Camellia fiber modal fabric preparation process and equipment thereof
Camellia modal fiber was prepared by loading camellia extract onto a porous carrier during the spinning process, which solved the problem of the antibacterial agent affecting the breathability of modal fiber and achieved the preparation of highly efficient antibacterial, breathable and comfortable fiber.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-18
- Publication Date
- 2026-04-07
AI Technical Summary
Existing antibacterial agents for modal fibers form a film on the fiber surface, affecting the fabric's breathability and comfort, resulting in a less comfortable feel when worn in hot environments.
Camellia extract was loaded onto a porous carrier during the spinning process to prepare camellia modal fibers. Combining the properties of modal fibers, bacterial growth was directly inhibited without the need for surface coating. The fibers were prepared using a wet spinning process.
Camellia modal fiber has natural antibacterial properties, maintains good breathability and comfort, softness and moisture absorption, while improving production efficiency.
Smart Images

Figure CN119800538B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of fiber preparation, and more particularly to a camellia flower modal fiber preparation process and equipment thereof. BACKGROUND
[0002] Modal fiber is a regenerated cellulose fiber, and its chemical composition is cellulose. The international standard ISO2076:1999 (E) defines modal fiber, which is a regenerated cellulose fiber made of a specific viscose and a regenerated bath composition, with high wet modulus and high breaking strength, and can achieve a higher degree of molecular orientation when the fiber is stretched and coagulated. Modal fiber has good moisture absorption, stable performance, comfortable wearing and other advantages, and is an ideal close-fitting fabric and health care clothing product.
[0003] Modal fiber has been widely used in many clothing and home products due to its excellent softness, moisture absorption and comfort, but its antibacterial performance is weak, so it needs to be treated with antibacterial agent to enhance its antibacterial performance. However, the existing modal fiber antibacterial treatment materials (such as antibacterial agent or antibacterial coating) can improve the antibacterial property to some extent, but also have some disadvantages and limitations, for example, the addition of antibacterial agent is mainly after the formation of fiber, a thin film is formed on the surface of modal fiber to improve the antibacterial effect, but the existence of the coating will affect the air permeability and comfort of the fabric, and the wearer will not feel cool enough in hot environment, affecting the wearing experience. SUMMARY
[0004] The present application provides a camellia flower modal fiber preparation process and equipment, which solves the problem that the existing addition of modal fiber antibacterial agent is mainly after the formation of fiber, a thin film is formed on the surface of modal fiber, but the existence of the coating will affect the air permeability and comfort of the fabric, and the wearer will not feel cool enough in hot environment, affecting the wearing experience.
[0005] To achieve the above purpose, the present application provides the following technical scheme: a camellia flower modal fiber preparation process, comprising the following steps:
[0006] Step one, prepare a porous carrier, hexadecyl trimethyl ammonium bromide and polyethylene glycol PEG-6000 are put into deionized water, stirred for 30 min, then continue to put mesitylene, stir for 30 min, then put water glass at a feeding rate of 1 g / min, continue to stir for 1.5 h after the water glass feeding is completed, adjust the PH value of the solution to 10, transfer to the reactor for crystallization, then filter out the crystal grains through the filtering equipment, wash and dry at 80℃ for 18 h, and calcine at 450℃ for 4 h to prepare the porous carrier;
[0007] Step 2: Modification of the porous carrier. The porous carrier was added to 35 parts by weight of ethanol solution and ultrasonically dispersed evenly. Under stirring, silane coupling agent KH-550 and silane coupling agent KH-580 were added dropwise at a rate of 2 mL / min. After the addition was completed, the pH was adjusted to 4.5, stirred and heated to 50°C, kept at this temperature, and stirred under reflux for 5 hours. The solid was separated by centrifugation, washed, and dried at 45°C to obtain the modified porous carrier.
[0008] Step 3: Preparation of functional components. Under light-protected conditions, the modified porous carrier is added to a solution containing 90 parts by weight of camellia components. The temperature is raised to 30°C, and the mixture is stirred at 50 rpm for 20 hours for adsorption. After washing, the mixture is dried at 45°C under a vacuum of 0.01 MPa until the moisture content is 1 wt%, thus obtaining the functional components, namely the modified porous carrier loaded with camellia.
[0009] Step 4: Prepare spinning solution. Add a modified porous carrier loaded with camellia flowers to the spinning solution, mix evenly, and then stir and dissolve under vacuum for 5 hours. Degas and filter to obtain a uniform and stable spinning solution.
[0010] Step 5: Spinning. Camellia modal fiber is produced by wet spinning process.
[0011] In a preferred embodiment, in step one, when cetyltrimethylammonium bromide and polyethylene glycol PEG-6000 are added to deionized water at a temperature of 35°C, a 2 mol / L hydrochloric acid solution is used as an adjusting agent to adjust the pH value. After pH adjustment, the solution is kept at this temperature and allowed to stand for 12 hours. During crystallization, the temperature is raised to 105°C and crystallized for 20 hours. In step two, acetic acid is used as an adjusting agent to adjust the pH value. The stirring process after pH adjustment is carried out under nitrogen protection and in the dark.
[0012] In a preferred embodiment, the washing process in step one uses 12 times the volume of deionized water, the washing process in step two first uses 8 times the volume of anhydrous ethanol 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.
[0013] In a preferred embodiment, the pH adjustment reagent used in steps one and two is added in two stages. In the first stage, three-quarters of the reagent is added and stirred. Then, the second stage of pH adjustment is carried out drop by drop while stirring continuously to ensure that the acetic acid added each time is fully mixed until the pH value stabilizes within the required range. After stopping the addition of acetic acid, stirring is continued for a few minutes to ensure that the pH value no longer changes. Then, the pH value is measured again to confirm the final pH value.
[0014] Step five, the wet spinning process, includes the following steps:
[0015] Step a: The spinning solution from step four is extruded through the small holes of the spinneret to form a thin stream. The thin stream enters the coagulation bath, where phase separation occurs, the solvent is replaced, and the polymer coagulates to form solid fibers.
[0016] Step b: After leaving the coagulation bath, the newly formed fibers are stretched by a stretching device, and the fiber stretching ratio is 1-1.5.
[0017] Step c: Soak the nascent fibers in an oil, wash, dehydrate, and dry them to obtain the final fiber material. The oil is an aqueous solution of amino silicone oil with a volume percentage concentration of 0.05-0.5% and a soaking time of 2-12 hours.
[0018] Step d: Roll up and package the treated fibers for subsequent textile processing.
[0019] A camellia modal fiber preparation device includes a filtration device, which includes a separation box. The top of the separation box is provided with a cylindrical part, and the bottom of the separation box is provided with a liquid outlet. The top of the cylindrical part is provided with a feeding pipe, and one side of the cylindrical part is provided with a crystal discharge pipe. The cylindrical part is provided with a main filtration assembly, which includes an eccentric rotating shaft. The bottom of the cylindrical part is provided with an arc-shaped filter plate.
[0020] In a preferred embodiment, an eccentric shaft is rotatably mounted inside the cylindrical section. The eccentric shaft is located below the axis of the cylindrical section and close to the grain discharge pipe. A rotating frame is fixedly mounted on the outside of the eccentric shaft. Multiple sets of gradient pressure plates are provided on the circumferential sidewall of the rotating frame. The end of the gradient pressure plate near the rotating frame is rotatably connected to the rotating frame. The gradient pressure plate is inclined on the rotating frame along the side opposite to the rotation direction of the rotating frame. A torsional elastic element is provided between the gradient pressure plate and the rotating frame. The torsional elastic element is used to provide a spring force to the gradient pressure plate to flip away from the rotating frame.
[0021] In a preferred embodiment, a scraper is fixedly connected to the end of the gradient pressure plate away from the rotating frame. The scraper has a convex structure and a liquid release groove is provided in the middle of the scraper. An inner punch is provided on one side of the scraper corresponding to the gradient pressure plate. The inner punch communicates with 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 diluent. The diluent supply system is used to supply diluent to the liquid release groove.
[0022] In a preferred embodiment, the eccentric rotating shaft is provided with an inner liner tube, which is fixedly installed in the cylindrical part. The rotating frame is a solid structure. A liquid outlet slit is provided on the side of the inner liner tube opposite to the grain discharge pipe. A liquid outlet channel is provided inside the rotating frame corresponding to each gradient pressure plate. The connecting pipe on each gradient pressure plate is connected to the corresponding liquid outlet channel, and the liquid outlet channel is provided corresponding to the liquid outlet slit. The inner cavity of the inner liner tube is connected to the high-pressure pump through a pipe.
[0023] In a preferred embodiment, a secondary filtration assembly is provided below the arc-shaped filter plate. The secondary filtration assembly includes a filter belt and a support roller assembly. The support roller assembly is installed inside the separation box, and the filter belt is located outside the support roller assembly. The support roller assembly supports the filter belt to form a track-like structure, so that the filter belt forms an upper region and a lower region. The secondary filtration assembly also includes a discharge box, which is installed below the filter belt. A centralized guide hopper is provided in the separation box. The centralized guide hopper is located between the arc-shaped filter plate and the filter belt. The bottom of the centralized guide hopper has a constriction structure. A soft scraper is fixedly installed in the discharge box. The top of the soft scraper contacts the lower region of the filter belt, and a leakage port is provided in the middle of the discharge box corresponding to the position of the centralized guide hopper. A transfer filter is fixedly installed on the bottom wall of the discharge box. The discharge box and the separation box are detachable.
[0024] In a preferred embodiment, the support roller group includes two sets of fixed rotating rollers and two sets of movable rotating rollers. Both the fixed rotating rollers and the movable rotating rollers are rotatably disposed inside the separation box. The fixed rotating rollers are rotatably connected to the separation box. The separation box is provided with a sliding groove at the position corresponding to the end of the movable rotating roller. A slider is rotatably installed at the end of the movable rotating roller. The slider is slidably installed in the sliding groove, and a thrust elastic element is installed between the slider and the sliding groove.
[0025] The beneficial effects of this invention are as follows: The camellia modal fiber obtained by this invention naturally contains camellia extract. Since camellia itself has certain antibacterial properties, combined with the characteristics of modal fiber, this fiber can inhibit bacterial growth and reduce odor. Therefore, there is no need to form a coating on the fiber surface, thus ensuring that the subsequently manufactured fabric has good breathability. Moreover, camellia is a natural plant component, making the resulting fiber gentler on the skin, further enhancing the softness and comfort of the fabric, while also providing excellent breathability and moisture absorption. The gradual pressure plate movement of this invention also drives the crystal movement until the squeezed crystals slide out of the crystal discharge pipe, achieving crystal separation. This avoids the problem of crystals accumulating in the same area during filtration, making it difficult for the solution to penetrate downwards. Simultaneously, the gradual squeezing of the gradual pressure plate also improves the separation efficiency between the solution and the crystals. This not only achieves sufficient solution separation but also enables continuous operation of the equipment, adapting to large-scale crystal filtration production and greatly improving the production efficiency of camellia modal fiber. Attached Figure Description
[0026] Figure 1 This is a flowchart of the preparation method of the present invention.
[0027] Figure 2 This is a flow chart of the wet spinning process of the present invention.
[0028] Figure 3This is a schematic diagram of the overall structure of the filtration device of the present invention.
[0029] Figure 4 This is a schematic diagram of the internal structure of the filtration device of the present invention.
[0030] Figure 5 This is a schematic diagram of the overall structure of the main filter component of the present invention.
[0031] Figure 6 This is a schematic diagram of the overall structure of the secondary filter component of the present invention.
[0032] Figure 7 For the present invention Figure 6 A schematic diagram of the structure of part A.
[0033] Figure 8 This is a schematic diagram of the improved main filter assembly of the present invention.
[0034] Figure 9 For the present invention Figure 8 Enlarged view of the structure of part B.
[0035] Figure 10 This is a diagram showing the state of the diluent being released from the release tank of the present invention.
[0036] Figure 11 This is a schematic diagram of the inner liner tube of the present invention.
[0037] Figure 12 This is a diagram showing the fit between the inner liner tube and the eccentric rotating shaft of the present invention.
[0038] The attached figures are labeled as follows: 1. Filtration equipment; 11. Separation box; 111. Liquid outlet; 12. Cylindrical section; 121. Feeding pipe; 122. Crystal discharge pipe; 123. Arc-shaped filter plate; 13. Centralized guide hopper; 14. Slide chute; 2. Main filtration assembly; 21. Eccentric rotating shaft; 22. Rotating frame; 221. Liquid outlet channel; 222. Connecting pipe; 23. Gradient pressure plate; 231. Scraper; 232. Liquid release tank; 233. Inner punch slit; 24. Inner liner pipe; 241. Liquid outlet slit; 3. Secondary filtration assembly; 31. Filter belt; 311. Upper area; 312. Lower area; 32. Support roller group; 321. Fixed rotating roller; 322. Moving rotating roller; 323. Sliding block; 324. Annular groove; 33. Discharge box; 331. Transfer filter screen; 34. Soft scraper. Detailed Implementation
[0039] The present application will now be described in further detail with reference to the accompanying drawings. It should be noted that the following specific embodiments are only used to further illustrate the present application and should not be construed as limiting the scope of protection of the present application. Those skilled in the art can make some non-essential improvements and adjustments to the present application based on the above application content.
[0040] Example 1, refer to the appendix of the instruction manual Figure 1 A process for preparing camellia modal fiber includes the following steps:
[0041] Step 1: Preparation of porous support. Cetyltrimethylammonium bromide and polyethylene glycol PEG-6000 were added to deionized water at 35°C and stirred for 30 min. Then, mesitylene was added and stirred for another 30 min. Water glass was added at a feeding rate of 1 g / min. After the water glass was added, stirring was continued for 1.5 h. The pH was adjusted to 10 with a 2 mol / L hydrochloric acid solution and kept at this temperature for 12 h. Then, the mixture was transferred to a reactor, heated to 105°C, and kept at this temperature for crystallization for 20 h. The crystals were filtered out using filter 1, washed with 12 times the volume of deionized water, dried at 80°C for 18 h, and calcined at 450°C for 4 h to obtain the porous support.
[0042] Step 2: Modification of the porous carrier. The porous carrier was added to 35 parts by weight of ethanol solution and ultrasonically dispersed evenly. Under stirring conditions, silane coupling agent KH-550 and silane coupling agent KH-580 were added dropwise at a rate of 2 mL / min. After the addition was completed, the pH value was adjusted to 4.5 with acetic acid. Under nitrogen protection and in the dark, the mixture was stirred and heated to 50°C, kept at this temperature, and stirred under reflux for 5 hours. The solid was separated by centrifugation, washed with 8 volumes of anhydrous ethanol, then washed with 18 volumes of deionized water, and finally dried at 45°C to obtain the modified porous carrier.
[0043] Step 3: Preparation of functional components. Under light-protected conditions, the modified porous carrier is added to a solution containing 90 parts by weight of camellia components. The temperature is raised to 30°C, and the mixture is stirred at 50 rpm for 20 hours for adsorption. Then, it is washed with 12 times the volume of deionized water and dried at 45°C under a vacuum of 0.01 MPa until the moisture content is 1 wt%, thus obtaining the functional components, namely the modified porous carrier loaded with camellia.
[0044] Step 4: Prepare spinning solution. Add a modified porous carrier loaded with camellia flowers to the spinning solution, mix evenly, and then stir and dissolve under vacuum for 5 hours. Degas and filter to obtain a uniform and stable spinning solution.
[0045] Step 5: Spinning. Camellia modal fiber is produced by wet spinning process.
[0046] The camellia-containing solution used in the above embodiments is a pre-prepared material. Dried camellia petals or leaves are selected as the source of the extract to ensure that the raw material is free of impurities and mold. Water is selected as the solvent, and supercritical carbon dioxide extraction is used. During extraction, a supercritical carbon dioxide extraction device is used. The camellia raw material is loaded into the extraction tank, and the pressure and temperature are adjusted (e.g., 30-40 MPa, 35-45℃) to make the carbon dioxide in a supercritical state. By adjusting the flow rate and extraction time (e.g., 1-3 h), the effective components in the camellia are extracted. The extracted liquid is collected and separated under reduced pressure to obtain a solution rich in camellia components.
[0047] The extract is then further purified using nanofiltration or reverse osmosis membrane separation technology to remove macromolecular impurities and insoluble substances. Activated carbon can also be used to adsorb and remove pigments and other impurities, improving the color and purity of the extract.
[0048] The prepared camellia extract solution was analyzed using HPLC, gas chromatography (GC), and mass spectrometry (MS) to determine the content and proportion of the main components in the extract to ensure that it met expectations. Then, it was stored in a light-proof and low-temperature environment (such as 4°C) to avoid the decomposition of active ingredients caused by light and high temperature.
[0049] In the above embodiment, the pH adjustment reagents used in steps one and two (i.e., hydrochloric acid in step one and acetic acid in step two) are added in two stages. In the first stage, three-quarters of the amount is added and stirred. Then, the adjustment reagent is added drop by drop using a dropper for the second stage of addition, while stirring continuously to ensure that the acetic acid added each time is fully mixed. After each addition of a certain amount of acetic acid, wait for a moment (about 10-30 seconds) to allow the pH value to stabilize, and then measure the pH value again.
[0050] When the pH value is very close to the target value, use a micropipette to make extremely fine adjustments until the pH value stabilizes within the required 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 value no longer changes, and then measure again to confirm the final pH value.
[0051] Further, please refer to the appendix to the instruction manual. Figure 2 Step five, the wet spinning process, includes the following steps:
[0052] Step a: The spinning solution from step four is extruded through the small orifices of the spinneret (micropores on the spinneret) to form a fine stream. This stream enters the coagulation bath, where phase separation occurs, the solvent is displaced, and the polymer coagulates to form solid fibers. The coagulation bath is a crucial part of wet spinning; it typically 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 the coagulation bath medium in the production of polyacrylonitrile fibers because it can effectively extract the solvent from the spinning solution.
[0053] Step b: After leaving the coagulation bath, the newly formed fibers are stretched by a stretching device, and the fiber stretching ratio is 1-1.5.
[0054] Step c: Soak the nascent fibers in an oil, wash, dehydrate, and dry them to obtain the final fiber material. The oil 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 a soaking time of 2-12 hours.
[0055] Step d: Roll up and package the treated fibers for subsequent textile processing.
[0056] It should be noted that the camellia modal fiber provided by this 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 odor. Therefore, there is no need to form a coating on the fiber surface, thus ensuring that the fabric produced has good breathability. Moreover, camellia is a natural plant component, and the resulting fiber is gentler on the skin, further enhancing the softness and comfort of the fabric. At the same time, it also gives the fabric excellent breathability and moisture absorption.
[0057] Example 2: In the preparation process of the above-mentioned camellia modal fiber, after crystallization, it is necessary to filter out the crystal grains. In the process of filtering out the crystal grains, a filtration device is required. In specific operation, the solution is input into the filtration device for filtration. If necessary, the filtration device can be connected to a vacuum device to extract the solution by using vacuum suction, thereby accelerating the filtration of crystal grains.
[0058] However, as the solution is continuously poured in, the number and thickness of the crystals on the filter element increase. During filtration, the solution poured in later is drawn out from top to bottom. In other words, as the solution is poured in, it needs to pass through the crystals that have already been filtered out before it can be filtered out. As the thickness gradually increases, the suction force required for filtration also increases, making filtration increasingly difficult. When the crystals reach a certain thickness, they must be removed from the filter element before filtration can continue, resulting in a discontinuous filtration process and low efficiency.
[0059] Therefore, the present invention also provides a camellia modal fiber preparation device, specifically, please refer to the appendix of the specification. Figures 3 to 12 The filter includes a filter device 1, which includes a separation box 11. The top of the separation box 11 is provided with a cylindrical part 12, and the bottom of the separation box 11 is provided with a liquid outlet 111. The main filter assembly 2 is provided in the cylindrical part 12.
[0060] The main filter assembly 2 includes an eccentric rotating shaft 21, a feeding pipe 121 at the top of the cylindrical part 12, and a crystal discharge pipe 122 on one side of the cylindrical part 12. In actual use, the feeding pipe 121 is connected to the crystallization reactor, and the formed crystals and solution are fed into the cylindrical part 12 together. The liquid outlet 111 is connected to a vacuum device to accelerate the passage of liquid through the main filter assembly 2. The crystal discharge pipe 122 is connected to a closed container for collecting the separated crystals. The bottom of the cylindrical part 12 is set as an arc-shaped filter plate 123. The cylindrical part 12 and the arc-shaped filter plate 123 together form a horizontally arranged cylindrical structure.
[0061] The eccentric shaft 21 is rotatably installed inside the cylindrical part 12. A drive motor for driving the eccentric shaft 21 to rotate is provided on the separation box 11. The eccentric shaft 21 is located below the axis of the cylindrical part 12 and close to the crystal discharge pipe 122. A rotating frame 22 is fixedly installed on the outside of the eccentric shaft 21. Multiple sets of gradient pressure plates 23 are provided on the circumferential side wall of the rotating frame 22. The end of the gradient pressure plate 23 near the rotating frame 22 is rotatably connected to the rotating frame 22. The gradient pressure plate 23 is inclined on the rotating frame 22 along the side opposite to the rotation direction of the rotating frame 22. A torsional elastic element is provided between the gradient pressure plate 23 and the rotating frame 22. The torsional elastic element is preferably a torsional spring. The torsional elastic element is used to provide a spring force to the gradient pressure plate 23 to flip away from the rotating frame 22. Under the action of this spring force, the end of the gradient pressure plate 23 away from the rotating frame 22 is in contact with the arc-shaped filter plate 123 or the inner side wall of the cylindrical part 12.
[0062] It should be noted that by setting the eccentric rotating shaft 21 eccentrically, the distance between the eccentric rotating shaft 21 and the cylindrical part 12 or the arc-shaped filter plate 123 varies, thus forming short-spacing and long-spacing regions. In use, the crystallization solution after the crystallization reaction is input through the feeding pipe 121, and the rotating frame 22 is driven by a drive motor. The crystallization solution first falls between two adjacent sets of gradient pressure plates 23. When the solution and crystals move to the arc-shaped filter plate 123, the solution flows downwards to form filtration, and the crystals are filtered onto the inner wall of the arc-shaped filter plate 123. As the gradient pressure plate 23 moves, the crystals gradually enter the lower region of the gradient pressure plate 23. When the gradient pressure plate 23, following the rotating frame 22, gradually rotates to the short-spacing region between the eccentric rotating shaft 21 and the arc-shaped filter plate 123, the gradient pressure plate 23 and the arc-shaped filter plate 123 form a... The pressure plate 23 is compressed, which in turn compresses the crystals on the arc-shaped filter plate 123, squeezing out the residual solution in the crystals and continuing filtration. As the gradient pressure plate 23 continues to move, and because the tail end of the gradient pressure plate 23 is always in contact with the arc-shaped filter plate 123 under the action of the torsional elastic element, the movement of the gradient pressure plate 23 also drives the crystals to move, until the compressed crystals are carried to the crystal discharge pipe 122 and slide out, realizing the separation of crystals. This avoids the problem of crystals accumulating in the same area during filtration, which makes it difficult for the solution to penetrate downwards into the crystals. At the same time, with the gradual compression of the gradient pressure plate 23, the separation efficiency between the solution and the crystals can also be improved. This not only achieves the function of fully separating the solution, but also realizes the continuous operation of the equipment, which can adapt to large-scale crystal filtration production and greatly improve the production efficiency of camellia modal fiber.
[0063] Furthermore, in order to ensure that the end of the gradient pressure plate 23 can always fit against the arc-shaped filter plate 123 and the cylindrical part 12 and drive the crystals to move, a scraper 231 is fixedly connected to the end of the gradient pressure plate 23 away from the rotating frame 22. The scraper 231 has a convex structure. The scraper 231 moves together with the gradient pressure plate 23, which can prevent the arc-shaped filter plate 123 from clogging and improve the filtration effect and the cleaning effect on the arc-shaped filter plate 123.
[0064] Furthermore, in the above embodiment, the pH value of the solution needs to be adjusted to 10 before the crystallization reaction. Therefore, the pH value of the overall solution after crystallization is relatively high, which will cause some corrosion to the material. Each processing equipment can be treated with anti-corrosion on its surface. However, under the action of the torsion elastic element, 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. To this end, this embodiment also provides the following technical solution: Specifically, a liquid release groove 232 is provided in the middle of the scraper 231, and an inner punch 233 is provided on one side of the scraper 231 corresponding to the gradient pressure plate 23. The inner punch 233 is connected to the liquid release groove 232, and the liquid release groove 232 is connected to a diluent supply system through a connecting pipe 222. The system includes a high-pressure pump and a diluent. The diluent is supplied to the release tank 232, thereby adjusting the pH value of the solution around the scraper 231 and reducing the corrosive effect of the solution on the scraper 231. At the same time, the diluent output from the release tank 232 has a certain pressure, which provides a thrust to the scraper 231 away from the surface of the arc-shaped filter plate 123, reducing the pressure between the scraper 231 and the arc-shaped filter plate 123, thereby reducing wear and increasing the service life of the gradient pressure plate 23. Meanwhile, the diluent output from the release tank 232 also flows outward from the inner punch 233, which will create a certain outward impact on the grains gathered at the scraper 231, avoiding abrasion between the scraper 231 and the grains, and further improving the filtration effect on the grains.
[0065] It should be noted that the above-mentioned diluent can be deionized water or other acidic solutions that do not affect the grains, thereby effectively neutralizing or diluting the solution near the scraper 231 and reducing the corrosive effect on the scraper 231.
[0066] Furthermore, when the gradient pressure plate 23 moves toward the crystal discharge pipe 122, the filtration is complete. At this time, the liquid release tank 232 should not output diluent. Therefore, the diluent supply system needs to stop supplying diluent when the gradient pressure plate 23 is about to reach the crystal discharge pipe 122. To this end, this embodiment also provides the following technical solution: an inner liner 24 is provided inside the eccentric rotating shaft 21. The inner liner 24 is fixedly installed in the cylindrical part 12 (only one end of the eccentric rotating shaft 21 passes through the side wall of the cylindrical part 12 and is rotatably connected to the cylindrical part 12; the inner liner 24 is fixedly connected to the cylindrical part 12 at the position corresponding to the other end of the eccentric rotating shaft 21, thereby achieving a fixed connection between the inner liner 24 and the cylindrical part 12 under the premise of forming a rotational support for the eccentric rotating shaft 21). The rotating frame 22 is a solid structure. A liquid outlet slit 241 is provided on the side of the inner liner 24 away from the crystal discharge pipe 122. A diluent supply slit 241 is provided inside the rotating frame 22 corresponding to each gradient pressure plate 23. The device is equipped with a liquid outlet channel 221. The connecting pipes 222 on each gradient pressure plate 23 are connected to the corresponding liquid outlet channel 221, and the liquid outlet channel 221 is set with a corresponding liquid outlet slit 241. The inner cavity of the inner liner tube 24 is connected to the high-pressure pump through a pipe, thereby realizing the connection between the connecting pipe 222 and the diluent supply system. In actual use, before the gradient pressure plate 23 approaches the crystal discharge pipe 122, its corresponding liquid outlet channel 221 is connected to the liquid outlet slit 241. Therefore, liquid can be guaranteed to be discharged from the release tank 232 during this process. When the gradient pressure plate 23 approaches the crystal discharge pipe 122 and the scraper 231 gradually reaches the crystal discharge pipe 122, the corresponding liquid outlet channel 221 is separated from the liquid outlet slit 241 and gradually goes around to the side of the inner liner tube 24 away from the liquid outlet slit 241, thereby blocking the liquid outlet channel 221. At this time, the release tank 232 no longer discharges liquid and will not affect the discharge of crystals from the crystal discharge pipe 122.
[0067] In the aforementioned method, some fine crystals may pass through the arc-shaped filter plate 123 along with the solution, causing filtration leakage, which in turn leads to material waste and may even affect the vacuum equipment. Therefore, this embodiment provides the following solution: Specifically, a secondary filter assembly 3 is provided below the arc-shaped filter plate 123. The secondary filter assembly 3 includes a filter belt 31 and a support roller group 32. The support roller group 32 is installed inside the separation box 11, and the filter belt 31 is disposed outside the support roller group 32, forming a track-like structure supported by the support roller group 32. This allows the filter belt 31 to form an upper region 311 and a lower region 312. The support roller group 32 is connected to a driving device, which is used for... The drive filter belt 31 moves like a track. The secondary filter assembly 3 also includes a discharge box 33, which is installed below the filter belt 31. A centralized guide hopper 13 is provided in the separation box 11. The centralized guide hopper 13 is located between the arc-shaped filter plate 123 and the filter belt 31. The bottom of the centralized guide hopper 13 has a constriction 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. A leakage port is provided in the middle of the discharge box 33 corresponding to the position of the centralized guide hopper 13. A transfer filter screen 331 is fixedly installed on the bottom wall of the discharge box 33. The discharge box 33 and the separation box 11 can be detachably installed.
[0068] Furthermore, both the filter belt 31 and the intermediate filter screen 331 are made of filter cloth material, and the support roller group 32 includes two sets of fixed rotating rollers 321 and two sets of moving rotating rollers 322. The two sets of moving rotating rollers 322 are located above the two sets of fixed rotating rollers 321. Both the fixed rotating rollers 321 and the moving rotating rollers 322 are rotatably arranged inside the separation box 11. The driving device is a drive motor, which is fixedly installed outside the separation box 11 and is connected to one of the sets of fixed rotating rollers 321.
[0069] The side wall of the separation box 11 has an installation port, and the interior of the separation box 11 is equipped with a support frame structure. The discharge box 33 is inserted into the support frame structure through the installation port and slides with the separation box 11 to form a pull-out drawer. Thus, the discharge box 33 can be pulled out for cleaning when needed (the soft scraper 34 is an elastic component. When the discharge box 33 is pulled out, the soft scraper 34 can deform adaptively without affecting the pulling out and putting in the discharge box 33).
[0070] In actual use, the movement of the filter belt 31 is periodically controlled to exchange the materials in the upper region 311 and the lower region 312. The filtered crystals are scraped into the discharge box 33 by the soft scraper 34. At the same time, the filter belt 31 always has a clean surface facing the solution, so as to achieve sufficient 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 filtration. The leaked crystals scraped into the discharge box 33 can be periodically removed and cleaned. When the discharge box 33 is removed, the filter belt 31 is still filtering in the separation box 11.
[0071] Furthermore, in order to ensure that the filter belt 31 has sufficient elasticity and fully contacts the soft scraper 34, this embodiment also provides the following technical solution: the fixed roller 321 is fixed in position relative to the separation box 11, and the fixed roller 321 is directly rotatably connected to the separation box 11. The separation box 11 is provided with a sliding groove 14 at the position corresponding to the end of the moving roller 322. A slider 323 is rotatably installed at the end of the moving roller 322. The slider 323 is slidably installed in the sliding groove 14, and a thrust elastic element is installed between the slider 323 and the sliding groove 14. The thrust elastic element is used to provide a tensioning force to the slider 323 to tighten the filter belt 31, so that the filter belt 31 can effectively contact the soft scraper 34.
[0072] The embodiments described above are merely examples of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention.
Claims
1. A process device for preparing camellia modal fiber, comprising a filtration device (1), wherein the filtration device (1) includes a separation box (11), the top of the separation box (11) is provided with a cylindrical part (12), the bottom of the separation box (11) is provided with a liquid outlet (111), the top of the cylindrical part (12) is provided with a feeding pipe (121), and one side of the cylindrical part (12) is provided with a crystal discharge pipe (122), characterized in that: The cylindrical part (12) is provided with a main filter assembly (2), the main filter assembly (2) includes an eccentric rotating shaft (21), and the bottom of the cylindrical part (12) is provided with an arc-shaped filter plate (123). The eccentric shaft (21) is rotatably installed inside the cylindrical part (12). The eccentric shaft (21) is located below the axis of the cylindrical part (12) and close to the grain discharge pipe (122). A rotating frame (22) is fixedly installed on the outside of the eccentric shaft (21). Multiple sets of gradient pressure plates (23) are provided on the circumferential side wall of the rotating frame (22). The 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 inclined on the rotating frame (22) along the side opposite to the rotation direction of the rotating frame (22). A torsional elastic element is provided between the gradient pressure plate (23) and the rotating frame (22). The torsional elastic element is used to provide elastic force to the gradient pressure plate (23) to flip away from the rotating frame (22).
2. The equipment for preparing camellia modal fiber according to claim 1, characterized in that: The end of the gradient pressure plate (23) away from the rotating frame (22) is fixedly connected to a scraper (231). The scraper (231) has a convex structure. A liquid release groove (232) is provided in the middle of the scraper (231). An inner punch (233) is provided on one side of the scraper (231) corresponding to the gradient pressure plate (23). The inner punch (233) is connected to the liquid release groove (232). The liquid release groove (232) is connected to a diluent supply system through a connecting pipe (222). The diluent supply system includes a high-pressure pump and diluent. The diluent supply system is used to supply diluent to the liquid release groove (232).
3. The equipment for preparing camellia modal fiber according to claim 2, characterized in that: The eccentric rotating shaft (21) is provided with an inner liner tube (24), which is fixedly installed in the cylindrical part (12). The rotating frame (22) is a solid structure. A liquid outlet slit (241) is provided on the side of the inner liner tube (24) away from the grain discharge pipe (122). A liquid outlet channel (221) is provided inside the rotating frame (22) corresponding to each gradient pressure plate (23). The connecting pipe (222) on each gradient pressure plate (23) is connected to the corresponding liquid outlet channel (221). The liquid outlet channel (221) is provided corresponding to the liquid outlet slit (241). The inner cavity of the inner liner tube (24) is connected to the high-pressure pump through a pipe.
4. The equipment for preparing camellia modal fiber according to claim 3, characterized in that: A secondary filter assembly (3) is provided below the arc-shaped filter plate (123). The secondary filter assembly (3) includes a filter belt (31) and a support roller group (32). The support roller group (32) is installed inside the separation box (11). The filter belt (31) is located outside the support roller group (32) and is supported by the support roller group (32) to form a track-like structure, so that the filter belt (31) forms an upper region (311) and a lower region (312). The secondary filter assembly (3) also includes a discharge box (33), which is installed below the filter belt (31). The separation box (11) 11) is provided with a centralized guide bucket (13), which is located between the arc-shaped filter plate (123) and the filter belt (31). The bottom of the centralized guide bucket (13) is a constriction structure. A soft scraper (34) is fixedly installed in the discharge box (33). The top of the soft scraper (34) contacts the lower area (312) of the filter belt (31). A 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). The discharge box (33) and the separation box (11) are detachable.
5. The equipment for preparing camellia modal fiber according to claim 4, characterized in that: The support roller group (32) includes two sets of fixed rotating rollers (321) and two sets of moving rotating rollers (322). The fixed rotating rollers (321) and the moving rotating rollers (322) are rotatably arranged inside the separation box (11). The fixed rotating rollers (321) are rotatably connected to the separation box (11). The separation box (11) is provided with a sliding groove (14) at the position corresponding to the end of the moving rotating roller (322). A slider (323) is rotatably installed at the end of the moving rotating roller (322). The slider (323) is slidably installed in the sliding groove (14), and a thrust elastic element is installed between the slider (323) and the sliding groove (14).
6. A process for preparing camellia modal fiber, characterized in that, The preparation process using the equipment described in claim 5 for camellia modal fiber includes the following steps: Step 1: Prepare a porous carrier. Add hexadecyltrimethylammonium bromide and polyethylene glycol PEG-6000 to deionized water and stir for 30 min. Then add mesitylene and stir for another 30 min. Add water glass at a feeding rate of 1 g / min. After the water glass is added, continue stirring for 1.5 h. Adjust the pH of the solution to 10 and transfer it to the reactor for crystallization. Then filter out the crystals through a filter (1). After washing, dry at 80°C for 18 h and calcine at 450°C for 4 h to prepare a porous carrier. Step 2: Modification of the porous carrier. The porous carrier was added to 35 parts by weight of ethanol solution and ultrasonically dispersed evenly. Under stirring, silane coupling agent KH-550 and silane coupling agent KH-580 were added dropwise at a rate of 2 mL / min. After the addition was completed, the pH was adjusted to 4.5, stirred and heated to 50°C, kept at this temperature, and stirred under reflux for 5 hours. The solid was separated by centrifugation, washed, and dried at 45°C to obtain the modified porous carrier. Step 3: Preparation of functional components. Under light-protected conditions, the modified porous carrier is added to a solution containing 90 parts by weight of camellia components. The temperature is raised to 30°C, and the mixture is stirred at 50 rpm for 20 hours for adsorption. After washing, the mixture is dried at 45°C under a vacuum of 0.01 MPa until the moisture content is 1 wt%, thus obtaining the functional components, namely the modified porous carrier loaded with camellia. Step 4: Prepare spinning solution. Add a modified porous carrier loaded with camellia flowers to the spinning solution, mix evenly, and then stir and dissolve under vacuum for 5 hours. Degas and filter to obtain a uniform and stable spinning solution. Step 5: Spinning. Camellia modal fiber is produced by wet spinning process.
7. The process for preparing camellia modal fiber according to claim 6, characterized in that: In step one, when cetyltrimethylammonium bromide and polyethylene glycol PEG-6000 are added to deionized water at a temperature of 35°C, a 2 mol / L hydrochloric acid solution is used as an adjusting agent to adjust the pH value. After pH adjustment, the solution is kept at this temperature and allowed to stand for 12 hours. During crystallization, the temperature is raised to 105°C and crystallized for 20 hours. In step two, acetic acid is used as an adjusting agent to adjust the pH value. The stirring process after pH adjustment is carried out under nitrogen protection and in the dark.
8. The camellia modal fiber preparation process according to claim 7, characterized in that: In step one, the washing process uses 12 times the volume of deionized water. In step two, the washing process first uses 8 times the volume of anhydrous ethanol, and then uses 18 times the volume of deionized water. In step three, the washing process uses 12 times the volume of deionized water.
9. The process for preparing camellia modal fiber according to claim 8, characterized in that: The pH adjustment reagent used in steps one and two is added in two stages. In the first stage, three-quarters of the reagent is added and stirred. Then, the second stage of addition is carried out drop by drop while stirring continuously to ensure that the acetic acid added each time is fully mixed until the pH value stabilizes within the required range. After stopping the addition of acetic acid, continue stirring for a few minutes to ensure that the pH value no longer changes. Then, measure again to confirm the final pH value.
10. The process for preparing camellia modal fiber according to claim 9, characterized in that, The wet spinning process in step five includes the following steps: Step a: The spinning solution from step four is extruded through the small holes of the spinneret to form a thin stream. The thin stream enters the coagulation bath, where phase separation occurs, the solvent is replaced, and the polymer coagulates to form solid fibers. Step b: After leaving the coagulation bath, the newly formed fibers are stretched by a stretching device, and the fiber stretching ratio is 1-1.
5. Step c: Soak the nascent fibers in an oil, wash, dehydrate, and dry them to obtain the final fiber material. The oil is an aqueous solution of amino silicone oil with a volume percentage concentration of 0.05-0.5% and a soaking time of 2-12 hours. Step d: Roll up and package the treated fibers for subsequent textile processing.
Citation Information
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