CN112779612A - Efficient production and manufacturing method and device for lyocell fibers - Google Patents
Efficient production and manufacturing method and device for lyocell fibers Download PDFInfo
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- CN112779612A CN112779612A CN202110019459.6A CN202110019459A CN112779612A CN 112779612 A CN112779612 A CN 112779612A CN 202110019459 A CN202110019459 A CN 202110019459A CN 112779612 A CN112779612 A CN 112779612A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 34
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- 238000009987 spinning Methods 0.000 claims abstract description 69
- 238000000034 method Methods 0.000 claims abstract description 60
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Images
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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- 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
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D13/00—Complete machines for producing artificial threads
-
- 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
-
- 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
-
- 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)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention belongs to the technical field of fiber production and manufacture, and relates to a method and equipment for efficiently producing and manufacturing lyocell fibers. Adding the spinning solution prepared by dissolving into a screw extruder, shearing and dissolving at a certain temperature, then spraying out after filtering, a static mixer, a metering pump and a spinning assembly, directionally stretching the sprayed tows in the air, then entering a coagulating bath, reducing the concentration of the solvent due to solvent diffusion, separating out cellulose, coagulating and forming the tows, and then carrying out water washing, oiling and drying post-treatment processes to inspect and pack to prepare the short fibers.
Description
Technical Field
The invention belongs to the technical field of fiber production and manufacture, and relates to a method and equipment for efficiently producing and manufacturing lyocell fibers.
Background
Cellulose is a main component of plant cell walls, can be derived from trees, cotton, hemp and other plants, and is widely distributed, inexhaustible and inexhaustible in nature. Generally, most organic substances containing hydroxyl groups are readily soluble in water, such as alcohol, glucose, and the like, but cellulose is insoluble in water and most organic solvents. The molecular weight of cellulose is generally large, and is hundreds of low, and is tens of thousands of high, and intramolecular and intermolecular hydrogen bonds are easily formed, and the acting force covers the affinity action of a part of hydroxyl groups to water, so that the cellulose is insoluble in water or common organic solvents.
As petroleum resources are gradually reduced and influenced by factors such as the consciousness of advocating nature, health and environmental protection, people gradually turn to regenerated cellulose fibers. Lyocell fiber (Lyocell) is commonly called as "velveteen", is made from natural plant fiber as a raw material, is known in the middle of the 90 s of the 20 th century, and is known as the most valuable product in artificial fiber history in the last half century. The Lyocell fiber has various excellent performances of natural fiber and synthetic fiber, Lyocell is green fiber, raw materials of Lyocell are inexhaustible cellulose in nature, a production process has no chemical reaction, a used solvent is nontoxic, the recovery rate of the solvent can reach more than 99%, and the production process is green and environment-friendly, so the Lyocell fiber is called as '21 st century green fiber'.
The lyocell fiber production technology is a relatively mature solvent method regenerated cellulose fiber industrialized production technology at present, and domestic and foreign enterprises, colleges and scientific research institutions have more relevant researches, but relatively few lyocell fiber complete production technologies can be really mastered, and as a foreign enterprise which monopolizes the lyocell fiber production technology for a long time, the lyocell fiber production technology mastered a series of most advanced lyocell fiber relevant technologies such as lyocell fiber production equipment and production technology, breaks through the blockade of the production technology and equipment by the foreign enterprise, develops a mature and reliable lyocell fiber production technology and equipment, and can powerfully promote the development of the field of new fiber materials.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method and equipment for efficiently producing and manufacturing lyocell fibers.
A high-efficiency production and manufacturing device of lyocell fibers comprises a separating machine or a traction machine connected with a coarse powder machine, a coarse powder machine connected with a fine powder machine through a fan, a fine powder machine connected with a bin, a weighing belt device connected with a premixer, a premixer connected with a mixing bin, a thin film evaporator connected with the mixing bin through a screw pump, an evaporator connected with a discharge pump connected with a glue solution filter, a spinning metering pump connected with a spinning assembly, a coagulating bath connected with a coagulating bath tank, a coagulating bath tank and a winding machine respectively connected with the coagulating bath tank, a rinsing water tank and a clarifying tank respectively connected with the coagulating bath tank, a clarifying tank connected with an air attachment device, an air attachment device connected with an anion exchange resin device, an anion exchange resin device connected with a cation exchange resin device, a cation exchange resin device connected with the evaporator, and an evaporator connected with a concentrated NMMO tank, the concentrated NMMO jar is connected the mixing bunker, and the winder connects three-section rinsing machine and washes the water pitcher respectively, and washing basin, cutter and washing water pitcher are connected respectively to three-section rinsing machine, and the fine groove is given in the cutter connection, gives the fine groove and connects the refiner, and the refiner is connected device, washing basin and the scouring basin of oiling respectively, and drying device is connected to the device of oiling, and packing apparatus is connected to drying device.
The coagulation bath barrel is in circulating connection with the coagulation bath, and the water washing tank is in circulating connection with the refiner.
A high-efficiency production method of lyocell fibers comprises the following steps: adding the spinning solution prepared by dissolving into a screw extruder, shearing and dissolving at a certain temperature, then spraying out after filtering, a static mixer, a metering pump and a spinning assembly, directionally stretching the sprayed tows in the air, then entering a coagulating bath, reducing the concentration of the solvent due to solvent diffusion, separating out cellulose, coagulating and forming the tows, and then carrying out post-treatment procedures of washing, oiling, drying and the like to inspect and pack to prepare the short fibers.
Also comprises the following steps:
step 1), solvent selection:
NMMO containing a certain amount of water is selected, the concentration of NMMO solvent is 65-85%, and the solvent temperature is 55-85 ℃. The water concentration of a certain amount is 65-85%, namely the water content is 15-35%.
Step 2), pulp treatment:
conveying the pulp to a strong shredding machine set through a separating machine or a tractor, carrying out secondary fine crushing treatment through a fine crusher after coarse crushing, filtering the fine crushed pulp through a filter plate, and then feeding the fine crushed pulp into a storage bin, wherein the large pulp separated by the filter plate returns to the fine crushing for recycling treatment.
Step 3), NMMO impregnation:
the pulp entering the bin and finely crushed falls to a belt weigher through a star discharger, the weighed pulp is conveyed to a pre-mixer through a belt, a solvent is sprayed into the pre-mixer, the materials and the solvent are fully mixed to generate porridge, and the porridge is conveyed to a mixed porridge tank.
Step 4), dissolving pulp:
dissolving the crushed pulp to obtain a plastic cellulose solution, adding excessive water to the raw material at the beginning of dissolving, and gradually removing water until NMMO and H2The proportion of O meets the requirements: the concentration is 65-85%.
Step 5), fiber forming and post-treatment:
the plastic cellulose solution is delivered to the spinning section by a discharge pump through a delivery pipeline, the spinning stock solution is quantitatively delivered to a spinning assembly by a metering pump, extruded by a spinneret orifice and then enters a coagulating bath through a section of air gap. The filament and the coagulating liquid are subjected to convective diffusion mass transfer in the coagulating bath, and the coagulating liquid enters a recovery cycle. The spinning post-treatment comprises the steps of drawing by a winder, washing by water, cutting, refining and drying, and the spinning post-treatment is carried out in a coagulating bath to obtain fibers.
Step 6), solvent recovery:
air-float filtering, decolouring, ion exchange and flash evaporation concentration to obtain pure low-concentration NMMO solution, and concentrating the recovered solution in multi-effect flash evaporation system, and multi-stage evaporating the solution in flash evaporation tank under negative pressure to remove water, so as to obtain 80-84% NMMO solution.
The core of the spinning in the method of the invention is as follows:
temperature of the spinning solution: the continuous vacuum film pushes the interior of the reactor to be vacuumized, the reactor adopts a jacket type heating mode, the jacket layer is divided into three independent circulating heating areas which are named as the upper part, the middle part and the lower part of the reactor respectively, slurry is added to the upper part, and the lower part is discharged. The heating temperature of the upper part of the reactor is controlled to be 45-65 ℃, the temperature of the middle part is controlled to be 65-85 ℃, the temperature of the lower part is controlled to be 85-105 ℃, and the vacuum degree in the reactor is controlled to be-85-125 bar. The plastic cellulose true solution prepared by the film evaporator is delivered to a spinning section by a delivery pump through a delivery pipeline, the requirement on temperature stability in the delivery process is very high, and the requirement is controlled within 80-120 ℃.
According to the spinneret plate assembly adopted in the invention, hole arrays on the spinneret plate are annularly arranged, a spinning disc of a single-spindle spinning assembly is 72000-75000 holes, glue solution is pressurized and then sent into the spinneret plate assembly, and is extruded into filaments from the holes, and filament bundles sprayed out of the whole spinneret plate are annular.
Air gap blowing speed: the spinning stock solution is quantitatively delivered to a spinning assembly through a metering pump, extruded from a spinneret orifice and then enters a coagulating bath through a section of air gap. The air gap medium is air, and in the process, the thin flow is drawn into a coagulating bath to form filaments under certain conditions. In the process, the air gap air temperature is controlled to be 12-22 ℃, the air speed is controlled to be 2.5-6.5 m/S, the coagulation bath temperature is controlled to be 15-25 ℃, the concentration of NMMO in the coagulation bath is lower than 30%, and the circulation volume of the coagulation bath of the single-spindle spinning machine is 2.5-5.5 m3/h。
The parameters will have different degrees of influence on the spinning formation. Since the drawing process of the cellulose fiber must be completed in the air gap between the spinneret and the coagulation bath for a very short time, the drawing and cooling process, the air-gap blowing speed, and the wind field uniformity need to be strictly controlled. Also comprises special spinning beam, spinneret plate, NMMO content variation in coagulating bath, etc.
The invention has the advantages that:
the wet glue-making production process is adopted in domestic lyocell production factories, the process utilizes hydropulper equipment to fully mix raw material pulp plates with water to form fluid pulp gruel-shaped materials with pulp concentration of about 4% -5%, the fluid pulp gruel-shaped materials are conveyed to squeezer equipment by a pump to be squeezed to obtain pulp with dryness of about 35%, wet pulp is smashed by coarse smashing and fine smashing, NMMO solution is fully mixed, and colloid is prepared. The wet glue making process has obvious defects that firstly, the pulp dryness of the squeezed pulp fluctuates, the concentration of NMMO (cellulose suspension) of the cellulose suspension prepared by mixing the squeezed pulp with the NMMO solution fluctuates, and the quality of subsequent glue making and the stability of a finished product are influenced; and secondly, redundant water is brought into a production system, so that the quantity of subsequent solvent recovery is increased, and the recovery cost and the investment cost of the recovered solvent are increased. Breaks through the technical blockade of the foreign lyocell fiber production process, breaks through the limitation of the foreign lyocell fiber technology on the productivity, and reduces the investment and the operation cost of the production line. The production process is more stable, and the quality fluctuation of the finished product is reduced.
Drawings
A more complete appreciation of the invention and many of the attendant advantages thereof will be readily obtained as the same becomes better understood by reference to the following detailed description when considered in connection with the accompanying drawings, wherein the accompanying drawings are included to provide a further understanding of the invention and form a part of this specification, and wherein the illustrated embodiments of the invention and the description thereof are intended to illustrate and not limit the invention, as illustrated in the accompanying drawings, in which:
FIG. 1 is a schematic diagram of the structure and process of the present invention.
The invention is further illustrated with reference to the following figures and examples.
Detailed Description
It will be apparent that those skilled in the art can make many modifications and variations based on the spirit of the present invention.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. It will be understood that when an element, component or section is referred to as being "connected" to another element, component or section, it can be directly connected to the other element or section or intervening elements or sections may also be present. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art.
The following examples are further illustrative in order to facilitate the understanding of the embodiments, and the present invention is not limited to the examples.
Example 1: as shown in figure 1, a high-efficiency production manufacturing device of lyocell fibers, a separating machine or a traction machine is connected with a coarse powder machine, a coarse powder machine is connected with a fine powder machine through a fan, a fine powder machine is connected with a bin, the bin is connected with a weighing belt device, the weighing belt device is connected with a premixer, the premixer is connected with a mixing bin, the mixing bin is connected with a thin film evaporator through a screw pump, the evaporator is connected with a discharge pump, the discharge pump is connected with a glue solution filter, the glue solution filter is connected with a spinning metering pump, the spinning metering pump is connected with a spinning assembly, the spinning assembly is connected with a coagulating bath tank, the coagulating bath tank is respectively connected with a coagulating bath barrel and a winding machine, the coagulating bath barrel is respectively connected with a flushing water tank and a clarifying tank, the clarifying tank is connected with an air-adhering device, the air-adhering, concentrated NMMO jar is connected to the evaporimeter, and concentrated NMMO jar is connected the mixing bunker, and three-section rinsing machine and wash the water pitcher are connected respectively to the winder, and washing basin, cutter and wash the water pitcher are connected respectively to the three-section rinsing machine, and fine groove is given in the cutter connection, gives fine groove connection refiner, and device, washing basin and the dashing hair basin of oiling are connected respectively to the refiner, and drying device connects drying device, and drying device connects packing apparatus.
The coagulating bath barrel is in circulating connection with the coagulating bath, and the water washing tank is in circulating connection with the refiner and conveys fibers to the fiber tank.
Example 2: as shown in figure 1, a set of mature and reliable lyocell fiber production process is developed by a high-efficiency lyocell fiber production method, so that the production cost and the investment cost are reduced, the localization process of lyocell fine fibers is promoted, and the development of the new fiber material field in China is further powerfully promoted.
Step 1), solvent selection:
the selection of the solvent is critical to the preparation of the cellulose fiber, since the rigid molecular chains and intramolecular and intermolecular hydrogen bonding networks of cellulose make it insoluble in water and conventional organic solvents.
Reacting diglycol with ammonia to obtain morpholine, methylating, and reacting with hydrogen peroxide (H)2O2) Oxidation to obtain an aliphatic cyclic tertiary amine oxide (i.e., NMMO). The N-O bond has strong polarity, so that hydrogen bonds among cellulose molecules can be broken to form hydrogen bond complexes and ion interaction, so that NMMO generates strong dissolving capacity on cellulose and cellulose derivatives are not generated. To reduce the cost of solvent use, NMMO containing a certain amount of water can also be used. In the electron donor-acceptor interaction between cellulose and NMMO, water can act as a solvent activation point, and hydrogen bonds with oxygen atoms and hydrogen atoms in the hydroxyl groups of cellulose and solvent NMMO & H2H in O2The interaction between O molecules achieves the aim of effectively dissolving cellulose. The concentration of the NMMO solvent used in the method is 65-85%, and the temperature of the solvent is 55-85 ℃.
Step 2), pulp treatment:
the lyocell fibers have special requirements on the quality of raw material pulp, the index control range of the raw material pulp is respectively DP (degree of polymerization) 450-770, the content of methyl fiber is 88-95%, whiteness is more than or equal to 92%, moisture is 8-15%, iron content is less than or equal to 15mg/kg, and ash content is less than or equal to 0.1 mg/kg. Conveying pulp meeting the quality requirement to a strong shredding unit through a separating machine or a tractor, performing secondary fine crushing treatment through a fine crusher after coarse crushing, filtering the fine crushed pulp through a filter plate, feeding the fine crushed pulp into a storage bin, and returning large pulp isolated by the filter plate to the fine crushing for recycling treatment, wherein the size of the filter plate is 2-8 mm.
Step 3), NMMO impregnation:
the pulp entering the fine crushing bin falls to a belt weigher through a star discharger, the weighed pulp is conveyed to a pre-mixer through a belt, a plurality of solvent spray nozzles are arranged on two sides of the pre-mixer, the weighing quantity and a solvent conveying system are in a logical relation, a PLC system calculates the adding amount of a solvent according to the weighing quantity, the solvent adding amount is quantitatively and regularly sprayed into the pre-mixer, materials and the solvent are fully mixed to generate porridge, and the porridge is conveyed to a mixed porridge tank. The concentration of the solvent is 65-85%, the temperature of the solvent is 55-85 ℃, the N/C ratio is controlled to be 5.5-8.5, a certain amount of antioxidant needs to be added in the solvent, and the adding proportion of the antioxidant is 0.5-2 per mill.
Step 4), dissolving pulp:
adding the crushed pulp into the NMMO aqueous solution meeting the requirements of concentration and temperature, fully soaking the pulp in a mixed pulp porridge tank, and homogenizing to obtain the cellulose suspension. The activated cellulose is then continuously mixed in a solvent to form a homogeneous suspension, and the slurry is fed into a thin-film evaporator, where the premix is applied in the upper region by means of a centrally positioned rotor and is fed downwards through the evaporator, the suspension is concentrated by vacuum pressure reduction and heating, and the pulp is gradually dissolved with decreasing water content and converted into a plastic cellulose solution. Because the dissolution of NMMO to cellulose can only be carried out in a very narrow NMMO/H range2The O mixed solvent can not be dissolved under the condition of proportion and has strict requirements on temperature, so that the water in the raw materials is excessive at the beginning of the dissolution, and then the water is gradually removed until NMMO and H are reached2The proportion concentration of O is 65-85%.
The process is briefly described as follows: at present, the preparation of Lyocell fiber spinning solution at home and abroad mainly comprises 4 technologies, namely an intermittent kettle type dissolving technology, a continuous double-screw extruder dissolving technology, a continuous vacuum full-mixing propulsion dissolving technology and a continuous vacuum film propulsion dissolving technology. The reactor in the process of the invention is a continuous vacuum film propelling reactor. The continuous vacuum film pushes the interior of the reactor to be vacuumized, the reactor adopts a jacket type heating mode, the jacket layer is divided into four independent heating areas which are respectively an upper part, a middle part, a lower part and a cone part heating area of the reactor, slurry and porridge enter from the upper part, and the slurry and porridge are discharged from the lower part. The temperature of the slurry at the upper part of the reactor is controlled to be 45-65 ℃, the temperature at the middle part is controlled to be 65-85 ℃, the temperature at the lower part is controlled to be 85-105 ℃, and the vacuum degree in the reactor is controlled to be-85-125 mbar.
The degree of polymerization of pulp directly affects the dissolution rate of the solvent and the properties of the fiber. The lower the degree of polymerization, the faster the dissolution rate and the better the filtration performance, but the poorer the performance of the cellulose fiber product; the higher the degree of polymerization, the better the properties of the fiber product produced. Factors that have a large influence on the spinnability of the fiber include the dissolution rate of the solution, the filtration performance, and the viscosity of the spinning solution. When the degree of polymerization is the same, wood pulp dissolves faster than cotton pulp in the ammonium oxide solvent (NMMO).
In the production process of Lyocell, the key point of high-performance fiber production is to prepare a spinning solution which is uniform, has proper viscosity and meets the requirements of various indexes, so the process control in the dissolving process of dissolving pulp is very important, and the finally prepared colloid index is controlled to be nD 50: 0.8-2, cellulose content: 8-14%, NMMO content: 65-85%, N/C: 5.5-8.5, viscosity: 300 to 600 Pa.s. nD50 means the refractive index of the glue solution at 50 ℃, and the content of the solvent in the glue solution can be reflected by the refractive index; N/C means the mass ratio of solvent NMMO to oven dried cellulose.
The paste is scraped and formed into a film in a film evaporator, and a foamless real solution is quickly formed under the action of a certain temperature and vacuum. The process has the characteristics of relatively simple equipment structure, low manufacturing cost, high efficiency and short solution forming time of materials, reduces the degradation of cellulose, greatly reduces the possibility of solvent decomposition, has small material holding amount in a system, and is favorable for safe production and large-scale production.
Step 5), fiber forming and post-treatment:
the plastic cellulose true solution prepared by the film evaporator is conveyed to a spinning working section by a discharge pump through a conveying pipeline, the requirement on temperature stability in the conveying process is very high, and the requirement is controlled within 80-120 ℃. The spinning stock solution is quantitatively delivered to a spinning assembly through a metering pump, extruded from a spinneret orifice and then enters a coagulating bath through a section of air gap. The air gap medium is air, and in the process, the thin flow is drawn into a coagulating bath to form filaments under certain conditions. In the process, the air gap air temperature is controlled to be 12-22 ℃, the air speed is controlled to be 2.5-6.5 m/s, the coagulation bath temperature is controlled to be 15-25 ℃, the concentration of NMMO in the coagulation bath is lower than 30%, and the circulation amount of the coagulation bath of the single-spindle spinning machine is 2.5-5.5 m/h. In order to reduce the investment and the manufacturing cost, the novel developed spinneret plate assembly is adopted, and the spinning disc of the single-spindle spinning assembly meets the configuration requirement of 72000-75000 holes, so that the investment and the manufacturing cost are greatly reduced.
The filament and the coagulating liquid are subjected to convective diffusion mass transfer in the coagulating bath, and the coagulating liquid enters a recovery cycle. The spinning post-treatment mainly comprises the steps of drawing by a winding machine, washing by water, cutting, refining, drying and the like. The filaments which are still in a partial swelling state after spinning and stretching are continuously stretched by multi-section water washing, water comes from condensed water after solvent recovery and evaporation, and is recycled in a countercurrent step mode, and fresh desalted water is supplemented when the filaments are washed after refining. The procedures of water washing, oiling refining, drying and the like after cutting are similar to those of common viscose fibers, and the smoothness, cohesion, antistatic property and the like of the fibers are endowed by oiling. The crimped wet fibers are subjected to steam heat treatment and then dried in a dryer to further improve the fiber performance. The traditional viscose fiber spinning needs to complete the chemical process of decomposing cellulose sulfonate in the spinning process, so a wet spinning process is needed, in the Lyocell fiber spinning, hydroxyl in cellulose macromolecules is not esterified to form cellulose sulfonate, if stock solution flows out of a spinneret orifice and directly enters a coagulating bath, intermolecular hydrogen bonds are interacted instantly, so that the molecules are difficult to slide, high-nozzle drawing is needed immediately after the spinning solution in flow state is sprayed out of the spinneret orifice, so that the cellulose supramolecular structure is fixed, then the spinning solution enters the coagulating bath to obtain fibers with a certain orientation structure, therefore, the process adopts a dry-jet wet spinning process, the spinning stock solution prepared by dissolving is added into a screw extruder, is sheared and dissolved at a certain temperature, is sprayed out after being filtered, a static mixer, a metering pump and a spinning assembly, and the sprayed tows are oriented and drawn in the air, and then the fiber enters a coagulating bath, the concentration of the solvent is reduced due to solvent diffusion, cellulose is separated out, the tows are coagulated and formed, and then the short fiber can be detected and packaged through the post-treatment procedures of water washing, oiling, drying and the like. Parameters such as the temperature of the spinning solution, the design of a spinneret plate component, the air gap blowing air speed, the temperature of the coagulation bath and the like can influence the spinning formation to different degrees.
Since the drawing process of the cellulose fiber must be completed in the air gap between the spinneret and the coagulation bath for a very short time, the drawing and cooling process, the air-gap blowing speed, and the wind field uniformity need to be strictly controlled. That is, the traction force during stretching is uniform and cannot fluctuate too much; the cooling temperature is required to be uniform and stable at 15-25 ℃, the wind speed is controlled at 2.5-6.5 m/S, and once the parameters are determined, the parameters cannot fluctuate greatly.
Besides, the industrial production also comprises special spinning beam, spinneret, NMMO content change in coagulation bath, and the like, and is the core part of the spinning in the process of the invention.
Step 6), solvent recovery:
the NMMO solvent recovery process plays a crucial role in the Lyocll fiber production process, and although the toxicity of the NMMO solvent is low, the NMMO solvent is expensive. The solution recovered from the coagulation bath and the water washing solution contains NMMO, suspended impurities, colored impurity N-methylmorpholine (NMM), metal ions, and the like. The dissolution of cellulose pulp needs to be carried out at high temperature, due to NMMO/H during the dissolution process2The O/cellulose ternary system is easy to decompose at high temperature to generate colored impurities, NMM, morpholine (M) and CO2During the dissolution and spinning processes, undissolved cellulose is present in the solution in colloidal form, forming suspended impurities which, through the accumulation of constant circulation, reduce the dissolution properties of the solvent. Metal ions in solution, e.g. Fe3+、Cu2+、Mn2 +、Cr3+Etc. also catalyze the decomposition of NMMO and cellulose, and the heat generated in the decomposition can potentially cause the system to explode.
The NMMO solvent recovery mainly comprises an air flotation filtration method, an adsorption method, an oxidation method, an ion exchange method and the like. The filtration method can only remove suspended impurities, the NMMO is difficult to recover, and the filtration effect is limited; the adsorption method adopts alumina, activated carbon and the like as adsorbents, so that NMMO to be recycled is adsorbed while impurities are removed, and the recovery rate of a solvent is reduced; the oxidation method generally adopts hydrogen peroxide to oxidize NMM in a solvent to generate an effective component NMMO, but the oxidation recovery process is complex and new substances are easy to introduce; the ion exchange method achieves the purpose of separation through ion exchange reaction on ion exchange resin. The ion exchange resin comprises cation exchange resin and anion exchange resin, different types of ion exchange resin can only remove corresponding types of impurities, for example, the cation exchange resin can only remove cations in the solution, but the anions in the solution cannot be removed, and the resin has short service life, frequent regeneration and high consumption. It can be seen that the recovery process of a single method is difficult to achieve ideal effects, and a plurality of methods are adopted in the process flow of the invention to be matched for use to recover the solvent.
The solvent recovery mainly adopts the processes of air-float filtration, decolorization, ion exchange, flash evaporation concentration and the like, and condensed water is used for the washing section of the fiber. The solvent recovery is carried out in a closed solvent recovery system. And (3) pumping all the glue washing water in the glue making process and the coagulating bath in the spinning process to an air flotation filter, and adding 0.8ppm of polyacrylamide flocculant into a buffer pipe. The recovered solution is specially filtered and then sequentially enters an anion exchange tower and a cation exchange tower to be decolorized to remove morpholine and Fe3+、Cu2+And preparing a pure low-concentration NMMO solution, finally concentrating the recovered solution in a multi-effect flash evaporation system, and removing water from the solution in a flash evaporation tank through multi-stage evaporation under a negative pressure state to realize concentration so as to finally prepare the 80-84% NMMO solution.
As described above, although the embodiments of the present invention have been described in detail, it will be apparent to those skilled in the art that many modifications are possible without substantially departing from the spirit and scope of the present invention. Therefore, such modifications are also all included in the scope of protection of the present invention.
Claims (9)
1. A high-efficiency production method of lyocell fibre is characterized by that the spinning dope obtained by dissolving is fed into screw extruder, the temp. of spinning solution is controlled, after the spinning solution is sheared and dissolved, it is passed through the processes of filtering, static mixer, metering pump and spinning component, and sprayed out, and the air gap air-blowing speed is controlled, and the sprayed fibre bundle is oriented and stretched in the air, and then fed into coagulating bath, and due to solvent diffusion, the solvent concentration is reduced, cellulose is separated out, and the fibre bundle is coagulated and formed, then passed through the processes of water-washing, oiling and drying, and can be tested and packaged so as to obtain the invented short fibre.
2. The method for efficiently producing lyocell fiber according to claim 1, further comprising the steps of:
step 1), solvent selection:
selecting NMMO containing a certain amount of water, wherein the concentration of NMMO solvent is 65-85%, and the temperature of the solvent is 55-85 ℃; a certain amount of water concentration is 65-85%, namely the water content is 15-35%;
step 2), pulp treatment:
conveying pulp to a strong shredding machine set through a separating machine or a tractor, performing secondary fine crushing treatment through a fine crusher after coarse crushing, filtering the fine crushed pulp through a filter plate, and then feeding the fine crushed pulp into a storage bin, wherein the large pulp separated by the filter plate returns to the fine crushing for recycling treatment;
step 3), NMMO impregnation:
the pulp entering the bin and finely crushed falls to a belt weigher through a star discharger, the weighed pulp is conveyed to a premixer through a belt, a solvent is sprayed into the premixer, the material and the solvent are fully mixed to generate porridge, and the porridge is conveyed to a mixed porridge tank;
step 4), dissolving pulp:
dissolving the crushed pulp to obtain a plastic cellulose solution, adding excessive water to the raw material at the beginning of dissolving, and gradually removing water until NMMO and H2The proportion of O meets the requirements;
step 5), fiber forming and post-treatment:
the plastic cellulose true solution is delivered to a spinning section by a delivery pump through a delivery pipeline, the spinning stock solution is quantitatively delivered to a spinning assembly by a metering pump, extruded by a spinneret orifice and then enters a coagulating bath through a section of air gap; the strand silk and the solidification liquid carry out convection diffusion mass transfer in the solidification bath, and the solidification liquid enters a recovery cycle; the spinning post-treatment comprises the steps of drawing, washing, cutting, refining and drying by a winder, and the spinning post-treatment is carried out in a coagulating bath to obtain fibers;
step 6), solvent recovery:
air-float filtering, decolouring, ion exchange and flash evaporation concentration to obtain pure low-concentration NMMO solution, and concentrating the recovered solution in multi-effect flash evaporation system, and multi-stage evaporating the solution in flash evaporation tank under negative pressure to remove water, so as to obtain 80-84% NMMO solution.
3. The process for efficiently producing lyocell fibers according to claim 1, wherein the temperature control step of the spinning dope comprises: the continuous vacuum film is pushed into the reactor to vacuumize, the reactor adopts a jacket type heating mode, a jacket layer is divided into three independent circulating heating areas which are named as an upper heating area, a middle heating area and a lower heating area of the reactor respectively, slurry is added into the upper part of the reactor, and the slurry is discharged from the lower part of the reactor; the heating temperature of the upper part of the reactor is controlled to be 45-65 ℃, the temperature of the middle part is controlled to be 65-85 ℃, the temperature of the lower part is controlled to be 85-105 ℃, and the vacuum degree in the reactor is controlled to be-85-125 bar; the plastic cellulose true solution prepared by the film evaporator is delivered to a spinning section by a delivery pump through a delivery pipeline, the requirement on temperature stability in the delivery process is very high, and the requirement is controlled within 80-120 ℃.
4. The method for efficiently producing lyocell fibers according to claim 1, wherein the air-gap blowing wind speed step comprises: quantitatively feeding the spinning stock solution to a spinning assembly through a metering pump, extruding the spinning stock solution from a spinneret orifice, and then feeding the extruded spinning stock solution into a coagulating bath through a section of air gap; the air gap medium is air, and in the process, the thin flow is drawn into a coagulating bath to form filaments under certain conditions; in the process, the air gap air temperature is controlled to be 12-22 ℃, the air speed is controlled to be 2.5-6.5 m/S, the coagulation bath temperature is controlled to be 15-25 ℃, the concentration of NMMO in the coagulation bath is lower than 30%, and the circulation volume of the coagulation bath of the single-spindle spinning machine is 2.5-5.5 m3/h。
5. The method for efficiently producing lyocell fibers according to claim 1, wherein the step 2) of treating the pulp further comprises the steps of: the lyocell fibers have special requirements on the quality of raw material pulp, the index control range of the raw material pulp is respectively DP (degree of polymerization) 450-770, the content of methyl fiber is 88-95%, whiteness is more than or equal to 92%, moisture is 8-15%, iron content is less than or equal to 15mg/kg, and ash content is less than or equal to 0.1 mg/kg; conveying pulp meeting the quality requirement to a strong shredding unit through a separating machine or a tractor, performing secondary fine crushing treatment through a fine crusher after coarse crushing, filtering the fine crushed pulp through a filter plate, feeding the fine crushed pulp into a storage bin, and returning large pulp isolated by the filter plate to the fine crushing for recycling treatment, wherein the size of the filter plate is 2-8 mm.
6. The method for efficiently producing lyocell fiber according to claim 1, wherein the step 3) and the NMMO impregnation further comprise the steps of: a plurality of solvent nozzles are arranged on two sides of the premixer, a logical relation is established between the weighing quantity and the solvent conveying system, the PLC system calculates the adding quantity of the solvent according to the weighing quantity, the solvent is quantitatively and regularly sprayed into the premixer, so that the materials and the solvent are fully mixed to generate the slurry porridge, and the slurry porridge is conveyed into the mixed slurry porridge tank. The concentration of the solvent is 65-85%, the temperature of the solvent is 55-85 ℃, the N/C ratio is controlled to be 5.5-8.5, a certain amount of antioxidant needs to be added in the solvent, and the adding proportion of the antioxidant is 0.5-2 per mill.
7. The method for efficiently producing lyocell fibers according to claim 1, wherein the dissolving step 4) of the pulp further comprises the steps of: continuously mixing activated cellulose in a solvent to form a homogeneous suspension, feeding the slurry to a thin film evaporator, applying a pre-mixture to the upper region of the evaporator with a centrally located rotor, feeding the pre-mixture downwards through the evaporator, concentrating the suspension under reduced pressure and heating under vacuum, the pulp dissolving gradually and being converted into a plastic cellulose solution as the water content decreasesUntil NMMO and H are reached2The proportion concentration of O is 65-85%.
8. The method for efficiently producing lyocell fiber according to claim 1, wherein the solvent recovery in step 6) further comprises the following steps: the recovered solution is specially filtered and then sequentially enters an anion exchange tower and a cation exchange tower to be decolorized to remove morpholine and Fe3+、Cu2+And preparing a pure low-concentration NMMO solution, finally concentrating the recovered solution in a multi-effect flash evaporation system, and removing water from the solution in a flash evaporation tank through multi-stage evaporation under a negative pressure state to realize concentration so as to finally prepare the 80-84% NMMO solution.
9. An efficient production and manufacturing device for lyocell fibers is characterized in that a separating machine or a traction machine is connected with a coarse powder machine, a coarse powder machine is connected with a fine powder machine through a fan, a fine powder machine is connected with a bin, the bin is connected with a weighing belt device, the weighing belt device is connected with a premixer, the premixer is connected with a mixing bin, the mixing bin is connected with a thin film evaporator through a screw pump, the evaporator is connected with a discharge pump, the discharge pump is connected with a glue solution filter, the glue solution filter is connected with a spinning metering pump, the spinning metering pump is connected with a spinning assembly, the spinning assembly is connected with a coagulating bath tank, the coagulating bath tank is respectively connected with a coagulating bath barrel and a winding machine, the coagulating bath barrel is respectively connected with a flushing water tank and a clarifying tank, the clarifying tank is connected with an air adhesion device, the air adhesion device is connected with, concentrated NMMO jar is connected to the evaporimeter, and concentrated NMMO jar is connected the mixing bunker, and three-section rinsing machine and wash the water pitcher are connected respectively to the winder, and washing basin, cutter and wash the water pitcher are connected respectively to the three-section rinsing machine, and fine groove is given in the cutter connection, gives fine groove connection refiner, and device, washing basin and the dashing hair basin of oiling are connected respectively to the refiner, and drying device connects drying device, and drying device connects packing apparatus.
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CN113529195A (en) * | 2021-06-17 | 2021-10-22 | 杭州融凯盛科技有限公司 | Method for producing Lyocell bamboo fiber |
CN113388897A (en) * | 2021-06-29 | 2021-09-14 | 北京三联虹普新合纤技术服务股份有限公司 | High-capacity Lyocell cellulose stock solution and continuous preparation process thereof |
CN113388897B (en) * | 2021-06-29 | 2022-06-10 | 北京三联虹普新合纤技术服务股份有限公司 | High-capacity Lyocell cellulose stock solution and continuous preparation process thereof |
CN117448981A (en) * | 2023-12-22 | 2024-01-26 | 山东鸿泰鼎新材料科技有限公司 | Method for preparing functional lyocell fiber containing apocynum venetum active ingredient |
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