Polyphenylene sulfide composite hollow fiber and high-flux membrane-covered filter material prepared from polyphenylene sulfide composite hollow fiber
Through the composite spinning technology of polyphenylene sulfide and polypropylene, high-porosity PPS/PP composite hollow fibers and PTFE membranes are prepared, which solves the problems of high resistance and high energy consumption of PTFE membrane filter materials, achieves a balance between high flux and low resistance, and improves the strength and service life of the filter materials.
Patent Information
- Application Number
- CN202510790173.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-13
- Publication Date
- 2025-09-09
AI Technical Summary
Existing PTFE membrane filter materials have high filtration accuracy but also have the problems of high initial resistance and high energy consumption, making it difficult to meet the requirements of low operating resistance and high throughput.
The composite spinning technology of polyphenylene sulfide (PPS) and polypropylene (PP) is adopted, and the melt mixing of the two is promoted by a heterogeneous regulator to prepare a high-porosity PPS/PP composite hollow fiber, which is then compounded with a PTFE membrane filter layer to form a high-flux membrane filter material.
It achieves a balance between high filtration accuracy and low operating resistance, reduces production energy consumption and costs, and at the same time improves the strength and service life of the filter material.
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Figure CN120608342A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of composite hollow fibers and air filter materials, in particular to a polyphenylene sulfide composite hollow fiber and a high-throughput membrane filter material prepared therefrom. Background Art
[0002] Under the current trend, the emission requirements for various industrial flue gases such as chemical, steel, metallurgy, cement, electricity, and waste incineration are becoming increasingly higher, reaching a zero emission level of 10mg / Nm3 or even below 5mg / Nm3. This is also a challenge for the above industries, which also increases the technical requirements for the environmental protection industry. In view of this, PTFE coated products play an important role in the field of dust removal and filtration due to their high filtration accuracy.
[0003] In addition to having the characteristics of high filtration accuracy and easy dust cleaning, PTFE coated products also have certain shortcomings. After coating, the filter material generally has high initial resistance. While ensuring high filtration accuracy, it is impossible to take into account low operating resistance, resulting in high energy consumption of the dust removal system during operation. Therefore, the problem of high resistance and high energy consumption of coated filter materials needs to be solved urgently, which is also a pain point that clients have always faced.
[0004] Patent publication number KR1020180024670A discloses a sheath-core composite spinning solution-dyed polyphenylene sulfide composite fiber. The sheath is composed of a polyphenylene sulfide resin, and the core is a polyester, polyamide, polyolefin, or a solution-dyed polyphenylene sulfide conjugate fiber. The fiber is cis-core conjugate spun with a black masterbatch added to any vinyl compound, improving spinning processability and providing excellent heat resistance. However, the patent does not disclose the preparation method of the polyphenylene sulfide composite fiber of the present invention. Summary of the Invention
[0005] The technical problem to be solved by the present invention is how to provide a method for preparing polyphenylene sulfide composite hollow fibers and a high-throughput membrane filter material prepared therefrom.
[0006] The present invention solves the above technical problems through the following technical means:
[0007] A first aspect of the present invention provides a method for preparing a high-porosity polyphenylene sulfide composite hollow fiber, comprising the following steps:
[0008] (1) Preparation of PPS / PP composite particles:
[0009] Mixing PPS resin, PP resin and heterogeneous regulator to obtain a mixture, and letting it stand; then granulating the mixture to obtain PPS / PP / heterogeneous regulator composite particles;
[0010] (2) Preparation of PPS / PP composite fiber:
[0011] The PPS / PP / heterogeneous phase regulator composite particles are melted and extruded into a uniform composite melt, which is then transported to a composite spinning manifold. The hollow fibers in the composite spinning assembly are extruded and pre-stretched to obtain pre-drawn fibers. The pre-drawn fibers are then shaped through a drawing and shaping process to obtain PPS / PP composite hollow fibers.
[0012] Preferably, in step (1), the PPS resin content is 65-95 wt%, the PP resin content is 4-25 wt%, and the heterogeneous regulator content is 1-10 wt%.
[0013] Preferably, the preparation method of the heterogeneous regulator comprises the following steps:
[0014] Epoxy resin, benzoic acid sorbitol, and zinc oxide are mixed and reacted under a specific temperature, pressure, and time (temperature 150-380°C, pressure 0.5-6.0 MPa, time 80-320 minutes) under the catalytic action of zinc oxide (epoxy resin accounts for 30-40wt%, benzoic acid sorbitol accounts for 40-50wt%, and zinc oxide accounts for 10-30wt%) to produce a composite compound (heterogeneous phase modifier) with both benzene ring hydroxyl groups and carbon chain polyhydroxyl groups. (The characteristic benzene ring of the epoxy resin reacts with the polyhydroxyl structure of benzoic acid sorbitol, and the hydroxyl groups of benzoic acid sorbitol are grafted onto the benzene ring of the epoxy resin, forming a composite compound (heterogeneous phase modifier) with both benzene ring hydroxyl groups and carbon chain polyhydroxyl groups. This gives the heterogeneous phase modifier two properties: promoting mixing of PPS and PP during melting, promoting PP crystal transformation, and uniform pore formation.)
[0015] Preferably, the melting temperature in step (2) is 250-380°C.
[0016] Preferably, the temperature inside the composite spinning box in step (2) is 250-380°C.
[0017] Preferably, the spinning speed of the pre-drawing in step (2) is 250-600 m / min.
[0018] Preferably, the stretching and shaping temperature in step (2) is 300-450° C., the stretching ratio is 5-10, and the stretching speed is 350-650 m / min.
[0019] The second aspect of the present invention provides a PPS / PP composite hollow fiber prepared by the above preparation method.
[0020] A third aspect of the present invention provides a method for preparing a high-throughput PPS / PP film-coated filter material, comprising the following steps:
[0021] 1) Preparation of PPS / PP needle-punched felt support layer:
[0022] The PPS / PP composite hollow fibers are opened, carded, laid and needled to form PPS / PP composite needle-punched felt.
[0023] 2) Preparation of PPS / PP high-throughput membrane filter material:
[0024] The PPS / PP composite needle-punched felt is compounded with the PTFE membrane filter layer to form a PPS / PP high-throughput membrane filter material.
[0025] Preferably, the composite method in step 2) is an asymmetric structure, the laminating temperature is 100-220° C., the laminating pressure is 0.1-0.5 MPa, and the laminating speed is 8-20 m / min.
[0026] The fourth aspect of the present invention provides a high-throughput PPS / PP membrane-coated filter material prepared by the above-mentioned preparation method.
[0027] The beneficial effects of the present invention are:
[0028] The present invention composites polypropylene (PP) with polyphenylene sulfide resin (PPS) and uses composite spinning technology to prepare PPS / PP composite hollow fibers. The hollow structure has two advantages: (1) pores can be formed on the fiber surface, increasing the flux of airflow through the filter material, ensuring high filtration efficiency of the coated filter material while taking into account the high flux and low resistance characteristics. (2) The hollow fiber can maintain the same gram weight as conventional filter material (when the weight of the raw materials is the same, the traditional single-layer or few-layer fiber mesh can be designed into a multi-layer fiber mesh). By increasing the number of fiber layers, the overall thickness of the filter material is increased, thereby improving the overall strength of the filter material and effectively reducing the impact of dust erosion during use on the product life.
[0029] Among them: when the PP melt is extruded, it crystallizes under the action of tensile stress and cools to form a parallel crystalline structure. When the composite fiber after heat treatment is stretched, the PP crystals will separate and slit-shaped micropores will appear, thereby producing a high-porosity PPS / PP composite hollow fiber; when the composite fiber is used as a raw material to prepare a PPS / PP composite filter material, on the one hand: when the PTFE membrane filter layer is thermally composited with the PPS / PP composite needle-punched felt support layer, there is no need to chemically treat the support layer. The thermoplasticity of PP can itself serve as a binder to composite the filter layer and the support layer. Avoiding the chemical treatment process can avoid environmental pollution. At the same time, the composite temperature is also lower than that of traditional PPS coated filter materials, which can reduce the damage of chemical treatment and high temperature to the performance indicators of the filter material product, including air permeability, strength, microstructure, etc., and design a green, low-damage composite technology. This invention technology reduces production energy consumption, improves production efficiency, and significantly reduces manufacturing costs;
[0030] On the other hand: when the needle-punched felt made of high-porosity PPS / PP composite fiber is compounded with the PTFE membrane filter layer, due to the high-porosity microstructure of the composite fiber surface, the clean gas can directly pass through the pores on the surface of the PPS / PP composite fiber to reach the clean gas surface of the filter material. Combined with the green, low-damage coating technology, the PPS / PP coated filter material ensures high-throughput performance. This technology ensures high filtration accuracy of the coated filter material while taking into account the low operating resistance characteristics.
[0031] Finally, due to the large difference in polarity between PPS and PP resins, agglomeration and uneven mixing are prone to occur during the physical melt mixing process, resulting in uneven micropores (wide pore size distribution), low porosity, and local microfiber breakage. There are stress concentration points, which lead to insufficient strength of the product during use. In view of this, the characteristic functional groups at both ends of the heterogeneous regulator are used to connect PPS and PP resins with a large polarity difference to promote physical melt mixing between the two. In response to the problem of uneven micropores in composite hollow fibers, the heterogeneous regulator can adjust the crystal form, structure and distribution of PP particles during micropore molding, promote mixing of PPS and PP during melting and PP crystal form transformation, and the crystal form transformation will refine the crystal size and increase the crystallinity. Under the action of external tensile force, PPS / PP composite fibers with uniform micropores (narrow pore size distribution), high porosity and high strength can be formed. BRIEF DESCRIPTION OF THE DRAWINGS
[0032] Figure 1 Schematic diagram of the structure of the PPS / PP composite fiber manufactured by the present invention;
[0033] Figure 2 This is a flow chart for manufacturing PPS / PP high-throughput membrane filter material according to the present invention. DETAILED DESCRIPTION
[0034] To make the objectives, technical solutions, and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts shall fall within the scope of protection of the present invention.
[0035] Unless otherwise specified, the test materials and reagents used in the following examples can be obtained from commercial sources.
[0036] If no specific techniques or conditions are specified in the examples, they can be carried out according to the techniques or conditions described in the literature in the field or according to the product instructions.
[0037] Example 1:
[0038] The preparation of the heterogeneous regulator comprises the following steps:
[0039] Epoxy resin, sorbitol and zinc oxide are mixed and reacted under certain temperature, pressure and time (temperature 235°C, pressure 3MPa, time 120min), (the proportion of epoxy resin in the system is 30wt%, the proportion of sorbitol in the system is 50wt%, and the proportion of zinc oxide in the system is 20wt%).
[0040] A method for preparing a high-porosity polyphenylene sulfide composite hollow fiber comprises the following steps:
[0041] (1) Preparation of PPS / PP composite particles:
[0042] Mixing: PPS resin (90 kg), PP resin (9 kg) and heterogeneous phase regulator (1 kg) were mixed in a U-type mixer, and the mixture was allowed to stand at room temperature. The content of PPS resin was 90 wt%, the content of PP resin was 9 wt%, and the content of heterogeneous phase regulator was 1 wt%. The standing time was 12 h.
[0043] Granulation: The mixed material is granulated through a single screw extruder to form uniformly mixed PPS / PP / lignoacid composite particles, wherein: the temperature of the screw extruder zone 1 is 240°C, the temperature of zone 2 is 260°C, and the temperature of zone 3 is 280°C; the temperature of the extrusion die zone 1 is 300°C, and the temperatures of zones 2 and 3 are 310°C;
[0044] (2) PPS / PP composite fiber manufacturing:
[0045] The PPS / PP / heterogeneous phase regulator composite particles are melt-extruded through a screw extruder to prepare a uniform composite melt, wherein: the extrusion die temperature is 300°C;
[0046] The composite melt is conveyed to the composite spinning box, where the temperature inside the composite spinning box is 310°C;
[0047] The hollow fibers in the composite spinning assembly are extruded and pre-stretched to obtain pre-drawn fibers, with a spinning speed of 350 m / min.
[0048] The pre-drawn fibers are subjected to a drawing and shaping process in a heating zone at 320° C. to obtain PPS / PP composite hollow fibers; wherein: the drawing and shaping temperature is 350° C., the drawing ratio is 6.4, and the drawing speed is 440 m / min.
[0049] The mechanical properties of the composite hollow fiber prepared in this example were tested: breaking strength was 20.62 cN / dtex, and breaking elongation was 24.35%.
[0050] Schematic diagram of PPS / PP composite fiber structure Figure 1 As shown, from Figure 1 It can be seen from the figure that the PPS / PP composite fiber presents a hollow morphology in the microstructure, and there are micropores distributed on the surface of the composite fiber.
[0051] A high-throughput PPS / PP coated filter material comprises the following steps:
[0052] 1) PPS / PP needle felt support layer manufacturing:
[0053] The PPS / PP composite hollow fibers prepared above are opened, carded, laid and needled to form a PPS / PP composite needled felt; (the PPS / PP composite needled felt in this embodiment is a "sandwich" structure, that is, fiber layers are distributed on the upper and lower sides of the base fabric layer, the base fabric is a PTFE plain weave fabric, and the surface layer and bottom fiber layer are both formed by PPS / PP composite fibers after opening, carding, laying and needled; the needled step is pre-needled (needle density 66p / cm 2 , needling depth 13mm) and main needling (needling density 552p / cm 2 After the needle punching depth reaches 8mm, the top and bottom fiber layers are tightly bonded with the base fabric layer to form a PPS / PP composite needle-punched felt with a sandwich structure;
[0054] 2) PPS / PP high-throughput membrane filter material manufacturing:
[0055] The PPS / PP composite needle-punched felt is compounded with the PTFE membrane filter layer through green and low-damage laminating technology to form a PPS / PP high-throughput laminating filter material, wherein: the laminating method is an asymmetric structure, the laminating temperature is 150°C, the laminating pressure is 0.2MPa, and the laminating speed is 10m / min.
[0056] Performance testing of finished PPS / PP high-throughput membrane filter media:
[0057] Air permeability 9.3m / min@200Pa, filtration efficiency 99.987% (dust particle size 1μm), initial resistance 125Pa, weight 655g / m 2 , thickness 2.89mm, warp strength 1537N, weft strength 2318N.
[0058] Example 2:
[0059] The preparation of the heterogeneous regulator comprises the following steps:
[0060] Epoxy resin, sorbitol and zinc oxide are mixed and reacted under certain temperature, pressure and time (temperature 150°C, pressure 0.5 MPa, time 320 min), (the proportion of epoxy resin in the system is 32wt%, the proportion of sorbitol in the system is 40wt%, and the proportion of zinc oxide in the system is 28wt%).
[0061] A method for preparing a high-porosity polyphenylene sulfide composite hollow fiber comprises the following steps:
[0062] (1) Preparation of PPS / PP composite particles:
[0063] Mixing: PPS resin (94 kg), PP resin (4 kg) and heterogeneous phase regulator (2 kg) were mixed in a U-type mixer, and the mixture was allowed to stand at room temperature. The content of PPS resin was 94 wt%, the content of PP resin was 4 wt%, and the content of heterogeneous phase regulator was 2 wt%. The standing time was 12 h.
[0064] Granulation: The mixed material is granulated through a single screw extruder to form uniformly mixed PPS / PP / lignoacid composite particles, wherein: the temperature of the screw extruder zone 1 is 240°C, the temperature of zone 2 is 260°C, and the temperature of zone 3 is 280°C; the temperature of the extrusion die zone 1 is 300°C, and the temperatures of zones 2 and 3 are 310°C;
[0065] (2) PPS / PP composite fiber manufacturing:
[0066] The PPS / PP / heterogeneous phase regulator composite particles are melt-extruded into a uniform composite melt by a screw extruder, wherein: the extrusion die temperature is 380°C;
[0067] The composite melt is transported to the composite spinning box, and the temperature inside the composite spinning box is 250°C;
[0068] The hollow fibers in the composite spinning assembly are extruded and pre-stretched to obtain pre-drawn fibers, with a spinning speed of 600 m / min.
[0069] The pre-drawn fibers are subjected to a drawing and shaping process in a heating zone at 320° C. to obtain PPS / PP composite hollow fibers; wherein the drawing and shaping temperature is 450° C., the drawing ratio is 10, and the drawing speed is 650 m / min.
[0070] The mechanical properties of the composite hollow fiber prepared in this example were tested: breaking strength was 28.49 cN / dtex, and breaking elongation was 20.16%.
[0071] A high-throughput PPS / PP coated filter material comprises the following steps:
[0072] 1) PPS / PP needle felt support layer manufacturing:
[0073] The PPS / PP composite hollow fibers prepared above are opened, carded, laid and needled to form a PPS / PP composite needled felt; (the PPS / PP composite needled felt in this embodiment is a "sandwich" structure, that is, fiber layers are distributed on the upper and lower sides of the base fabric layer, the base fabric is a PTFE plain weave fabric, and the surface layer and bottom fiber layer are both formed by PPS / PP composite fibers after opening, carding, laying and needled; the needled step is pre-needled (needle density 66p / cm 2 , needling depth 13mm) and main needling (needling density 552p / cm 2 After the needle punching depth is 8mm), the surface and bottom fiber layers are tightly bonded with the base fabric layer to form a PPS / PP composite needle-punched felt with a sandwich structure.
[0074] 2) PPS / PP high-throughput membrane filter material manufacturing:
[0075] The PPS / PP composite needle-punched felt is compounded with the PTFE membrane filter layer through green and low-damage laminating technology to form a PPS / PP high-throughput laminating filter material, wherein: the laminating method is an asymmetric structure, the laminating temperature is 220℃, the laminating pressure is 0.5MPa, and the laminating speed is 20m / min.
[0076] Performance testing of finished PPS / PP high-throughput membrane filter media:
[0077] Air permeability 8.5m / min@200Pa, filtration efficiency 99.992% (dust particle size 1μm), initial resistance 137Pa, weight 657g / m 2 , thickness 2.87mm, warp strength 1602N, weft strength 2355N.
[0078] Example 3:
[0079] The preparation of the heterogeneous regulator comprises the following steps:
[0080] Epoxy resin, sorbitol and zinc oxide are mixed and reacted under certain temperature, pressure and time (temperature 380°C, pressure 6.0 MPa, time 80 min), (the proportion of epoxy resin in the system is 40wt%, the proportion of sorbitol in the system is 45wt%, and the proportion of zinc oxide in the system is 15wt%).
[0081] A method for preparing a high-porosity polyphenylene sulfide composite hollow fiber comprises the following steps:
[0082] (1) Preparation of PPS / PP composite particles:
[0083] Mixing: PPS resin (65 kg), PP resin (25 kg) and heterogeneous phase regulator (10 kg) were mixed in a U-type mixer, and the mixture was allowed to stand at room temperature. The content of PPS resin was 65 wt%, the content of PP resin was 25 wt%, and the content of heterogeneous phase regulator was 10 wt%. The standing time was 12 h.
[0084] Granulation: The mixed material is granulated through a single screw extruder to form uniformly mixed PPS / PP / lignoacid composite particles, wherein: the temperature of the screw extruder zone 1 is 240°C, the temperature of zone 2 is 260°C, and the temperature of zone 3 is 280°C; the temperature of the extrusion die zone 1 is 300°C, and the temperatures of zones 2 and 3 are 310°C;
[0085] (2) PPS / PP composite fiber manufacturing:
[0086] The PPS / PP / heterogeneous phase regulator composite particles were melt-extruded through a screw extruder to prepare a uniform composite melt, wherein: the extrusion die temperature was 250°C;
[0087] The composite melt is transported to the composite spinning box, where the temperature inside the composite spinning box is 380°C;
[0088] The hollow fibers in the composite spinning assembly are extruded and pre-stretched to obtain pre-drawn fibers, with a spinning speed of 250 m / min.
[0089] The pre-drawn fibers are subjected to a drawing and shaping process in a heating zone at 320° C. to obtain PPS / PP composite hollow fibers; wherein: the drawing and shaping temperature is 300° C., the drawing ratio is 5, and the drawing speed is 350 m / min.
[0090] The mechanical properties of the composite hollow fiber prepared in this example were tested: breaking strength was 18.11 cN / dtex, and breaking elongation was 25.33%.
[0091] A high-throughput PPS / PP coated filter material comprises the following steps:
[0092] 1) PPS / PP needle felt support layer manufacturing:
[0093] The PPS / PP composite hollow fibers prepared above are opened, carded, laid and needled to form a PPS / PP composite needled felt; (the PPS / PP composite needled felt in this embodiment is a "sandwich" structure, that is, fiber layers are distributed on the upper and lower sides of the base fabric layer, the base fabric is a PTFE plain weave fabric, and the surface layer and bottom fiber layer are both formed by PPS / PP composite fibers after opening, carding, laying and needled; the needled step is pre-needled (needle density 66p / cm 2 , needling depth 13mm) and main needling (needling density 552p / cm2 After the needle punching depth is 8mm), the surface and bottom fiber layers are tightly bonded with the base fabric layer to form a PPS / PP composite needle-punched felt with a sandwich structure.
[0094] 2) PPS / PP high-throughput membrane filter material manufacturing:
[0095] The PPS / PP composite needle-punched felt is compounded with the PTFE membrane filter layer through green and low-damage laminating technology to form a PPS / PP high-throughput laminating filter material, wherein: the laminating method is an asymmetric structure, the laminating temperature is 100°C, the laminating pressure is 0.1MPa, and the laminating speed is 8m / min.
[0096] Performance testing of finished PPS / PP high-throughput membrane filter media:
[0097] Air permeability 11.3m / min@200Pa, filtration efficiency 99.985% (dust particle size 1μm), initial resistance 102Pa, gram weight 654g / m 2 , thickness 2.88mm, warp strength 1524N, weft strength 2308N.
[0098] Comparative Example 1:
[0099] Compared with Example 1, this comparative example differs in that: no heterogeneous regulator and PP are added, only PPS is used to make the support layer to make the PPS film-coated filter material, and the rest is the same as Example 1.
[0100] The mechanical properties of the PPS hollow fiber prepared in this comparative example were tested: breaking strength was 3.22 cN / dtex, and breaking elongation was 14.7%.
[0101] PPS membrane filter material, including the following steps:
[0102] Performance test of finished PPS coated filter material:
[0103] Air permeability 1.4m / min@200Pa, filtration efficiency 99.954% (dust particle size 1μm), initial resistance 947Pa, gram weight 652g / m 2 , thickness 2.54mm, warp strength 768N, weft strength 1147N.
[0104] Comparative Example 2:
[0105] This comparative example is compared with Example 1, except that: no heterogeneous regulator is added, the PPS resin content is 90wt%, the PP resin content is 10wt%, PPS and PP are used to make the support layer to make PPS / PP high-flux membrane filter material, and the rest is the same as Example 1.
[0106] The mechanical properties of the composite hollow fiber of this comparative example were tested: breaking strength was 2.14 cN / dtex, and breaking elongation was 11.9%.
[0107] The performance test of the finished product of PPS / PP high-flux membrane filter material in this comparative example is as follows: air permeability 3.1m / min@200Pa, filtration efficiency 99.285% (dust particle size 1μm), initial resistance 687Pa, gram weight 648g / m 2 , thickness 2.77mm, warp strength 532N, weft strength 897N.
[0108] Comparative Example 3:
[0109] This comparative example is different from Example 1 in that the heterogeneous regulator is replaced with a conventional compatibilizer: m-isopropenyl-2,2-dimethylphenyl isocyanate. Other conditions are the same as those in Example 1.
[0110] The mechanical properties of the composite hollow fiber prepared in this comparative example were tested: breaking strength was 4.17 cN / dtex, and breaking elongation was 15.8%.
[0111] The performance test of the finished product of PPS / PP high-throughput membrane filter material prepared in this comparative example is as follows: air permeability 5.4m / min@200Pa, filtration efficiency 99.744% (dust particle size 1μm), initial resistance 479Pa, gram weight 661g / m 2 , thickness 2.73mm, warp strength 732N, weft strength 1145N.
[0112] Comparative Example 4:
[0113] This comparative example is different from Example 1 in that no heterogeneous regulator is added, and only conventional compatibilizer m-isopropenyl-2,2-dimethylphenyl isocyanate and nucleating agent lignin are added.
[0114] That is, mixing: PPS resin (90 kg), PP resin (8 kg), m-isopropenyl-2,2-dimethylphenyl isocyanate (1 kg), and lignin (1 kg) are mixed by a U-type mixer, and the rest is the same as in Example 1.
[0115] The mechanical properties of the composite hollow fiber prepared in this comparative example were tested: breaking strength was 7.55 cN / dtex, and breaking elongation was 18.3%.
[0116] The performance test of the finished product of PPS / PP high-flux membrane filter material prepared in this comparative example is as follows: air permeability 6.1m / min@200Pa, filtration efficiency 99.833% (dust particle size 1μm), initial resistance 425Pa, gram weight 639g / m 2, thickness 2.81mm, warp strength 829N, weft strength 1533N.
[0117] As can be seen from Comparative Example 4, the effect of adding the conventional compatibilizer and nucleating agent simultaneously is not ideal. In Example 1, the compatibilizer and the nucleating agent are synthesized first, so that the homogeneous regulator has the functions of both the compatibilizer and the nucleating agent.
[0118] Test method:
[0119] 1. Air permeability test method:
[0120] A 210cm*60cm sample is cut with a circular sampler in an area of 100cm, with each sample piece not being in the same position in the warp and weft directions. 2 For circular specimens, refer to GB / T 5453:1997 and select an air permeability tester for testing. The setting parameters are: unit m 3 / m 2 / min, pressure difference 200Pa, sample area 20cm 2 .
[0121] 2. Warp and weft strength test method:
[0122] Cut samples from the sample to be tested. The sample area should be free of obvious defects, wrinkles, and damage. Take samples with a width of 50mm in the warp and weft directions on the filter material. The sample length should meet the nominal clamping distance of 200mm±1mm. Cut at least 5 groups of samples from each sample, that is, 5 samples in the warp and weft directions. Lines must be drawn on both sides for sampling. The samples should be at least 100mm away from the edge of the fabric. Refer to GB / T 3923 to select a tensile strength tester for testing. Set the parameters as follows: initial position 200mm, rising speed 100mm / min, and descending speed 500mm / min.
[0123] 3. Initial resistance and filtration efficiency test method:
[0124] The dynamic filtration performance of the filter media was tested on the DLC-2004 filter media dynamic filtration performance tester, including initial resistance and filtration efficiency. The test was carried out in accordance with GB / T 6719-2009. The dust filtration performance of the initial filter media sample was determined as follows:
[0125] (a) Install the filter media sample on the filter media fixture. The filter media sample specification is 150mm in diameter. When the pressure loss reaches 1000Pa, clean the dust. After repeating 30 times, measure the weight gain of the high-efficiency filter membrane and the dust concentration at the outlet and record them;
[0126] (b) Aging treatment: During the dust filtration process, back-blowing is performed at intervals of 5 seconds, and repeated 10,000 times;
[0127] (c) Stabilization: To stabilize the dust filtration performance of the aged filter media sample, perform the dust filtration and dust cleaning operation 10 times according to (a). (d) Determination of dust filtration performance of the stabilized filter media: For the filter cloth that has undergone the above stabilization treatment, perform the dust filtration and dust cleaning operation 30 times according to (a). Test and record the dust throughput and outlet dust concentration. (e) In tests (ad), record the instantaneous resistance values throughout the entire process. Test conditions are as follows:
[0128] project Value / Type Test dust Alumina Inlet dust concentration <![CDATA[5g / m 3 ]]> Filtration speed 2m / min Cleaning resistance 1000Pa Blowing pressure 500kPa Pulse injection time 50ms
[0129] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the various embodiments of the present invention.
Claims
1. A method for preparing a high-porosity polyphenylene sulfide composite hollow fiber, characterized in that: The following steps are involved: (1) Preparation of PPS / PP composite particles: Mixing PPS resin, PP resin and heterogeneous regulator to obtain a mixture, and letting it stand; then granulating the mixture to obtain PPS / PP / heterogeneous regulator composite particles; (2) Preparation of PPS / PP composite fiber: The PPS / PP / heterogeneous phase regulator composite particles are melted and extruded into a uniform composite melt, which is then transported to a composite spinning manifold. The hollow fibers in the composite spinning assembly are extruded and pre-stretched to obtain pre-drawn fibers. The pre-drawn fibers are then shaped through a drawing and shaping process to obtain PPS / PP composite hollow fibers.
2. The method for preparing a high-porosity polyphenylene sulfide composite hollow fiber according to claim 1, characterized in that: In the step (1), the content of PPS resin is 65-95 wt%, the content of PP resin is 4-25 wt%, and the content of heterogeneous regulator is 1-10 wt%.
3. The method for preparing a high-porosity polyphenylene sulfide composite hollow fiber according to claim 1, characterized in that: The preparation method of the heterogeneous regulator comprises the following steps: The epoxy resin, sorbitol and zinc oxide are mixed and reacted at a temperature of 150-380° C. and a pressure of 0.5-6.0 MPa for 80-320 minutes to obtain a product; the epoxy resin accounts for 30-40wt% in the system, the sorbitol accounts for 40-50wt% in the system, and the zinc oxide accounts for 10-30wt% in the system.
4. The method for preparing a high-porosity polyphenylene sulfide composite hollow fiber according to claim 1, characterized in that: In the step (2), the melting temperature is 250-380°C; and the temperature inside the composite spinning box is 250-380°C.
5. The method for preparing a high-porosity polyphenylene sulfide composite hollow fiber according to claim 1, characterized in that: The spinning speed of the pre-drawing in step (2) is 250-600 m / min.
6. The method for preparing a high-porosity polyphenylene sulfide composite hollow fiber according to claim 1, characterized in that: The drawing and shaping temperature in step (2) is 300-450° C., the drawing ratio is 5-10, and the drawing speed is 350-650 m / min.
7. PPS / PP composite hollow fiber prepared by the preparation method according to any one of claims 1 to 6.
8. A method for preparing a high-throughput PPS / PP film-coated filter material, characterized in that: The following steps are involved: 1) Preparation of PPS / PP needle-punched felt support layer: The PPS / PP composite hollow fiber according to claim 7 is formed into a PPS / PP composite needle-punched felt after being opened, carded, laid and needle-punched; 2) Preparation of PPS / PP high-throughput membrane filter material: The PPS / PP composite needle-punched felt is compounded with the PTFE membrane filter layer to form a PPS / PP high-throughput membrane filter material.
9. The method for preparing a high-throughput PPS / PP film-coated filter material according to claim 8, characterized in that: The composite method of step 2) is an asymmetric structure, the laminating temperature is 100-220° C., the laminating pressure is 0.1-0.5 MPa, and the laminating speed is 8-20 m / min.
10. The high-throughput PPS / PP membrane-coated filter material prepared by the preparation method according to any one of claims 8 to 9.
Citation Information
Patent Citations
Dope Dyed Polyphenylene Sulfide Composite Fiber Prepared By Sheath-Core Complex Spinning
KR1020180024670A