CN114933312A - Method for synthesizing Na-P type zeolite molecular sieve from waste clay brick powder and application thereof - Google Patents
Method for synthesizing Na-P type zeolite molecular sieve from waste clay brick powder and application thereof Download PDFInfo
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- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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Abstract
The invention relates to the field of building solid waste resource utilization, in particular to a method for synthesizing a Na-P type zeolite molecular sieve by using waste clay brick powder and an application thereof, which comprises the following steps: s1: ball-milling and sieving the waste clay bricks to obtain waste clay brick powder; s2: pretreating waste clay brick powder; s3: mixing and grinding the pretreated waste clay brick powder with NaOH and NaF to obtain a mixed product; s4: calcining the mixed product to obtain an activated product; s5: dissolving the activated product in deionized water and carrying out ultrasonic treatment to obtain a mixed solution; s6: carrying out hydrothermal reaction on the mixed solution to obtain a reactant; s7: and (3) carrying out solid-liquid separation on the reactants, and cleaning and drying the solid obtained by separation to obtain the Na-P type zeolite molecular sieve. Compared with the prior art, the invention can obviously improve the added value of the waste clay brick, thereby promoting the recycling of the clay brick and reducing the environmental pollution caused by building solid waste.
Description
Technical Field
The invention relates to the field of building solid waste resource utilization, in particular to a method for synthesizing a Na-P type zeolite molecular sieve from waste clay brick powder and application thereof.
Background
With the accelerated urbanization process, China will generate a large amount of solid waste of buildings every year. The waste clay brick is one of the main components of the solid waste of the building. Currently, the main disposal of waste clay bricks is in landfills or as low-end building materials, including recycled aggregates, mineral admixtures, fillers, etc. The added value of the waste clay brick is low, the disposal cost of the waste clay brick is higher than the market value of the waste clay brick, and the recycling rate of the waste clay brick is low. The large accumulation of building waste solids can create serious environmental problems. Therefore, an approach for upgrading the utilization of the waste clay bricks and preparing waste clay brick derivative products with high added values is urgently needed.
Zeolite molecular sieve is a kind of microporous aluminosilicate with three-dimensional network structure, and its skeleton is made of SiO 4 Tetrahedron and AlO 4 Tetrahedrons are connected by oxygen atoms and have been widely used in the fields of petrochemical industry, water purification, catalysis, etc. The demand of China for zeolite molecular sieves is large, and natural zeolite can not meet the current demand. The synthesis of zeolite requires the use of soluble silicates and aluminates of high purity as raw materials, which is costly. Researches show that most solid wastes contain rich silicon-aluminum elements, so that the cheap solid wastes are used as raw materials for synthesizing the zeolite, and the method has important significance for reducing the zeolite cost, reducing the environmental pollution of the solid wastes and improving the additional value of the solid wastes.
Currently, various industrial solid wastes have been successfully used for synthesizing zeolite molecular sieves. However, the applicant consults a large amount of domestic patents and literature data through a system, and does not find a relevant report of synthesizing the zeolite molecular sieve by using the construction solid wastes (especially the waste clay brick powder) as raw materials. Based on that the waste clay brick contains a large amount of SiO 2 And Al 2 O 3 The zeolite molecular sieve can be used as a synthetic raw material of the zeolite molecular sieve, and the clay brick contains a certain glass phase substance, so that the zeolite molecular sieve has high activity, favorable conditions are provided for dissolving out silicon-aluminum elements, the problem of short supply of zeolite raw materials can be relieved by a large amount of waste clay bricks, and the resource utilization and high value-added utilization of the waste clay bricks can be realized by synthesizing the zeolite.
The waste clay brick is a large amount of building solid waste, and the resource utilization of the waste clay brick is greatly limited due to low additional value at present, so that serious environmental load is brought. However, the waste clay brick contains abundant silicon and aluminum elements and is a potential raw material for synthesizing zeolite. The traditional thermal activation can cause higher energy consumption, and because the raw materials often contain quartz and other inert substances, the raw materials need to be activated at high temperature, so that the dissolution rate of the silicon-aluminum element in the alkali solution is increased, the activation temperature usually reaches 600-.
Disclosure of Invention
The invention aims to solve at least one of the problems, and provides a method for synthesizing a Na-P type zeolite molecular sieve by using waste clay brick powder and an application thereof.
The purpose of the invention is realized by the following technical scheme:
the first aspect of the invention discloses a method for synthesizing a Na-P type zeolite molecular sieve by using waste clay brick powder, which comprises the following steps:
s1: ball-milling and sieving the waste clay bricks to obtain waste clay brick powder;
s2: pretreating the waste clay brick powder obtained in the step S1;
s3: mixing and grinding the pretreated waste clay brick powder obtained in the step S2 with NaOH and NaF to obtain a mixed product;
s4: calcining the mixed product obtained in the step S3 to obtain an activated product;
s5: dissolving the activated product obtained in the step S4 in deionized water and carrying out ultrasonic treatment to obtain a mixed solution;
s6: carrying out hydrothermal reaction on the mixed solution obtained in the step S5 to obtain a reactant;
s7: and (4) carrying out solid-liquid separation on the reactant obtained in the step (S6), and washing and drying the solid obtained by separation to obtain the Na-P type zeolite molecular sieve.
Preferably, SiO of the waste clay brick described in step S1 2 And Al 2 O 3 The mass content of the silicon-aluminum alloy is not less than 80 percent, and the Si/Al molar ratio is 2-4. The waste clay bricks have rough and porous surfaces and high water absorption, and the waste clay bricks from different sources have large differences in physical and chemical properties, so that the waste clay bricks can be utilized in a large scale on the premise of ensuring stable product performance, and certain challenges exist. On the other hand, however, the waste clay bricks have a rich content of silicon and aluminum, SiO thereof 2 And Al 2 O 3 The sum of the contents of the components exceeds 80 percent, the Si/Al molar ratio is 2-4, the zeolite molecular sieve is very suitable for synthesizing the zeolite molecular sieve theoretically, and the waste clay brick contains a part of high-activity glass phase substances after being fired at high temperature, which is beneficial to providing rich silicon-aluminum sources under alkaline conditions.
Preferably, the mesh size of the screen used in the screening described in step S1 is not greater than 100 mesh.
In step S1, batch ball milling is performed on the waste clay bricks from different sources to obtain powder, so as to realize homogenization treatment of the waste clay brick powder.
Preferably, the pretreatment in step S2 includes acid washing, filtering and drying, the acid solution used in the acid washing process is hydrochloric acid with a mass concentration of 2%, the temperature of the acid washing is 90 ℃, and the time is 2 h.
In step S2, acid liquor pretreatment purification is carried out to reduce C a2+ And Fe 3+ And the like.
Preferably, the mass ratio of the NaOH to the waste clay brick powder in the step S3 is 1-1.4, and the mass of the NaF is 1% of the waste clay brick powder.
The NaOH-NaF composite mineralizer is added in the step S3, so that the activation temperature of the waste clay brick powder is greatly reduced, and a large amount of Na is provided + A source, promoting the formation of Na-P type zeolite.
Preferably, the calcination temperature in step S4 is 350-550 ℃ and the calcination time is 2 h.
Preferably, the solid-to-liquid ratio of the activated product to the deionized water in step S5 is 1g/10L, and the time of the ultrasonic treatment is 30 min. The silicon-aluminum element dissolution is accelerated through ultrasonic treatment, and the higher yield of the zeolite can be realized without adding a silicon-aluminum source.
Preferably, the hydrothermal reaction in step S6 is carried out at 80-120 deg.C for no less than 12 h.
Preferably, the solid-liquid separation described in step S7 is centrifugation.
The invention also discloses an application of the method for synthesizing the Na-P type zeolite molecular sieve by using the waste clay brick powder in the field of sewage treatment.
The Na-P type zeolite molecular sieve has excellent adsorption performance and ion exchange capacity, and is widely applied in the field of sewage treatment.
Compared with the prior art, the invention has the following beneficial effects:
1. the Na-P type zeolite molecular sieve is synthesized by using the building solid wastes, so that the cost of the zeolite is reduced, the resources are saved, the added value of the waste clay brick is improved, the environmental pollution caused by building solid waste accumulation is reduced, and the Na-P type zeolite molecular sieve has important economic benefits and social environmental benefits.
2. The NaOH-NaF composite mineralizer is used, so that the activation temperature of the waste clay brick can be obviously reduced, and the quartz can generate lattice distortion in a lower temperature range (350-.
3. High concentration of Na + The introduction of the Na-P type zeolite can promote the crystallization of the Na-P type zeolite and improve the crystallinity of the Na-P type zeolite.
4. The ultrasonic treatment can accelerate the dissolution of silicon-aluminum elements, improve the concentration of silicon-aluminum ions in the solution, and improve the yield of the zeolite molecular sieve without adding a silicon-aluminum source.
5. And (3) batch ball-milling the waste clay bricks from different sources into powder to realize homogenization treatment of the waste clay brick powder. Then carrying out acid liquor pretreatment and purification to reduce Ca 2+ And Fe 3+ The content of impurities is equal, NaOH-NaF composite mineralizer is added, the activation temperature of waste clay brick powder is greatly reduced, and simultaneously, a large amount of Na is provided + And (3) promoting the formation of Na-P type zeolite, and finally synthesizing the Na-P type zeolite molecular sieve with higher purity by adopting low-temperature hydrothermal treatment. The technical route not only can overcome the influence of the property difference of different waste clay bricks on the product performance, but also can solve the problem that the property difference of different waste clay bricks has influence on the product performanceSynthesizing Na-P type zeolite with low energy consumption, and simultaneously using the Na-P type zeolite for adsorbing and removing organic matters in water.
Drawings
FIG. 1 is a microscopic morphology diagram of waste clay brick powder;
FIG. 2 is an X-ray diffraction diagram of waste clay brick powder, activated waste clay brick powder and Na-P type zeolite molecular sieve;
FIG. 3 is a microscopic morphology of a Na-P type zeolite molecular sieve;
FIG. 4 is a process flow chart of synthesizing Na-P type zeolite molecular sieve from waste clay brick powder.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
The components and mass contents of the waste clay bricks used in the following examples are shown in Table 1, and the overall preparation process flow is shown in FIG. 4. Other reagents may be commercially available products which can be obtained conventionally by those skilled in the art, unless otherwise specified.
Table 1 mass fraction of waste clay brick (%)
| Na 2 O | MgO | Al 2 O 3 | SiO 2 | P 2 O 5 | K 2 O | CaO | TiO 2 | Fe 2 O 3 | Other |
| 1.573 | 2.402 | 16.415 | 66.257 | 0.205 | 2.496 | 4.192 | 0.647 | 4.891 | 0.922 |
FIG. 1 is a microscopic morphology of waste clay brick powder, which shows that the waste clay brick powder has rough surface and irregular particle shape; FIG. 2 is an X-ray diffraction diagram of waste clay brick powder, activated waste clay brick powder and Na-P type zeolite molecular sieve, which shows that the main crystal phase of the waste clay brick powder is quartz, and after alkali activation, the diffraction peak of the quartz is weakened, and stronger Na appears 2 SiO 3 Diffraction peaks, which show that the method for activating the composite mineralizer at low temperature can effectively activate the waste clay bricks, and after hydrothermal crystallization treatment, the diffraction peaks of the Na-P type zeolite are obvious; spherical particulate matter appears in fig. 3, which is a microscopic topography of a typical Na-P type zeolite molecular sieve. The microstructure characterization result fully shows that the method and the technical route can fully utilize the waste clay brick powder to efficiently synthesize the Na-P type zeolite molecular sieve.
Example 1
Grinding the waste clay bricks into powder and sieving the powder by a 100-mesh sieve. Then, pretreating the waste clay brick powder in acid liquor at 90 ℃ for 2 hours, wherein the acid liquor is hydrochloric acid with the mass concentration of 2%, and then filtering and drying to obtain the waste clay brick powder. Mixing and grinding the pretreated waste clay brick powder with a certain amount of NaOH and NaF, wherein the mass ratio of the NaOH to the waste clay brick powder is (alkali-ash ratio) 1.4, and the doping amount of the NaF is 1% of the mass of the waste clay brick powder. The mixed product was calcined in a muffle furnace at 350 ℃ for 2 hours. Then, the activated product was dissolved in a certain amount of deionized water at a solid/liquid ratio of 1g/10L, followed by ultrasonic treatment for 30 minutes. And finally, pouring the mixed solution into a polytetrafluoroethylene container, carrying out hydrothermal reaction for 12 hours at 120 ℃, filtering and drying to obtain the Na-P type zeolite molecular sieve. The removal rate of methylene blue by the performance test is 80.78%, as shown in table 2.
Example 2
Grinding waste clay bricks into powder by ball milling, and sieving with a 100-mesh sieve. And then, pretreating the waste clay brick powder in acid liquor at 90 ℃ for 2 hours, wherein the acid liquor is hydrochloric acid with the mass concentration of 2%, and then filtering and drying to obtain the waste clay brick powder. Mixing and grinding the pretreated waste clay brick powder with a certain amount of NaOH and NaF, wherein the mass ratio of the NaOH to the waste clay brick powder is (alkali-ash ratio) 1.2, and the doping amount of the NaF is 1% of the mass of the waste clay brick powder. The mixed product was calcined in a muffle furnace at a temperature of 450 ℃ for 2 hours. Then, the activated product was dissolved in a certain amount of deionized water at a solid/liquid ratio of 1g/10L, followed by ultrasonic treatment for 30 minutes. And finally, pouring the mixed solution into a polytetrafluoroethylene container, carrying out hydrothermal reaction for 12 hours at the temperature of 100 ℃, filtering and drying to obtain the Na-P type zeolite molecular sieve. The removal rate of methylene blue by the performance test is 90.54%, as shown in table 2.
Example 3
Grinding the waste clay bricks into powder and sieving the powder by a 100-mesh sieve. And then, pretreating the waste clay brick powder in acid liquor at 90 ℃ for 2 hours, wherein the acid liquor is hydrochloric acid with the mass concentration of 2%, and then filtering and drying to obtain the waste clay brick powder. Mixing and grinding the pretreated waste clay brick powder with a certain amount of NaOH and NaF, wherein the mass ratio (alkali-ash ratio) of the NaOH to the waste clay brick powder is 1.2, and the doping amount of the NaF is 1% of the mass of the waste clay brick powder. The mixed product was calcined in a muffle furnace at 550 ℃ for 2 hours. Then, the activated product was dissolved in a certain amount of deionized water at a solid/liquid ratio of 1g/10L, followed by ultrasonic treatment for 30 minutes. And finally, pouring the mixed solution into a polytetrafluoroethylene container, carrying out hydrothermal reaction for 12 hours at the temperature of 80 ℃, filtering and drying to obtain the Na-P type zeolite molecular sieve. The removal rate of methylene blue by the performance test is 85.94%, as shown in table 2.
Comparative example
Grinding the waste clay bricks into powder and sieving the powder by a 100-mesh sieve. Then, the waste clay brick powder is pretreated in acid liquor at 90 ℃ for 2 hours, the acid liquor is hydrochloric acid with the mass concentration of 2%, then the waste clay brick powder is obtained through filtration and drying, and the removal rate of methylene blue is 13.19% through performance tests, and is shown in table 2.
Table 2 results of performance testing
Through the adsorption result of embodiment and comparative example, can find, abandonment clay brick powder has certain adsorption, but the adsorption capacity is less, and adsorption efficiency is lower. The Na-P type zeolite molecular sieve is synthesized, the adsorption efficiency of the Na-P type zeolite molecular sieve on methylene blue is obviously improved, and the removal efficiency of the methylene blue exceeds 80%, so that the Na-P type zeolite molecular sieve has higher adsorption capacity and has greater application prospect in water pollution treatment.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A method for synthesizing a Na-P type zeolite molecular sieve by using waste clay brick powder is characterized by comprising the following steps:
s1: ball-milling and sieving the waste clay bricks to obtain waste clay brick powder;
s2: pretreating the waste clay brick powder obtained in the step S1;
s3: mixing and grinding the pretreated waste clay brick powder obtained in the step S2 with NaOH and NaF to obtain a mixed product;
s4: calcining the mixed product obtained in the step S3 to obtain an activated product;
s5: dissolving the activated product obtained in the step S4 in deionized water and carrying out ultrasonic treatment to obtain a mixed solution;
s6: carrying out hydrothermal reaction on the mixed solution obtained in the step S5 to obtain a reactant;
s7: and (4) carrying out solid-liquid separation on the reactant obtained in the step (S6), and washing and drying the solid obtained by separation to obtain the Na-P type zeolite molecular sieve.
2. The method for synthesizing Na-P type zeolite molecular sieve from waste clay brick powder as claimed in claim 1, wherein SiO of waste clay brick is in step S1 2 And Al 2 O 3 The mass content of the silicon-aluminum alloy is not less than 80 percent, and the Si/Al molar ratio is 2-4.
3. The method for synthesizing the Na-P type zeolite molecular sieve from the waste clay brick powder as claimed in claim 1, wherein the mesh number of the sieve used in the sieving in step S1 is not more than 100.
4. The method for synthesizing the Na-P type zeolite molecular sieve from the waste clay brick powder as claimed in claim 1, wherein the pretreatment in step S2 comprises acid washing, filtering and drying, the acid solution used in the acid washing process is hydrochloric acid with a mass concentration of 2%, the acid washing temperature is 90 ℃ and the acid washing time is 2 hours.
5. The method for synthesizing Na-P type zeolite molecular sieve from waste clay brick powder as claimed in claim 1, wherein the mass ratio of NaOH to waste clay brick powder in step S3 is 1-1.4, and the mass of NaF is 1% of waste clay brick powder.
6. The method for synthesizing Na-P type zeolite molecular sieve from waste clay brick powder as claimed in claim 1, wherein the calcination temperature in step S4 is 350-550 ℃ for 2 h.
7. The method for synthesizing the Na-P type zeolite molecular sieve from the waste clay brick powder as claimed in claim 1, wherein the solid-to-liquid ratio of the activated product to the deionized water in step S5 is 1g/10L, and the time of the ultrasonic treatment is 30 min.
8. The method for synthesizing the Na-P type zeolite molecular sieve from the waste clay brick powder as claimed in claim 1, wherein the temperature of the hydrothermal reaction in step S6 is 80-120 ℃ and the time is not less than 12 h.
9. The method for synthesizing the Na-P type zeolite molecular sieve from the waste clay brick powder as claimed in claim 1, wherein the solid-liquid separation in step S7 is centrifugation.
10. The application of the method for synthesizing Na-P type zeolite molecular sieve from waste clay brick powder as claimed in any one of claims 1-9 in the field of sewage treatment.
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