CN116850700A - Multifunctional dedusting and denitration filter material with flower-shaped catalytic interface, preparation method and application - Google Patents

Multifunctional dedusting and denitration filter material with flower-shaped catalytic interface, preparation method and application Download PDF

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CN116850700A
CN116850700A CN202311067118.1A CN202311067118A CN116850700A CN 116850700 A CN116850700 A CN 116850700A CN 202311067118 A CN202311067118 A CN 202311067118A CN 116850700 A CN116850700 A CN 116850700A
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filter material
salt
flower
denitration
multifunctional
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杨波
王刘莹
汪振辉
黄琼
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Nanjing University of Information Science and Technology
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Nanjing University of Information Science and Technology
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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
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • 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
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
    • 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
    • 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
    • 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
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J15/00—Arrangements of devices for treating smoke or fumes
    • F23J15/003—Arrangements of devices for treating smoke or fumes for supplying chemicals to fumes, e.g. using injection devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J15/00—Arrangements of devices for treating smoke or fumes
    • F23J15/02—Arrangements of devices for treating smoke or fumes of purifiers, e.g. for removing noxious material
    • F23J15/022—Arrangements of devices for treating smoke or fumes of purifiers, e.g. for removing noxious material for removing solid particulate material from the gasflow
    • F23J15/025—Arrangements of devices for treating smoke or fumes of purifiers, e.g. for removing noxious material for removing solid particulate material from the gasflow using filters
    • 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

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Abstract

The invention belongs to the technical field of functional composite filter materials, and particularly relates to a dust-removing and denitration multifunctional filter material with a flower-shaped catalytic interface, a preparation method and application thereof; the preparation raw materials of the dedusting and denitration multifunctional filter material comprise active stock solution and a filter material substrate; the active stock solution comprises the following components in percentage by mass: 10-45% of active component precursor and 5-15% of morphology auxiliary agent; the active component precursor comprises: titanium salt, chromium salt, manganese salt and lanthanum salt, and the mol ratio of Ti/Cr/Mn/La elements in the active component precursor is 1: (0.5-0.8): (0.3-0.9): (0.1-0.4); the morphology auxiliary agent comprises: bismuth salt, nitrogen salt, cerium salt and molybdenum salt, wherein the mole ratio of Bi/N/Ce/Mo elements in the morphology auxiliary agent is 1: (0.1-0.7): (0.3-0.8): (0.1-0.5). The dedusting and denitration multifunctional filter material consists of a filter material substrate and a flower-shaped catalytic interface wrapped on the surface of the filter material substrate; the invention has important significance for popularization and application of the collaborative dedusting and denitration technology in industries such as ceramics and the like.

Description

Multifunctional dedusting and denitration filter material with flower-shaped catalytic interface, preparation method and application
Technical Field
The invention belongs to the technical field of functional composite filter materials, and particularly relates to a dust-removing and denitration multifunctional filter material with a flower-shaped catalytic interface, a preparation method and application thereof.
Background
The ceramic industry is one of the traditional dominant industries with long history in China and plays an important role in national economy. The statistics show that the total amount of the flue gas generated by the ceramic industrial kiln in 2017 is about 11674 trillion m 3 If the standard emission concentration is calculated, the ceramic industry particles and SO 2 、NO x The annual emission total amounts are respectively about 3.5 ten thousand tons, 5.8 ten thousand tons and 21 ten thousand tons, the annual national industrial emission proportions are respectively 0.44 percent, 0.66 percent and 1.67 percent, and the emission amount is larger. Therefore, the ceramic industry is an important industry for controlling the atmospheric pollution in China, and has important significance for controlling the atmospheric pollution. At present, the focus of the treatment of atmospheric pollutants in the ceramic industry is on the ceramic industry of buildings, and the dust removal and desulfurization treatment technology is mature and has high popularity, so that the environmental protection requirement can be met. However, the denitration technology is still imperfect, and fluoride, chloride and heavy metal in the flue gas are mainly controlled cooperatively through dust removal, desulfurization and denitration facilities, and the sintering process is optimized and the raw materials are controlled, so that the emission standard requirement can be basically met. In the aspect of denitration, the ceramic industry has two technologies, a Selective Non-catalytic reduction technology (SNCR) is adopted for denitration, the effect is poor, the denitration efficiency is only 10% -30%, and the reducing agent has an influence on equipment and products. The kiln adopts a selective catalytic reduction technology (Selective Catalytic Reduction, SCR) to achieve high denitration efficiency, mature technology and denitration efficiency of about 80 percent. However, SCR technology has few cases of application in the ceramic industry due to limitations in operating conditions, costs, and the like.
Dust removal and denitration dual-function filter material can realize simultaneous removal of dust and NO x However, at present, no patent aiming at the dedusting and denitration dual-function filter material in the ceramic industry exists. Has the following componentsIn the patent related to dedusting and denitration filter materials, the patent (CN 114699845A) uses polyphenylene sulfide as a basic filter material, and sodium alginate is adopted to modify the polyphenylene sulfide; loading denitration active component MnO by adopting excessive impregnation method 2 -CeO 2 -Co 3 O 4 The method comprises the steps of carrying out a first treatment on the surface of the And (3) spraying polytetrafluoroethylene slurry with the concentration of 5% after the polyphenylene sulfide functional filter material is immersed to prepare the dedusting and denitration integrated filter material. The patent (CN 112704959A) adds sodium alginate powder into a precursor solution to form a sol system, and adopts a blending method or a two-step method to prepare the dedusting and denitration integrated filter material. The catalyst is only coated on the surface of the filter material, and the direct coating mode can lead to uneven distribution, easy falling-off and short service life of the catalyst particles; meanwhile, the catalyst is easy to be poisoned and deactivated by the influence of chlorine, fluorine and the like in ceramic industrial flue gas.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a dust-removing and denitration multifunctional filter material with a flower-shaped catalytic interface, a preparation method and application thereof. N in the catalytic interface of the flower-like morphology 2 The catalyst has high selectivity and NOx removal activity, and simultaneously has excellent chlorine resistance, fluoride resistance and SO resistance 2 Poisoning performance. The multifunctional filter material does not need to modify any equipment when in use, can be suitable for roller kilns, tunnel kilns, shuttle kilns and the like in the ceramic industry, and can remove dust and NO in a dust remover at the same time x The denitration rate is more than or equal to 98 percent in the temperature range of 140-180 ℃.
The aim of the invention can be achieved by the following technical scheme:
the preparation raw materials of the dust-removing and denitration multifunctional filter material with the flower-shaped catalytic interface comprise active stock solution and a filter material substrate;
the active stock solution comprises the following components in percentage by mass:
10 to 45 percent of active component precursor,
5-15% of morphology auxiliary agent;
the active component precursor comprises: titanium salt, chromium salt, manganese salt and lanthanum salt, and the mol ratio of Ti/Cr/Mn/La elements in the active component precursor is 1: (0.5-0.8): (0.3-0.9): (0.1-0.4); the morphology auxiliary agent comprises: bismuth salt, nitrogen salt, cerium salt and molybdenum salt, wherein the mole ratio of Bi/N/Ce/Mo elements in the morphology auxiliary agent is 1: (0.1-0.7): (0.3-0.8): (0.1-0.5).
Preferably, the titanium salt is one of titanium dioxide and titanium tetrachloride, the chromium salt is one of chromium nitrate, chromium chloride and chromium sulfate, the manganese salt is one of manganese nitrate and manganese sulfate, and the lanthanum salt is one of lanthanum chloride and lanthanum nitrate.
Preferably, the bismuth salt is one of bismuth trichloride and bismuth oxide, the nitrogen salt is one of 1-methyl-2-pyrrolidone and N, N-dimethylformamide, the cerium salt is one of cerium nitrate and cerium sulfate, and the molybdenum salt is molybdenum sulfate.
Preferably, the filter material substrate is one of PPS fiber filter material, PTFE fiber filter material, glass fiber filter material, P84 filter material or Flumes filter material.
Preferably, the active stock solution further comprises the following components in percentage by mass:
10 to 25 percent of activated coupling agent,
1 to 15 percent of cosolvent,
25-74% of deionized water.
Preferably, the activated coupling agent is one of sodium hydroxide or sodium hypochlorite; the cosolvent is one of isopropanol, acetone and ethyl acetate.
The preparation method of the dust-removing and denitration multifunctional filter material with the flower-shaped catalytic interface comprises the following steps of:
(1) Preparation of active stock solution
Adding the active component precursor, the morphology auxiliary agent, the activated coupling agent and the cosolvent into deionized water, and magnetically stirring at a constant temperature of 20-50 ℃ at a stirring speed of 150-260 r/min to completely dissolve each component in the deionized water to obtain an active stock solution;
(2) In situ growth of catalytic interface
Firstly, immersing a filter material substrate in an active stock solution, and continuously oscillating and stirring to pretreat the filter material substrate; transferring the pretreated filter material substrate and the active stock solution into a reaction kettle, fixing the reaction kettle on a reactor, and mechanically mixing the filter material substrate and the active stock solution in the reactor, so that active components with flower-shaped catalytic interfaces are generated in situ on the surface of the filter material substrate, and the active components with flower-shaped catalytic interfaces are wrapped on the fiber surface of the filter material substrate;
(3) Flower-like catalytic interface solidification shaping
Taking out the filter material substrate obtained in the step (2), soaking and washing for 3 times by using a curing agent, curing and shaping the catalytic interface morphology, and soaking and washing for 3 times by using deionized water to remove surface impurities; finally, drying to obtain the dust-removing and denitration multifunctional filter material with the flower-shaped catalytic interface.
Preferably, in the step (2), when the filter material base material and the active stock solution are moved into a reaction kettle together for reaction, the reaction kettle is required to be fixed on a rotating bracket of a reactor; the reaction temperature in the reaction kettle is set to be 90-170 ℃, the reaction time is 20-30 hours, and the rotating speed of the rotating bracket is 240-400 rpm;
the equipment used for drying in the step (3) is a forced air drying oven, and the drying conditions are as follows: drying at 50-120deg.C for 40-110 min, and heating to 111-300deg.C for 60-350 min.
Preferably, the curing agent in the step (3) is one of polyurethane, vinyl chloride or ammonium sulfate.
Preferably, the multifunctional filter material with the flower-shaped catalytic interface for dust removal and denitration is applied to the aspect of absorbing smoke dust in the ceramic manufacturing industry.
The invention has the beneficial effects that:
(1) The invention provides a flower-shaped catalytic interface dedusting and denitration multifunctional filter material, active components loaded on the filter material have flower-shaped morphology, and the flower-shaped catalytic interface N 2 Selectivity and NO x High removal activity and excellent chlorine resistanceFluoride and SO 2 Poisoning performance;
(2) The flower-like catalytic interface dedusting and denitration multifunctional filter material provided by the invention has the advantage that denitration is more than or equal to 98% in a temperature range of 140-180 ℃;
(3) The preparation method is simple and has high production feasibility;
(4) The invention has important significance for popularization and application of the gas collaborative dust removal denitration technology in the ceramic industry of buildings, and can be applied to industrial scenes such as roller kilns, tunnel kilns, shuttle kilns and the like in the ceramic industry.
Drawings
In order to more clearly illustrate the embodiments of the present disclosure or the prior art, the drawings that are required for the description of the embodiments or the prior art will be briefly described, and it will be apparent to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is an SEM image of the finished product of the dust removal and denitration multifunctional filter material with the flower-shaped catalytic interface under different scales.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) Preparing precursor stock solution
10g (10%) of active component precursors, 5g (5%) of morphology auxiliary agents, 10g (10%) of activated coupling agents, 1g (1%) of cosolvents and 74g (74%) of deionized water are weighed. The element mol ratio of Ti/Cr/Mn/La is 1:0.5:0.3:0.1; the element mol ratio of Bi/N/Ce/Mo is 1:0.1:0.3:0.1, the addition amounts of active component precursors of titanium dioxide, chromium nitrate, manganese nitrate, lanthanum chloride, morphology auxiliary agent bismuth trichloride, 1-methyl-2-pyrrolidone, cerium nitrate and molybdenum sulfate are calculated respectively, and are dissolved in deionized water; and weighing the activated coupling agent sodium hydroxide and cosolvent isopropanol with corresponding masses, adding the activated coupling agent sodium hydroxide and cosolvent isopropanol into deionized water, and magnetically stirring at a constant temperature of 20 ℃ at a stirring speed of 150 revolutions per minute to completely dissolve the activated coupling agent sodium hydroxide and cosolvent isopropanol.
(2) In situ growth of catalytic interface
Immersing the PPS fiber filter material into the precursor solution stirred in the step (1), and carrying out ultrasonic oscillation for 40 minutes at 20 ℃, wherein the stirring speed is 100 revolutions per minute; the treated dedusting filter material and the precursor solution are moved into a reactor together, the reactor is fixed on a rotating bracket of a homogeneous reactor, the homogeneous reaction time is 20 hours, and the reaction temperature is 90 ℃; the rotational speed of the rotating support is 240 revolutions per minute.
(3) Catalytic interfacial curing shaping
Taking out the dedusting filter material obtained in the step (2), soaking and washing for 3 times by using curing agent polyurethane, and soaking and washing for 3 times by using deionized water; drying in a forced air drying oven, drying at 50 ℃ for 50 minutes, and then heating to 111 ℃ for 60 minutes to obtain the flower-shaped multifunctional filter material for dust removal and denitration of the catalytic interface.
And performing performance measurement on the prepared dedusting and denitration composite multifunctional filter material.
NO x The removal efficiency test method is as follows:
the experimental device consists of a gas distribution system, a flow control (mass flow device), a gas mixer, a gas preheater, a catalytic reactor and a flue gas analysis system. The inner diameter Φ=20 mm. Cutting the filter cloth into round pieces with phi=20mm, standing in a fixed reactor, maintaining the temperature of a constant temperature area where the filter cloth is positioned, and then placing the reactor into a fixed tubular reactor. The simulated flue gas composition was NO (500 ppm), NH 3 (500 ppm), chlorine (100 ppm), hydrogen fluoride (100 ppm), SO 2 (200ppm)、O 2 (8%) and carrier gas N 2 Composition, filter wind speed 1m/min, NH 3 No=1, and the reaction temperature was controlled at 200 ℃. Each gas flow is controlled by a mass flow meter. The gases are mixed by a gas mixer before entering the reactorHeated by a heater. NO of air inlet and air outlet x The concentration was determined by KM9106 (kane) flue gas analyzer. To eliminate the effect of surface adsorption, the system was run stable for 20-30 minutes at aeration to begin the acquisition test.
The catalytic activity of the catalyst is mainly achieved by NO x Is reflected by the denitration activity of (2) NO x The denitration activity of (2) is calculated by the following formula:
c in the formula 0 The initial concentration, the concentration after treatment of the C flue gas.
The method for testing the removal efficiency of the flue gas dust comprises the following steps:
a VDI filter material simulation testing device is adopted to test the filtering performance of a sample, and Pural NF alumina dust is selected for use, wherein the dust concentration is 5g/m 3 Filtering air speed 2m/min, ash removal pressure difference 1000Pa, test area 0.0154m 2 The pulse blowing interval is 5s, the tank pressure is 0.5MPa, the humidity is less than 50%, and the pulse valve opening time is 60ms. The dust removal rate is calculated by the following formula:
wherein u is the initial concentration, u 0 Is the concentration of the flue gas after treatment.
NO x Removal efficiency and dust removal efficiency:
sample of Temperature (temperature) Denitration Activity Dust removal rate
Example 1 200℃ 83％ 99％
Example 2
(1) Preparing precursor stock solution
15g (15%) of active component precursor, 7g (7%) of morphology auxiliary agent, 15g (15%) of activated coupling agent, 3g (3%) of cosolvent and 60g (60%) of deionized water are weighed. The element mol ratio of Ti/Cr/Mn/La is 1:0.6:0.5:0.2; the element mol ratio of Bi/N/Ce/Mo is 1:0.2:0.4:0.2, and the addition amounts of active component precursors titanium tetrachloride, chromium chloride, manganese sulfate, lanthanum nitrate, morphology auxiliary agents bismuth chloride, N-dimethyl-methyl-Coolamine, cerium sulfate and molybdenum sulfate are respectively calculated and dissolved in deionized water; and weighing the sodium hypochlorite serving as an active coupling agent and propanol serving as a cosolvent with corresponding mass, adding the sodium hypochlorite and propanol serving as the active coupling agent into deionized water, and magnetically stirring at a constant temperature of 30 ℃ at a stirring speed of 180 revolutions per minute to completely dissolve the sodium hypochlorite and propanol serving as the active coupling agent.
(2) In situ growth of catalytic interface
Immersing the P84 filter material into the precursor solution stirred in the step (1), and carrying out ultrasonic oscillation for 60 minutes at 30 ℃, wherein the stirring speed is 100 revolutions per minute; the treated dedusting filter material and the precursor solution are moved into a reactor together, the reactor is fixed on a rotating bracket of a homogeneous reactor, the homogeneous reaction time is 23 hours, and the reaction temperature is 120 ℃; the rotational speed of the rotating support is 280 revolutions per minute.
(3) Catalytic interfacial curing shaping
Taking out the dedusting filter material obtained in the step (2), soaking and washing for 3 times by using curing agent chloroethylene, and soaking and washing for 3 times by using deionized water; drying in a forced air drying oven, drying at 70 ℃ for 70 minutes, and then heating to 160 ℃ for drying for 100 minutes to obtain the flower-shaped multifunctional filter material for dust removal and denitration of the catalytic interface.
Performance test is carried out on the prepared dedusting and denitration multifunctional filter material, and NO X The dust removal rate test method was the same as in example 1.
The test results were as follows:
sample of Temperature (temperature) Denitration Activity Dust removal rate
Example 2 200℃ 89％ 99％
Example 3
(1) Preparing precursor stock solution
30g (30%) of active component precursors, 12g (12%) of morphology auxiliary agents, 20g (20%) of activated coupling agents, 5g (5%) of cosolvents and 33g (33%) of deionized water are weighed. The element mol ratio of Ti/Cr/Mn/La is 1:0.7:0.7:0.3; the element mol ratio of Bi/N/Ce/Mo is 1:0.5:0.6:0.3, and the addition amounts of active component precursors of titanium dioxide, chromium nitrate, manganese nitrate, lanthanum chloride, morphology auxiliary agent bismuth trichloride, 1-methyl-2-pyrrolidone, cerium nitrate and molybdenum sulfate are respectively calculated and dissolved in deionized water; and weighing the activated coupling agent sodium hydroxide and cosolvent isopropanol with corresponding masses, adding the activated coupling agent sodium hydroxide and cosolvent isopropanol into deionized water, and magnetically stirring at a constant temperature of 40 ℃ at a stirring speed of 220 rpm to completely dissolve the activated coupling agent sodium hydroxide and cosolvent isopropanol.
(2) In situ growth of catalytic interface
Immersing the PTFE fiber filter material into the precursor solution stirred in the step (1), and carrying out ultrasonic oscillation for 120 minutes at 40 ℃, wherein the stirring speed is 300 revolutions per minute; the treated dedusting filter material and the precursor solution are moved into a reactor together, the reactor is fixed on a rotating bracket of a homogeneous reactor, the homogeneous reaction time is 26 hours, and the reaction temperature is 140 ℃; the rotational speed of the rotating support is 350 revolutions per minute.
(3) Catalytic interfacial curing shaping
Taking out the dedusting filter material obtained in the step (2), soaking and washing for 3 times by using curing agent polyurethane, and soaking and washing for 3 times by using deionized water; drying in a forced air drying oven, drying at 100 ℃ for 80 minutes, and then heating to 240 ℃ for drying for 280 minutes to obtain the flower-shaped multifunctional filter material for dust removal and denitration of the catalytic interface.
Performance test is carried out on the prepared dedusting and denitration multifunctional filter material, and NO x The dust removal rate test method was the same as in example 1.
The test results were as follows:
sample of Temperature (temperature) Denitration Activity Dust removal rate
Example 3 200℃ 98％ 99.9％
Example 4
(1) Preparing precursor stock solution
40g (40%) of active component precursor, 8g (8%) of morphology auxiliary agent, 19g (19%) of activated coupling agent, 8g (8%) of cosolvent and 25g (25%) of deionized water are weighed. The element mol ratio of Ti/Cr/Mn/La is 1:0.8:0.9:0.4; the element mol ratio of Bi/N/Ce/Mo is 1:0.7:0.8:0.5, and the addition amounts of active component precursors titanium tetrachloride, chromium sulfate, manganese sulfate, lanthanum nitrate, morphology auxiliary agents bismuth chloride, N-dimethyl-methyl-Coolamine, cerium sulfate and molybdenum sulfate are respectively calculated and dissolved in deionized water; and weighing the sodium hypochlorite serving as an active coupling agent and ethyl acetate serving as a cosolvent with corresponding mass, adding the sodium hypochlorite and the ethyl acetate serving as the cosolvent into deionized water, and magnetically stirring at a constant temperature of 50 ℃ at a stirring speed of 260 revolutions per minute to completely dissolve the sodium hypochlorite and the ethyl acetate.
(2) In situ growth of catalytic interface
Immersing the glass fiber filter material into the precursor solution stirred in the step (1), and carrying out ultrasonic oscillation for 150 minutes at 50 ℃, wherein the stirring speed is 400 revolutions per minute; the treated dedusting filter material and the precursor solution are moved into a reactor together, the reactor is fixed on a rotating bracket of a homogeneous reactor, the homogeneous reaction time is 30 hours, and the reaction temperature is 170 ℃; the rotational speed of the rotating support is 350 revolutions per minute.
(3) Catalytic interfacial curing shaping
Taking out the dedusting filter material obtained in the step (2), soaking and washing for 3 times by using ammonium sulfate as a curing agent, and soaking and washing for 3 times by using deionized water; drying in a forced air drying oven, drying at 120 ℃ for 100 minutes, and then heating to 240 ℃ for drying for 300 minutes to obtain the flower-shaped multifunctional filter material for dust removal and denitration of the catalytic interface.
Performance test is carried out on the prepared dedusting and denitration multifunctional filter material, and NO x The dust removal rate test method was the same as in example 1.
The test results were as follows:
sample of Temperature (temperature) Denitration Activity Dust removal rate
Example 4 200℃ 91％ 99％
Comparative example 1
(1) Preparing precursor stock solution
12g (12%) of morphology aid, 20g (20%) of activated coupling agent, 5g (5%) of cosolvent and 63g (63%) of deionized water are weighed. The element mol ratio of Bi/N/Ce/Mo is 1:0.5:0.6:0.3, the addition amounts of morphology auxiliary agents bismuth trichloride, 1-methyl-2-pyrrolidone, cerium nitrate and molybdenum sulfate are calculated respectively, and the morphology auxiliary agents bismuth trichloride, 1-methyl-2-pyrrolidone, cerium nitrate and molybdenum sulfate are dissolved in deionized water; and weighing the activated coupling agent sodium hydroxide and cosolvent isopropanol with corresponding masses, adding the activated coupling agent sodium hydroxide and cosolvent isopropanol into deionized water, and magnetically stirring at a constant temperature of 40 ℃ at a stirring speed of 220 rpm to completely dissolve the activated coupling agent sodium hydroxide and cosolvent isopropanol.
(2) In situ growth of catalytic interface
Immersing the PTFE fiber filter material into the precursor solution stirred in the step (1), and carrying out ultrasonic oscillation for 120 minutes at 40 ℃, wherein the stirring speed is 300 revolutions per minute; the treated dedusting filter material and the precursor solution are moved into a reactor together, the reactor is fixed on a rotating bracket of a homogeneous reactor, the homogeneous reaction time is 26 hours, and the reaction temperature is 140 ℃; the rotational speed of the rotating support is 350 revolutions per minute.
(3) Catalytic interfacial curing shaping
Taking out the dedusting filter material obtained in the step (2), soaking and washing for 3 times by using curing agent polyurethane, and soaking and washing for 3 times by using deionized water; drying in a forced air drying oven, drying at 100 ℃ for 80 minutes, and then heating to 240 ℃ for drying for 280 minutes to obtain the flower-shaped multifunctional filter material for dust removal and denitration of the catalytic interface.
Performance test is carried out on the prepared dedusting and denitration multifunctional filter material, and NO x The dust removal rate test method was the same as in example 1.
The test results were as follows:
sample of Temperature (temperature) Denitration Activity Dust removal rate
Comparative example 1 200℃ 12％ 99％
Comparative example 2
(1) Preparing precursor stock solution
30g (30%) of active component precursor, 20g (20%) of activated coupling agent, 5g (5%) of cosolvent and 45g (45%) of deionized water are weighed. The element mol ratio of Ti/Cr/Mn/La is 1:0.7:0.7:0.3; respectively calculating the addition amounts of active component precursors of titanium dioxide, chromium nitrate, manganese nitrate and lanthanum chloride, and dissolving the active component precursors in deionized water; and weighing the activated coupling agent sodium hydroxide and cosolvent isopropanol with corresponding masses, adding the activated coupling agent sodium hydroxide and cosolvent isopropanol into deionized water, and magnetically stirring at a constant temperature of 40 ℃ at a stirring speed of 220 rpm to completely dissolve the activated coupling agent sodium hydroxide and cosolvent isopropanol.
(2) In situ growth of catalytic interface
Immersing the PTFE fiber filter material into the precursor solution stirred in the step (1), and carrying out ultrasonic oscillation for 120 minutes at 40 ℃, wherein the stirring speed is 300 revolutions per minute; the treated dedusting filter material and the precursor solution are moved into a reactor together, the reactor is fixed on a rotating bracket of a homogeneous reactor, the homogeneous reaction time is 26 hours, and the reaction temperature is 140 ℃; the rotational speed of the rotating support is 350 revolutions per minute.
(3) Catalytic interfacial curing shaping
Taking out the dedusting filter material obtained in the step (2), soaking and washing for 3 times by using curing agent polyurethane, and soaking and washing for 3 times by using deionized water; drying in a forced air drying oven, drying at 100 ℃ for 80 minutes, and then heating to 240 ℃ for drying for 280 minutes to obtain the flower-shaped multifunctional filter material for dust removal and denitration of the catalytic interface.
Performance test is carried out on the prepared dedusting and denitration multifunctional filter material, and NO x The dust removal rate test method was the same as in example 1.
The test results were as follows:
sample of Temperature (temperature) Denitration Activity Dust removal rate
Comparative example 2 200℃ 65％ 99％
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims.

Claims (10)

1. The multifunctional filter material with the flower-shaped catalytic interface for dust removal and denitration is characterized in that the preparation raw materials of the multifunctional filter material with the flower-shaped catalytic interface for dust removal and denitration comprise active stock solution and a filter material substrate;
the active stock solution comprises the following components in percentage by mass:
10 to 45 percent of active component precursor,
5-15% of morphology auxiliary agent;
the active component precursor comprises: titanium salt, chromium salt, manganese salt and lanthanum salt, and the mol ratio of Ti/Cr/Mn/La elements in the active component precursor is 1: (0.5-0.8): (0.3-0.9): (0.1-0.4); the morphology auxiliary agent comprises: bismuth salt, nitrogen salt, cerium salt and molybdenum salt, wherein the mole ratio of Bi/N/Ce/Mo elements in the morphology auxiliary agent is 1: (0.1-0.7): (0.3-0.8): (0.1-0.5).
2. The multifunctional dedusting and denitration filter material with the flower-shaped catalytic interface as claimed in claim 1, which is characterized in that: the titanium salt is one of titanium dioxide and titanium tetrachloride, the chromium salt is one of chromium nitrate, chromium chloride and chromium sulfate, the manganese salt is one of manganese nitrate and manganese sulfate, and the lanthanum salt is one of lanthanum chloride and lanthanum nitrate.
3. The multifunctional dedusting and denitration filter material with the flower-shaped catalytic interface as claimed in claim 2, which is characterized in that: the bismuth salt is one of bismuth trichloride and bismuth oxide, the nitrogen salt is one of 1-methyl-2-pyrrolidone and N, N-dimethylformamide, the cerium salt is one of cerium nitrate and cerium sulfate, and the molybdenum salt is molybdenum sulfate.
4. The multifunctional dedusting and denitration filter material with the flower-shaped catalytic interface as claimed in claim 1, which is characterized in that: the filter material substrate is one of PPS fiber filter material, PTFE fiber filter material, glass fiber filter material, P84 filter material or Flumesi filter material.
5. The multifunctional dedusting and denitration filter material with the flower-shaped catalytic interface as claimed in claim 1, which is characterized in that: the active stock solution comprises the following components in percentage by mass:
10 to 25 percent of activated coupling agent,
1 to 15 percent of cosolvent,
25-74% of deionized water.
6. The multifunctional dedusting and denitration filter material with the flower-shaped catalytic interface as claimed in claim 1, which is characterized in that: the activated coupling agent is one of sodium hydroxide or sodium hypochlorite; the cosolvent is one of isopropanol, acetone and ethyl acetate.
7. The preparation method of the dust-removing and denitration multifunctional filter material with the flower-shaped catalytic interface is characterized by comprising the following steps of:
(1) Preparation of active stock solution
Adding the active component precursor, the morphology auxiliary agent, the activated coupling agent and the cosolvent into deionized water, and magnetically stirring at a constant temperature of 20-50 ℃ at a stirring speed of 150-260 r/min to completely dissolve each component in the deionized water to obtain an active stock solution;
(2) In situ growth of catalytic interface
Firstly, immersing a filter material substrate in an active stock solution, and continuously oscillating and stirring to pretreat the filter material substrate; transferring the pretreated filter material substrate and the active stock solution into a reaction kettle, fixing the reaction kettle on a reactor, and mechanically mixing the filter material substrate and the active stock solution in the reactor, so that active components with flower-shaped catalytic interfaces are generated in situ on the surface of the filter material substrate, and the active components with flower-shaped catalytic interfaces are wrapped on the fiber surface of the filter material substrate;
(3) Flower-like catalytic interface solidification shaping
Taking out the filter material substrate obtained in the step (2), soaking and washing for 3 times by using a curing agent, curing and shaping the catalytic interface morphology, and soaking and washing for 3 times by using deionized water to remove surface impurities; finally, drying to obtain the dust-removing and denitration multifunctional filter material with the flower-shaped catalytic interface.
8. The method of manufacturing according to claim 7, wherein: in the step (2), when the filter material base material and the active stock solution are moved into a reaction kettle together for reaction, the reaction kettle is required to be fixed on a rotary bracket of a reactor; the reaction temperature in the reaction kettle is set to be 90-170 ℃, the reaction time is 20-30 hours, and the rotating speed of the rotating bracket is 240-400 rpm;
the equipment used for drying in the step (3) is a forced air drying oven, and the drying conditions are as follows: drying at 50-120deg.C for 40-110 min, and heating to 111-300deg.C for 60-350 min.
9. The method of manufacturing according to claim 7, wherein: the curing agent in the step (3) is one of polyurethane, chloroethylene or ammonium sulfate.
10. The application of the multifunctional filter material with flower-shaped catalytic interface for dust removal and denitration as defined in any one of claims 1 to 6 or the multifunctional filter material with flower-shaped catalytic interface prepared by the preparation method as defined in any one of claims 7 to 9 in the aspect of smoke adsorption in ceramic manufacturing industry.
CN202311067118.1A 2023-08-23 2023-08-23 Multifunctional dedusting and denitration filter material with flower-shaped catalytic interface, preparation method and application Pending CN116850700A (en)

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