CN110180261B - Preparation method of denitration filter material - Google Patents
Preparation method of denitration filter material Download PDFInfo
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- CN110180261B CN110180261B CN201910400248.XA CN201910400248A CN110180261B CN 110180261 B CN110180261 B CN 110180261B CN 201910400248 A CN201910400248 A CN 201910400248A CN 110180261 B CN110180261 B CN 110180261B
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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
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- 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
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- 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
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- 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
- B01D2239/0464—Impregnants
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- 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
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- 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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- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
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- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
A preparation method of a denitration filter material comprises the steps of firstly preparing low-temperature SCR catalyst powder by using a sol-gel method, then preparing modified polytetrafluoroethylene chopped fibers by using the powder as a modifier through a membrane cracking method, and finally blending the obtained modified polytetrafluoroethylene chopped fibers with unmodified chopped fibers to obtain the denitration filter material. The method disclosed by the invention not only improves the dispersibility of the active components of the denitration catalyst on the filter cloth and the bonding strength of the active components and the filter cloth, but also can simply regulate and control the denitration performance of the prepared filter material, and has smaller mutual influence on the denitration performance and the dedusting performance. The denitration filter bag products with good comprehensive performance can be obtained, and the denitration filter bag products have wide application prospect in the field of industrial boiler (kiln) flue gas denitration.
Description
Technical Field
The invention belongs to the technical field of flue gas purification of industrial boilers (kilns), and particularly relates to a preparation method of a denitration filter material.
Background
The purification of industrial boiler (kiln) flue gas is the key point of the treatment of atmospheric pollutants in recent years. Among them, denitration of flue gas is a difficult point of treatment technology. Because of low smoke temperature and complex smoke components, the denitration technology commonly used in the power industry is not suitable for industrial boiler (kiln) furnaces. The filter bag denitration is a novel flue gas denitration technology, and the flue gas denitration is realized at low temperature by using a filter bag with a catalytic function and a bag type dust removal process. The technology is widely applied to foreign industrial boiler (kiln) furnaces. The key point of the filter bag denitration lies in the development of the denitration filter bag. At present, the preparation methods of the denitration filter bag mainly comprise a coating method (CN108970269A, CN104607015A, CN108479218A, CN104524886A and CN108635983A) and a dipping method (CN108816220A, CN105435534A, CN105442305B and CN 105521659A). Although the denitration filter material can be prepared by the method, the denitration active component is poor in dispersity, the bonding strength of the catalyst and the filter bag fibers is weak, the denitration efficiency of the filter bag is low, the service life of the filter bag is short, and the engineering application of the filter bag is limited greatly. Therefore, it is necessary and important to develop a novel preparation technology of the denitration filter material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a denitration filter material.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of denitration filter material comprises the steps of uniformly mixing polytetrafluoroethylene powder, dioctyl phthalate and Ce-V/Ti catalyst powder, heating and prepressing the mixture to form columnar mold material, and rolling the columnar mold material to form a polytetrafluoroethylene base belt; guiding the polytetrafluoroethylene base band into a slitting mechanism for slitting, and combining the slit monofilaments into bundles; carrying out two-pass hot drawing on the combined monofilaments to obtain polytetrafluoroethylene long fibers, and cutting after heat setting to obtain low-temperature SCR catalyst modified polytetrafluoroethylene chopped fibers; and (3) blending the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fibers and the chopped fibers to obtain the denitration filter material.
A further improvement of the invention is that the Ce-V/Ti catalyst powder is prepared by the following process: the catalyst is prepared by a sol-gel method at room temperature by using tetrabutyl titanate, cerium nitrate, ammonium metavanadate and water as raw materials, absolute ethyl alcohol as a solvent and nitric acid as a hydrolysis inhibitor.
A further improvement of the invention is that the Ce-V/Ti catalyst powder is prepared by the following process: and (3) tetrabutyl titanate according to molar ratio: anhydrous ethanol: water: nitric acid: ammonium metavanadate: cerium nitrate 1:8:6: 1: (0.04-0.09): (0.1-0.2), mixing tetrabutyl titanate, absolute ethyl alcohol, water, nitric acid, ammonium metavanadate and cerium nitrate, reacting until the viscosity is not increased any more, drying and calcining to obtain the Ce-V/Ti catalyst powder.
A further improvement of the invention is that the calcination is carried out at a temperature of 400 ℃ for a period of 2 hours.
The further improvement of the invention is that the mass ratio of the polytetrafluoroethylene powder, the dioctyl phthalate and the Ce-V/Ti catalyst powder is 100: 20: (10-20).
The invention is further improved in that the heating temperature is 50-60 ℃ and the heating time is 24 hours.
The invention is further improved in that the columnar mold material is rolled into the polytetrafluoroethylene base belt at the linear speed of 0.5m/min at the temperature of 50-60 ℃.
The further improvement of the invention is that before the polytetrafluoroethylene tape is introduced into a slitting mechanism for slitting, the polytetrafluoroethylene tape is rinsed by ethanol and dried; slitting was carried out at a linear speed of 1 m/min.
The further improvement of the invention is that when the two-stage hot drawing is carried out, the first-stage drawing temperature is 195-205 ℃, and the second-stage drawing temperature is 245-255 ℃; the draw ratio of hot drawing is 1: 1000; heat setting is carried out at 360 ℃.
The invention is further improved in that the chopped fiber is polytetrafluoroethylene chopped fiber or polyimide chopped fiber.
The further improvement of the invention is that the specific blending process comprises the following steps: opening, mixing, carding, lapping, needling, calendering and singeing; in the denitration filter material, the mass percentage of the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fiber is 10-30%.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the preparation process of the filter material fiber, catalyst powder and polytetrafluoroethylene powder are mixed to prepare catalyst modified chopped fiber, and the catalyst modified chopped fiber is blended into the denitration filter material. The catalyst powder and the polytetrafluoroethylene powder can be uniformly mixed through a simple blending process, so that the Ce-V/Ti catalyst has high dispersibility in each chopped fiber and the whole filter material. The preparation process of the chopped fiber is subjected to processes of high-temperature melting-cooling solidification and the like, and the Ce-V/Ti catalyst is firmly (semi-) wrapped in the chopped fiber, so that the catalyst and the fiber have high bonding strength. The porosity of the denitration filter material depends on the blending process and is irrelevant to the addition of the catalyst, so that the load of the catalyst has little influence on the resistance of the filter material. The addition of the Ce-V/Ti catalyst has little influence on the preparation process of the chopped fibers, so that the denitration filter material can realize high catalyst loading. The invention can obtain the denitration filter material with excellent comprehensive performance.
(2) The denitration performance of the filter material prepared by the invention can be simply regulated and controlled through blending proportion, the mutual influence of the dust removal performance and the denitration performance is small, the filter material is beneficial to obtaining a denitration filter bag product with excellent comprehensive performance, and the filter material has wide application prospect in the field of flue gas denitration of industrial boiler (kiln).
Detailed Description
The present invention will be described in detail with reference to examples.
The preparation method of the denitration filter material comprises the following three steps:
(1) preparation of low temperature SCR catalyst powder
Tetrabutyl titanate (1mol), cerium nitrate (0.1-0.2 mol), ammonium metavanadate (0.04-0.09 mol) and water (6mol) are used as raw materials, absolute ethyl alcohol (8mol) is used as a solvent, nitric acid (1mol) is used as a hydrolysis inhibitor, and the reaction is carried out at room temperature until the viscosity of the system is not increased any more. And drying the obtained gel at about 100 ℃ for 24h, and then calcining the gel at 400 ℃ for 2 h to obtain the low-temperature SCR catalyst powder Ce-V/Ti.
(2) Preparation of catalyst modified polytetrafluoroethylene chopped fiber
Uniformly mixing 100g of polytetrafluoroethylene powder, 20g of dioctyl phthalate and 10-20 g of Ce-V/Ti catalyst powder, standing at 50-60 ℃ for 24 hours, prepressing at the normal temperature under the pressure of 0.6MPa to form a columnar mold material, and calendering the columnar mold material at the linear speed of 0.5m/min at 50-60 ℃ to prepare the polytetrafluoroethylene base belt. Rinsing the polytetrafluoroethylene base belt with ethanol to remove the lubricant, drying at 45 ℃, guiding the dried polytetrafluoroethylene base belt into a slitting mechanism to slit at a linear speed of 1m/min, and combining the slit monofilaments into a bundle. And (3) carrying out two-stage (the first stage stretching temperature is 200 ℃, the second stage stretching temperature is 250 ℃) hot drawing (the stretching ratio is 1:1000) on the combined monofilaments to obtain polytetrafluoroethylene long fibers, carrying out 360 ℃ hot setting, and then cutting by using a cutting machine to obtain the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fibers.
(3) Blending of catalyst modified polytetrafluoroethylene chopped fiber and other fibers
Blending the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fiber and other unmodified chopped fibers according to the following process: opening → mixing → carding → lapping → needling → calendaring → singeing → product, thus obtaining the denitration filter material. Wherein the unmodified chopped fiber is one of polytetrafluoroethylene chopped fiber (PTFE) and polyimide (P84) chopped fiber, the percentage of the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fiber is 10-30 (w/w)%, namely, in the denitration filter material, the mass fraction of the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fiber is 10-30%.
And (3) evaluating the low-temperature denitration performance of the obtained denitration filter material on an SCR denitration test bed by using simulated flue gas, wherein the denitration efficiency is measured by a flue gas analyzer.
Example 1
(1) Preparation of low temperature SCR catalyst powder
The method comprises the following steps of taking 1mol of tetrabutyl titanate, 0.15mol of cerium nitrate, 0.04mol of ammonium metavanadate and 6mol of water as raw materials, taking 8mol of absolute ethyl alcohol as a solvent, taking 1mol of nitric acid with the mass concentration of 65-68% as a hydrolysis inhibitor, and reacting at room temperature until the viscosity of a system is not increased any more. And drying the obtained gel at about 100 ℃ for 24h, and then calcining the gel at 400 ℃ for 2 h to obtain low-temperature SCR catalyst powder, namely Ce-V/Ti catalyst powder.
(2) Preparation of catalyst modified polytetrafluoroethylene chopped fiber
Uniformly mixing 100g of polytetrafluoroethylene powder, 20g of dioctyl phthalate serving as a lubricant and 15g of Ce-V/Ti catalyst powder, standing at 50-60 ℃ for 24 hours, prepressing at the normal temperature under the pressure of 0.6MPa to form a columnar mold material, and rolling the columnar mold material at the linear speed of 0.5m/min at 50-60 ℃ to prepare the polytetrafluoroethylene base belt. Rinsing the polytetrafluoroethylene base belt with ethanol to remove the lubricant, drying at 45 ℃, guiding the dried polytetrafluoroethylene base belt into a slitting mechanism to slit at a linear speed of 1m/min, and combining the slit monofilaments into a bundle. And (3) carrying out two-stage (the first stage stretching temperature is 200 ℃, the second stage stretching temperature is 250 ℃) hot drawing (the stretching ratio is 1:1000) on the combined monofilaments to obtain polytetrafluoroethylene long fibers, carrying out 360 ℃ hot setting, and then cutting by using a cutting machine to obtain the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fibers.
(3) Blending of catalyst modified polytetrafluoroethylene chopped fiber and other fibers
Blending the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fiber and other unmodified chopped fibers according to the following process: opening → mixing → carding → lapping → needling → calendaring → singeing → product, thus obtaining the denitration filter material. Wherein the unmodified chopped fiber is polytetrafluoroethylene chopped fiber (PTFE), and the proportion of the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fiber is 20 (w/w)%.
Examples 2-11 were otherwise identical to those of example 1 except for the details given in Table 1.
TABLE 1 results of examples 1-11
As can be seen from Table 1, the denitration efficiency of the denitration filter material prepared by the method is over 90 percent and can reach as high as 98 percent.
The method comprises the steps of firstly preparing low-temperature SCR catalyst powder by using a sol-gel method, then preparing modified polytetrafluoroethylene chopped fibers by using a membrane cracking method by using the powder as a modifier, and finally blending the obtained modified polytetrafluoroethylene chopped fibers with unmodified chopped fibers to obtain the denitration filter material.
The preparation process of the chopped fiber is subjected to processes of high-temperature melting-cooling solidification and the like, and the Ce-V/Ti catalyst is firmly (semi-) wrapped in the chopped fiber (surface), so that the catalyst and the fiber have high bonding strength. The porosity of the denitration filter material depends on the blending process and is irrelevant to the addition of the catalyst, so that the load of the catalyst has little influence on the resistance of the filter material. The addition of the Ce-V/Ti catalyst has little influence on the preparation process (mainly stretching) of the chopped fibers, so that the denitration filter material can realize high catalyst loading. In contrast, in the prior art, a coating method is to load a catalyst on the surface of a conventional filter material in a coating manner to form a denitration filter material, the catalyst can block part of filter material pores to increase the resistance of the filter material, the interfacial adhesion between the catalyst and the filter material is poor, the resistance is considered, and the loading amount of the catalyst is limited; the impregnation method generally uses suspension or emulsion of the catalyst as impregnation liquid to impregnate the conventional filter material to prepare the denitration filter material, and due to poor wettability of the fiber and poor uniformity of the suspension or emulsion, the catalyst has poor dispersibility in the filter material and weak bonding strength with the fiber. The invention can overcome the problems of the coating method and the dipping method in the prior art.
Compared with the common method, the method disclosed by the invention not only improves the dispersibility of the active component of the denitration catalyst on the filter cloth and the bonding strength of the active component and the filter cloth, but also can simply regulate and control the denitration performance of the prepared filter material, and the mutual influence of the denitration performance and the dust removal performance is small. The denitration filter bag products with good comprehensive performance can be obtained, and the denitration filter bag products have wide application prospect in the field of industrial boiler (kiln) flue gas denitration.
Claims (1)
1. A preparation method of a denitration filter material is characterized in that polytetrafluoroethylene powder, dioctyl phthalate and Ce-V/Ti catalyst powder are uniformly mixed, heated and pre-pressed into a columnar mold material, and then the columnar mold material is rolled to prepare a polytetrafluoroethylene base belt; guiding the polytetrafluoroethylene base band into a slitting mechanism for slitting, and combining the slit monofilaments into bundles; carrying out two-pass hot drawing on the combined monofilaments to obtain polytetrafluoroethylene long fibers, and cutting after heat setting to obtain low-temperature SCR catalyst modified polytetrafluoroethylene chopped fibers; blending the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fibers and the chopped fibers to obtain a denitration filter material;
the Ce-V/Ti catalyst powder was prepared by the following procedure: the preparation method comprises the following steps of (1) preparing the nano-composite material by a sol-gel method at room temperature by using tetrabutyl titanate, cerium nitrate, ammonium metavanadate and water as raw materials, absolute ethyl alcohol as a solvent and nitric acid as a hydrolysis inhibitor;
rolling the columnar mold material at 50-60 ℃ at a linear speed of 0.5m/min to prepare a polytetrafluoroethylene base belt;
when the two-stage hot drawing is carried out, the first-stage drawing temperature is 195-205 ℃, and the second-stage drawing temperature is 245-255 ℃; the draw ratio of hot drawing is 1: 1000; heat setting is carried out at 360 ℃;
the Ce-V/Ti catalyst powder was prepared by the following procedure: and (3) tetrabutyl titanate according to molar ratio: anhydrous ethanol: water: nitric acid: ammonium metavanadate: cerium nitrate 1:8:6: 1: (0.04-0.09): (0.1-0.2), mixing tetrabutyl titanate, absolute ethyl alcohol, water, nitric acid, ammonium metavanadate and cerium nitrate, reacting until the viscosity is not increased any more, drying and calcining to obtain Ce-V/Ti catalyst powder;
the mass ratio of the polytetrafluoroethylene powder, the dioctyl phthalate and the Ce-V/Ti catalyst powder is 100: 20: (10-20);
the heating temperature is 50-60 ℃, and the time is 24 hours;
before the polytetrafluoroethylene base band is introduced into a slitting mechanism for slitting, rinsing the polytetrafluoroethylene base band by adopting ethanol, and drying; slitting at a linear speed of 1 m/min;
the chopped fiber is polytetrafluoroethylene chopped fiber or polyimide chopped fiber;
the specific process of blending is as follows: opening, mixing, carding, lapping, needling, calendering and singeing; in the denitration filter material, the mass percentage of the low-temperature SCR catalyst modified polytetrafluoroethylene chopped fiber is 10-30%.
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| CN112044176B (en) * | 2020-09-29 | 2022-04-19 | 西安热工研究院有限公司 | NO catalytic oxidation filter bag for rapid SCR reaction and preparation method thereof |
| CN112044177B (en) * | 2020-09-29 | 2022-04-26 | 西安热工研究院有限公司 | Preparation method of denitration filter bag |
| CN113457731B (en) * | 2021-07-06 | 2022-08-19 | 中国科学院过程工程研究所 | Molecular sieve catalytic inorganic fiber, preparation method thereof and dust removal and denitration integrated application |
| CN114471104A (en) * | 2022-03-09 | 2022-05-13 | 清源创新实验室 | Flue gas full-working-condition dry desulfurization and catalytic filter bag dust removal-SCR denitration system and method |
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