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WO2022267335A1 - Matériau filtrant, sa méthode de préparation, et son application - Google Patents

Matériau filtrant, sa méthode de préparation, et son application Download PDF

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Publication number
WO2022267335A1
WO2022267335A1 PCT/CN2021/133271 CN2021133271W WO2022267335A1 WO 2022267335 A1 WO2022267335 A1 WO 2022267335A1 CN 2021133271 W CN2021133271 W CN 2021133271W WO 2022267335 A1 WO2022267335 A1 WO 2022267335A1
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WIPO (PCT)
Prior art keywords
filter material
solution
preparation
metal salt
substrate
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Application number
PCT/CN2021/133271
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English (en)
Chinese (zh)
Inventor
张振
郭晓蓓
高政
王屹
尹奕玲
徐涛
费传军
余佳彬
匡新波
吴涛
Original Assignee
南京玻璃纤维研究设计院有限公司
中材科技股份有限公司
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Priority to KR1020237039027A priority Critical patent/KR20230170740A/ko
Publication of WO2022267335A1 publication Critical patent/WO2022267335A1/fr

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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
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/0001—Making filtering elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B01D53/8628—Processes characterised by a specific catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B01D53/8631—Processes characterised by a specific device
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
    • B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04—Additives and treatments of the filtering material
    • B01D2239/0407—Additives and treatments of the filtering material comprising particulate additives, e.g. adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10—Filtering material manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases

Definitions

  • the invention belongs to the technical field of filter material preparation, and in particular relates to a filter material and its preparation method and application.
  • bag filter In the field of industrial flue gas post-treatment, bag filter has been widely used in coal-fired power plants, waste incineration, cement and other fields due to its high dust removal efficiency, good operation stability, and easy recycling.
  • the filter material is the core of the bag filter, such as glass fiber, PTFE and so on.
  • the use temperature of conventional bag filter media (about 150-200°C) is far lower than the temperature of catalytic reaction, which limits the development of multifunctional filter media with denitrification.
  • the integrated filter material for denitrification and dust removal is a material that enables the filter material to intercept dust and at the same time has the function of catalytically removing pollutants such as nitrogen oxides, sulfur oxides or heavy metals. It can realize the coordinated removal of multiple pollutions and effectively avoid the above problems.
  • the realization of integrated filter material for denitrification and dust removal is mainly to assemble the catalyst and the filter material base material by impregnation or coating.
  • This method is difficult to solve the problem of low bonding fastness and uneven dispersion of catalyst powder and filter material base material
  • the disadvantages are that the service life of the filter material and the catalytic stability are insufficient.
  • the treated metal fiber felt is immersed in a metal salt solution, and the in-situ deposition agent is added to adjust the pH and then calcined to obtain a filter material.
  • the catalyst and filter The surface bonding fastness of the material base material is high, but the air permeability of the obtained filter material is not good, and it is easy to harden, resulting in a low service life of the filter material. At the same time, the catalyst will also have the problem of uneven dispersion on the filter material base material.
  • the technical problem to be solved in the present invention is to overcome the defects that the integrated filter material for denitrification and dust removal in the prior art cannot simultaneously ensure the high binding fastness between the filter material and the catalyst, the uniform distribution of the catalyst, and the good air permeability of the integrated filter material. Therefore, a filter material and its preparation method and application are provided.
  • the present invention provides the following technical solutions.
  • the invention provides a kind of preparation method of filter material, comprises the following steps,
  • the mass concentration of the urea solution is 5-40%
  • the volume concentration of the ammonia solution is 35-60%;
  • the volume concentration of the hydrogen peroxide is 10-45%.
  • step (2) spray urea solution and/or ammonia solution on the surface of the filter material substrate under the condition of 55-80°C, and then spray the hydrogen peroxide solution on the surface of the filter material substrate under the condition of 55-80°C;
  • the spraying amount of ammonia solution is 150-330ml/m 2 ;
  • the amount of urea solution sprayed is 150-230ml/m 2 in terms of per square meter of filter material substrate;
  • the spraying amount of the hydrogen peroxide solution is 120-300ml/m 2 .
  • step (1) the time for the filter substrate to be immersed in the metal salt solution is greater than 30s;
  • the metal salt solution includes at least one of titanium salt, cerium salt and manganese salt;
  • the mass concentration of the metal salt solution is 30-35%.
  • the metal salt solution includes titanium salt, cerium salt and manganese salt
  • the molar ratio of titanium, cerium and manganese in the metal salt solution is (10-12):(0.7-1.3):(4-5).
  • the temperature of the heat treatment is 250-300° C., and the time is 20-30 minutes.
  • the heat treatment step also includes the step of spraying polytetrafluoroethylene composite emulsion on the surface of the filter material base material, and after sintering, heat-press lamination with polytetrafluoroethylene expanded microporous membrane.
  • the process parameters of the hot-press lamination the temperature is 260-380°C, the vehicle speed is 1-10m/min, and the pressure is 0.2-0.5MPa;
  • the polytetrafluoroethylene composite emulsion includes a mass ratio of (20-50): (10-20): (0.5-1.5): (1.5-5) polytetrafluoroethylene emulsion, fluorine-containing silane waterproofing agent, coupling agent and inorganic water repellent;
  • the sintering temperature is 260-320° C., and the sintering time is 4-10 minutes.
  • a drying step is also included between the steps of heat treatment and spraying the polytetrafluoroethylene composite emulsion; wherein, the drying temperature is 100-120°C.
  • the present invention also provides a filter material prepared by the above method.
  • the filter material is an integrated filter material for dust removal and denitrification, which can have the functions of dust removal and denitrification at the same time.
  • the present invention also provides a filter material prepared by the above method or an application of the above filter material in catalytic denitrification.
  • the invention provides a kind of preparation method of filter material, comprising, (1) at 55-70 °C, filter material substrate is immersed in metal salt solution; (2) filter material substrate surface after dipping Spraying urea solution and/or ammonia solution, and then spraying hydrogen peroxide solution on the surface of the filter material substrate; (3) obtaining the filter material after heat treatment.
  • the denitrification and dust removal integrated filter material obtained by the method can ensure high binding fastness between the filter material base material and the catalyst, and can also make the catalyst evenly distributed on the filter material base material, and the presence of the catalyst does not affect the air permeability of the filter material.
  • the base material of the filter material is immersed in the metal salt solution under the condition of 55-70°C.
  • the metal salt solution can ensure that the metal salt solution is in a uniform state, so that the metal ions are evenly loaded on the surface of the fiber of the filter material base material.
  • the catalyst particles will not block the pores of the filter material and affect the air permeability of the filter material; on the other hand, at this temperature, the metal salt solution is in a stable state and will not form a suspension. It has good wettability to the base material of the filter material, so that the metal salt solution can evenly cover the base material of the filter material, and the base material of the filter material has good wettability.
  • the urea solution and/or ammonia solution is sprayed on the surface of the filter substrate by spraying, so that the urea and/or ammonia react with the metal ions on the surface of the filter substrate to form catalyst particles on the surface of the filter substrate, making the catalyst particles Firmly attached to the surface of the filter material base material, the bonding fastness is strong; compared with the direct dipping method adopted in the prior art, the spraying method adopted in the present invention has little influence on the air permeability of the filter material and the denitrification efficiency of the catalyst, and the catalyst is formed on the surface of the filter material Particles, reducing the phenomenon of particles inside the filter material blocking the pores and the phenomenon of filter material compaction, improving the filtering effect and service life.
  • Spraying urea solution and/or ammonia solution has a good reduction effect and a wide range of sources, and can be popularized and applied to the removal of nitrogen oxides in industrial flue gas.
  • Spraying the hydrogen peroxide solution on the filter base material by spraying can further improve the stability of the metal ion valence state in the metal complex and improve the denitrification efficiency of the catalyst. During use, no other metal ions will be introduced and the stability of the catalytic system will not be affected. , low price, no pollution.
  • the preparation method of the filter material provided by the invention is suitable for high-temperature-resistant filter material substrates such as glass fiber, polytetrafluoroethylene, polyimide, aramid fiber, and metal fiber.
  • the preparation method of the filter material provided by the present invention is under the condition of 55-80 °C, sprays reductant and oxidizing agent on the surface of filter material base material, can prevent the metal ion in the metal salt solution from separating out, settling, metal
  • sprays reductant and oxidizing agent on the surface of filter material base material can prevent the metal ion in the metal salt solution from separating out, settling, metal
  • the salt solution reacts with the reducing agent, there will be no problem of agglomeration, so that the metal salt solution, the reducing agent and the oxidizing agent can fully contact and react, and an integrated filter material with uniform catalyst distribution can be obtained.
  • this method metal salt solution comprises titanium salt, cerium salt and manganese salt, can improve the catalytic efficiency of catalyst on the one hand, when this filter material is used for catalytic denitrification on the other hand, can Lower the reaction temperature.
  • the heat treatment temperature is reduced while the integrated filter material for dedusting and denitrification is prepared, thereby saving energy and protecting the environment.
  • Fig. 1 is a scanning electron microscope image of the filter material in Example 1 of the present invention.
  • the coupling agent used in the comparative example is KH1100
  • the fluorine-containing silane waterproofing agent is FLW-99 type
  • the inorganic waterproofing agent is nano inorganic silicon waterproofing agent.
  • the present embodiment provides a kind of preparation method of filter material, comprises the following steps,
  • the metal salt solution includes titanyl sulfate, cerium nitrate and acetic acid in a molar ratio of 11:1:4.5 Manganese, the mass concentration of the metal salt solution is 15wt%.
  • the glass fiber base material is placed under the atmosphere of 65 °C, and the volume concentration of 40% ammonia solution and the hydrogen peroxide solution of 30% volume concentration are sprayed successively on the surface of the glass fiber base material after immersion, and the per square meter filter Based on the base material, the spraying amount of ammonia solution is 220ml/m 2 , and the spraying amount of hydrogen peroxide solution is 160ml/m 2 . After spraying, dry the glass fiber substrate at 120°C to remove excess water and other liquids. .
  • the polytetrafluoroethylene composite emulsion includes polytetrafluoroethylene emulsion with a mass ratio of 45:15:1.5:1.5:37, fluorine-containing silane waterproofing agent, coupling agent, inorganic waterproofing agent and water, and the spraying amount is glass fiber-based 4% of the material mass; the temperature of hot-press lamination is 345°C, the pressure is 0.3MPa, and the vehicle speed is 4m/min.
  • Figure 1 is a topographical view of the filter material of this embodiment, from which it can be seen that the catalyst is evenly distributed on the surface of the filter material substrate.
  • the present embodiment provides a kind of preparation method of filter material, comprises the following steps,
  • the metal salt solution includes sulfuric acid oxygen with a molar ratio of 11:1:4.5 Titanium, cerium nitrate and manganese acetate, the concentration of the metal salt solution is 10wt%.
  • the polyimide needle felt base material is placed under the atmosphere of 70 °C, and the polyimide needle felt base material surface after dipping is sprayed successively that mass concentration is 40% urea aqueous solution and volume concentration is 12 % hydrogen peroxide solution, in terms of per square meter of filter material base material, the spraying amount of urea aqueous solution is 200ml/m 2 , the spraying amount of hydrogen peroxide solution is 140ml/m 2 , after spraying, the polyimide needle felt base The material is dried at 120°C to remove excess water and other liquids.
  • the polytetrafluoroethylene composite emulsion includes polytetrafluoroethylene emulsion with a mass ratio of 40:15:1:2:42, fluorine-containing silane waterproofing agent, coupling agent, inorganic waterproofing agent and water, and the spraying amount is polyimide 4wt% of the mass of the amine needle felt substrate; the temperature of hot-press lamination is 328°C, the pressure is 0.45MPa, and the vehicle speed is 5m/min.
  • the present embodiment provides a kind of preparation method of filter material, comprises the following steps,
  • the glass fiber and polyimide composite needle felt substrate were immersed in the metal salt solution, and the immersion time was 0.8min; wherein, the metal salt solution included a molar ratio of 11:1: 4.5 titanyl sulfate, cerium nitrate and manganese acetate, the concentration of the metal salt solution is 35wt%.
  • the composite needle felt base material is then placed in an atmosphere of 70° C., and the volume concentration of 40% ammonia solution and the volume concentration of 40% hydrogen peroxide solution are sprayed on the surface of the impregnated composite needle felt base material successively, with Calculated per square meter of filter material substrate, the spraying amount of ammonia solution is 320ml/m 2 , and the spraying amount of hydrogen peroxide solution is 270ml/m 2 . After spraying, put the composite needle felt substrate at 120°C to dry , to remove excess water and other liquids.
  • the polytetrafluoroethylene composite emulsion includes polytetrafluoroethylene emulsion with a mass ratio of 50:10:1.5:1.5:37, a fluorine-containing silane waterproofing agent, a coupling agent, an inorganic waterproofing agent and water, and the spraying amount is the composite acupuncture 4wt% of the mass of the felt substrate; the temperature of hot-press lamination is 320° C., the pressure is 0.5 MPa, and the vehicle speed is 10 m/min.
  • the present embodiment provides a kind of preparation method of filter material, comprises the following steps,
  • the metal salt solution includes titanyl sulfate, cerium nitrate and Manganese acetate, the concentration of the metal salt solution is 10wt%.
  • the glass fiber substrate is placed in an atmosphere of 60°C, and the volume concentration of 35% ammonia solution and 20% hydrogen peroxide solution are sprayed on the surface of the impregnated glass fiber substrate successively.
  • the spraying amount of ammonia solution is 160ml/m 2
  • the spraying amount of hydrogen peroxide solution is 120ml/m 2 .
  • the polytetrafluoroethylene composite emulsion includes polytetrafluoroethylene emulsion with a mass ratio of 50:10:1:2:36, fluorine-containing silane waterproofing agent, coupling agent, inorganic waterproofing agent and water, and the spraying amount is glass fiber-based 4wt% of the material weight; the temperature of hot-press lamination is 340°C, the pressure is 0.35MPa, and the vehicle speed is 6m/min.
  • This comparative example provides a kind of preparation method of filter material, comprises the following steps,
  • the metal salt solution includes titanyl sulfate, cerium nitrate and acetic acid in a molar ratio of 11:1:4.5 Manganese, the concentration of the metal salt solution is 15wt%.
  • the glass fiber substrate is placed in an atmosphere of 70°C, and the volume concentration of 40% ammonia solution and 30% hydrogen peroxide solution are sprayed on the surface of the impregnated glass fiber substrate successively.
  • the spraying amount of ammonia solution is 220ml/m 2
  • the spraying amount of hydrogen peroxide solution is 160ml/m 2 .
  • the polytetrafluoroethylene composite emulsion includes polytetrafluoroethylene emulsion with a mass ratio of 45:15:1.5:1.5:37, fluorine-containing silane waterproofing agent, coupling agent, inorganic waterproofing agent and water, and the spraying amount is glass fiber-based 4wt% of the material mass; the temperature of hot-press lamination is 345°C, the pressure is 0.3MPa, and the vehicle speed is 4m/min.
  • This comparative example provides a kind of preparation method of filter material, comprises the following steps,
  • the metal salt solution includes titanyl sulfate, cerium nitrate and manganese acetate in a molar ratio of 11:1:4.5, and the mass concentration of the metal salt solution is 15 wt%.
  • the polytetrafluoroethylene composite emulsion includes polytetrafluoroethylene emulsion with a mass ratio of 45:15:1.5:1.5:37, fluorine-containing silane waterproofing agent, coupling agent, inorganic waterproofing agent and water, and the spraying amount is glass fiber-based 4wt% of the material mass; the temperature of hot-press lamination is 345°C, the pressure is 0.3MPa, and the vehicle speed is 4m/min.
  • This test example provides the performance tests and test results of the filter materials prepared in Examples 1-4 and Comparative Examples 1-2.
  • the test methods are as follows, and the test results are shown in Table 1.
  • the weight deviation of the catalyst loaded on the filter material per square meter is in accordance with Section 9.1 of the standard GB/T6719-2009c;
  • the air permeability of the filter material is in accordance with the standard GB/T6719-2009c section 9.2;
  • the filtration resistance of the filter material is in accordance with section 9.5 of the standard GB/T6719-2009c.
  • the test method for the catalytic denitrification efficiency of the filter material is: test the denitrification efficiency at 250°C, specifically, after the nitrogen oxide gas meter passes through the disc-shaped filter material with a diameter of 10cm at a speed of 0.5m/min, the concentration of nitrogen oxides decreases by the percentage.
  • the catalyst prepared by the present invention has a small deviation in the loaded square meter gram weight, indicating that the catalyst is evenly distributed on the filter material substrate, and the filter material is used for denitrification, and the denitrification efficiency is high; the smaller the filtration resistance, the more breathable The greater the permeability, the better the air permeability of the filter material.
  • the filter material prepared in Example 1-4 of the present invention with both dust removal and catalytic denitrification functions is not easy to fall off during use, and the filter material prepared in Comparative Example 1-2 is not easy to fall off during use.
  • the filter material prepared by the present invention has higher binding fastness to the catalyst, and on the basis of ensuring the binding fastness, the distribution uniformity and air permeability of the catalyst are further improved.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

L'invention concerne un matériau filtrant, son procédé de préparation, et son application. La méthode de préparation consiste à : (1) tremper un substrat de matériau de filtrant dans une solution de sel métallique à 55-70 °C ; (2) pulvériser une solution d'urée et/ou une solution d'eau d'ammoniac sur la surface du substrat de matériau filtrant trempé, puis pulvériser une solution de peroxyde d'hydrogène sur la surface du substrat de matériau filtrant ; et (3) réaliser un traitement thermique pour obtenir le matériau filtrant.
PCT/CN2021/133271 2021-06-22 2021-11-25 Matériau filtrant, sa méthode de préparation, et son application WO2022267335A1 (fr)

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CN202110691710.3A CN113476958B (zh) 2021-06-22 2021-06-22 一种滤料及其制备方法和应用

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CN103230813A (zh) * 2013-04-27 2013-08-07 北京工业大学 一种适用于水泥窑炉的抗碱中毒的脱硝催化剂的制备方法
CN103463871A (zh) * 2013-09-02 2013-12-25 安徽锦鸿环保科技有限公司 一种脱硝除尘玻璃纤维覆膜滤料
JP2017144430A (ja) * 2016-02-18 2017-08-24 ユニチカ株式会社 集塵フィルター用ガラス繊維布帛及び該布帛を備えるバグフィルター
CN109847580A (zh) * 2019-03-21 2019-06-07 青岛大学 基于等离子体前处理和浸渍法的脱硝滤料及其制备方法
CN113476958A (zh) * 2021-06-22 2021-10-08 南京玻璃纤维研究设计院有限公司 一种滤料及其制备方法和应用

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