WO2016041099A1 - 一种玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法 - Google Patents

一种玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法 Download PDF

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WO2016041099A1
WO2016041099A1 PCT/CN2014/000857 CN2014000857W WO2016041099A1 WO 2016041099 A1 WO2016041099 A1 WO 2016041099A1 CN 2014000857 W CN2014000857 W CN 2014000857W WO 2016041099 A1 WO2016041099 A1 WO 2016041099A1
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emulsion
polyphenylene sulfide
polytetrafluoroethylene
modified polyphenylene
filter material
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PCT/CN2014/000857
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English (en)
French (fr)
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袁振其
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太仓苏纶纺织化纤有限公司
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Priority to PCT/CN2014/000857 priority Critical patent/WO2016041099A1/zh
Publication of WO2016041099A1 publication Critical patent/WO2016041099A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
    • D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/63—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing sulfur in the main chain, e.g. polysulfones

Definitions

  • the invention relates to a coating method of basalt fiber filter material, in particular to a layered coating method of modified polyphenylene sulfide/polytetrachloroethylene of basalt fiber filter material.
  • Filter media is a major component of gas-solid separation devices, and its performance directly determines the quality of the filtration.
  • post-finishing technology such as dipping, coating and laminating to improve the surface layer and internal structure of the filter material, thereby obtaining uniform structure and size. Stable and efficient filtration material.
  • the single polyphenylene sulfide needle felt has poor oxidation resistance and cannot be adapted to the purification effect under high oxygen conditions.
  • a single PTFE fiber needle felt has water repellency and oxidation resistance, it is expensive, requires high post-treatment equipment, and increases production costs.
  • the coating prepared by coating the polytetrafluoroethylene powder on the filter base fabric can improve the anti-adhesiveness of the filter material, but the mechanical properties of the filter material are not completely melted due to the high melt viscosity of the polytetrafluoroethylene. Poor, easy to pinhole, low bonding ability of the coating.
  • Basalt fiber has the characteristics of high temperature resistance, oxidation resistance and radiation resistance, and can be widely used in filter material production.
  • the use of basalt fiber as the filter base fabric can improve the dimensional stability of the composite material at high temperatures, and at the same time improve its acid and alkali resistance. Due to the large surface tension of basalt fiber, poor cohesion between fibers, easy generation of static electricity, large modulus of elasticity, etc., the use of post-preparation techniques such as dipping, coating, and film coating on the base fabric can improve the filter material. Surface and internal structure to obtain a highly efficient filter material with uniform structure and dimensional stability.
  • Hyperbranched polyphenylene sulfide has a chemical composition similar to that of linear polyphenylene sulfide, and both contain a benzene ring and a sulfur atom, but have different chemical structures.
  • the blending of hyperbranched polyphenylene sulfide and linear polyphenylene sulfide in a certain ratio can reduce the melt viscosity and improve the performance of the finished product while maintaining good compatibility between the two.
  • the method provides a layered coating method of modified polyphenylene sulfide/polytetrafluoroethylene for basalt fiber filter.
  • the basalt fiber is used as the filter base cloth, and the modified polyphenylene sulfide and polytetrafluoroethylene are respectively prepared into coating materials, and the modified polyphenylene sulfide having strong binding ability of the primer layer and the base cloth is adopted by the layer coating method.
  • the surface layer is coated with anti-adhesive polytetrafluoroethylene to improve the mechanical strength, high temperature stability, acid and alkali resistance of the filter material, and at the same time, provide the roughness of the composite coating on the surface of the filter layer, and promote the combination of the coating and the skin. And to improve the dispersion and density of the fiber.
  • a modified polyphenylene sulfide/polytetrafluoroethylene layer coating method for basalt fiber filter material comprising:
  • the modified polyphenylene sulfide emulsion in the step 2) is composed of a linear polyphenylene sulfide powder of 5-10% by mass, a 3-5% hyperbranched polyphenylene sulfide powder, and the balance being water;
  • the primer in the step 3) is composed of a modified polyphenylene sulfide emulsion having a percentage of 35-55%, a 40-60% polytetrafluoroethylene emulsion, and a 5%-10% fluorine-containing silane coupling agent;
  • the topcoat described in 4) consists of a 40-50% polytetrafluoroethylene emulsion, 38-48% F 46 emulsion, and the balance being water.
  • the modified polyphenylene sulfide emulsion in the step 2) is composed of a linear polyphenylene sulfide powder of 8% by mass, a 4% hyperbranched polyphenylene sulfide powder, and the balance being water; in step 3)
  • the primer consists of a 40% modified polyphenylene sulfide emulsion, a 55% polytetrafluoroethylene emulsion and a 5% fluorine-containing silane coupling agent; the topcoat described in step 4) is percentage It is a 45% polytetrafluoroethylene emulsion, 40% F 46 emulsion, and the balance is water.
  • the hyperbranched polyphenylene sulfide is added to 0.8 M N-methylpyrrolidone by 50 mmol of dichlorothiophenol and 100 mmol of anhydrous potassium carbonate, heated to 150 ° C, and kept for 8.5 hours, and the product is washed with hydrochloric acid. After filtration, it was dissolved in tetrahydrofuran, extracted with hexane, and dried by filtration, and the degree of polymerization was 8-12.
  • the top coat layer has a thickness of 4-6 ⁇ m, and the top layer is sprayed with 1-2 layers.
  • the base fabric of the present invention uses hyperbranched polyphenylene sulfide and linear polyphenylene sulfide as a primer layer, and its crystallization temperature and crystallization rate are higher than that of a pure linear polyphenylene sulfide coating, thereby improving The thermal stability and leveling properties of the filter material make it easier to process.
  • Base fabric made of basalt. Because basalt fiber has the characteristics of high temperature resistance, oxidation resistance and radiation resistance, it has stronger bonding ability with surface coating. After the surface is coated with fluoropolymer, the degree of adhesion of surrounding fibers is improved. The structure of the web becomes denser, the roughness of the smooth fiber surface is increased, the dust in the flue gas is easily entered between the filter materials, the running resistance of the filter material is increased, and the filtration performance and mechanical properties of the filter material are improved.
  • the bottom layer is coated with modified polyphenylene sulfide with strong binding ability, and the surface layer is coated with anti-sticky polytetrafluoroethylene to provide mechanical strength of the coating and prevent polyphenylene sulfide. Decomposition occurs and a rough coating surface is obtained.
  • the filter material produced by the preparation method of the invention has good thermal stability and corrosion resistance It can improve the dispersibility and compactness of the finished fiber, and has a simple manufacturing process and low cost, and is suitable for large-scale industrial production.
  • basalt filter material base cloth the basalt fiber is opened, combed into a net, cross-laid, and made into a filter base cloth.
  • modified polyphenylene sulfide fiber emulsion according to the mass percentage of 5% linear polyphenylene sulfide powder, 5% hyperbranched polyphenylene sulfide powder, the balance is the proportion of water, and then evenly mixed by ultrasonic cleaning machine, Formulated as an emulsion.
  • Preparation of primer mixed in proportion of 35% by mass of modified polyphenylene sulfide emulsion, 60% of polytetrafluoroethylene emulsion and 5% of fluorinated silane coupling agent, and then uniformly mixed by ultrasonic cleaner Into an emulsion.
  • top coat 40% by mass of polytetrafluoroethylene emulsion, 48% of F 46 emulsion, the balance of water is mixed, and then evenly mixed by ultrasonic cleaning machine to prepare emulsion.
  • the cleaned filter base cloth is immersed in the primer coating emulsion, and then rolled by rolling mill, pre-baked, the temperature is 90 ° C, baking, the temperature is 160 ° C, cooling with the furnace, the bottom layer
  • the coating thickness is 8-10 ⁇ m.
  • Spray coating method spray the top coat on the bottom surface with a spray gun.
  • the thickness of each layer is 4-6 ⁇ m. No blast and accumulation, spray 1-2 layers and put into the oven at 60°C. Preheated for 30 minutes, and then plasticized at 360 °C.
  • basalt filter base fabric opening basalt fiber, combing into a net, cross-laying, making Filter into a base fabric.
  • modified polyphenylene sulfide fiber emulsion 10% by mass of linear polyphenylene sulfide powder, 3% hyperbranched polyphenylene sulfide powder, the balance is water ratio, and then evenly mixed by ultrasonic cleaning machine, Formulated as an emulsion.
  • Preparation of primer mixed in a proportion of 45% by mass of modified polyphenylene sulfide emulsion, 45% of polytetrafluoroethylene emulsion and 10% of fluorine-containing silane coupling agent, and then uniformly mixed by ultrasonic cleaning machine to prepare Into an emulsion.
  • top coat 50% by mass of polytetrafluoroethylene emulsion, 38% of F 46 emulsion, the balance of water is mixed, and then evenly mixed by ultrasonic cleaner to prepare emulsion.
  • the cleaned filter base cloth is immersed in the primer coating emulsion, and then rolled by rolling mill, pre-baked, the temperature is 90 ° C, baking, the temperature is 160 ° C, cooling with the furnace, the bottom layer
  • the coating thickness is 8-10 ⁇ m.
  • Spray coating method Spray the top coat on the surface of the bottom layer with a spray gun.
  • the thickness of each layer is 4-6 ⁇ m. Between the 1-2 layers and the oven at 65°C, no air enthalpy and accumulation will occur. Preheated for 25 minutes, and then plasticized at 360 °C.
  • basalt filter material base cloth the basalt fiber is opened, combed into a net, cross-laid, and made into a filter base cloth.
  • modified polyphenylene sulfide fiber emulsion linear polyphenylene sulfide powder of 8% by mass At the end, 4% hyperbranched polyphenylene sulfide powder is mixed with the balance of water, and then uniformly mixed by an ultrasonic cleaner to prepare an emulsion.
  • Preparation of primer mixed in a proportion of 40% by mass of modified polyphenylene sulfide emulsion, 55% of polytetrafluoroethylene emulsion and 5% of fluorinated silane coupling agent, and then uniformly mixed by ultrasonic cleaning machine. Into an emulsion.
  • Preparation of the top coat 45% by mass of the polytetrafluoroethylene emulsion, 40% of the F 46 emulsion, the balance is the proportion of water, and then evenly mixed by an ultrasonic cleaner to prepare an emulsion.
  • the cleaned filter base cloth is immersed in the primer coating emulsion, and then rolled by rolling mill, pre-baked, the temperature is 90 ° C, baking, the temperature is 160 ° C, cooling with the furnace, the bottom layer
  • the coating thickness is 8-10 ⁇ m.
  • Spray coating method spray the top coat on the bottom surface with a spray gun.
  • the thickness of each layer is 4-6 ⁇ m. No blast and accumulation, spray 1-2 layers and put into the oven at 60°C. Preheated for 30 minutes, and then plasticized at 360 °C.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Filtering Materials (AREA)

Abstract

一种玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法，包括：将玄武岩纤维制成滤料基布的步骤；将线性聚苯硫醚和超支链聚苯硫醚混合制成改性聚苯硫醚乳液的步骤；将改性聚苯硫醚乳液、聚四氟乙烯乳液和含氟硅烷偶联剂混合制成底层涂料的步骤；将聚四氟乙烯乳液、含氟硅烷偶联剂和F46乳液混合制成面层涂料的步骤；将所述滤料基布浸渍在所述底层涂料中，高温固化、随炉冷却、制成底层的步骤；用喷枪将面层涂料喷涂在底层表面，高温塑化后，得到成品的步骤。通过本发明的制备方法，制造的复合滤料具有良好的热稳定性、耐腐蚀性、较强机械强度，提高成品纤维的分散性和致密程度并且制造工艺简单，成本较低，适合大规模工业生产。

Description

一种玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法 技术领域
本发明涉及玄武岩纤维滤料的涂覆方法，特别是涉及一种玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法。
背景技术
目前，耐高温过滤材料已被广泛运用于发电、水泥等工业领域，滤料是气固分离装置的主要组成部分，其性能直接决定过滤效果的好坏。为了提高过滤精度，人们除了在生产中不断改善滤料本身制备工艺外，还运用浸渍、涂层和覆膜等后整理技术，旨在改善滤材的表层和内部结构，从而得到结构均匀、尺寸稳定的高效过滤材料。
在实际生产中发现，单一的聚苯硫醚针刺毡的耐氧化性不好，无法适应高氧状态下的净化效果。单一的聚四氟乙烯纤维针刺毡虽然具有拒水性，耐氧化性能也好，但是其价格昂贵，对后处理设备要求也很高，增加生产成本。另外，用聚四氟乙烯粉末制备涂层涂覆在滤料基布上可以提高滤料防粘性，但是由于聚四氟乙烯因熔融黏度大无法完全熔融流平，因此这种滤料的机械性能差，易出针孔，涂层的结合能力低。
玄武岩纤维具有耐高温、抗氧化和防辐射的特点，可广泛用于滤料生产。以玄武岩纤维为滤料基布能够改善复合了材料高温下的尺寸稳定性，同时也能提高其耐酸耐碱性。由于玄武岩纤维表面张力大，纤维之间抱合力差，容易产生静电，弹性模量大等诸多原因，在此基布上继续运用浸渍、涂层、覆膜等后整理技术，能够改善滤材的表面和内部结构，从而得到结构均匀、尺寸稳定的高效过滤材料。
综上所述，目前迫切需要一种滤料的制备方法，能够改善复合滤料的 高温稳定性、提高其耐酸耐碱性并且促进复合材料相互结合，从而提高成品的过滤性能。
发明内容
超支化聚苯硫醚具有与线型聚苯硫醚相类似的化学组成，都含有苯环和硫原子，但化学结构不同。将超支化聚苯硫醚和线型的聚苯硫醚按一定配比共混,能够在降低熔体黏度、改善成品性能的同时,保持两者较好的相容性。本方法提供了一种玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法。以玄武岩纤维作为滤料基布，分别将改性聚苯硫醚和聚四氟乙烯制备成涂料，采用分层涂覆的方法，底层涂层与基布结合能力强的改性聚苯硫醚，表层涂覆具有防粘性的聚四氟乙烯，从而提高滤料机械强度、高温稳定性、耐酸耐碱性，同时提供滤层表面复合涂层的粗糙程度，促进涂层和之间相互结合，并且提高纤维的分散性和致密程度。
为实现上述发明目的，本发明所提供的技术方案是：
一种玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法，包括：
1)将玄武岩纤维制成滤料基布；
2)将线性聚苯硫醚和超支链聚苯硫醚混合制成改性聚苯硫醚乳液；
3)将改性聚苯硫醚乳液、聚四氟乙烯乳液和含氟硅烷偶联剂混合制成底层涂料；
4)将聚四氟乙烯乳液、含氟硅烷偶联剂和F46乳液混合制成面层涂料；
5)将所述滤料基布浸渍在所述底层涂料中，高温固化、随炉冷却、制成底层；
6)用喷枪将面层涂料喷涂在底层表面，高温塑化后，得到成品。
进一步地，步骤2)中所述改性聚苯硫醚乳液由质量百分比为5-10％的线性聚苯硫醚粉末、3-5％超支化聚苯硫醚粉末，余量为水组成；步骤3) 中所述底层涂料由百分比为35-55％的改性聚苯硫醚乳液、40-60％的聚四氟乙烯乳液和5％-10％的含氟硅烷偶联剂组成；步骤4)中所述的面层涂料由百分比为40-50％的聚四氟乙烯乳液、38-48％的F46乳液，余量为水组成。
进一步地，步骤2)中所述改性聚苯硫醚乳液由质量百分比为8％的线性聚苯硫醚粉末、4％超支化聚苯硫醚粉末，余量为水组成；步骤3)中所述底层涂料由百分比为40％的改性聚苯硫醚乳液、55％的聚四氟乙烯乳液和5％的含氟硅烷偶联剂组成；步骤4)中所述的面层涂料由百分比为45％的聚四氟乙烯乳液、40％的F46乳液，余量为水组成。
进一步地，所述超支化聚苯硫醚是由50mmol的二氯硫酚和100mmol的无水碳酸钾加入到0.8M的N-甲基吡咯烷酮中，加热到150℃，保温8.5小时，产物盐酸洗涤过滤后，加入四氢呋喃溶解，己烷萃取，过滤烘干制成，聚合度为8-12。
进一步地，其中所述底层涂料的厚度为8-10μm，面层涂层厚度为4-6μm，面层喷涂1-2层。
采用上述技术方案，本发明的有益效果有：
1.在本发明中的基布使用超支化聚苯硫醚和线性聚苯硫醚共混作为底层涂层，其结晶温度和结晶速度高于单纯线性的聚苯硫醚涂层，因此能够提高滤料的热稳定性和流平性能，更易于加工。
2.采用玄武岩制成基布，由于玄武岩纤维具有耐高温、抗氧化和防辐射的特点，其与表面涂层的结合能力更强，表面涂覆含氟聚合物后，周围纤维黏连程度提高，使得纤网结构变得更加致密，增加光滑的纤维表面的粗糙程度，方便烟气中粉尘进入滤料之间，增加滤料运行阻力，提高了滤料的过滤性能和力学性能。
3.采用分层涂覆的方法，底层涂覆结合能力强的改性聚苯硫醚，面层涂覆具有防粘性的聚四氟乙烯，提供涂层的机械强度、同时防止聚苯硫醚分解现象的发生，同时能够得到粗糙的涂层表面。
4.通过本发明的制备方法制造的滤料具有良好的热稳定性、耐腐蚀 性，同时能够提高成品纤维的分散性和致密程度，并且制造工艺简单，成本较低，适合大规模工业生产。
具体实施方式
实施例1
制备玄武岩滤料基布：将玄武岩纤维开松，梳理成网，交叉铺网，制成滤料基布。
制备超支化聚苯硫醚：在250mL三颈瓶中加入10g 3,4-二氯硫酚和13.4g无水碳酸钾及80mL的N-甲基吡咯烷酮,加热到150℃,保温8.5h。产物用盐酸洗涤过滤后,加入四氢呋喃溶解,用己烷萃取,过滤烘干,得浅褐色超支化PPS粉末，其聚合度为8-12。
制备改性聚苯硫醚纤维乳液：按质量百分比为5％的线性聚苯硫醚粉末、5％超支化聚苯硫醚粉末，余量为水的比例混合，再通过超声波清洗机混合均匀，配制成乳液。
制备底层涂料：按质量百分比为35％的改性聚苯硫醚乳液、60％的聚四氟乙烯乳液和5％的含氟硅烷偶联剂的比例混合，再通过超声波清洗机混合均匀，配制成乳液。
制备面层涂料：按质量百分比为40％的聚四氟乙烯乳液、48％的F46乳液，余量为水的比例混合，再通过超声波清洗机混合均匀，配制成乳液。
浸渍法涂覆底层涂料：将清洗后的滤料基布浸渍在底层涂料乳液中，再通过轧车轧压，预烘，温度为90℃，焙烘，温度为160℃，随炉冷却，底层涂料厚度为8-10μm。
喷涂法涂覆面层涂料：用喷枪将面层涂料乳液均匀喷涂在底层表面，每层厚度为4-6μm，以不出现气呛和积聚为准，喷涂1-2层，放入60℃的烘箱中预热30min，再在360℃高温中塑化成型。
实施例2
制备玄武岩滤料基布：将玄武岩纤维开松，梳理成网，交叉铺网，制 成滤料基布。
制备超支化聚苯硫醚：在250mL三颈瓶中加入10g 3,4-二氯硫酚和13.4g无水碳酸钾及80mL的N-甲基吡咯烷酮,加热到150℃,保温8.5h。产物用盐酸洗涤过滤后,加入四氢呋喃溶解,用己烷萃取,过滤烘干,得浅褐色超支化PPS粉末，其聚合度为8-12。
制备改性聚苯硫醚纤维乳液：按质量百分比为10％的线性聚苯硫醚粉末、3％超支化聚苯硫醚粉末，余量为水的比例混合，再通过超声波清洗机混合均匀，配制成乳液。
制备底层涂料：按质量百分比为45％的改性聚苯硫醚乳液、45％的聚四氟乙烯乳液和10％的含氟硅烷偶联剂的比例混合，再通过超声波清洗机混合均匀，配制成乳液。
制备面层涂料：按质量百分比为50％的聚四氟乙烯乳液、38％的F46乳液，余量为水的比例混合，再通过超声波清洗机混合均匀，配制成乳液。
浸渍法涂覆底层涂料：将清洗后的滤料基布浸渍在底层涂料乳液中，再通过轧车轧压，预烘，温度为90℃，焙烘，温度为160℃，随炉冷却，底层涂料厚度为8-10μm。
喷涂法涂覆面层涂料：用喷枪将面层涂料乳液均匀喷涂在底层表面，每层厚度为4-6μm，以不出现气呛和积聚为准，喷涂1-2层，放入65℃的烘箱中预热25min，再在360℃高温中塑化成型。
实施例3
制备玄武岩滤料基布：将玄武岩纤维开松，梳理成网，交叉铺网，制成滤料基布。
制备超支化聚苯硫醚：在250mL三颈瓶中加入10g 3,4-二氯硫酚和13.4g无水碳酸钾及80mL的N-甲基吡咯烷酮,加热到150℃,保温8.5h。产物用盐酸洗涤过滤后,加入四氢呋喃溶解,用己烷萃取,过滤烘干,得浅褐色超支化PPS粉末，其聚合度为8-12。
制备改性聚苯硫醚纤维乳液：按质量百分比为8％的线性聚苯硫醚粉 末、4％超支化聚苯硫醚粉末，余量为水的比例混合，再通过超声波清洗机混合均匀，配制成乳液。
制备底层涂料：按质量百分比为40％的改性聚苯硫醚乳液、55％的聚四氟乙烯乳液和5％的含氟硅烷偶联剂的比例混合，再通过超声波清洗机混合均匀，配制成乳液。
制备面层涂料：按质量百分比为45％的聚四氟乙烯乳液、40％的F46乳液，余量为水的比例混合，再通过超声波清洗机混合均匀，配制成乳液。
浸渍法涂覆底层涂料：将清洗后的滤料基布浸渍在底层涂料乳液中，再通过轧车轧压，预烘，温度为90℃，焙烘，温度为160℃，随炉冷却，底层涂料厚度为8-10μm。
喷涂法涂覆面层涂料：用喷枪将面层涂料乳液均匀喷涂在底层表面，每层厚度为4-6μm，以不出现气呛和积聚为准，喷涂1-2层，放入60℃的烘箱中预热30min，再在360℃高温中塑化成型。
实施例1、2、3中成品的性能参数见下表：
Figure PCTCN2014000857-appb-000001
以上所述实施例仅表达了本发明的实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对 于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。

Claims (5)

  1. 一种玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法，其特征在于，包括：
    1)将玄武岩纤维制成滤料基布；
    2)将线性聚苯硫醚和超支链聚苯硫醚混合制成改性聚苯硫醚乳液；
    3)将改性聚苯硫醚乳液、聚四氟乙烯乳液和含氟硅烷偶联剂混合制成底层涂料；
    4)将聚四氟乙烯乳液、含氟硅烷偶联剂和F46乳液混合制成面层涂料；
    5)将所述滤料基布浸渍在所述底层涂料中，高温固化、随炉冷却、制成底层；
    6)用喷枪将面层涂料喷涂在底层表面，高温塑化后，得到成品。
  2. 根据权利要求1所述的玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法，其特征在于，步骤2)中所述改性聚苯硫醚乳液由质量百分比为5-10％的线性聚苯硫醚粉末、3-5％超支化聚苯硫醚粉末，余量为水组成；步骤3)中所述底层涂料由百分比为35-55％的改性聚苯硫醚乳液、40-60％的聚四氟乙烯乳液和5％-10％的含氟硅烷偶联剂组成；步骤4)中所述的面层涂料由百分比为40-50％的聚四氟乙烯乳液、38-48％的F46乳液，余量为水组成。
  3. 根据权利要求1所述的玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法，其特征在于，步骤2)中所述改性聚苯硫醚乳液由质量百分比为8％的线性聚苯硫醚粉末、4％超支化聚苯硫醚粉末，余量为水组成；步骤3)中所述底层涂料由百分比为40％的改性聚苯硫醚乳液、55％的聚四氟乙烯乳液和5％的含氟硅烷偶联剂组成；步骤4)中所述的面层涂料由百分比为45％的聚四氟乙烯乳液、40％的F46乳液，余量为水组成。
  4. 根据权利要求1-3任一项所述的玄武岩纤维滤料的改性聚苯硫醚/ 聚四氯乙烯分层涂覆方法，其特征在于，所述超支化聚苯硫醚是由50mmol的二氯硫酚和100mmol的无水碳酸钾加入到0.8M的N-甲基吡咯烷酮中，加热到150℃，保温8.5小时，产物盐酸洗涤过滤后，加入四氢呋喃溶解，己烷萃取，过滤烘干制成，聚合度为8-12。
  5. 根据权利要求1-3任一项所述的玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法，其特征在于，其中所述底层涂料的厚度为8-10μm，面层涂层厚度为4-6μm，面层喷涂1-2层。
PCT/CN2014/000857 2014-09-19 2014-09-19 一种玄武岩纤维滤料的改性聚苯硫醚/聚四氯乙烯分层涂覆方法 WO2016041099A1 (zh)

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CN109663413A (zh) * 2019-03-01 2019-04-23 抚顺天成环保科技有限公司 一种高温过滤材料用耐高温覆膜的制备方法
CN111804063A (zh) * 2020-08-05 2020-10-23 山东兴国新力环保科技股份有限公司 一种耐高温过滤材料的制备方法
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