary drum at a feeding speed of 1.06t/min, the rotary drum keeps normal and stable operation, and the rotary drum rotation speed is 3-5rpm. Thus, the pulp feed rate of 1.06t/min corresponds to a rate of injection of pure NMMO of 6.4t/min (satisfying the NMMO/cellulose=6.4 relationship). In this operation, NMMO concentration was 80% and the injection rate of aqueous NMMO solution was 8.0t/min. Solvent NMMO was all fed from the feed inlet at a rate of 8t/min at 78 degrees Celsius.
In this operation, the swelling time was controlled to 150 minutes (i.e., the time from entry of pulp into the drum to exit of pulp from the drum).
Through the operation, the finally swelled material can directly enter a reaction kettle for evaporation and dissolution.
2Kg of each of 3 parts of the materials swelled by the operation are taken and the swelling ratio is tested.
The first centrifuged material had a weight of 1.89kg, the second centrifuged material had a weight of 1.90kg, and the third centrifuged material had a weight of 1.89kg. Thus, the corresponding swelling ratios were 94.7%, 95.0% and 94.7%, respectively, and the average swelling ratio was 94.80%.
The swelling rate of the prior art is generally 88-92%, and compared with the prior art, the swelled material obtained by the operation has excellent swelling effect.
In addition, after the materials with poor swelling effect are evaporated and dissolved to prepare spinning stock solution, more white cores still remain in the solution. Based on this, in order to further demonstrate the above-mentioned swelling effect, 1 part of the stock solution was taken out from the solution dissolved by the present operation, and placed under an environment excellent in sunlight, and observed with a magnifying glass at a magnification of 5 times, substantially no white core particles were found (see fig. 7). This is almost impossible with conventional dissolution processes.
The test proves that the pulp and the solvent form a mixed material, and the solvent and the pulp can be promoted to be fully swelled by repeated beating under the self gravity, probably because the beating process can lead the solvent to repeatedly try to enter the molecular gap of the pulp from different angles, and the pulp is uniform and soft, thereby avoiding the external force from tearing and pulling and affecting the physical and chemical properties of cellulose.
In addition, the use of a drum-type swelling device has the great advantage of greatly increasing the single line energy yield of the cellulose fibers. In the prior art, whether dry or other wet processes mentioned in the background, it is necessary to use a hydraulic pulper or a pulping device like an in-water pulper, which is not only small in volume, but also directly agitates the material by rotation of the blades, which determines a limited weight of pulp added. Currently, annual single-line productivity is difficult to break through by 2 ten thousand tons. By adopting the technology of the invention, single-line productivity can be greatly improved, and the annual productivity of hundreds of thousands or more can be achieved. The method is unexpected in the prior art, improves single-line productivity, undoubtedly reduces the product cost, and creates a wide prospect for product popularization.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications to these embodiments can be made by those skilled in the art without departing from the technical principles of the present invention, and these modifications should also be considered as the scope of the present invention.
Claims (6)
1. A preparation system of lyocell spinning solution comprises a swelling device and a dissolving device, wherein dry pulp is swelled by the swelling device and then enters the dissolving device to be dissolved into spinning solution, the swelling device is used for swelling the dry pulp by NMMO solution, the preparation system is characterized in that the swelling device is a rotary drum, the two ends of the length direction of the rotary drum are respectively provided with a feed inlet and a discharge outlet, the rotary drum is provided with an inclined angle relative to the horizontal direction, and materials in the rotary drum are brought to a position close to the top from the bottom and then freely fall back to the bottom through a rotating mode, and simultaneously the swollen materials are conveyed towards the discharge outlet;
A spraying belt is arranged at the top of the shell of the rotary drum or near the top of the shell of the rotary drum and extends along the axial direction of the shell of the rotary drum, and NMMO solution is sprayed into the rotary drum from the spraying belt;
The rotary drum is characterized in that a shell of the rotary drum is fixed, a rotatable material stirring part is arranged in the shell of the rotary drum, the material stirring part is a material stirring cross beam fixedly provided with a plurality of beater arms, the beater arms are driven by the material stirring cross beam, and the material stirring part drives materials to freely fall back to the bottom from the bottom of the rotary drum to a position close to the top;
Or the rotary drum is characterized in that the shell of the rotary drum rotates, a material stirring part rotating along with the rotary drum is arranged in the shell of the rotary drum, the material stirring part is a material stirring cross beam fixedly provided with a plurality of beater arms, the material stirring cross beam and the beater arms rotate along with the shell, and the material stirring part drives materials to freely fall back to the bottom from the bottom of the rotary drum to a position close to the top.
2. The manufacturing system of claim 1, wherein the shower belt ends extend to respective ends of the housing of the drum.
3. The manufacturing system of claim 2, wherein the drum has an adjustable tilt angle of 0-10 °.
4. A method for preparing lyocell spinning solution using the preparation system according to any one of claims 1 to 3, comprising the steps of:
The method comprises the steps of adding dry pulp and NMMO solution into a rotary drum, rotating the rotary drum to repeatedly beat a material formed by mixing the dry pulp and the NMMO solution in the rotary drum to obtain a swelled material, adding the NMMO solution into the rotary drum through a spraying assembly, and forming a spraying belt extending along the axial direction of the rotary drum through the spraying assembly;
Discharging the swelled material from the rotary drum, and feeding the swelled material into a dissolving device for dissolution to obtain the lyocell spinning solution.
5. The preparation method of the spray belt according to claim 4, wherein the spray belt comprises two spray sections, namely a first front spray section and a second rear spray section, the mass concentration of the first spray section NMMO is 72-78%, and the spray temperature is 75-82 ℃.
6. The method of claim 5, wherein the material is spray mixed in the first spray section for a longer period of time than in the second spray section.
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| CN114016141B (en) * | 2021-12-09 | 2023-03-21 | 赛得利(常州)纤维有限公司 | Method for preparing fiber spinning solution by direct dissolution method |
| CN116145449A (en) * | 2022-12-29 | 2023-05-23 | 唐山三友集团兴达化纤有限公司 | Lyocell fiber pulp fluffing liquid and preparation method thereof |
| CN118497906A (en) * | 2023-02-23 | 2024-08-16 | 四川丝丽雅纤维科技有限公司 | Preparation method of glue solution suitable for lyocell fibers |
| CN120738775B (en) * | 2025-08-29 | 2025-11-14 | 上海里奥纤维企业发展有限公司 | Heating circulation system and heating circulation method for lyocell fiber production |
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