CN112642394A - Preparation method of honeycomb zeolite molecular sieve adsorbent - Google Patents
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- CN112642394A CN112642394A CN201910959009.8A CN201910959009A CN112642394A CN 112642394 A CN112642394 A CN 112642394A CN 201910959009 A CN201910959009 A CN 201910959009A CN 112642394 A CN112642394 A CN 112642394A
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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
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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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
- B01D53/02—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
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
- B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
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- 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
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Abstract
The invention relates to the technical field of organic waste gas treatment, in particular to a preparation method of a honeycomb zeolite molecular sieve adsorbent, which comprises the following formula raw materials in percentage by weight of 25-35% of a stone molecular sieve, 5-15% of aluminum hydroxide, 30-40% of molecular sieve raw powder, 5-15% of silicon dioxide, 10-20% of a pore-forming agent, a plasticizer and a binder, and the preparation method comprises the following steps: batching → stirring and kneading → vacuum mixing → aging → extrusion molding → drying → cutting → sintering → quality inspection → qualified product. The honeycomb zeolite molecular sieve adsorbent prepared by the zeolite molecular sieve has the advantages of strong adsorption selectivity: the molecular sieve is uniform in pore size and is an ionic adsorbent; strong adsorption capacity: even if the composition concentration of the gas is very low, the gas still has adsorption capacity; the novel synthesis method has the advantages of simple process, environmental protection and low price, and is used for preparing the honeycomb zeolite molecular sieve adsorbent which has higher adsorption capacity, high-temperature desorption, pertinence, selectivity and stable operation.
Description
Technical Field
The invention relates to the technical field of organic waste gas treatment, in particular to a preparation method of a honeycomb zeolite molecular sieve adsorbent.
Background
Atmospheric pollution is one of the most outstanding environmental problems in China at present, and industrial waste gas is an important source of atmospheric pollutants. A large amount of industrial waste gas is discharged into the atmosphere, so that the quality of the atmospheric environment is inevitably reduced, serious harm is brought to the human health, and huge loss is caused to national economy. Therefore, the treatment and purification of the organic waste gas are imperative.
The existing waste gas treatment technology mainly comprises the following steps: adsorption recovery technology, adsorption concentration technology, catalytic combustion technology and high-temperature incineration technology. The current application technology for organic waste gas with large air quantity and low concentration is adsorption concentration and catalytic combustion. The drawbacks of this process are as follows:
1. the safety of the active carbon material as an adsorbent is very poor, and when the temperature of the regeneration hot gas flow reaches above 100 ℃, the heat accumulation in the adsorption bed is easy to ignite;
2. the hot air flow is adopted to purge and regenerate the activated carbon, the regeneration temperature usually can not exceed 120 ℃, when the desorption period is finished, partial high-boiling-point compounds can not be desorbed completely, and can be accumulated in an activated carbon bed layer to cause the reduction of the adsorption performance, so the method is not suitable for the purification of the high-boiling-point organic compounds;
3. usually, the activated carbon has strong water absorption capacity, and when the humidity of the waste gas is higher, the purification capacity of the organic compounds is rapidly reduced;
4. the replaced activated carbon is classified as hazardous waste, causing secondary pollution.
Disclosure of Invention
The present invention is directed to a method for preparing a honeycomb zeolite molecular sieve adsorbent, which solves one or more of the problems set forth in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a honeycomb zeolite molecular sieve adsorbent comprises the following formula raw materials: the zeolite molecular sieve, aluminum hydroxide, molecular sieve raw powder, silicon dioxide, pore-forming agent and binder, the proportion of the raw materials of each formula is 25-35% of the zeolite molecular sieve, 5-15% of the aluminum hydroxide, 30-40% of the molecular sieve raw powder, 5-15% of the silicon dioxide and 10-20% of the pore-forming agent and the binder, and the preparation method comprises the following steps: batching → stirring and kneading → vacuum mixing → aging → extrusion molding → drying → cutting → sintering → quality inspection → qualified product.
Preferably, the raw materials of the formula comprise 30% of zeolite molecular sieve, 10% of aluminum hydroxide, 35% of molecular sieve raw powder, 10% of silicon dioxide and 15% of pore-forming agent and binder.
Preferably, cellulose is used as the binder, and graphene is used as the pore-forming agent.
Preferably, glycerin is used as the plasticizer.
Preferably, the formulation of the zeolite molecular sieve specifically comprises the following steps:
s1: selecting zeolite based on SiO2And Al2O3The molecular ratio of (A) is different, and molecular sieves with different apertures are obtained;
s2: grinding the selected zeolite into zeolite powder with the particle size of 300-;
s3: adding the powder material after iron removal into NaOH solid particles according to the ratio of 2:1, fully mixing, adding sodium metaaluminate into the mixture to adjust the silicon-aluminum molar ratio and SiO2:AI2O3=2.2-3.0, putting the solid mixture into a ball mill for ball milling for 60-70 minutes;
s4: adding 180% of deionized water into the ball mill according to the weight of the materials, continuously grinding uniformly, heating to 90 ℃ for crystal bloom, stopping the ball mill after about 4 hours to obtain a crystal shield, removing the crystal shield from the ball mill, performing suction filtration and washing until the pH is less than 9, and drying in an environment with the temperature of 80 ℃ to obtain the zeolite molecular sieve.
Preferably, the stirring and kneading is to stir and knead the self-made zeolite molecular sieve and other raw materials, and then to perform vacuum kneading and aging.
Preferably, the vacuum kneading and the aging are carried out simultaneously, and the frequency of the vacuum kneading and the aging is 2 to 3 times per day, and the interval between every two times is 3 to 5 hours.
Preferably, the drying mode adopts spontaneous combustion drying, steam drying, far infrared drying or microwave drying.
Preferably, the drying method is microwave drying.
Compared with the prior art, the invention has the beneficial effects that:
1. the cellular zeolite molecular sieve adsorbent is prepared by the preparation method, and the mechanism of the zeolite molecular sieve for adsorbing VOCs organic matters is that the molecular sieve is modified to have a certain pore diameter to adsorb gas molecules, and Fe can be added3+、Fe2+、Mg2+、Mn2+、Sr2+The preparation method of the honeycomb zeolite molecular sieve adsorbent has the advantages of simple process, environmental protection and low price, so as to prepare the honeycomb zeolite molecular sieve adsorbent which has higher adsorption capacity, high-temperature desorption, pertinence, selectivity and stable operation.
2. The preparation method of the honeycomb zeolite molecular sieve adsorbent has the advantages that the honeycomb zeolite molecular sieve adsorbent is prepared by the zeolite molecular sieve, and has strong adsorption selectivity: the molecular sieve is uniform in pore size and is an ionic adsorbent; strong adsorption capacity: even if the composition concentration of the gas is very low, the gas still has adsorption capacity; the molecular sieve still has larger adsorption capacity at higher temperature, and other adsorbents are greatly influenced by the temperature, so that the adsorption capacity of the molecular sieve is large under the same temperature condition; the regeneration can be carried out at high temperature, the regeneration efficiency is high, and the safety is high; the polarity of the lewis centers on the surface is strong; the central cage or channel is very small, so that the gravitational field is very strong, therefore, the adsorption capacity of the central cage or channel on adsorbate molecules is far superior to that of other types of adsorbents, and the adsorption capacity is very considerable even if the concentration of the adsorbate is very low; the molecular sieve adsorbent is the only available high-temperature adsorbent, and has good thermal stability; selecting different zeolite molecular sieves according to the diameter of adsorbate
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a honeycomb zeolite molecular sieve adsorbent comprises the following formula raw materials: the zeolite molecular sieve, aluminum hydroxide, molecular sieve raw powder, silicon dioxide, pore-forming agent, plasticizer and binder, wherein the raw materials of the formula comprise 25-35% of the zeolite molecular sieve, 5-15% of the aluminum hydroxide, 30-40% of the molecular sieve raw powder, 5-15% of the silicon dioxide, and 10-20% of the pore-forming agent, the plasticizer and the binder, and the preparation method comprises the following steps: batching → stirring and kneading → vacuum mixing → aging → extrusion molding → drying → cutting → sintering → quality inspection → qualified product.
In the preferred embodiment, the formulation comprises 30% of zeolite molecular sieve, 10% of aluminum hydroxide, 35% of molecular sieve raw powder, 10% of silica, and 15% of pore-forming agent, plasticizer and binder.
Furthermore, the adhesive is cellulose, the pore-forming agent is graphene, and the plasticizer is glycerin, so that the plasticity and the fluidity of the pug are improved.
Specifically, the formulation of the zeolite molecular sieve specifically comprises the following steps:
s1: selecting zeolite based on SiO2And Al2O3The molecular ratio of (A) is different, and molecular sieves with different apertures are obtained;
s2: grinding the selected zeolite into zeolite powder with the particle size of 300-;
s3: adding the powder material after iron removal into NaOH solid particles according to the ratio of 2:1, fully mixing, adding sodium metaaluminate into the mixture to adjust the silicon-aluminum molar ratio and SiO2:AI2O3=2.2-3.0, putting the solid mixture into a ball mill for ball milling for 60-70 minutes;
s4: adding 180% of deionized water into the ball mill according to the weight of the materials, continuously grinding uniformly, heating to 90 ℃ for crystal bloom, stopping the ball mill after about 4 hours to obtain a crystal substance shield, removing the crystal substance shield from the ball mill, performing suction filtration and washing until the pH value is less than 9, and drying in an environment with the temperature of 80 ℃ to obtain the zeolite molecular sieve.
It is worth to be noted that the stirring kneading is to stir and knead the self-made zeolite molecular sieve and other raw materials, and then to perform vacuum kneading and aging.
In addition, the vacuum mulling and the aging are carried out synchronously, the frequency of the vacuum mulling and the aging is 2-3 times per day, and the interval of each time is 3-5 hours, so that the density and the plasticity of the pug are improved, the tissue of the pug is uniform, the forming performance is improved, the drying strength and the mechanical strength after forming are improved, and the aging can promote the uniform distribution of water in the pug.
It should be noted that the drying mode is spontaneous combustion drying, steam drying, far infrared drying or microwave drying, as the preferred mode of this embodiment, the drying mode is microwave drying, drying after pug that will be kneaded, stirred and aged is formed, drying is the key link in the production process, make it dewater and shape rapidly, then send to the cutting workshop to cut and shape, send to the kiln and sinter.
The principle of the invention is as follows: the raw materials are mixed and diffused among the whole amorphous silicon oxide at the initial stage of the synthesis reaction, then the temperature of the system is raised, silicon hydroxyl groups are continuously condensed in the process of material diffusion to generate water through condensation polymerization, the amorphous silicon oxide is gradually converted to crystals, the crystallization process is continuously carried out, and the continuous condensation of the silicon hydroxyl groups finally enables the solid raw materials to be converted into molecular sieve crystals in a solid phase state.
The reaction process of solid phase synthesis is a diffusion rearrangement process between materials, the reaction occurs between homomorphic reactants, the dissolution like that in liquid phase gel does not exist, and the rearrangement regrowth process, because the water content in a solid phase system is extremely low, only water molecules with the properties of the reactants can be provided, and the water molecules play a role of a reaction initiator. It can be seen that the rearrangement between the materials at the initial stage of the reaction has a great influence on the reaction process, and the difference between the liquid phase mechanism and the W phase diffusion mechanism is most obvious at this time. In the case of the solid-phase thermal synthesis method, a part of micropores are formed already in the amorphous stage in the early stage of the reaction, and the crystals are not grown yet. The pore size is larger than the standard pore size (5.2-5.5A) of the molecular sieve crystal because the molecular sieve is in a loose amorphous state. With the further growth, the amorphous silicon skeleton further grows and condenses to gradually grow into a crystal structure with standard pore diameter. Compared with the traditional hydrothermal method for synthesizing the molecular sieve, the solid-phase synthesis method has the following obvious characteristics: high molecular sieve product yield, greatly increased single kettle utilization rate of the reaction kettle, obviously reduced pollutants and simplified synthesis steps.
The honeycomb zeolite molecular sieve adsorbent is an adsorbent for treating waste gas, which is prepared by modifying, proportioning and extruding a zeolite molecular sieve, has the advantages of thermodynamic property, low resistance and consumption, high adsorption rate and the like, has excellent adsorption performance in the treatment of organic waste gas with large air volume and low concentration, is in a porous honeycomb structure, and has the advantages of developed pore structure, large specific surface area, small fluid resistance and the like.
The industrial principle is as follows: the waste gas containing organic matters passes through the molecular sieve adsorption layer under the action of the fan, harmful substances are adsorbed in the molecular sieve, and clean gas is discharged; after a period of time, when the molecular sieve adsorbent is saturated, the catalytic combustion device is started after the molecular sieve adsorbent is switched by each valve, the catalytic combustion device continuously sends hot air into the molecular sieve adsorption bed, when the hot air source reaches the boiling point of the organic matters, the organic matters are volatilized from the molecular sieve, and enter the catalytic chamber through the pipeline to be catalytically decomposed into water and carbon dioxide, and simultaneously, energy is released. Then the released energy is utilized to enter the adsorption bed for desorption. The molecular sieve is recycled, organic matters are decomposed, and no secondary pollution is generated.
The preparation method of the honeycomb zeolite molecular sieve adsorbent has the advantages that the honeycomb zeolite molecular sieve adsorbent is prepared by the zeolite molecular sieve: the adsorption selectivity is strong: the molecular sieve is uniform in pore size and is an ionic adsorbent; strong adsorption capacity: even if the composition concentration of the gas is very low, the gas still has adsorption capacity; the molecular sieve still has larger adsorption capacity at higher temperature, and other adsorbents are greatly influenced by the temperature, so that the adsorption capacity of the molecular sieve is large under the same temperature condition; the regeneration can be carried out at high temperature, the regeneration efficiency is high, and the safety is high; the polarity of the lewis centers on the surface is strong; the central cage or channel is very small, so that the gravitational field is very strong, therefore, the adsorption capacity of the central cage or channel on adsorbate molecules is far superior to that of other types of adsorbents, and the adsorption capacity is very considerable even if the concentration of the adsorbate is very low; the molecular sieve adsorbent is the only available high-temperature adsorbent, and has good thermal stability; different zeolite molecular sieves are selected according to the diameter of the adsorbate.
The foregoing shows and describes the general principles, essential 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 the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A preparation method of a honeycomb zeolite molecular sieve adsorbent is characterized by comprising the following steps: comprises the following formula raw materials: the zeolite molecular sieve, aluminum hydroxide, molecular sieve raw powder, silicon dioxide, pore-forming agent, plasticizer and binder, wherein the raw materials of the formula comprise 25-35% of the zeolite molecular sieve, 5-15% of the aluminum hydroxide, 30-40% of the molecular sieve raw powder, 5-15% of the silicon dioxide, and 10-20% of the pore-forming agent, the plasticizer and the binder, and the preparation method comprises the following steps: batching → stirring and kneading → vacuum mixing → aging → extrusion molding → drying → cutting → sintering → quality inspection → qualified product.
2. The method for preparing a honeycomb zeolite molecular sieve adsorbent according to claim 1, characterized in that: the raw materials of each formula account for 30 percent of zeolite molecular sieve, 10 percent of aluminum hydroxide, 35 percent of molecular sieve raw powder, 10 percent of silicon dioxide, and 15 percent of pore-forming agent, plasticizer and binder.
3. The method for preparing a honeycomb zeolite molecular sieve adsorbent according to claim 2, characterized in that: the binder is cellulose, and the pore-forming agent is graphene.
4. The method for preparing a honeycomb zeolite molecular sieve adsorbent according to claim 2, characterized in that: the plasticizer is glycerol.
5. The method for preparing a honeycomb zeolite molecular sieve adsorbent according to claim 1, characterized in that: the preparation method of the zeolite molecular sieve specifically comprises the following steps:
s1: selecting zeolite based on SiO2And Al2O3The molecular ratio of (A) is different, and molecular sieves with different apertures are obtained;
s2: grinding the selected zeolite into zeolite powder with the particle size of 300-;
s3: adding the powder material after iron removal into NaOH solid particles according to the ratio of 2:1, fully mixing, adding sodium metaaluminate into the mixture to adjust the silicon-aluminum molar ratio and SiO2：AI2O3=2.2-3.0, putting the solid mixture into a ball mill for ball milling for 60-70 minutes;
s4: adding 180% of deionized water into the ball mill according to the weight of the materials, continuously grinding uniformly, heating to 90 ℃ for crystal bloom, stopping the ball mill after about 4 hours to obtain a crystal shield, removing the crystal shield from the ball mill, performing suction filtration and washing until the pH is less than 9, and drying in an environment with the temperature of 80 ℃ to obtain the zeolite molecular sieve.
6. The method for preparing a honeycomb zeolite molecular sieve adsorbent according to claim 1, characterized in that: the stirring kneading is to stir and knead the self-made zeolite molecular sieve and other raw materials, and then to carry out vacuum mulling and staling.
7. The method for preparing a honeycomb zeolite molecular sieve adsorbent according to claim 1, characterized in that: the vacuum mixing and aging are carried out synchronously, the frequency of the vacuum mixing and aging is 2-3 times per day, and the interval of each time is 3-5 hours.
8. The method for preparing a honeycomb zeolite molecular sieve adsorbent according to claim 1, characterized in that: the drying mode adopts spontaneous combustion drying, steam drying, far infrared drying or microwave drying.
9. The method for preparing a honeycomb zeolite molecular sieve adsorbent according to claim 8, wherein: the drying mode is microwave drying.
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Cited By (5)
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| CN113171748A (en) * | 2021-05-25 | 2021-07-27 | 山东亮剑环保新材料有限公司 | High surface area honeycomb zeolite and production method thereof |
| CN113426406A (en) * | 2021-07-09 | 2021-09-24 | 山东亮剑环保新材料有限公司 | High-strength low-density honeycomb zeolite and production method thereof |
| CN113426407A (en) * | 2021-07-09 | 2021-09-24 | 山东亮剑环保新材料有限公司 | Zero-drying-period honeycomb zeolite and preparation method thereof |
| CN113731106A (en) * | 2021-09-28 | 2021-12-03 | 江西萍乡龙发实业股份有限公司 | Method and device for treating organic waste gas by using renewable honeycomb adsorbent |
| CN117181185A (en) * | 2023-09-07 | 2023-12-08 | 硅宝石(武汉)高新装备股份有限公司 | Preparation method of NMP honeycomb zeolite adsorption material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113171748A (en) * | 2021-05-25 | 2021-07-27 | 山东亮剑环保新材料有限公司 | High surface area honeycomb zeolite and production method thereof |
| CN113426406A (en) * | 2021-07-09 | 2021-09-24 | 山东亮剑环保新材料有限公司 | High-strength low-density honeycomb zeolite and production method thereof |
| CN113426407A (en) * | 2021-07-09 | 2021-09-24 | 山东亮剑环保新材料有限公司 | Zero-drying-period honeycomb zeolite and preparation method thereof |
| CN113731106A (en) * | 2021-09-28 | 2021-12-03 | 江西萍乡龙发实业股份有限公司 | Method and device for treating organic waste gas by using renewable honeycomb adsorbent |
| CN117181185A (en) * | 2023-09-07 | 2023-12-08 | 硅宝石(武汉)高新装备股份有限公司 | Preparation method of NMP honeycomb zeolite adsorption material |
| CN117181185B (en) * | 2023-09-07 | 2024-02-20 | 硅宝石(武汉)高新装备股份有限公司 | Preparation method of NMP honeycomb zeolite adsorption material |
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Application publication date: 20210413 |