Camellia modal fiber preparation process and equipment thereof

Abstract

The invention discloses a camellia modal fiber preparation process and equipment thereof, and particularly relates to the technical field of fiber preparation, the process comprises the following steps: preparing a porous carrier, modifying the porous carrier, preparing a functional component, putting the modified porous carrier into 90 times of a camellia component-containing solution in parts by weight under a dark condition, preparing a spinning solution, and preparing the camellia modal fiber. The preparation method comprises the following steps: adding a modified porous carrier loaded with camellia into a spinning stock solution, uniformly mixing, stirring and dissolving in vacuum for 5 hours, defoaming, filtering, finally preparing a uniform and stable spinning solution, spinning by adopting a wet spinning process and the like, and finally preparing the camellia modal fiber. According to the invention, the camellia extract is combined with the characteristics of the modal fiber, so that the growth of bacteria can be inhibited, the generation of peculiar smell is reduced, and a film does not need to be formed on the surface of the fiber, thereby ensuring that the subsequently manufactured fabric has good air permeability.

Description

Technical Field

[0001] The invention relates to the technical field of fiber preparation, and more specifically to a camellia modal fiber preparation process and equipment thereof. Background Art

[0002] Modal fiber is a regenerated cellulose fiber, and its chemical composition is cellulose. The international standard ISO2076:1999 (E) defines Modal fiber as a regenerated cellulose fiber with high wet modulus and high breaking strength made from a specific viscose and regeneration bath composition, which can achieve a higher degree of molecular orientation when the fiber is stretched and condensed. Modal fiber has the advantages of good hygroscopicity, stable performance, and comfortable wearing, and is an ideal close-fitting fabric and health care clothing product.

[0003] Modal fiber has been widely used in many garments and household items due to its excellent softness, moisture absorption and comfort, but its own antibacterial properties are weak, so it needs to be enhanced through antibacterial treatment. However, although the existing antibacterial treatment materials for modal fibers (such as antibacterial agents or antibacterial coatings) can improve the antibacterial properties to a certain extent, they also have some disadvantages and limitations. For example, the addition of antibacterial agents is mainly to form a thin film on the surface of modal fibers after the fibers are formed, so as to improve the antibacterial effect. However, the presence of the coating will affect the breathability and comfort of the fabric, and the wearer will not feel refreshed enough in a hot environment, affecting the wearing experience. Summary of the invention

[0004] The invention provides a camellia modal fiber preparation process and equipment thereof, and aims to solve the following problem: the existing modal fiber antibacterial agent is added mainly to form a thin film on the surface of the modal fiber after the fiber is formed; however, the presence of the coating affects the air permeability and comfort of the fabric, and the wearer feels not cool enough in a hot environment, which affects the wearing experience.

[0005] To achieve the above object, the present invention provides the following technical solution: a process for preparing camellia modal fiber, comprising the following steps: Step 1, preparing a porous carrier, adding hexadecyltrimethylammonium bromide and polyethylene glycol PEG-6000 into deionized water, stirring for 30 minutes, then adding mesitylene, stirring for 30 minutes, adding water glass at a feeding rate of 1g / min, and after the water glass is added, stirring is continued for 1.5 hours, the solution is adjusted to a pH value of 10, transferred to a reactor for crystallization, and then filtered out the crystals through a filtering device, washed, dried at 80°C for 18 hours, and calcined at 450°C for 4 hours to obtain a porous carrier; Step 2, modification of the porous carrier, the porous carrier is put into 35 times the weight of the ethanol solution, ultrasonically dispersed evenly, under stirring, silane coupling agent KH-550 and silane coupling agent KH-580 are added at the same time at a dropping rate of 2 mL / min, after the addition is completed, the pH value is adjusted to 4.5, stirred and heated to 50° C., kept warm, stirred and refluxed for 5 hours; the solid matter is separated by centrifugation, washed and dried at 45° C. to obtain a modified porous carrier; Step 3: Prepare the functional component. In a light-proof condition, put the modified porous carrier into a solution containing 90 times the weight of the camellia component, heat it to 30°C, stir and adsorb it at 50 rpm for 20 hours, wash it, and dry it at 45°C under a vacuum degree of 0.01 MPa until the moisture content is 1 wt%, to obtain the functional component, i.e., the modified porous carrier loaded with camellia. Step 4, preparing a spinning solution, adding a modified porous carrier loaded with camellia to the spinning solution, mixing evenly, dissolving in a vacuum stirring for 5 hours, degassing, filtering, and finally obtaining a uniform and stable spinning solution; Step 5: spinning, using a wet spinning process to produce camellia modal fiber.

[0006] In a preferred embodiment, in step 1, when cetyltrimethylammonium bromide and polyethylene glycol PEG-6000 are added to deionized water, the temperature of the deionized water is 35°C, and a hydrochloric acid solution with a concentration of 2 mol / L is used as an adjusting agent to adjust the pH value. After the pH value is adjusted, the mixture is kept warm for 12 hours, and the temperature is raised to 105°C during crystallization, and the mixture is kept warm for crystallization for 20 hours. In step 2, acetic acid is used as an adjusting agent to adjust the pH value, and the stirring process after the pH value is adjusted is carried out under nitrogen protection and light-proof conditions.

[0007] In a preferred embodiment, the washing process in step one uses 12 times the volume of deionized water for washing, the washing process in step two first uses 8 times the volume of anhydrous ethanol for washing and then uses 18 times the volume of deionized water, and the washing process in step three uses 12 times the volume of deionized water.

[0008] In a preferred embodiment, the adjusting reagent used for pH adjustment in step 1 and step 2 is added in two stages. In the first stage, three quarters of the amount is added. After stirring, the adjusting reagent is added dropwise for the second stage, and stirring is continued to ensure that the acetic acid added each time can be fully mixed until the pH value stabilizes within the desired range. After stopping the addition of acetic acid, stirring is continued for a few minutes to ensure that the pH value does not change any more, and then measurement is performed again to confirm the final pH value.

[0009] The wet spinning process in step 5 includes the following steps: Step a, extruding the spinning solution in step 4 through the small holes of the spinneret to form a thin stream, and the thin stream enters the coagulation bath, during which phase separation occurs, the solvent is replaced, and the polymer is coagulated to form solid fibers; Step b, the newly formed fiber is stretched by a stretching device after leaving the coagulation bath, and the stretching ratio of the fiber is 1-1.5; Step c, soaking the spun fiber in an oil agent, washing, dehydrating and drying it to obtain the final fiber material, wherein the oil agent is an aqueous solution of amino silicone oil with a volume percentage concentration of 0.05-0.5%, and the soaking time is 2-12 hours; Step d: rolling and packaging the treated fibers for subsequent textile processing.

[0010] A camellia modal fiber preparation device comprises a filtering device, the filtering device comprises a separation box, a cylindrical portion is arranged on the top of the separation box, a liquid outlet is arranged on the bottom of the separation box, a delivery pipe is arranged on the top of the cylindrical portion, a crystal grain discharge pipe is arranged on one side of the cylindrical portion, a main filtering assembly is arranged in the cylindrical portion, the main filtering assembly comprises an eccentric rotating shaft, and an arc-shaped filtering plate is arranged on the bottom of the cylindrical portion; In a preferred embodiment, the eccentric rotating shaft is rotatably installed inside the cylindrical part, the eccentric rotating shaft is located below the axis of the cylindrical part and is arranged close to the grain discharge pipe, a rotating frame is fixedly installed outside the eccentric rotating shaft, a plurality of groups of gradient pressure plates are arranged on the circumferential side wall of the rotating frame, one end of the gradient pressure plate close to the rotating frame is rotatably connected to the rotating frame, the gradient pressure plate is inclined on the rotating frame along a side away from the rotation direction of the rotating frame, and a torsion elastic member is arranged between the gradient pressure plate and the rotating frame, the torsion elastic member is used to provide elastic force for the gradient pressure plate to flip in the direction away from the rotating frame.

[0011] In a preferred embodiment, a scraper strip is fixedly connected to one end of the gradual pressure plate away from the rotating frame. The scraper strip is a convex strip structure. A liquid release groove is arranged in the middle of the scraper strip. An inner punched seam is arranged on the side of the scraper strip corresponding to the gradual pressure plate. The inner punched seam is connected to the liquid release groove. The liquid release groove is connected to a diluent supply system through a connecting pipe. The diluent supply system includes a high-pressure pump and a diluent. The diluent supply system is used to provide the diluent to the liquid release groove.

[0012] In a preferred embodiment, an inner lining tube is provided inside the eccentric rotating shaft, and the inner lining tube is fixedly installed in the cylindrical part. The rotating frame is a solid structure. A liquid outlet gap is provided on the side of the inner lining tube away from the grain discharge pipe. Liquid outlet channels are provided inside the rotating frame corresponding to each gradient pressure plate. The connecting tubes on each gradient pressure plate are respectively connected to the corresponding liquid outlet channels, and the liquid outlet channels are provided corresponding to the liquid outlet gaps. The inner cavity of the inner lining tube is connected to the high-pressure pump through a pipeline.

[0013] In a preferred embodiment, a secondary filter assembly is arranged below the arc filter plate, the secondary filter assembly includes a filter belt and a support roller group, the support roller group is installed in the separation box, the filter belt is arranged outside the support roller group, and the filter belt is supported by the support roller group to form a crawler structure, so that the filter belt forms an upper area and a lower area of ​​the upper and lower parts, the secondary filter assembly also includes a discharge box, the discharge box is installed below the filter belt, a centralized guide bucket is arranged in the separation box, the centralized guide bucket is located between the arc filter plate and the filter belt, the bottom of the centralized guide bucket is a contraction structure, a soft scraper is fixedly installed in the discharge box, the top of the soft scraper is in contact with the lower area of ​​the filter belt, and a liquid leakage port is arranged in the middle of the discharge box corresponding to the position of the centralized guide bucket, a transfer filter is fixedly installed on the bottom wall of the discharge box, and the discharge box and the separation box are detachably installed.

[0014] In a preferred embodiment, the support roller group includes two groups of fixed rollers and two groups of movable rollers. The fixed rollers and the movable rollers are rotatably arranged inside a separation box. The fixed rollers are rotatably connected to the separation box. Slide grooves are provided at positions of the separation box corresponding to the ends of the movable rollers. Slide blocks are rotatably installed at the ends of the movable rollers. The slide blocks are slidably installed in the slide grooves, and thrust elastic parts are installed between the slide blocks and the slide grooves.

[0015] The beneficial effects of the present invention are as follows: the camellia modal fiber prepared by the present invention contains camellia extract itself. Since camellia itself has a certain antibacterial effect, combined with the characteristics of modal fiber, this fiber can inhibit bacterial growth and reduce the generation of odor. Therefore, there is no need to form a coating on the fiber surface, thereby ensuring that the fabric made subsequently has good air permeability. Moreover, camellia is a natural plant component, and the prepared fiber is more gentle to the skin, further enhancing the softness and comfort of the fabric. At the same time, the fabric can also have excellent air permeability and hygroscopicity. The movement of the gradient pressing plate of the present invention will also drive the movement of the grains until the extruded grains are driven to slide out of the grain discharge pipe to achieve the separation of the grains, thereby avoiding the problem that the grains converge in the same area during the filtration process, causing the solution to be difficult to penetrate the grains downward. At the same time, with the gradual extrusion of the gradient pressing plate, the separation efficiency between the solution and the grains can also be improved, not only realizing the full separation function of the solution, but also realizing the continuous operation of the equipment, which can adapt to large-scale grain filtration production, and greatly improving the production efficiency of the camellia modal fiber. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a flow chart of the preparation method of the present invention.

[0017] Figure 2 It is a flow chart of the wet spinning process of the present invention.

[0018] Figure 3 It is a schematic diagram of the overall structure of the filtering device of the present invention.

[0019] Figure 4 It is a schematic diagram of the internal structure of the filtering device of the present invention.

[0020] Figure 5 It is a schematic diagram of the overall structure of the main filter assembly of the present invention.

[0021] Figure 6 It is a schematic diagram of the overall structure of the auxiliary filtering component of the present invention.

[0022] Figure 7 For the present invention Figure 6 Schematic diagram of the A part structure.

[0023] Figure 8 This is a schematic structural diagram of the improved main filter assembly of the present invention.

[0024] Fig. 9 For the present invention Figure 8 Enlarged view of the structure of part B.

[0025] Fig.10 This is a state diagram of the liquid release tank of the present invention releasing the diluent.

[0026] Fig.11 It is a schematic diagram of the structure of the liner pipe of the present invention.

[0027] Fig.12 This is a diagram showing the matching state between the inner liner pipe and the eccentric rotating shaft of the present invention.

[0028] The accompanying drawings are marked as follows: 1. filtration equipment; 11. separation box; 111. liquid outlet; 12. cylinder; 121. delivery pipe; 122. grain discharge pipe; 123. arc filter plate; 13. centralized guide bucket; 14. slide; 2. main filter assembly; 21. eccentric shaft; 22. rotating frame; 221. liquid outlet channel; 222. connecting pipe; 23. gradient pressure plate; 231. scraper strip; 232. liquid release groove; 233. inner punching seam; 24. lining tube; 241. liquid outlet seam; 3. auxiliary filter assembly; 31. filter belt; 311. upper area; 312. lower area; 32. support roller group; 321. fixed roller; 322. movable roller; 323. slider; 324. annular slot; 33. discharge box; 331. transfer filter; 34. soft scraper. DETAILED DESCRIPTION

[0029] The present application is further described in detail below in conjunction with the accompanying drawings. It is necessary to point out here that the following specific implementation methods are only used to further illustrate the present application and cannot be understood as limiting the scope of protection of the present application. Technical personnel in this field can make some non-essential improvements and adjustments to the present application based on the above application content.

[0030] Embodiment 1, refer to the attached specification Figure 1 , a camellia modal fiber preparation process, comprising the following steps: Step 1, prepare a porous carrier, add hexadecyltrimethylammonium bromide and polyethylene glycol PEG-6000 into 35°C deionized water, stir for 30 minutes, then continue to add mesitylene and stir for 30 minutes; add water glass at a feeding rate of 1g / min, and after the water glass is added, continue to stir for 1.5h; use a 2mol / L hydrochloric acid solution to adjust the pH value to 10, keep it warm and let it stand for 12h; then transfer it into a reactor, heat it to 105°C, keep it warm and crystallize for 20h; use filtering equipment 1 to filter out the grains, wash them with 12 times the volume of deionized water, dry them at 80°C for 18h, and calcine them at 450°C for 4h to obtain a porous carrier.

[0031] Step 2, porous carrier modification, the porous carrier is put into 35 times the weight of ethanol solution, and ultrasonically dispersed evenly; under stirring conditions, silane coupling agent KH-550 and silane coupling agent KH-580 are added at the same time at a dropping rate of 2 mL / min. After the addition is completed, acetic acid is used to adjust the pH value to 4.5; under nitrogen protection and light protection conditions, the mixture is stirred and heated to 50°C, kept warm, and stirred and refluxed for 5 hours; the solid matter is separated by centrifugation, washed with 8 times the volume of anhydrous ethanol, washed with 18 times the volume of deionized water, and then dried at 45°C to obtain a modified porous carrier.

[0032] Step 3: prepare the functional component. Under light-proof conditions, place the modified porous carrier into 90 times the weight of a solution containing camellia components, heat to 30°C, stir and adsorb at 50rpm for 20 hours, wash with 12 times the volume of deionized water, and then dry at 45°C under a vacuum degree of 0.01MPa to a moisture content of 1wt%, to obtain the functional component, i.e., the modified porous carrier loaded with camellia.

[0033] Step 4, preparing a spinning solution, adding a modified porous carrier loaded with camellia to the spinning solution, mixing evenly, dissolving in a vacuum stirring for 5 hours, degassing, filtering, and finally obtaining a uniform and stable spinning solution; Step 5: spinning, using a wet spinning process to produce camellia modal fiber.

[0034] The solution containing camellia components used in the above-mentioned embodiment is a pre-prepared material. Dried camellia petals or leaves are selected as the source of the extract to ensure that the raw materials are free of impurities and mildew. Water is selected as the solvent and supercritical carbon dioxide extraction is used. During the extraction, supercritical carbon dioxide extraction equipment is used to load the camellia raw material into an extraction tank, and the pressure and temperature (such as 30-40MPa, 35-45°C) are adjusted to make the carbon dioxide in a supercritical state. By adjusting the flow rate and extraction time (such as 1-3h), the effective ingredients in the camellia are extracted, and the extracted liquid is collected and separated under reduced pressure to obtain a solution rich in camellia components.

[0035] Nanofiltration or reverse osmosis membrane separation technology is then used to further purify the extract to remove large molecular impurities and insoluble substances. At the same time, activated carbon adsorption can also be used to remove pigments and other impurities to improve the color and purity of the extract.

[0036] The prepared camellia component solution is analyzed using HPLC, gas chromatography (GC), mass spectrometry (MS) and other analytical methods to determine the content and proportion of the main components in the extract to ensure that it meets expectations. The solution is then stored in a light-proof, low-temperature (such as 4°C) environment to prevent decomposition of the active ingredients due to light and high temperature.

[0037] In the above embodiment, the adjusting reagents used for pH adjustment in step 1 and step 2 (i.e., hydrochloric acid in step 1 and acetic acid in step 2) are added in two stages. In the first stage, three quarters of the amount is added. After stirring, the adjusting reagent is added dropwise using a dropper for the second stage. At the same time, stirring is continued to ensure that the acetic acid added each time can be fully mixed. After adding a certain amount of acetic acid, wait for a while (about 10-30 seconds) to allow the pH value to stabilize, and then measure the pH value again.

[0038] When the pH is very close to the target value, use a micropipette to make extremely fine adjustments until the pH stabilizes in the desired range (e.g., 4.5 ± 0.1). After stopping the addition of acetic acid, continue stirring for a few minutes to ensure that the pH does not change any more, then measure again to confirm the final pH.

[0039] For further information, please refer to the attached manual. Figure 2 In step 5, the wet spinning process comprises the following steps: Step a: Extrude the spinning solution in step 4 through the small holes of the spinneret (micropores on the spinneret) to form a thin stream, which enters the coagulation bath. Phase separation occurs during this process, the solvent is replaced, and the polymer coagulates to form solid fibers. The coagulation bath is a key part of wet spinning, and it usually consists of a liquid that can exchange with the solvent in the spinning solution but does not dissolve the polymer. For example, water is often used as a coagulation bath medium for polyacrylonitrile fiber production because it can effectively extract the solvent from the spinning solution. Step b, the newly formed fiber is stretched by a stretching device after leaving the coagulation bath, and the stretching ratio of the fiber is 1-1.5; Step c, soaking the spun fiber in an oil agent, washing, dehydrating and drying it to obtain the final fiber material, wherein the oil agent is an aqueous solution of silicone oil, dimethyl silicone oil or amino silicone oil, with a volume percentage concentration of 0.05-0.5%, and the soaking time is 2-12 hours; Step d: rolling and packaging the treated fibers for subsequent textile processing.

[0040] It should be noted that the camellia modal fiber provided by the present invention contains camellia extract. Since camellia itself has a certain antibacterial effect, combined with the characteristics of modal fiber, this fiber can inhibit bacterial growth and reduce the generation of odor. Therefore, there is no need to form a coating on the fiber surface, thereby ensuring that the subsequent fabric has good air permeability. Moreover, camellia is a natural plant ingredient, and the prepared fiber is more gentle on the skin, further enhancing the softness and comfort of the fabric. At the same time, it can also make the fabric have excellent air permeability and moisture absorption.

[0041] Example 2: During the preparation process of the camellia modal fiber, after crystallization is completed, it is necessary to filter out the crystals. In the process of filtering out the crystals, a filtering device is required. During the specific operation, the solution is input into the filtering device for filtering. If necessary, the filtering device can be connected to a vacuum device to utilize vacuum suction to extract the solution and accelerate the filtering out of the crystals.

[0042] However, as the solution is continuously poured in, the number of crystals on the filter component increases and the thickness is also increasing. During filtration, the solution poured in later is extracted from top to bottom. That is to say, as the solution is poured in, the solution poured in later needs to pass downward through the crystals that have been filtered out previously before it can be filtered out. As the thickness gradually increases, the suction force required for filtration is also increasing, making filtration increasingly difficult. When the crystals reach a certain thickness, the crystals must be removed from the filter component before filtration can continue, resulting in discontinuous filtration and low efficiency.

[0043] Therefore, the present invention also provides a camellia modal fiber preparation device, specifically, refer to the attached specification Figures 3 to 12 , including a filtering device 1, the filtering device 1 includes a separation box 11, a cylindrical portion 12 is arranged on the top of the separation box 11, a liquid outlet 111 is arranged on the bottom of the separation box 11, and a main filtering component 2 is arranged in the cylindrical portion 12.

[0044] The main filter assembly 2 includes an eccentric rotating shaft 21, a delivery pipe 121 is arranged on the top of the cylindrical portion 12, and a grain discharge pipe 122 is arranged on one side of the cylindrical portion 12. In actual use, the delivery pipe 121 is connected to the crystallization reactor, and the formed grains and the solution are input into the cylindrical portion 12 together. The liquid outlet 111 is connected to the vacuum pumping equipment to accelerate the liquid to pass through the main filter assembly 2. The grain discharge pipe 122 is connected to a closed container for collecting the separated grains. The bottom of the cylindrical portion 12 is arranged as an arc-shaped filter plate 123, and the cylindrical portion 12 and the arc-shaped filter plate 123 together form a horizontally arranged cylindrical structure.

[0045] Among them, the eccentric rotating shaft 21 is rotatably installed inside the cylindrical part 12, and a driving motor for driving the eccentric rotating shaft 21 to rotate is arranged on the separation box 11, and the eccentric rotating shaft 21 is located below the axis of the cylindrical part 12 and is arranged close to the grain discharge pipe 122, and a rotating frame 22 is fixedly installed outside the eccentric rotating shaft 21, and a plurality of groups of gradual pressure plates 23 are arranged on the circumferential side wall of the rotating frame 22, and the gradual pressure plate 23 is rotatably connected to the rotating frame 22 at one end close to the rotating frame 22, and the gradual pressure plate 23 is inclined on the rotating frame 22 along a side away from the rotation direction of the rotating frame 22, and a torsion elastic member is arranged between the gradual pressure plate 23 and the rotating frame 22, and the torsion elastic member is preferably a torsion spring, which is used to provide an elastic force for the gradual pressure plate 23 to flip in the direction away from the rotating frame 22, and under the action of the elastic force, the end of the gradual pressure plate 23 away from the rotating frame 22 is in contact with the arc filter plate 123 or the inner wall of the cylindrical part 12.

[0046] It should be noted that by eccentrically setting the eccentric shaft 21, the distance between the eccentric shaft 21 and the cylindrical portion 12 or the arc-shaped filter plate 123 is long and short, thereby forming a short spacing area and a long spacing area. When in use, the crystal solution after the crystallization reaction is input from the delivery pipe 121, and the rotating frame 22 is driven by the driving motor to rotate. The crystal solution first falls between two adjacent groups of gradient pressure plates 23. When the solution and the crystals move to the arc-shaped filter plate 123, the solution flows downward to form filtration. The crystals are filtered on the inner wall of the arc-shaped filter plate 123, and with the movement of the gradient pressure plate 23, the crystals gradually enter the area below the gradient pressure plate 23. When the gradient pressure plate 23 follows the rotating frame 22 to gradually rotate to the short spacing area between the eccentric shaft 21 and the arc-shaped filter plate 123, the gradient pressure plate 23 and the arc-shaped filter plate 123 are in contact with each other. The crystal grains on the arc filter plate 123 are squeezed, and the residual solution in the crystal grains is squeezed out and continues to be filtered. As the gradient pressing plate 23 continues to move, and because the tail end of the gradient pressing plate 23 is always in contact with the arc filter plate 123 under the action of the torsion elastic member, the movement of the gradient pressing plate 23 will also drive the crystal grains to move until the squeezed crystal grains are driven to the crystal grain discharge pipe 122 and slide out, so as to achieve the separation of the crystal grains, thereby avoiding the problem that the crystal grains gather in the same area during the filtration process, making it difficult for the solution to penetrate the crystal grains downward. At the same time, with the help of the gradual squeezing of the gradient pressing plate 23, the separation efficiency between the solution and the crystal grains can also be improved, which not only realizes the full separation function of the solution, but also realizes the continuous operation of the equipment, can adapt to large-scale crystal grain filtration production, and greatly improves the production efficiency of camellia modal fiber.

[0047] Furthermore, in order to ensure that the end of the gradient pressure plate 23 can always fit with the arc filter plate 123 and the cylindrical portion 12, and drive the movement of the grains, the end of the gradient pressure plate 23 away from the rotating frame 22 is fixedly connected with a scraper bar 231, and the scraper bar 231 is a convex strip structure. The scraper bar 231 moves together with the gradient pressure plate 23, which can avoid clogging of the arc filter plate 123 and improve the filtering effect and the cleaning effect of the arc filter plate 123.

[0048] Furthermore, in the above-mentioned embodiment, before the crystallization reaction, the pH value of the solution needs to be adjusted to 10. Therefore, the pH value of the overall solution after the final crystallization is completed is relatively high, which will cause certain corrosion to the material. Each processing equipment can perform anti-corrosion treatment on its surface. However, under the action of the torsion elastic member, the scraper 231 is always in contact with the arc-shaped filter plate 123. During the movement, long-term friction will be generated, which will reduce the anti-corrosion effect of the scraper 231 and affect the service life of the gradient pressure plate 23. For this reason, the present embodiment also provides the following technical solutions. Specifically, a liquid release groove 232 is provided in the middle of the scraper 231, and an inner punching slit 233 is provided on one side of the scraper 231 corresponding to the gradient pressure plate 23. The inner punching slit 233 is connected to the liquid release groove 232, and the liquid release groove 232 is connected to the diluent providing system through the connecting pipe 222. The diluent supply system includes a high-pressure pump and a diluent. The diluent is supplied to the liquid release tank 232 through the diluent supply system, so that the pH value of the solution around the scraper 231 can be adjusted, thereby reducing the corrosion effect of the solution on the scraper 231. At the same time, since the diluent output from the liquid release tank 232 has a certain pressure, it can provide a thrust to the scraper 231 away from the surface of the arc filter plate 123, thereby reducing the pressure between the scraper 231 and the arc filter plate 123, thereby reducing wear and improving the service life of the gradient pressure plate 23. At the same time, the diluent output from the liquid release tank 232 will also flow outward from the inner punching seam 233, thereby forming a certain outward impact on the grains gathered at the scraper 231, avoiding grinding between the scraper 231 and the grains, and further improving the filtering effect on the grains.

[0049] It should be noted that the diluent may be deionized water or other acidic solutions that have no effect on the grains, thereby fully neutralizing or diluting the solution near the scraper bar 231 and reducing the corrosion effect on the scraper bar 231 .

[0050] Furthermore, when the gradient pressure plate 23 moves toward the crystal grain discharge pipe 122, it is in the filtering completion state. At this time, the liquid release tank 232 should no longer output the dilution liquid. Therefore, the dilution liquid providing system needs to stop providing when the gradient pressure plate 23 is about to reach the crystal grain discharge pipe 122. To this end, the present embodiment also provides the following technical scheme: an inner lining tube 24 is provided inside the eccentric rotating shaft 21, and the inner lining tube 24 is fixedly installed in the cylindrical portion 12 (only one end of the eccentric rotating shaft 21 passes through the side wall of the cylindrical portion 12 and is rotatably connected to the cylindrical portion 12, and the position of the inner lining tube 24 corresponding to the other end of the eccentric rotating shaft 21 is fixedly connected to the cylindrical portion 12, thereby realizing the fixed connection between the inner lining tube 24 and the cylindrical portion 12 under the premise of forming a rotation support for the eccentric rotating shaft 21), the rotating frame 22 is a solid structure, and a liquid outlet gap 241 is provided on the side of the inner lining tube 24 away from the crystal grain discharge pipe 122, and each gradient pressure plate 23 is provided inside the rotating frame 22 A liquid outlet channel 221 is provided, and the connecting pipes 222 on each gradient pressure plate 23 are respectively connected to the corresponding liquid outlet channel 221, and the liquid outlet channel 221 is arranged corresponding to the liquid outlet gap 241. The inner cavity of the lining tube 24 is connected to the high-pressure pump through a pipeline, thereby realizing the connection between the connecting pipe 222 and the diluent providing system. In actual use, before the gradient pressure plate 23 approaches the grain discharge pipe 122, its corresponding liquid outlet channel 221 is connected to the liquid outlet gap 241 to achieve connection. Therefore, the liquid discharge of the liquid release groove 232 can be guaranteed in this process. When the gradient pressure plate 23 approaches the grain discharge pipe 122 and the scraper 231 gradually reaches the grain discharge pipe 122, the corresponding liquid outlet channel 221 is separated from the liquid outlet gap 241 and gradually goes around to the side of the lining tube 24 away from the liquid outlet gap 241, thereby realizing the blocking of the liquid outlet channel 221. At this time, the liquid release groove 232 no longer discharges liquid, and will not affect the discharge of grains from the grain discharge pipe 122.

[0051] In the above-mentioned fact mode, some fine crystals will pass through the arc filter plate 123 along with the solution, resulting in leakage, which will further cause material waste and even affect the vacuum equipment. For this reason, the present embodiment also provides the following scheme. Specifically, a sub-filter assembly 3 is arranged below the arc filter plate 123. The sub-filter assembly 3 includes a filter belt 31 and a support roller group 32. The support roller group 32 is installed in the separation box 11. The filter belt 31 is arranged outside the support roller group 32, and the filter belt 31 is supported by the support roller group 32 to form a crawler structure, so that the filter belt 31 forms an upper area 311 and a lower area 312 of the upper and lower parts. The support roller group 32 is connected to a driving device, which is used to The filter belt 31 is driven to move like a crawler track. The auxiliary filter assembly 3 also includes a discharge box 33, which is installed below the filter belt 31. A centralized guide bucket 13 is provided in the separation box 11. The centralized guide bucket 13 is located between the arc filter plate 123 and the filter belt 31. The bottom of the centralized guide bucket 13 is a contraction mouth structure. A soft scraper 34 is fixedly installed in the discharge box 33. The soft scraper 34 is an elastic component. The top of the soft scraper 34 contacts the lower area 312 of the filter belt 31, and a liquid leakage port is provided in the middle of the discharge box 33 corresponding to the position of the centralized guide bucket 13. A transfer filter 331 is fixedly installed on the bottom wall of the discharge box 33, and the discharge box 33 and the separation box 11 are detachably installed.

[0052] Furthermore, the filter belt 31 and the transfer filter screen 331 are both made of filter cloth materials, and the supporting roller group 32 includes two groups of fixed rollers 321 and two groups of movable rollers 322, the two groups of movable rollers 322 are located above the two groups of fixed rollers 321, the fixed rollers 321 and the movable rollers 322 are both rotatably arranged inside the separation box 11, and the driving device is a driving motor, which is fixedly installed on the outside of the separation box 11 and is transmission-connected to one of the groups of fixed rollers 321.

[0053] An installation opening is provided on the side wall of the separation box 11, and a support frame structure is provided inside the separation box 11. The discharge box 33 is inserted into the support frame structure through the installation opening and slidably cooperates with the separation box 11 to form a pull-out drawer, so that the discharge box 33 can be pulled out for cleaning when necessary (the soft scraper 34 is an elastic component, and when the discharge box 33 is pulled out and placed, the soft scraper 34 can be adaptively deformed without affecting the pulling out and placing in of the discharge box 33).

[0054] In actual use, the movement of the filter belt 31 is regularly controlled to exchange the materials in the upper area 311 and the lower area 312, and the filtered crystals are scraped into the discharge box 33 by the soft scraper 34. At the same time, the filter belt 31 can always have a clean surface facing the solution, thereby achieving full filtration of the leaked crystals in the solution, while also preventing the leaked crystals from accumulating and adhering to the filter belt 31 and affecting the filtration. The leaked crystals scraped into the discharge box 33 can be regularly taken out and cleaned. When the discharge box 33 is taken out, the filter belt 31 is still present in the separation box 11 for filtration.

[0055] Furthermore, in order to ensure that the filter belt 31 has sufficient elasticity to fully contact the soft scraper 34, the present embodiment also provides the following technical solutions: the fixed roller 321 is fixed relative to the separation box 11, and the fixed roller 321 is directly connected to the separation box 11 for rotation, and the separation box 11 is provided with a slide groove 14 at the position corresponding to the end of the movable roller 322, and a slider 323 is rotatably installed at the end of the movable roller 322, and the slider 323 is slidably installed in the slide groove 14, and a thrust elastic member is installed between the slider 323 and the slide groove 14, and the thrust elastic member is used to provide the slider 323 with an elastic force to tension the filter belt 31, so that the filter belt 31 can effectively contact the soft scraper 34.

[0056] The above-mentioned embodiments only express several implementation methods of the present invention, and the description is relatively specific and detailed, but it cannot be understood as limiting the scope of the present invention. It should be pointed out that for ordinary technicians in this field, several modifications and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention.

Claims

1. A process for preparing camellia modal fiber, characterized in that: The following steps are involved: Step 1, preparing a porous carrier, adding hexadecyltrimethylammonium bromide and polyethylene glycol PEG-6000 into deionized water, stirring for 30 minutes, then adding mesitylene, stirring for 30 minutes, adding water glass at a feeding rate of 1 g / min, and after the addition of water glass, continuing to stir for 1.5 hours, adjusting the pH value of the solution to 10, transferring it into a reactor for crystallization, and then filtering out the crystals through a filtering device (1), washing, drying at 80°C for 18 hours, and calcining at 450°C for 4 hours to obtain a porous carrier; Step 2, modification of the porous carrier, the porous carrier is put into 35 times the weight of the ethanol solution, ultrasonically dispersed evenly, under stirring, silane coupling agent KH-550 and silane coupling agent KH-580 are added at the same time at a dropping rate of 2 mL / min, after the addition is completed, the pH value is adjusted to 4.5, stirred and heated to 50° C., kept warm, stirred and refluxed for 5 hours; the solid matter is separated by centrifugation, washed and dried at 45° C. to obtain a modified porous carrier; Step 3: Prepare the functional component. In a light-proof condition, put the modified porous carrier into a solution containing 90 times the weight of the camellia component, heat it to 30°C, stir and adsorb it at 50 rpm for 20 hours, wash it, and dry it at 45°C under a vacuum degree of 0.01 MPa until the moisture content is 1 wt%, to obtain the functional component, i.e., the modified porous carrier loaded with camellia. Step 4, preparing a spinning solution, adding a modified porous carrier loaded with camellia to the spinning solution, mixing evenly, dissolving in a vacuum stirring for 5 hours, degassing, filtering, and finally obtaining a uniform and stable spinning solution; Step 5: spinning, using a wet spinning process to produce camellia modal fiber.

2. The process for preparing camellia modal fiber according to claim 1, characterized in that: In the step 1, when cetyltrimethylammonium bromide and polyethylene glycol PEG-6000 are added into deionized water, the temperature of the deionized water is 35° C., a hydrochloric acid solution with a concentration of 2 mol / L is used as a regulating agent to adjust the pH value, and after the pH value is adjusted, the solution is kept warm and allowed to stand for 12 hours. During crystallization, the temperature is raised to 105° C. and kept warm for crystallization for 20 hours. In the step 2, acetic acid is used as a regulating agent to adjust the pH value, and the stirring process after the pH value is adjusted is carried out under nitrogen protection and light-proof conditions.

3. The process for preparing camellia modal fiber according to claim 2, characterized in that: In the step 1, the washing process uses 12 times the volume of deionized water for washing, in the step 2, the washing process first uses 8 times the volume of anhydrous ethanol for washing, and then uses 18 times the volume of deionized water, and in the step 3, the washing process uses 12 times the volume of deionized water.

4. The process for preparing camellia modal fiber according to claim 3, characterized in that: The adjusting reagent used for pH adjustment in step 1 and step 2 is added in two stages. In the first stage, three quarters of the amount is added. After stirring, the adjusting reagent is added dropwise for the second stage. At the same time, stirring is continued to ensure that the acetic acid added each time can be fully mixed until the pH value is stabilized within the required range. After stopping the addition of acetic acid, stirring is continued for a few minutes to ensure that the pH value does not change any more, and then measurement is performed again to confirm the final pH value.

5. A process for preparing camellia modal fiber according to claim 4, characterized in that: The wet spinning process in step 5 comprises the following steps: Step a, extruding the spinning solution in step 4 through the small holes of the spinneret to form a thin stream, and the thin stream enters the coagulation bath, during which phase separation occurs, the solvent is replaced, and the polymer is coagulated to form solid fibers; Step b, the newly formed fiber is stretched by a stretching device after leaving the coagulation bath, and the stretching ratio of the fiber is 1-1.5; Step c, soaking the spun fiber in an oil agent, washing, dehydrating and drying it to obtain the final fiber material, wherein the oil agent is an aqueous solution of amino silicone oil with a volume percentage concentration of 0.05-0.5%, and the soaking time is 2-12 hours; Step d: rolling and packaging the treated fibers for subsequent textile processing.

6. An apparatus for preparing camellia modal fiber according to claim 5, comprising a filtering device (1), the filtering device (1) comprising a separation box (11), a cylindrical portion (12) being arranged at the top of the separation box (11), a liquid outlet (111) being arranged at the bottom of the separation box (11), a delivery pipe (121) being arranged at the top of the cylindrical portion (12), and a crystal grain discharge pipe (122) being arranged at one side of the cylindrical portion (12), characterized in that: A main filter assembly (2) is arranged in the cylindrical portion (12), the main filter assembly (2) comprising an eccentric rotating shaft (21), and the bottom of the cylindrical portion (12) is arranged as an arc-shaped filter plate (123); The eccentric rotating shaft (21) is rotatably mounted inside the cylindrical portion (12). The eccentric rotating shaft (21) is located below the axis of the cylindrical portion (12) and is arranged close to the crystal grain discharge pipe (122). A rotating frame (22) is fixedly mounted outside the eccentric rotating shaft (21). A plurality of groups of gradient pressure plates (23) are arranged on the circumferential side wall of the rotating frame (22). One end of the gradient pressure plate (23) close to the rotating frame (22) is rotatably connected to the rotating frame (22). The gradient pressure plate (23) is arranged on the rotating frame (22) at an angle away from the rotating direction of the rotating frame (22). A torsion elastic member is arranged between the gradient pressure plate (23) and the rotating frame (22). The torsion elastic member is used to provide an elastic force for the gradient pressure plate (23) to flip in a direction away from the rotating frame (22).

7. The equipment for preparing camellia modal fiber according to claim 6, characterized in that: A scraper (231) is fixedly connected to one end of the gradual change pressure plate (23) away from the rotating frame (22); the scraper (231) is a convex strip structure; a liquid release groove (232) is provided in the middle of the scraper (231); an inner punched seam (233) is provided on one side of the scraper (231) corresponding to the gradual change pressure plate (23); the inner punched seam (233) is communicated with the liquid release groove (232); the liquid release groove (232) is connected to a diluent supply system via a connecting pipe (222); the diluent supply system comprises a high-pressure pump and a diluent; the diluent supply system is used to supply the diluent to the liquid release groove (232).

8. The equipment for preparing camellia modal fiber according to claim 7, characterized in that: An inner lining tube (24) is arranged inside the eccentric rotating shaft (21), and the inner lining tube (24) is fixedly installed in the cylindrical portion (12). The rotating frame (22) is a solid structure. A liquid outlet slit (241) is arranged on the side of the inner lining tube (24) away from the grain discharge pipe (122). Liquid outlet channels (221) are arranged inside the rotating frame (22) corresponding to each gradient pressure plate (23). The connecting tubes (222) on each gradient pressure plate (23) are respectively connected to the corresponding liquid outlet channels (221), and the liquid outlet channels (221) are arranged corresponding to the liquid outlet slits (241). The inner cavity of the inner lining tube (24) is connected to the high-pressure pump through a pipeline.

9. The equipment for preparing camellia modal fiber according to claim 8, characterized in that: A secondary filter assembly (3) is arranged below the arc-shaped filter plate (123), the secondary filter assembly (3) comprising a filter belt (31) and a support roller group (32), the support roller group (32) being installed in the separation box (11), the filter belt (31) being arranged outside the support roller group (32), and the filter belt (31) being supported by the support roller group (32) to form a crawler-type structure, so that the filter belt (31) forms an upper region (311) and a lower region (312) of two upper and lower parts, the secondary filter assembly (3) further comprising a discharge box (33), the discharge box (33) being installed below the filter belt (31), and the separation box (11) A centralized guide bucket (13) is provided in the discharge box (11), the centralized guide bucket (13) is located between the arc-shaped filter plate (123) and the filter screen belt (31), the bottom of the centralized guide bucket (13) is a contraction opening structure, a soft scraper (34) is fixedly installed in the discharge box (33), the top end of the soft scraper (34) is in contact with the lower area (312) of the filter screen belt (31), and a liquid leakage port is provided in the middle of the discharge box (33) corresponding to the position of the centralized guide bucket (13), a transfer filter screen (331) is fixedly installed on the bottom wall of the discharge box (33), and the discharge box (33) and the separation box (11) are detachably installed.

10. The equipment for preparing camellia modal fiber according to claim 9, characterized in that: The supporting roller group (32) comprises two groups of fixed rotating rollers (321) and two groups of movable rotating rollers (322); the fixed rotating rollers (321) and the movable rotating rollers (322) are both rotatably arranged inside the separation box (11); the fixed rotating rollers (321) are rotatably connected to the separation box (11); a slide groove (14) is provided at a position of the separation box (11) corresponding to the end of the movable rotating roller (322); a slider (323) is rotatably installed at the end of the movable rotating roller (322); the slider (323) is slidably installed in the slide groove (14), and a thrust elastic member is installed between the slider (323) and the slide groove (14).

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