CN218320801U - Device for synthesizing modified NaA type molecular sieve by coal gangue - Google Patents
Device for synthesizing modified NaA type molecular sieve by coal gangue Download PDFInfo
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- CN218320801U CN218320801U CN202222662700.XU CN202222662700U CN218320801U CN 218320801 U CN218320801 U CN 218320801U CN 202222662700 U CN202222662700 U CN 202222662700U CN 218320801 U CN218320801 U CN 218320801U
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Abstract
The utility model provides a device of modified NaA type molecular sieve is synthesized to gangue, including ultrasonic generator, naOH liquid storage pot I, naAlO 2 A liquid storage tank and a NaOH liquid storage tank II, wherein a synthesis reaction kettle, the NaOH liquid storage tank I and NaAlO are arranged in the ultrasonic generator 2 The liquid storage pot is connected with the centrifugal pump through the pipeline respectively, and the centrifugal pump passes through the pipeline to be connected with synthetic reation kettle, and NaOH liquid storage pot II passes through the pipeline to be connected with synthetic reation kettle, and synthetic reation kettle top is provided with feed inlet and pressure gauge, and the feed inlet is furnished with sealed lid. The utility model discloses can be according to the productThe method requires flexible setting of synthesis conditions and modification treatment conditions to obtain a molecular sieve product with optimal performance, and solves the problems of complex process, single product performance, small specific surface area and the like of the NaA molecular sieve prepared by the existing method.
Description
Technical Field
The utility model relates to a molecular sieve preparation technical field, concretely relates to device of synthetic modified NaA type molecular sieve of gangue.
Background
With the rapid development of industry, the environmental problem is increasingly prominent, the treatment of bulk solid wastes is urgent, although the comprehensive treatment of coal gangue has obtained remarkable effect in recent years, the utilization rate is not high, the utilization mode is simple, and the generated economic benefit is low. Therefore, it is urgently needed to develop a high value-added utilization mode of coal gangue.
The molecular sieve is a porous material, has a uniform pore structure, a high specific surface area, good thermal stability and excellent ion exchange capacity, and can be widely applied to the fields of adsorbents, ion exchangers and heterogeneous catalysis. NaA molecular sieve is the most commercially used, and representative, molecular sieve material. The traditional preparation method is to use chemical raw materials, such as water glass, alumina and the like, as raw materials for preparation, and has high cost and complex process. At present, a lot of low-cost raw materials such as kaolin, coal gangue, diatomite and the like are used for replacing chemical raw materials to produce molecular sieves. Therefore, the application value of industrial waste coal gangue is fully utilized to prepare a chemical product NaA molecular sieve, heavy metal ions and macromolecular substances in environmental sewage are adsorbed, the waste problem of the coal gangue is solved, the production cost of the molecular sieve is reduced, the effect of treating waste by waste is achieved, and the NaA molecular sieve prepared by taking the coal gangue as a raw material has a single sieve pore channel structure and strong selectivity, but has the defects of small specific surface area and weak adsorption capacity.
Disclosure of Invention
The utility model provides a device of modified NaA molecular sieve is synthesized to gangue, the device can solve prior art NaA molecular sieve surface area less, the technical problem that adsorption efficiency is weaker.
The technical scheme of the utility model as follows:
a device for synthesizing a modified NaA molecular sieve by coal gangue comprises an ultrasonic generator and a NaOH liquid storage tankI、NaAlO 2 A liquid storage tank and a NaOH liquid storage tank II, wherein a synthesis reaction kettle, the NaOH liquid storage tank I and NaAlO are arranged in the ultrasonic generator 2 The liquid storage pot passes through the pipeline respectively and is connected with the centrifugal pump, and the centrifugal pump passes through the pipeline to be connected with synthetic reation kettle, and NaOH liquid storage pot II passes through the pipeline to be connected with synthetic reation kettle, and synthetic reation kettle top is provided with feed inlet and pressure gauge, and the feed inlet is furnished with sealed lid.
The synthesis reaction kettle is arranged on a bracket inside the ultrasonic generating device.
The NaOH liquid storage tank I and the NaAlO 2 And a flow meter and a control valve are respectively arranged on a pipeline for connecting the liquid storage tank with the centrifugal pump. Through the control valve and the flowmeter, quantitative materials can be input into the reaction kettle by setting the control valve, so that SiO 2 And Al 2 O 3 Is 2:1.
And a flow meter and a control valve are arranged on a pipeline for connecting the NaOH liquid storage tank II with the synthesis reaction kettle.
And a vibrating screen machine is arranged above the feeding hole. The screen cloth of sieving machine can be changed in a flexible way, according to the actual conditions adjustment screen cloth aperture size, preferred 100-300 mesh screen cloth, further preferred 200 mesh screen cloth.
The control panel of the ultrasonic generating device is provided with a power switch, an ultrasonic switch, a heating switch, a display instrument and an indicator lamp, wherein the display instrument comprises a display and a temperature adjusting button.
The utility model has the advantages that:
1. the utility model discloses a continuous alkali treatment and ultrasonic treatment take off partial structure in the molecular sieve, make it can form from outside to inside and distribute macropore-mesopore-micropore's multistage pore structure in proper order, greatly increased specific surface area, strengthened the adsorption efficiency to metal ion and macromolecular substance, make its processing that can the wide application in sewage.
2. The utility model discloses can also set up the service condition of device in a flexible way, according to the requirement of product, nimble setting synthesis condition and the condition of modified processing obtain the best molecular sieve product of performance, have solved that current method preparation NaA molecular sieve technology is complicated, product performance singleness scheduling problem.
3. Ultrasonic wave generating device can use in a flexible way in this device, both can regard as heating device to use in the synthetic process, also can carry out alkali corrosion and ultrasonic treatment to synthetic NaA molecular sieve in the aftertreatment process, modifies NaA molecular sieve to effectively promote the modification effect.
Drawings
FIG. 1 is a schematic view of the present invention;
wherein: 1-ultrasonic generating device, 2-synthesis reaction kettle, 3-pressure gauge, 4-feeding inlet, 5-control valve III, 6-flowmeter III,7-NaOH liquid storage tank II, 8-control valve II, 9-flowmeter II,10-NaAlO 2 The system comprises a liquid storage tank, 11-control valves I, 12-flow meters I,13-NaOH liquid storage tanks I, 14-centrifugal pumps, 15-ultrasonic indicator lamps, 16-heating indicator lamps, 17-power indicator lamps, 18-power switches, 19-heating switches, 20-ultrasonic switches, 21-control panels and 22-supports.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the present application, and the described embodiments are only some embodiments, not all embodiments, of the present invention. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative work belong to the protection scope of the present invention.
Example 1
As shown in figure 1, the utility model provides an apparatus for synthesizing modified NaA molecular sieve by using coal gangue, which comprises a synthesis reaction kettle 2, an ultrasonic generating device 1, a NaOH liquid storage tank I13, a NaOH liquid storage tank II 7 and NaAlO 2 A liquid storage tank 10, a NaOH liquid storage tank I13 and NaAlO 2 The liquid storage tank 10 is respectively connected with a centrifugal pump 14 through a pipeline, the centrifugal pump 14 is connected with the synthesis reaction kettle 2 through a pipeline, the NaOH liquid storage tank II 7 is connected with the synthesis reaction kettle 2 through a pipeline, a control valve I11 and a flow meter I12 are arranged on the pipeline connecting the NaOH liquid storage tank I13 and the centrifugal pump 14, and NaAlO 2 A control valve is arranged on a pipeline for connecting the liquid storage tank 10 and the centrifugal pump 14A flow meter III 5 and a control valve III 6 are arranged on a pipeline connecting the II 8 and the flow meter II 9 as well as the NaOH liquid storage tank II 7 and the synthesis reaction kettle 2. The top of the synthesis reaction kettle 2 is provided with a pressure gauge 3 and a feed inlet 4 with a sealing cover, the feed inlet 4 is provided with a vibrating screen, and the synthesis reaction kettle 2 is arranged on a bracket 22 in the ultrasonic generator 1; the control panel 21 of the ultrasonic wave generating device 2 is provided with a power switch 18, an ultrasonic switch 20, a heating switch 19, a display instrument and an indicator light, wherein the display instrument comprises a display and a temperature adjusting button.
The ultrasonic wave generating device in the device can be flexibly used, not only can be used as a heating device in the synthesis process, but also can carry out alkali corrosion and ultrasonic treatment on the synthesized NaA molecular sieve in the post-treatment process to modify the NaA molecular sieve.
The method for synthesizing the modified NaA molecular sieve by using the coal gangue comprises the following steps:
pretreatment: the coal gangue of Shanxi Shuozhou is selected as raw material, has few impurities and has SiO as main component 2 And Al 2 O 3 The mass ratio is about 1.3, and the molar mass ratio is about 2.2. Crushing the coal gangue into small particles in a crusher, adding the small particles into a ball mill for grinding, transferring the ball-milled raw materials into a rotary drying furnace for drying, placing the rotary drying furnace into an incinerator, roasting at the high temperature of 600 ℃ for 2 hours, cooling, adding the cooled raw materials into a vibrating screen machine, and sieving by a 200-mesh sieve for later use.
Preparation of the molecular sieve: adding the pretreated coal gangue into a synthesis reaction kettle 2 from a feed inlet 4, and adding a NaOH liquid storage tank I13 and NaAlO 2 NaOH solution and NaAlO in the liquid storage tank 10 2 The solution is conveyed into a synthesis reaction kettle, and NaOH solution and NaAlO are adjusted 2 The concentration and amount of the solution are such that SiO 2 And Al 2 O 3 Is about 2:1, fully stirred and then stands for aging for 12 hours. After aging, the power switch 18 and the heating switch 19 of the ultrasonic generator 1 were turned on, and the reaction was carried out at 90 ℃ for 3 hours under high temperature and high pressure. And after the reaction is finished, taking out the reaction liquid, filtering the reaction liquid by using a plate and frame filter, and transferring the precipitate to a rotary drying furnace for drying to obtain molecular sieve powder (unmodified molecular sieve).
Modification of the molecular sieve: and transferring the molecular sieve powder into the synthesis reaction kettle again, conveying the NaOH solution in the NaOH liquid storage tank II 7 into the synthesis reaction kettle, wherein the mass ratio of the molecular sieve to the added NaOH is 3:1, the concentration of NaOH solution is 3mol/L, then a power switch 18 and a heating switch 19 of an ultrasonic wave generating device are turned on, the temperature is set to be 90 ℃, alkali treatment is carried out for 2 hours, then an ultrasonic switch 20 of the ultrasonic wave generating device is turned on, and ultrasonic treatment is carried out for 40 minutes. And after ultrasonic treatment, filtering the treatment liquid by using a plate and frame filter, and transferring the precipitate to a rotary drying furnace for drying to obtain modified molecular sieve powder.
Molecular sieve testing
Subjecting the above molecular sieves (unmodified and modified) to Cu 2+ And (3) performing adsorption test, namely preparing 0.5M copper salt solution, putting the molecular sieve into the solution, stirring for 6 hours to ensure that the molecular sieve fully absorbs copper ions in the solution, filtering out the molecular sieve in the solution, and measuring the content of the residual copper ions in the solution to obtain the amount of the copper ions adsorbed by the molecular sieve.
The modified molecular sieve has better adsorption performance on heavy metal pollutants such as Cu commonly seen in chemical plants 2+ The adsorption rate of (2) is improved from 55% (unmodified) to 85%.
From pair Cu 2+ The adsorption result shows that the adsorption effect of the modified molecular sieve is obviously improved, and the continuous alkali treatment and the ultrasonic modification treatment can enlarge the pore diameter and form a multi-stage pore channel structure, thereby improving the Cu content 2+ The adsorption performance of (3).
Compared with the unmodified molecular sieve, the modified molecular sieve has more mesopores, more complex pore structures and higher specific surface area. Continuous alkali treatment and ultrasonic modification treatment, wherein Al-OH and Si-OH bonds of the molecular sieve are partially broken, so that the aperture of the molecular sieve can be expanded from micropores to mesopores, and a multi-level pore channel structure (a structure with macropores, mesopores and micropores coexisting) is formed. In addition, the modification treatment also effectively enlarges the BET specific surface area (which is 2.5 times of that of the unmodified molecular sieve), and enhances the effect of the modification treatment on Cu 2+ The adsorption performance of (3).
The molecular sieve prepared by the device has better adsorption performance on heavy metals, can flexibly set synthesis conditions and modification treatment conditions according to the requirements of products to obtain the molecular sieve product with the best performance, and solves the problems of complex process, single product performance and the like of the NaA molecular sieve prepared by the existing method.
Claims (8)
1. A device for synthesizing a modified NaA type molecular sieve by coal gangue is characterized in that: comprises an ultrasonic generating device (1), a NaOH liquid storage tank I (13) and NaAlO 2 A liquid storage tank (10) and a NaOH liquid storage tank II (7), wherein a synthesis reaction kettle (2), a NaOH liquid storage tank I (13) and NaAlO are arranged in the ultrasonic generating device (1) 2 Liquid storage pot (10) are connected with centrifugal pump (14) through the pipeline respectively, and centrifugal pump (14) are connected with synthetic reation kettle (2) through the pipeline, and NaOH liquid storage pot II (7) are connected with synthetic reation kettle (2) through the pipeline, and synthetic reation kettle (2) top is provided with feed inlet (4) and pressure gauge (3), and feed inlet (4) are furnished with sealed lid.
2. The device for synthesizing the modified NaA-type molecular sieve by using the coal gangue as claimed in claim 1, wherein the device comprises: the synthesis reaction kettle (2) is arranged on a bracket (22) in the ultrasonic generator (1).
3. The device for synthesizing the modified NaA-type molecular sieve by using the coal gangue as claimed in claim 1, wherein the device comprises: the NaOH liquid storage tank I (13) and NaAlO 2 The pipeline connecting the liquid storage tank (10) and the centrifugal pump (14) is respectively provided with a flowmeter and a control valve.
4. The apparatus for synthesizing modified NaA-type molecular sieve from coal gangue according to claim 1, wherein: and a flow meter and a control valve are arranged on a pipeline connecting the NaOH liquid storage tank II (7) and the synthesis reaction kettle (2).
5. The device for synthesizing the modified NaA-type molecular sieve by using the coal gangue as claimed in claim 1, wherein the device comprises: and a vibrating screen machine is arranged above the feeding hole (4).
6. The apparatus for synthesizing a modified NaA-type molecular sieve from coal gangue according to claim 5, wherein: the screen mesh of the vibrating screen machine is a 100-300 mesh screen mesh.
7. The device for synthesizing the modified NaA-type molecular sieve by using the coal gangue as claimed in claim 1, wherein the device comprises: a control panel (21) of the ultrasonic wave generating device (1) is provided with a power switch (18), an ultrasonic switch (19), a heating switch (20), a display instrument and an indicator light.
8. The apparatus for synthesizing a modified NaA type molecular sieve from coal gangue according to claim 7, wherein: the display instrument includes a display and a temperature adjustment button.
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