CN111545164B - Filtering material for purifying volatile organic compounds and preparation method thereof - Google Patents

Filtering material for purifying volatile organic compounds and preparation method thereof Download PDF

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Publication number
CN111545164B
CN111545164B CN202010344985.5A CN202010344985A CN111545164B CN 111545164 B CN111545164 B CN 111545164B CN 202010344985 A CN202010344985 A CN 202010344985A CN 111545164 B CN111545164 B CN 111545164B
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temperature
filter material
resistant fabric
fiber
molecular sieve
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CN111545164A (en
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郭行
史东军
李马刚
孙传凯
赵雪源
徐纪清
骆坚平
潘涛
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Beijing Longtao Environment Technology Co ltd
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Beijing Longtao Environment Technology Co ltd
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    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B01J20/183—Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation
    • 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
    • B01D53/02—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 by adsorption, e.g. preparative gas chromatography
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0251—Compounds of Si, Ge, Sn, Pb
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/708—Volatile organic compounds V.O.C.'s
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

Abstract

The invention belongs to the field of environmental protection, and particularly relates to a filtering material for purifying volatile organic compounds and a preparation method thereof. The high-temperature-resistant fabric comprises a filling layer and high-temperature-resistant fabric layers arranged on two sides of the filling layer; the filling layer comprises a three-dimensional porous fiber net and micron particles distributed in holes of the fiber net; the material of the fiber web comprises glass fiber and/or ceramic fiber; the material of the micron particles comprises a hydrophobic molecular sieve, an inorganic binder and silicon carbide in a weight ratio of 5-7:1.5-2:1-2; the weight ratio of the fiber web to the microparticles is 5-10: 70-80. The filter material of the invention has the characteristics of high temperature resistance, high molecular sieve content, light weight and the like, has the appearance similar to paper, belongs to flexible materials, and is convenient to process into various shapes. Meanwhile, the structure is stable, the service life is long, and the device is convenient to apply in actual production.

Description

Filtering material for purifying volatile organic compounds and preparation method thereof
Technical Field
The invention belongs to the field of environmental protection, and particularly relates to a filtering material for purifying volatile organic compounds and a preparation method thereof.
Background
Volatile organic compounds (Volatile Organic Compounds, VOCs) are the general term for volatile organic compounds having a melting point below room temperature and a boiling point in the range of 50 to 260 ℃. VOCs are important gaseous pollutants in the atmosphere, and not only have direct influence on human health, ecological environment and the like, but also can generate secondary pollutants by participating in atmospheric photochemical reaction. Therefore, the method for controlling the emission of VOCs and effectively treating VOCs has very important significance for human health and environmental protection.
The active carbon in the existing adsorption filter material has high adsorption capacity, but is not high-temperature resistant, has poor hydrophobicity, and has fast performance decay rate and short service life after cyclic regeneration; the waste belongs to dangerous waste and needs special institutions to treat the dangerous waste; continuous and stable operation cannot be ensured.
In the existing molecular sieve rotating wheel technology, the relative content of the molecular sieve in unit treatment volume is low, so that the adsorption capacity of organic matters is small when organic waste gas is treated, and the problems of powder falling and the like exist when the existing molecular sieve rotating wheel technology is processed by adopting a coating process. Meanwhile, the molecular sieve has small specific heat capacity, poor heat conduction performance and relatively large energy consumption. The integral extrusion molecular sieve honeycomb or particle has the advantages of large energy and mass per unit volume, large specific heat, low heating and cooling rate and high energy consumption. The deodorizing or filtering adsorption material at normal temperature has poor high temperature resistance although some flame retardance is added, but volatile organic matters, particularly high boiling point matters, are desorbed after being adsorbed at industrial normal temperature, and therefore the service life of the adsorption material is difficult to ensure.
CN103068468A discloses a flame-retardant deodorizing filter material, which adopts one of an activated carbon plate, cellulose fiber, polyvinyl alcohol fiber, polyacrylonitrile fiber and phenol fiber, the content of which is more than 30%, and at the same time contains phosphorus flame retardant; is used for deodorizing and purifying harmful gases; the temperature is usually-20 to 80 ℃. In the technical scheme, in order to realize flame retardance, a fiber fabric containing carbonized fibers during combustion is adopted as a covering material, and 10-70% of phosphorus flame retardant is added; in order to achieve the adsorption effect, activated carbon particles with high specific surface area are adopted; in order to prevent the active carbon particles from falling off, an upper layer of fiber fabric and a lower layer of fiber fabric are used for covering, and the active carbon particles are fixed through a thermoplastic resin adhesive. However, it has the following problems: 1. chemical fibers are adopted, and cannot resist high temperature, so that the chemical fibers can be decomposed at the temperature of 250-300 ℃; 2. after the active carbon itself adsorbs organic matters, the active carbon has the possibility of burning because the active carbon contains impurities in the preparation process; 3. the adhesive contains thermoplastic resin, and has poor high temperature resistance; 4. the two layers of fabrics are covered and are simply connected up and down by the thermoplastic resin adhesive, the air quantity and the air speed during passing are not related, and the problem of infirm adhesion can exist during large air quantity application.
CN102389773a discloses a method for manufacturing molecular sieve honeycomb body for adsorbing volatile organic compounds, which adopts 5-15% of paper pulp, 5-20% of ceramic fiber, binder and zeolite molecular sieve as raw materials, and the corrugated molecular sieve paperboard is manufactured by papermaking technology. However, it has the following problems: 1. the zeolite molecular sieve is a NaY molecular sieve, a 4A molecular sieve, a 13X molecular sieve, a zsm-5 molecular sieve or a hydrophobic molecular sieve, under the condition of high humidity, the first few molecular sieves are used for preferentially adsorbing water, the waste gas generally has certain humidity, and the molecular sieve is converted into a polar molecular sieve after water molecules are inhaled, so that the adsorption effect of the molecular sieve cannot be ensured; whereas the definition of hydrophobic molecular sieves is more ambiguous. 2. The powder type molecular sieve is adopted, so that powder is easy to fall off; meanwhile, the inorganic binder is used, so that the molecular sieve powder is easily wrapped by the binder to form a binder film, and gas adsorption is prevented; 3. the properties of silica sol and alumina sol are different, the alumina sol has larger water absorption, and the natural kaolin and the attapulgite have unstable properties; 4. the method adopts a papermaking method, the molecular sieve has small particle size and low retention rate.
CN101850239a discloses a method for preparing an organic solvent adsorption material, which comprises making a common molecular sieve into paper, forming into honeycomb, and using SiCl 4 The gas or the water vapor carries out chemical treatment on the honeycomb body, and adopts an acidic mode to remove the generated solid product, so that the common molecular sieve is dealuminized and silicon-supplemented to improve the hydrophobicity. However, it has the following problems: 1. the molecular sieve content cannot be ensured, and the molecular sieve has the possibility of falling off, no matter SiCl 4 Gas or water vapor treatment, when the gas or water vapor reacts with the molecular sieve and affects the honeycomb structure, the content of the molecular sieve cannot be ensured, and the stable structure of the honeycomb body is maintained; 2. it adopts acid washing means, although solid products are removed, the acid can damage the crystallinity of the molecular sieve, thereby reducing the specific surface area and further affectingSound adsorption performance; 3. the external support strength of the corrugations of the honeycomb can be compromised to varying degrees as the honeycomb repeatedly contacts both high temperature water vapor and acidic liquids.
Disclosure of Invention
First, the technical problem to be solved
Aiming at the defects existing in the prior art, the invention aims to provide a filtering material for purifying volatile organic compounds and a preparation method thereof, which are not only suitable for normal-temperature waste gas adsorption purification, but also suitable for industrial organic waste gas purification devices, can effectively purify high-boiling-point volatile organic waste gas, and have the advantages of excellent molecular sieve microsphere retention capacity, stable overall performance and long service life after repeated alternation of high temperature and low temperature.
(II) technical scheme
It has been found through intensive studies that the above problems can be solved by the technical means shown below, and the present invention has been completed.
Specifically, the invention firstly provides a filtering material for purifying volatile organic compounds, which comprises a filling layer and high-temperature-resistant fabric layers attached to two sides of the filling layer;
the filling layer comprises a three-dimensional porous fiber net and micron particles distributed in holes of the fiber net;
the material of the fiber web comprises glass fiber and/or ceramic fiber;
the material of the micron particles comprises a hydrophobic molecular sieve, an inorganic binder and silicon carbide in a weight ratio of 5-7:1.5-2:1-2;
the weight ratio of the fiber web to the microparticles is 5-10: 70-80.
According to the invention, under the structure, the molecular sieve content in the filter material can be improved to a large extent by controlling the weight ratio of the fiber net to the micron particles and optimizing the composition of the micron particles, and the high efficiency of the function of the filter material and the stability of the structure are ensured.
Furthermore, the invention optimizes the selection and parameters of each material in the scheme, so that the effect of the filter material is further improved.
Preferably, the hydrophobic molecular sieve is one or more of ZSM-5, USY and Beta; the dynamic water absorption of ZSM-5 is 0.1-8wt%, the dynamic water absorption of USY is 3-10wt%, and the dynamic water absorption of Beta is 1-8wt%.
Preferably, the inorganic binder is one or two of diatomite and kaolin;
preferably, the silicon carbide is hydrophobic silicon carbide modified by Y-aminopropyl triethoxysilane.
Preferably, in the microparticles, the hydrophobic molecular sieve has a specific surface area of 300 to 1000m 2 And/g, wherein the average particle size of the hydrophobic molecular sieve is kept consistent with that of the silicon carbide and is 500-800 mu m; the average particle diameter of the inorganic binder is 10-100 mu m.
In the fiber web, the fiber diameter of the glass fiber and the fiber diameter of the ceramic fiber are 0.02-0.1 mm, and the length thereof is 0.1-5 mm.
When the parameters of each material are controlled in the above range, the bonding property of the mixed material is more favorable to be increased, so that the stability of the structure is ensured, and the service life is prolonged.
Preferably, the high-temperature-resistant fabric layer is made of glass fiber paper and/or ceramic fiber paper;
preferably, the ratio of the total weight of the high-temperature-resistant fabric layer to the weight of the filling layer is 10:90-25:75;
preferably, the thickness of the filter material is 0.2-0.8 mm, and the single-layer thickness of the high-temperature-resistant fabric layer is 10-25% of the total thickness of the filter material.
The invention further provides a preparation method of the filter material, which comprises the following steps:
(1) Mixing a PVA solution with the microparticles and the raw materials of the fiber web to prepare a suspension mixed solution;
(2) Spraying the suspension mixture onto a high-temperature-resistant fabric layer, and then paving a high-temperature-resistant fabric layer above the suspension mixture; pumping out liquid substances in the suspension mixture to obtain a semi-dry-based filter material;
(3) Drying and shaping the semi-dry base filtering material, and performing hot press shaping at 150-200 ℃ and 0.5-3.0 Mpa to obtain a shaped semi-finished product;
(4) And removing organic matters from the shaped semi-finished product through high-temperature roasting to obtain a finished product.
Through the steps, the filter material disclosed by the invention can be conveniently and efficiently obtained. Wherein, by controlling the temperature and pressure of the hot pressing, the thermoplastic binder plays an expected role, and the compactness of the upper, middle and lower 3 layers of the filter material is ensured; and bringing the molecular sieve, the inorganic binder and the silicon carbide into further intimate contact. Thereby improving the pull-up degree and strength of the filter material and facilitating the post-processing treatment.
In order to improve the uniformity of the suspension mixture, it is preferable that the concentration of the PVA solution in step (1) is 2 to 10wt%; the weight ratio of the PVA solution to the total weight of the microparticles and the web material is 100:15 to 30, more preferably 100:18 to 20.
When the weight ratio of the web material to the microparticle material is 1-5:10-25 (more preferably 3-5:15), the ratio of the materials in the final product will fall within the limits of the product specifications.
Preferably, the raw materials of the microparticles comprise hydrophobic molecular sieve raw materials, binder raw materials and silicon carbide raw materials in a weight ratio of 5-7:2-3:1-2 (more preferably 5-7:3:1); the raw materials of the adhesive are inorganic adhesive and organic adhesive with the weight ratio of 5:1-5 (more preferably 5:2-4); the inorganic binder is one or two of diatomite and kaolin, and the organic binder is thermoplastic resin. The organic binder is added according to the proportion in the preparation process, so that the adhesiveness of the raw materials in the preparation process is improved, and further the expected structure and performance of the product can be further ensured.
Preferably, the average particle diameter of the organic binder is 10 to 100 μm.
The selection of the hydrophobic molecular sieve, silicon carbide and the web material is in accordance with the limitations in the product technology program.
Preferably, the web material is subjected to static elimination and beating prior to mixing with the PVA solution. For example, static electricity can be eliminated by adding an antistatic agent.
Preferably, the material of the microparticles is subjected to a pre-mixing treatment prior to mixing with the PVA solution.
Preferably, the step (2) specifically comprises: spraying the suspension mixture onto a high-density wire mesh with a high-temperature-resistant fabric layer laid at the bottom, and then laying a high-temperature-resistant fabric layer above the suspension mixture; the lower part of the high-density porous metal net is provided with a vacuum device, the vacuum degree is controlled to be 10-300 Pa, and liquid substances in the suspension mixed liquid are pumped away to obtain a semi-dry-base filter material; more preferably, the vacuum degree is 280 to 300Pa.
The liquid material is pumped away in a vacuum mode, the vacuum degree is controlled to be 10-300 Pa, the solution can be ensured to rapidly permeate under the high-density porous metal net, and the upper and lower high-temperature-resistant fiber fabric layers are further ensured to be closely connected with the middle filler layer.
Preferably, in the step (3), when the hot press forming is performed at 170 to 190 ℃ and 0.8 to 1.2Mpa, the adsorption performance of the obtained material is better.
Preferably, in the step (3), the temperature of the drying and shaping is 100-150 ℃ and the time is 10-25 minutes; the preferred drying means is microwave drying.
Drying in the above manner can rapidly remove water from the semi-dry base filter material and ensure uniformity of the filter material.
Preferably, in the step (4), the high-temperature roasting is specifically: raising the temperature to 550-650 ℃ at a heating rate of 1-2.5 ℃/min, and maintaining the temperature at 550-650 ℃ for 4-8 hours.
Under the above high temperature firing scheme, not only the organic matters remaining in the filter material can be removed, but also the inorganic binder can be made to further function. Especially under the temperature rising rate and the constant temperature time, the stability of the product is more facilitated.
The person skilled in the art can adjust the uniformity and thickness of the product by controlling the speed of spraying, without further limitation.
The person skilled in the art will appreciate from the disclosure that a combination of the above-described preferred embodiments provides a preferred embodiment of the invention.
(III) beneficial effects
(1) The invention is made of high temperature resistant material, and the application temperature range is wide. The obtained filter material can be used at normal temperature or at 100-600 ℃ and has wide application range.
(2) The filter material of the invention has high molecular sieve content and large adsorption capacity. According to the adsorption theory, the organic matters and the water molecules are subjected to competitive adsorption on the surface of the molecular sieve, and the molecular sieve subjected to hydrophobic modification is adopted, so that the adsorption of the water molecular sieve is reduced, and the adsorption capacity of the organic matters is increased; further improving the purifying effect of volatile organic compounds and prolonging the resolving period of material regeneration.
(3) The filter material has the characteristic of light weight, and the volume specific gravity in unit volume is reduced by about 25 percent compared with that of the conventional honeycomb activated carbon, so that the heat absorption capacity is reduced during use, and the energy consumption is further reduced. Meanwhile, because the hydrophobic molecular sieve is adopted in the invention, the energy consumption of the latent heat of water adsorption is reduced during desorption; the energy consumption is reduced overall.
(4) The filter material of the invention has the appearance similar to paper, belongs to flexible materials, and is convenient to process into various shapes such as honeycomb, round barrel, plain paper and the like.
(5) According to the invention, the silicon carbide is added, so that the heat conducting performance is improved, the heat transfer performance is improved, the temperature rising and reducing rate is increased, and the desorption time and the heat energy consumption are reduced; and continuous operation is facilitated.
(6) The filter material of the invention adopts the interweaved fiber net and is attached with the adhesive, thus ensuring that the micron particles of the molecular sieve do not fall off powder and prolonging the service life of the material.
(7) The preparation method provided by the invention has strong operability, and can basically realize automatic operation, so that continuous production is realized in industrial application.
Drawings
FIG. 1 is a flow chart of the preparation method in example 1;
fig. 2 is a schematic sectional structure in embodiment 1; in the figure, A, a high temperature resistant fabric layer; B. a filling layer; 1. hydrophobic molecular sieve particles; 2. silicon carbide particles; 3. glass fibers; 4. binder particles;
FIG. 3 shows the results of the firing experiments at various temperatures in test example 3.
Detailed Description
The following examples are illustrative of the invention and are not intended to limit the scope of the invention.
For better contrast, in the following embodiment, the hydrophobic molecular sieve is ZSM-5, and the dynamic water absorption is 3wt%; the inorganic binder is diatomite; the organic binder is thermoplastic resin; the silicon carbide is hydrophobic silicon carbide modified by Y-aminopropyl triethoxysilane; the high temperature resistant fabric layer is made of glass fiber paper.
The specific surface area of the hydrophobic molecular sieve is 350m 2 And/g, wherein the average particle size of the hydrophobic molecular sieve is kept consistent with that of the silicon carbide, and is 600 mu m; the average particle diameter of the binder was 60. Mu.m.
In practical applications, the above materials may also be other options mentioned in the summary.
In addition, "parts" in the following examples are parts by weight.
The specific techniques or conditions are not identified in the examples and are described in the literature in this field or are carried out in accordance with the product specifications. The reagents or equipment used were conventional products available for purchase by regular vendors without the manufacturer's attention.
Example 1
The embodiment provides a filter material, which is prepared by the following method (the flow chart is shown in fig. 1):
step 1: and (5) pretreatment of raw materials. Weighing 5 parts of glass fiber with the diameter of 0.02mm and the length of 5mm according to parts by weight, adding into a container containing 100 parts of deionized water, dripping 3 parts of antistatic agent, mechanically stirring for 20 minutes, and transferring into a beating machine for slightly beating; after filtration through a 200 mesh screen, washing with deionized water 5 times and drying for use, designated as A. Respectively weighing a hydrophobic molecular sieve, a binder and silicon carbide according to the mass part ratio of 5:2:1, and mechanically mixing uniformly for standby, wherein the mass part ratio of the inorganic binder to the organic binder in the binder is 5:1; preparing PVA solution with the concentration of 2% according to the parts by weight for standby, and marking as C;
step 2: and (3) preparing a suspension mixture. Weighing 5 parts of A and 25 parts of B in the step 1 according to parts by weight, respectively adding into 100 parts of C, continuously stirring at a rotating speed of 300 revolutions per minute, and marking as D;
step 3: and (5) spray forming. And pumping the suspension mixture D by a pump of a slurry spraying machine, spraying the suspension mixture D onto a high-density wire mesh with a single-layer high-temperature-resistant fabric layer paved at the bottom at a constant speed, and controlling the thickness of the slurry above the high-temperature-resistant fabric layer through the slurry spraying speed, so that the slurry spraying speed is regulated according to actual production requirements. Meanwhile, automatically paving a high-temperature-resistant fabric layer above the suspension mixture D; with the uniform motion of the wire mesh, the lower part of the high-density porous metal mesh is provided with a vacuum device, and liquid substances in the suspension mixture are extracted to obtain a semi-dry-based filter material; this step can control the speed of filtration of the suspension mixture by controlling the vacuum; the single-layer thickness of the high-temperature resistant fabric layers of the upper layer and the lower layer is 0.02mm; the vacuum degree is controlled to 300Pa;
step 4: microwave drying: filtering the semi-dry base obtained in the step S3, continuously passing through a microwave drying area, and drying and shaping the filtering material to obtain a dry base filtering material; the control temperature of microwave drying is 150 ℃; drying by microwaves for 10 minutes;
step 5: hot-pressing and shaping, namely continuously passing the dry-base filter material obtained in the step 4 through the middle of a heated double-wheel roller, and hot-pressing the dry-base filter material to obtain the dry-base filter material; the temperature of the heated double-wheel roller is controlled at 180 ℃, and the strength of the extruded dry-base filter material is 1.0MPa during hot pressing.
Step 6; roasting: roasting the dry-base filter material processed in the step 5 at a high temperature to remove organic matters, wherein the roasting temperature is 550 ℃, the heating rate is controlled to be 2.5 ℃/min, the roasting maintaining time is 8 hours, and finally, a high-temperature-resistant light-weight filter material product is obtained, and the total thickness of the filter material is 0.30mm;
the schematic cross-sectional structure of the high-temperature-resistant fabric is shown in fig. 2, and the high-temperature-resistant fabric comprises a filling layer B and high-temperature-resistant fabric layers A attached to two sides of the filling layer B; the filling layer comprises a three-dimensional porous fiber net and micron particles distributed in the holes of the fiber net. The material of the fiber net is glass fiber 3, and the material of the micron particles comprises hydrophobic molecular sieve particles 1, binder particles 4 and silicon carbide particles 2.
Example 2
The embodiment provides a filter material, which is prepared by the following method:
step 1: and (5) pretreatment of raw materials. According to the parts by weight, 1 part of ceramic fiber with the diameter of 0.1mm and the length of 0.1mm is weighed, added into a container containing 100 parts of deionized water, 3 parts of antistatic agent is dripped, and the ceramic fiber is transferred into a beating machine after being mechanically stirred for 20 minutes for slight beating; after filtration through a 200 mesh screen, washing with deionized water 5 times and drying for use, designated as A. Respectively weighing a hydrophobic molecular sieve, a binder and silicon carbide according to the mass part ratio of 5:2:1, and mechanically mixing uniformly for standby, wherein the mass part ratio of the inorganic binder to the organic binder in the binder is 5:1; preparing PVA solution with the concentration of 2% according to the parts by weight for standby, and marking as C;
step 2: and (3) preparing a suspension mixture. Weighing 1 part of A and 10 parts of B in the step 1 according to parts by weight, respectively adding into 100 parts of C, continuously stirring at a rotating speed of 300 revolutions per minute, and marking as D;
step 3: and (5) spray forming. And pumping the suspension mixture D by a pump of a slurry spraying machine, spraying the suspension mixture D onto a high-density wire mesh with a single-layer high-temperature-resistant fabric layer paved at the bottom at a constant speed, and controlling the thickness of the slurry above the high-temperature-resistant fabric layer through the slurry spraying speed, so that the slurry spraying speed is regulated according to actual production requirements. Meanwhile, automatically paving a high-temperature-resistant fabric layer above the suspension mixture D; with the uniform motion of the wire mesh, the lower part of the high-density porous metal mesh is provided with a vacuum device, and liquid substances in the suspension mixture are extracted to obtain a semi-dry-based filter material; this step can control the speed of filtration of the suspension mixture by controlling the vacuum; the single-layer thickness of the high-temperature resistant fabric layers of the upper layer and the lower layer is 0.2mm; the vacuum degree is controlled to be between 10 Pa;
steps 4 to 6 are the same as steps 4 to 6 in embodiment 1; finally obtaining the filter material product, wherein the total thickness of the filter material is 0.40mm.
Example 3
The embodiment provides a filter material, which is prepared by the following method:
step 1: and (5) pretreatment of raw materials. Weighing 5 parts of ceramic fibers with the diameter of 0.05mm and the length of 0.5mm according to parts by weight, adding into a container containing 100 parts of deionized water, dropwise adding 10 parts of antistatic agent, mechanically stirring for 20 minutes, and transferring into a beating machine for slightly beating; after filtration through a 200 mesh screen, washing with deionized water 5 times and drying for use, designated as A. Respectively weighing a hydrophobic molecular sieve, a binder and silicon carbide according to the mass part ratio of 7:3:2, and mechanically mixing uniformly for standby, wherein the mass part ratio of an inorganic binder to an organic binder in the binder is 5:5; preparing PVA solution with the concentration of 10% according to the parts by weight for standby, and marking as C;
step 2: and (3) preparing a suspension mixture. Weighing 5 parts of A and 25 parts of B in the step 1 according to parts by weight, respectively adding into 100 parts of C, continuously stirring at a rotating speed of 300 revolutions per minute, and marking as D;
step 3: and (5) spray forming. And pumping the suspension mixture D by a pump of a slurry spraying machine, spraying the suspension mixture D onto a high-density wire mesh with a single-layer high-temperature-resistant fabric layer paved at the bottom at a constant speed, and controlling the thickness of the slurry above the high-temperature-resistant fabric layer through the slurry spraying speed, so that the slurry spraying speed is regulated according to actual production requirements. Meanwhile, automatically paving a high-temperature-resistant fabric layer above the suspension mixture D; with the uniform motion of the wire mesh, the lower part of the high-density porous metal mesh is provided with a vacuum device, and liquid substances in the suspension mixture are extracted to obtain a semi-dry-based filter material; this step can control the speed of filtration of the suspension mixture by controlling the vacuum; the single-layer thickness of the high-temperature resistant fabric layers of the upper layer and the lower layer is 0.02mm; the vacuum degree is controlled to be 300Pa;
steps 4 to 6 are the same as steps 4 to 6 in embodiment 1; finally obtaining the filter material product, wherein the total thickness of the filter material is 0.35mm.
Example 4
The embodiment provides a filter material, which is prepared by the following method:
step 1: and (5) pretreatment of raw materials. Weighing 5 parts of glass fiber with the diameter of 0.05mm and the length of 0.5-mm according to parts by weight, adding into a container containing 100 parts of deionized water, dripping 10 parts of antistatic agent, mechanically stirring for 20 minutes, and transferring into a beating machine for slightly beating; after filtration through a 200 mesh screen, washing with deionized water 5 times and drying for use, designated as A. Respectively weighing a hydrophobic molecular sieve, a binder and silicon carbide according to the mass part ratio of 6:3:1, and mechanically mixing uniformly for standby, wherein the mass part ratio of an inorganic binder to an organic binder in the binder is 5:3; preparing PVA solution with the concentration of 10% according to the parts by weight for standby, and marking as C;
step 2: and (3) preparing a suspension mixture. Weighing 4 parts of A and 15 parts of B in the step 1 according to parts by weight, respectively adding the parts by weight into 100 parts of C, continuously stirring at a rotating speed of 300 revolutions per minute, and marking as D;
step 3: and (5) spray forming. And pumping the suspension mixture D by a pump of a slurry spraying machine, spraying the suspension mixture D onto a high-density wire mesh with a single-layer high-temperature-resistant fabric layer paved at the bottom at a constant speed, and controlling the thickness of the slurry above the high-temperature-resistant fabric layer through the slurry spraying speed, so that the slurry spraying speed is regulated according to actual production requirements. Meanwhile, automatically paving a high-temperature-resistant fabric layer above the suspension mixture D; with the uniform motion of the wire mesh, the lower part of the high-density porous metal mesh is provided with a vacuum device, and liquid substances in the suspension mixture are extracted to obtain a semi-dry-based filter material; this step can control the speed of filtration of the suspension mixture by controlling the vacuum; the single-layer thickness of the high-temperature resistant fabric layers of the upper layer and the lower layer is 0.1mm; the vacuum degree is controlled to 300Pa;
steps 4 to 6 are the same as steps 4 to 6 in embodiment 1; finally obtaining the filter material product, wherein the total thickness of the filter material is 0.35mm.
Example 5
The embodiment provides a filter material, which is prepared by the following method:
a preparation method of a high-temperature-resistant light-weight filtering material for purifying volatile organic compounds comprises the following steps:
step 1: and (5) pretreatment of raw materials. Weighing 5 parts of glass fiber with the diameter of 0.05mm and the length of 0.5mm according to parts by weight, adding into a container containing 100 parts of deionized water, dripping 3 parts of antistatic agent, mechanically stirring for 20 minutes, and transferring into a beating machine for slightly beating; after filtration through a 200 mesh screen, washing with deionized water 5 times and drying for use, designated as A. Respectively weighing a hydrophobic molecular sieve, a binder and silicon carbide according to the mass part ratio of 5:2:2, and mechanically mixing uniformly for standby, wherein the mass part ratio of the inorganic binder to the organic binder in the binder is 5:1; preparing PVA solution with the concentration of 10% according to the parts by weight for standby, and marking as C;
step 2: and (3) preparing a suspension mixture. Weighing 5 parts of A and 10 parts of B in the step 1 according to parts by weight, respectively adding into 100 parts of C, continuously stirring at a rotating speed of 300 revolutions per minute, and marking as D;
step 3: and (5) spray forming. And pumping the suspension mixture D by a pump of a slurry spraying machine, spraying the suspension mixture D onto a high-density wire mesh with a single-layer high-temperature-resistant fabric layer paved at the bottom at a constant speed, and controlling the thickness of the slurry above the high-temperature-resistant fabric layer through the slurry spraying speed, so that the slurry spraying speed is regulated according to actual production requirements. Meanwhile, automatically paving a high-temperature-resistant fabric layer above the suspension mixture D; with the uniform motion of the wire mesh, the lower part of the high-density porous metal mesh is provided with a vacuum device, and liquid substances in the suspension mixture are extracted to obtain a semi-dry-based filter material; this step can control the speed of filtration of the suspension mixture by controlling the vacuum; the single-layer thickness of the high-temperature resistant fabric layers of the upper layer and the lower layer is 0.1mm; the vacuum degree is controlled to be 300Pa;
steps 4 to 6 are the same as steps 4 to 6 in embodiment 1; finally obtaining the filter material product, wherein the total thickness of the filter material is 0.32mm.
Example 6
The embodiment provides a filter material, which is prepared by the following method:
a preparation method of a high-temperature-resistant light-weight filtering material for purifying volatile organic compounds comprises the following steps:
steps 1 to 4 are the same as steps 1 to 4 in example 4;
step 5: hot-pressing and shaping, namely continuously passing the dry-base filter material obtained in the step 4 through the middle of a heated double-wheel roller, and hot-pressing the dry-base filter material to obtain the dry-base filter material; the temperature of the heated two-wheel roller is controlled at 150 ℃, and the strength of the extruded dry-base filter material is 0.5MPa during hot pressing.
Step 6 is the same as step 6 in example 4.
Example 7
The embodiment provides a filter material, which is prepared by the following method:
a preparation method of a high-temperature-resistant light-weight filtering material for purifying volatile organic compounds comprises the following steps:
steps 1 to 4 are the same as steps 1 to 4 in example 4;
step 5: hot-pressing and shaping, namely continuously passing the dry-base filter material obtained in the step 4 through the middle of a heated double-wheel roller, and hot-pressing the dry-base filter material to obtain the dry-base filter material; the temperature of the heated two-wheel roller is controlled at 150 ℃, and the strength of the extruded dry-base filter material is 3.0MPa during hot pressing.
Step 6 is the same as step 6 in example 4.
Example 8
The embodiment provides a filter material, which is prepared by the following method:
a preparation method of a high-temperature-resistant light-weight filtering material for purifying volatile organic compounds comprises the following steps:
steps 1 to 4 are the same as steps 1 to 4 in example 4;
step 5: hot-pressing and shaping, namely continuously passing the dry-base filter material obtained in the step 4 through the middle of a heated double-wheel roller, and hot-pressing the dry-base filter material to obtain the dry-base filter material; the temperature of the heated two-wheel roller is controlled at 150 ℃, and the strength of the extruded dry-base filter material is 2.0MPa during hot pressing.
Step 6 is the same as step 6 in example 4.
Comparative example 1
The difference between this comparative example and example 4 is that: the proportion of the hydrophobic molecular sieve to the binder in the step 1 is 6:3, silicon carbide is not added, and the rest steps are the same.
Comparative example 2
The difference between this comparative example and example 4 is that: the proportion of the hydrophobic molecular sieve to the silicon carbide in the step 1 is 6:1, no binder is added, and the rest steps are the same.
Comparative example 3
The difference between this comparative example and example 4 is that: when the suspension mixture is prepared in the step 2, only 15 parts of B are weighed according to parts by weight, added into 100 parts of C, and continuously stirred at a rotating speed of 300 revolutions per minute, and marked as D, and the rest steps are the same.
Comparative example 4
The difference between this comparative example and example 4 is that: in the step 3, the pump of the slurry spraying machine is used for pumping the suspension mixture D, the suspension mixture D is sprayed onto a high-density wire mesh with a single-layer high-temperature-resistant fabric layer paved at the bottom at a constant speed, the thickness of the slurry above the high-temperature-resistant fabric layer can be controlled through the speed of slurry spraying, and the slurry spraying speed is regulated according to actual production requirements. Meanwhile, automatically paving a high-temperature-resistant fabric layer above the suspension mixture D; with the uniform motion of the wire mesh, the lower part of the high-density porous metal mesh is provided with a vacuum device, and liquid substances in the suspension mixture are extracted to obtain a semi-dry-based filter material; the vacuum device is turned off and the vacuum degree is not controlled. The remaining steps are the same.
Comparative example 5
The difference between this comparative example and example 4 is that: in the step 5, continuously passing the dry-base filter material obtained in the step 4 through the middle of a heated double-roller shaft, and hot-pressing the dry-base filter material to obtain the dry-base filter material; the temperature of the heated double-wheel roller is controlled at 200 ℃, and the strength of the extruded dry-base filter material is 5.0MPa during hot pressing.
Comparative example 6
The difference between this comparative example and example 4 is that: in the step 5, continuously passing the dry-base filter material obtained in the step 4 through the middle of a heated double-roller shaft, and hot-pressing the dry-base filter material to obtain the dry-base filter material; the temperature of the heated double-roller is controlled at 150 ℃, the strength of the extruded dry-based filter material is 0.01MPa during hot pressing, and the rest steps are the same.
Comparative example 7
The difference between this comparative example and example 4 is that: in step 1, the molecular sieve is a normal ZSM-5.
Comparative example 8
The difference between this comparative example and example 4 is that: the weight ratio of the hydrophobic molecular sieve to the binder to the silicon carbide is 8:1:1;
test example 1
The appearance of the filter materials obtained in examples 1 to 8 and comparative examples 1 to 6 was compared with each other, and the results were shown in Table 1 below.
TABLE 1
Figure BDA0002469744360000151
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Figure BDA0002469744360000161
From the results, it was found that a filter material having a satisfactory appearance was obtained within the scope of the present invention. In contrast, in comparative example 2, the binder was not added, and the molecular sieve and the silicon carbide microparticles were exfoliated, so the binder was a substance that must be added in the present invention. In the comparative example 3, glass fiber or ceramic fiber is not added in the middle filling layer, a net structure is not formed effectively, and the micro-nano particles in the middle layer are partially separated, so that the method is very critical in the step, has innovation, and prolongs the service life of the product. Comparative example 4 since the vacuum pump was not turned on, the liquid and solid portions in the suspension mixture D were not efficiently separated, resulting in failure of the filter material to be molded. In comparative example 5, the dry filter material was damaged due to the excessive extrusion pressure of the twin-roll roller, and the production process was destroyed. In comparative example 6, however, the high temperature fabric layer and the intermediate filling layer were not well contacted due to the excessively small extrusion pressure of the twin-roll rolls, the particles were loose from one another, and the hot melt adhesive was not effective, resulting in separation of the upper, middle and lower 3 layers of the filter material.
Test example 2
The filter materials prepared in example 3, example 4, example 6, comparative example 1 and comparative example 7 were randomly selected for performance testing. The specific test process is as follows:
the samples were individually sheared, 10cm in diameter and 10cm in height, and individually tested in a quartz reactor in an adsorption apparatus. The adsorption, desorption and temperature resistance of the filter material prepared by the invention are tested by taking dimethylbenzene and water as test adsorbates, preparing mixed gas of dimethylbenzene with certain concentration and humidity through bubbling and air dilution at certain temperature. Wherein the adsorption space-time tower speed is 1.2m/s, and the concentration of toluene at the inlet of the quartz reactor is 400mg/m 3 Humidity of 80%, constant temperature of 35 ℃, volume airspeed of 7000h -1 Testing under conditions. The detection means adopts a gas chromatograph to analyze and determine the concentration of toluene in the tail gas. In the adsorption process, the breakthrough point is set at which the outlet gas concentration reaches 5% of the inlet concentration, and the time from the start of adsorption to the breakthrough point is taken as breakthrough time when 100% is reached. The breakthrough adsorption capacity is the mass percent of paraxylene adsorbed per gram of filter material. The desorption experiment is carried out at 150 ℃, hot air is utilized to be introduced into a quartz reactor for kneading, and the volume space velocity during desorption is 5000h -1 And simultaneously monitoring the heating condition of the central part of the filter material within 20 minutes, and calculating the heating rate within the time. The dynamic water absorption test method refers to national standard GB ≡T 8770-2014. The results are averaged after 3 groups of parallel tests for each sample and the test results are shown in table 2.
TABLE 2
Figure BDA0002469744360000171
From the results, it was found that the product properties obtained by examples 3, 4 and 6 remained substantially uniform, and that the filter material of example 4 had a higher breakthrough adsorption capacity than examples 3 and 6. The difference between comparative example 1 and example 4 is that silicon carbide is not added in comparative example 1, so that under the same condition, the temperature rising rate is lower than that of example 4, which indicates that the addition of silicon carbide improves the heat conducting property of the product and can realize the function of rapid temperature rising. Comparative example 7 uses a conventional molecular sieve, which has a significantly higher dynamic water absorption than that of example, but has a temperature rise rate as low as that of examples 3, 4, 6 and comparative example 1 because it adsorbs a large amount of water.
Test example 3
In this test example, the filter material obtained in example 4 was baked at 320℃at 350℃at 380℃at 500℃and at 600℃at the same time, and the results are shown in FIG. 3. From the results, it was found that the filter material of the present invention remained intact at 600 ℃.
While the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.

Claims (24)

1. The preparation method of the filter material is characterized in that the filter material comprises a filling layer and high-temperature-resistant fabric layers attached to two sides of the filling layer;
the filling layer comprises a three-dimensional porous fiber net and micron particles distributed in holes of the fiber net;
the material of the fiber web comprises glass fiber and/or ceramic fiber;
the material of the micron particles comprises a hydrophobic molecular sieve, an inorganic binder and silicon carbide in a weight ratio of 5-7:1.5-2:1-2;
the weight ratio of the fiber web to the microparticles is 5-10: 70-80 parts;
the preparation method comprises the following steps:
(1) Mixing a PVA solution with the microparticles and the raw materials of the fiber web to prepare a suspension mixed solution;
(2) Spraying the suspension mixture onto a high-temperature-resistant fabric layer, and then paving a high-temperature-resistant fabric layer above the suspension mixture; pumping out liquid substances in the suspension mixture to obtain a semi-dry-based filter material;
(3) Drying and shaping the semi-dry base filtering material, and performing hot press shaping at 150-200 ℃ and 0.5-3.0 Mpa to obtain a shaped semi-finished product;
(4) And removing organic matters from the shaped semi-finished product through high-temperature roasting to obtain a finished product.
2. The method of claim 1, wherein the hydrophobic molecular sieve is one or more of ZSM-5, USY, beta; the dynamic water absorption of the ZSM-5 is 0.1-8wt%, the dynamic water absorption of the USY is 3-10wt% and the dynamic water absorption of the Beta is 1-8wt%;
and/or the inorganic binder is one or two of diatomite and kaolin;
and/or the silicon carbide is hydrophobic silicon carbide modified by Y-aminopropyl triethoxysilane.
3. The preparation method according to claim 1 or 2, wherein in the microparticles, the specific surface area of the hydrophobic molecular sieve is 300 to 1000m 2 And/g, wherein the average particle size of the hydrophobic molecular sieve is kept consistent with that of the silicon carbide and is 500-800 mu m; the average particle diameter of the inorganic binder is 10-100 mu m.
4. The production method according to claim 1 or 2, wherein in the fiber web, the fiber diameter of the glass fiber and the ceramic fiber is 0.02 to 0.1mm and the length is 0.1 to 5mm.
5. A method of producing according to claim 3, wherein in the fiber web, the glass fibers and the ceramic fibers have a fiber diameter of 0.02 to 0.1mm and a length of 0.1 to 5mm.
6. The method of claim 1, 2 or 5, wherein the material of the high temperature resistant fabric layer is glass fiber paper and/or ceramic fiber paper.
7. A method of making according to claim 3 wherein the material of the high temperature resistant fabric layer is fiberglass paper and/or ceramic fiber paper.
8. The method according to claim 4, wherein the material of the high temperature resistant fabric layer is glass fiber paper and/or ceramic fiber paper.
9. The method of claim 6, wherein the ratio of the total weight of the high temperature resistant fabric layer to the weight of the filler layer is 10:90 to 25:75.
10. The method of claim 7 or 8, wherein the ratio of the total weight of the high temperature resistant fabric layer to the weight of the filler layer is 10:90 to 25:75.
11. The method according to claim 6, wherein the thickness of the filter material is 0.2 to 0.8mm, and the single layer thickness of the high temperature resistant fabric layer is 10 to 25% of the total thickness of the filter material.
12. The method of claim 7 or 8, wherein the thickness of the filter material is 0.2 to 0.8mm, and the single layer thickness of the high temperature resistant fabric layer is 10 to 25% of the total thickness of the filter material.
13. The method according to claim 1, wherein in the step (1), the raw materials of the microparticles comprise a hydrophobic molecular sieve raw material, a binder raw material and a silicon carbide raw material in a weight ratio of 5 to 7:2 to 3:1 to 2; the raw materials of the adhesive are inorganic adhesive and organic adhesive in a weight ratio of 5:1-5; the inorganic binder is one or two of diatomite and kaolin, and the organic binder is thermoplastic resin.
14. The method of claim 13, wherein the weight ratio of web material to microparticle material is 1-5:10-25.
15. The method of claim 13, wherein the PVA solution has a concentration of 2wt% to 10wt%; the weight ratio of the PVA solution to the total weight of the microparticles and the web material is 100:15-30.
16. The preparation method according to any one of claims 1, 13 to 15, wherein step (2) specifically comprises: spraying the suspension mixture onto a high-density wire mesh with a high-temperature-resistant fabric layer laid at the bottom, and then laying a high-temperature-resistant fabric layer above the suspension mixture; the lower part of the high-density porous metal net is provided with a vacuum device, the vacuum degree is controlled to be 10-300 Pa, and liquid substances in the suspension mixed liquid are pumped away to obtain the semi-dry-base filter material.
17. The method according to any one of claims 1 and 13 to 15, wherein in the step (3), the drying and setting temperature is 100 to 150 ℃ and the time is 10 to 25 minutes.
18. The method according to claim 16, wherein in the step (3), the drying and setting temperature is 100 to 150 ℃ and the time is 10 to 25 minutes.
19. The method of claim 17, wherein the drying is microwave drying.
20. The method of claim 18, wherein the drying is microwave drying.
21. The method according to any one of claims 1, 13 to 15, 18 to 20, wherein in step (4), the high-temperature baking is specifically: raising the temperature to 550-650 ℃ at a heating rate of 1-2.5 ℃/min, and maintaining the temperature at 550-650 ℃ for 4-8 hours.
22. The method according to claim 16, wherein in the step (4), the high-temperature baking is specifically: raising the temperature to 550-650 ℃ at a heating rate of 1-2.5 ℃/min, and maintaining the temperature at 550-650 ℃ for 4-8 hours.
23. The method according to claim 17, wherein in the step (4), the high-temperature baking is specifically: raising the temperature to 550-650 ℃ at a heating rate of 1-2.5 ℃/min, and maintaining the temperature at 550-650 ℃ for 4-8 hours.
24. A filter material for purifying volatile organic compounds, characterized in that it is produced by the production method according to any one of claims 1 to 23.
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