CN115465871A - Method for preparing Silicalite-1 molecular sieve by using corn leaves - Google Patents

Method for preparing Silicalite-1 molecular sieve by using corn leaves Download PDF

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CN115465871A
CN115465871A CN202211157360.3A CN202211157360A CN115465871A CN 115465871 A CN115465871 A CN 115465871A CN 202211157360 A CN202211157360 A CN 202211157360A CN 115465871 A CN115465871 A CN 115465871A
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corn leaves
molecular sieve
biomass
silicalite
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CN115465871B (en
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赵海玲
安宏佳
赵威
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Zhao Hailing
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/02Separation 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B37/00Compounds having molecular sieve properties but not having base-exchange properties
    • C01B37/005Silicates, i.e. so-called metallosilicalites or metallozeosilites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2253/00Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10Inorganic adsorbents
    • B01D2253/116Molecular sieves other than zeolites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image

Abstract

The invention discloses a method for preparing a Silicalite-1 molecular sieve by using corn leaves, which comprises the steps of firstly, cleaning and drying the biomass corn leaves, secondly, carbonizing the biomass corn leaves to obtain white powder, thirdly, washing and filtering the white powder, then adding tetrapropylammonium hydroxide, alkali, water and seed crystals, mixing and stirring, fourthly, crystallizing the mixed solution to obtain a crystallized substance, and fifthly, roasting and curing the crystallized substance to obtain the zeolite molecular sieve; the invention adopts SiO in the biomass corn leaves 2 As a silicon source of the molecular sieve, the method effectively utilizes the characteristics of biomass, enriches the methods of biomass utilization technology, reduces the damage to the environment in the existing silicon dioxide mining process, and solves the problems of high energy consumption and high pollution in the silicon preparation process and the zeolite molecular sieve process in industry, and provides the method for preparing the molecular sieveThe synthesis route is green.

Description

Method for preparing Silicalite-1 molecular sieve by using corn leaves
Technical Field
The invention relates to the technical field of clean energy, in particular to a method for preparing a Silicalite-1 molecular sieve by using corn leaves.
Background
The current society faces the problems of energy shortage, increasingly serious environmental destruction and the like, biomass energy is used as renewable green energy, great development and utilization are of great significance to industry and social life, and the preparation of the molecular sieve by using biomass as a raw material is one of effective and feasible methods for converting biomass into a green molecular sieve synthetic route.
Corn is used as a biomass resource with the annual output of 2.57 hundred million tons in China, and the main components of corn leaves are cellulose, hemicellulose, lignin, silicon dioxide and inorganic metal ions, so that the corn leaf has great application potential as a biomass silicon source.
The corn leaves used in the form of silicon dioxide in the coating can obviously improve scratch resistance, abrasion resistance, hardness, modulus, thermal stability, rheological property, hydrophobicity and the like; the silicon element exists in the cell wall of the leaf of the corn leaf and can weaken the transpiration together with the cuticle; in order to extract the amorphous silica, inorganic acid such as sulfuric acid, hydrochloric acid and nitric acid solution is generally used for acid leaching to remove metal oxide impurities in the corn leaves, then a calcination mode is used for separating organic matters in the corn leaves, and strong acid is not suitable for being used in a large amount as an environmental pollutant, so that the invention provides a method for preparing the Silicalite-1 molecular sieve by using the corn leaves so as to solve the problems in the prior art.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a method for preparing the Silicalite-1 molecular sieve by using corn leaves, and the method for preparing the Silicalite-1 molecular sieve by using the corn leaves adopts SiO in biomass corn leaves 2 As a silicon source of the molecular sieve, the method effectively utilizes the characteristics of biomass, enriches the methods of biomass utilization technology, reduces the damage to the environment in the existing silicon dioxide mining process, and provides a green synthetic route for the problems of silicon preparation process and zeolite molecular sieve process with high energy consumption and high pollution in industry.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme: a method for preparing Silicalite-1 molecular sieve by using corn leaves comprises the following steps:
soaking biomass corn leaves in deionized water for 24 hours, repeatedly washing the biomass corn leaves with water for 3-4 times until the surfaces of the biomass corn leaves are free of mud and other dirt, and then putting the biomass corn leaves into a drying box for drying treatment to obtain dried biomass corn leaves;
step two, placing the biomass corn leaves into a citric acid solution for treatment to obtain a mixture, and preserving the temperature of the mixture in a muffle furnace at 600-800 ℃ for 5 hours in an air atmosphere to obtain white powder;
washing and filtering the obtained white powder to obtain pure white powder, and then strongly stirring tetrapropylammonium hydroxide, alkali, water and seed crystals with the pure white powder to prepare uniform mixed solution;
transferring the obtained mixed solution to a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining for crystallization treatment to obtain a crystallized substance;
and step five, washing the obtained crystallized substance with deionized water until the crystallized substance is nearly neutral, then placing the crystallized substance in a drying oven at the temperature of 3-150 ℃ for drying treatment, then placing the dried crystallized substance in a muffle furnace at the temperature of 400-700 ℃ for roasting for 4-20 hours, and curing to obtain the Silicalite-1 zeolite molecular sieve.
The further improvement lies in that: adding an acidic solution to remove metal ions when the biomass corn leaves are soaked in the first step, and drying the cleaned biomass corn leaves in the sun after washing; during the drying treatment, the biomass corn leaves are placed in a drying box and kept dry for 4 hours under the ventilation condition of 60 ℃.
The further improvement lies in that: and in the second step, the biomass corn leaves and the citric acid solution are subjected to azeotropy for 1h and then washed with distilled water for three times, and the steps are repeated for three times.
The further improvement is that: and in the third step, the seed crystal is a Silicalite-1 zeolite molecular sieve, and the Silicalite-1 crystal with the particle size of 100-300nm is obtained after ball milling.
The further improvement lies in that: the mixed solution after stirring in the third step consists of TPAOH and SiO 2 、Na 2 O、H 2 O and Seed, wherein TPAOH, siO 2 、Na 2 O、H 2 The molar mass ratio of O to Seed is 0.01-0.1.
The further improvement lies in that: the crystallization treatment in the fourth step is carried out for 1 to 5 days under the condition of 100 to 200 ℃ in a static or dynamic crystallization way, wherein the static crystallization treatment time is 1 to 2 days; the dynamic crystallization treatment time is 2-5 days, the dynamic purification treatment comprises crystallization under stirring and rotating conditions, and the pressure of crystallization reaction when water is heated is the pressure of the components in the mixed solution generated by heat.
The further improvement lies in that: the molecular sieve prepared by the method for preparing the Silicalite-1 molecular sieve by using the corn leaves is applied to gas separation.
The invention has the beneficial effects that: the invention adopts SiO in the biomass corn leaves 2 As a silicon source of the molecular sieve, the method effectively utilizes the characteristics of biomass, enriches the methods of biomass utilization technology, reduces the damage to the environment in the existing silicon dioxide mining process, and provides a green synthetic route for the problems of silicon preparation process and zeolite molecular sieve process with high energy consumption and high pollution in industry.
Drawings
FIG. 1 is a flowchart of a method of example 1 of the present invention.
FIG. 2 is a morphology chart of biomass Silicalite-1 of the invention.
FIG. 3 is an XRD pattern of the biomass Silicalite-1 of the present invention.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
Example 1
Referring to fig. 1, 2 and 3, this example provides a method for preparing Silicalite-1 molecular sieve from corn leaves, comprising the following steps:
soaking biomass corn leaves in deionized water for 24 hours, repeatedly washing the biomass corn leaves with water for 3-4 times until the surfaces of the biomass corn leaves have no soil or other dirt, then putting the biomass corn leaves into a drying oven for drying treatment, putting the biomass corn leaves into the drying oven during the drying treatment, and keeping the biomass corn leaves dry for 4 hours under a ventilation condition of 60 ℃ to obtain dry biomass corn leaves;
adding an acid solution to remove metal ions when the biomass corn leaves are soaked, placing the washed biomass corn leaves in the sun for drying, and then carrying out leaf drying treatment.
Step two, placing the biomass corn leaves into a citric acid solution for azeotropy for 1 hour, washing the biomass corn leaves with distilled water for three times, repeating the steps for three times to obtain a mixture after treatment, and preserving the temperature of the mixture in a muffle furnace at 600-800 ℃ for 5 hours in an air atmosphere to obtain white powder;
washing and filtering the obtained white powder to obtain pure white powder, and then strongly stirring tetrapropylammonium hydroxide, alkali, water and seed crystals with the pure white powder to prepare uniform mixed solution;
the mixed solution after stirring consists of TPAOH and SiO 2 、Na 2 O、H 2 O and Seed, wherein TPAOH, siO 2 、Na 2 O、H 2 The molar mass ratio of O to Seed is 0.01-0.1;
wherein the seed crystal is Silicalite-1 zeolite molecular sieve crystals with the particle size of 100-300nm obtained after ball milling.
Transferring the obtained mixed solution to a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining for crystallization treatment to obtain a crystallized substance;
the crystallization treatment is carried out for 1-5 days under the condition of 100-200 ℃, wherein the static crystallization treatment time is 1-2 days; the dynamic crystallization treatment time is 2-5 days, the dynamic purification treatment comprises crystallization under stirring and rotating conditions, and the pressure of crystallization reaction when water is heated is the self pressure of the components in the mixed solution generated by heat.
And step five, washing the obtained crystallized substance to be nearly neutral by deionized water, then placing the crystallized substance in a drying box at the temperature of 3-150 ℃ for drying treatment, then placing the dried crystallized substance in a muffle furnace at the temperature of 400-700 ℃ for roasting for 4-20 hours, and curing to obtain the Silicalite-1 zeolite molecular sieve.
The molecular sieve prepared by the method for preparing the Silicalite-1 molecular sieve by using the corn leaves is applied to gas separation.
Example 2
The embodiment provides a method for preparing Silicalite-1 molecular sieve by using corn leaves, which comprises the steps of soaking the corn leaves in deionized water for 20 hours, repeatedly washing the corn leaves for 3-4 times to remove soil and other dirt attached to the surfaces of the corn leaves, and then putting the corn leaves into a drying box to be kept at 60 ℃ for ventilation drying for 4 hours.
Azeotropy corn leaf and citric acid solution for 1h, washing with distilled water for 3 times, repeating the above steps for 3 times, placing pretreated corn leaf into muffle furnace, heating the furnace to 620 deg.C, and keeping the temperature for 6h to obtain white powder.
Washing and filtering the obtained white powder to obtain pure SiO 2 Product, 0.2g Silicalite-1 seed (0.2 wt%) was seeded with 5g biomass SiO at room temperature 2 The product (0.07 mol) is dissolved in 100gH 2 O was mixed well to form solution A, then NaOH (1.25 g,0.031 mol) and TPAOH (9.15g, 0.042mol) were dissolved in H 2 O (60g, 3.33mol) is evenly mixed to form a solution B, and then the A is slowly added into the solution B, wherein the molar mass ratio of the components is as follows: siO 2 2 :TPAOH:Na 2 O:H 2 O=1:0.56:0.19:111。
The resulting mixture was then transferred to a stainless steel autoclave with a teflon liner for static crystallization at 175 c for 1 day.
And (3) quenching to room temperature after crystallization, washing to obtain a completely crystallized product, drying, roasting for 8 hours at 550 ℃ in a muffle furnace, and solidifying the pore channel to obtain the Silicalite-1 zeolite molecular sieve.
Example 3
The embodiment provides a method for preparing Silicalite-1 molecular sieve by using corn leaves, which comprises the steps of soaking the corn leaves in deionized water for 20 hours, repeatedly washing the corn leaves for 3-4 times to remove soil and other dirt attached to the surfaces of the corn leaves, and then putting the corn leaves into a drying box to be kept at 60 ℃ for ventilation drying for 4 hours.
The corn leaves were azeotroped with the bulk citric acid solution for 1h and washed 3 times with distilled water, and the above steps were repeated 3 times. Placing the pretreated corn leaves into a muffle furnace, heating the furnace to 620 ℃, and preserving the temperature for 6 hours to obtain white powder.
The resulting white powder was washed and filtered toPure SiO is obtained 2 Product, 0.15g Silicalite-1 (0.15 wt%) seed with 4g Biomass SiO at room temperature 2 The product (0.064 mol) is dissolved in 100gH 2 O was mixed well to form solution A, then NaOH (2 g, 0.05 mol) and TPAOH (3.9 g, 0.019mol) were dissolved in H 2 O (120g, 6.66mol) is evenly mixed to form a solution B, and then A is slowly added into the solution B, wherein the molar mass ratio of the components is as follows: siO 2 2 :TPAOH:Na 2 O:H 2 O=1:0.3:0.39:190。
The resulting mixture was then transferred to a stainless steel autoclave with a teflon liner for static crystallization at 175 c for 1 day.
And (3) quenching to room temperature after crystallization, washing to obtain a completely crystallized product, drying, roasting in a muffle furnace at 550 ℃ for 8 hours, and solidifying the pore channel to obtain the Silicalite-1 zeolite molecular sieve.
Example 4
The embodiment provides a method for preparing Silicalite-1 molecular sieve by using corn leaves, which comprises the steps of soaking the corn leaves in deionized water for 20 hours, repeatedly washing the corn leaves for 3-4 times to remove soil and other dirt attached to the surfaces of the corn leaves, and then putting the corn leaves into a drying box to be kept at 60 ℃ for ventilation drying for 4 hours.
Azeotropy corn leaves and a body citric acid solution for 1h, washing with distilled water for 3 times, repeating the steps for 3 times, putting the pretreated corn leaves into a muffle furnace, heating the furnace to 620 ℃, and keeping the temperature for 6h to obtain white powder.
Washing and filtering the obtained white powder to obtain pure SiO 2 Product, 1g of Silicalite-1 seed (1 wt.%) was seeded with 5g of Biomass SiO at room temperature 2 The product (0.08 mol) is dissolved in 100gH 2 O was mixed to homogeneity to form solution A, then NaOH (1.25g, 0.0318 mol) and TPAOH (13.73g, 0.068 mol) were dissolved in H 2 O (200g, 11.11mol) is evenly mixed to form a solution B, and then A is slowly added into the solution B, wherein the molar mass ratio of each component is as follows: siO 2 2 :TPAOH:Na 2 O:H 2 O=1:0.85:0.19:208。
The resulting mixture was then transferred to a stainless steel autoclave with a teflon liner for static crystallization at 175 c for 1 day.
And (3) quenching to room temperature after crystallization, washing to obtain a completely crystallized product, drying, roasting in a muffle furnace at 550 ℃ for 8 hours, and solidifying the pore channel to obtain the Silicalite-1 zeolite molecular sieve.
Example 5
The embodiment provides a method for preparing Silicalite-1 molecular sieve by using corn leaves, which comprises the steps of soaking the corn leaves in deionized water for 20 hours, repeatedly washing the corn leaves for 3-4 times to remove soil and other dirt attached to the surfaces of the corn leaves, and then putting the corn leaves into a drying box to be kept at 60 ℃ for ventilation drying for 4 hours.
The leaves of corn were azeotroped with the citric acid solution for 1h and washed with distilled water 3 times, and the above procedure was repeated 3 times. Placing the pretreated corn leaves into a muffle furnace, heating the furnace to 620 ℃, and preserving the temperature for 6 hours to obtain white powder.
Washing and filtering the obtained white powder to obtain pure SiO 2 Product, 2g of Silicalite-1 seed (2 wt.%) with 5g of biomass SiO at room temperature 2 The product (0.08 mol) is dissolved in 100gH 2 O was mixed well to form solution A, then NaOH (2.5 g, 0.062mol) and TPAOH (16.47g, 0.081mol) were dissolved in H 2 O (300g, 16.67mol) is evenly mixed to form a solution B, and then A is slowly added into the solution B, wherein the molar mass ratio of each component is as follows: siO 2 2 :TPAOH:Na 2 O:H 2 O=1:1.01:0.39:278。
The resulting mixture was then transferred to a stainless steel autoclave with a teflon liner for static crystallization at 175 c for 1 day.
And (3) quenching to room temperature after crystallization, washing to obtain a completely crystallized product, drying, roasting in a muffle furnace at 550 ℃ for 8 hours, and solidifying the pore channel to obtain the Silicalite-1 zeolite molecular sieve.
Example 6
The embodiment provides a method for preparing Silicalite-1 molecular sieve by using corn leaves, which comprises the steps of soaking the corn leaves in deionized water for 20 hours, repeatedly washing the corn leaves for 3-4 times to remove soil and other dirt attached to the surfaces of the corn leaves, and then putting the corn leaves into a drying box to be kept at 60 ℃ for ventilation drying for 4 hours.
Azeotropy corn leaves and a body citric acid solution for 1h, washing with distilled water for 3 times, repeating the steps for 3 times, putting the pretreated corn leaves into a muffle furnace, heating the furnace to 620 ℃, and keeping the temperature for 6h to obtain white powder.
Washing and filtering the obtained white powder to obtain pure SiO 2 Product, 3g of Silicalite-1 seed (3 wt.%) with 5g of biomass SiO at room temperature 2 The product (0.08 mol) is dissolved in 100gH 2 O was stirred well to form solution A, then NaOH (2.5 g, 0.062mol) and TPAOH (32.94g, 0.162mol) were dissolved in H 2 O (400g, 22.22mol) is evenly mixed to form a solution B, and then A is slowly added into the solution B, wherein the molar mass ratio of each component is as follows: siO 2 2 :TPAOH:Na 2 O:H 2 O=1:2.02:0.39:347。
The resulting mixture was then transferred to a stainless steel autoclave with a teflon liner for static crystallization at 175 c for 1 day.
And (3) quenching to room temperature after crystallization, washing to obtain a completely crystallized product, drying, roasting for 8 hours at 550 ℃ in a muffle furnace, and solidifying the pore channel to obtain the Silicalite-1 zeolite molecular sieve.
Example 7
This example provides a molecular sieve test experiment for preparing a Silicalite-1 molecular sieve from corn leaves, and the adsorption separation performance of the Silicalite-1 molecular sieve is evaluated as follows: with CO 2 /N 2 、CO 2 /CH 4 The two-component mixed gas (50%: 50%) is used as raw material gas to carry out penetration separation experiment on the Silicalite-1 zeolite molecular sieve.
The usage amount of the Silicalite-1 zeolite molecular sieve is 4.862g, the time from the beginning of the adsorption of the mixed gas to the penetration of the weak adsorbate is defined as the penetration time, also called the co-adsorption time, the time from the penetration of the weak adsorbate to the penetration of the strong adsorbate is called the retention time, generally, the shorter the penetration time and the longer the retention time, the better the adsorption and separation effect of the material on the mixed gas, and the adsorption and separation effect is usually related to both the selectivity and the adsorption amount. The results of the reaction are shown in Table 1 below, which demonstrate that the Silicalite-1 zeolite molecules of the present inventionThe sieve has high gas adsorption capacity and gas adsorption selectivity, and can effectively adsorb and separate CO 2
TABLE 1 Silicalite-1 adsorption selectivity coefficient (Si/j)
Figure BDA0003859356070000101
It should be noted that the biomass corn leaves in the present application are not limited to pure corn leaves, but may be other biomass resources.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (7)

1. A method for preparing a Silicalite-1 molecular sieve by using corn leaves is characterized by comprising the following steps:
soaking biomass corn leaves in deionized water for 24 hours, repeatedly washing the biomass corn leaves with water for 3-4 times until the surfaces of the biomass corn leaves are free of mud and other dirt, and then putting the biomass corn leaves into a drying box for drying treatment to obtain dried biomass corn leaves;
step two, putting biomass corn leaves into a citric acid solution for treatment to obtain a mixture, and preserving the heat of the mixture in a muffle furnace at 600-800 ℃ for 5 hours in an air atmosphere to obtain white powder;
washing and filtering the obtained white powder to obtain pure white powder, and then strongly stirring tetrapropylammonium hydroxide, alkali, water and seed crystals with the pure white powder to prepare a uniform mixed solution;
transferring the obtained mixed solution to a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining for crystallization treatment to obtain a crystallized substance;
and step five, washing the obtained crystallized substance with deionized water until the crystallized substance is nearly neutral, then placing the crystallized substance in a drying oven at the temperature of 3-150 ℃ for drying treatment, then placing the dried crystallized substance in a muffle furnace at the temperature of 400-700 ℃ for roasting for 4-20 hours, and curing to obtain the Silicalite-1 zeolite molecular sieve.
2. The method for preparing the Silicalite-1 molecular sieve by using the corn leaves as the raw material according to claim 1, wherein the method comprises the following steps: adding an acid solution to remove metal ions when the biomass corn leaves are soaked in the first step, and drying the cleaned biomass corn leaves in the sun after washing; during the drying treatment, the biomass corn leaves are placed in a drying box and kept dry for 4 hours under the ventilation condition of 60 ℃.
3. The method for preparing the Silicalite-1 molecular sieve by using the corn leaves as claimed in claim 1, wherein the method comprises the following steps: and in the second step, the biomass corn leaves and the citric acid solution are subjected to azeotropy for 1h and then washed with distilled water for three times, and the steps are repeated for three times.
4. The method for preparing the Silicalite-1 molecular sieve by using the corn leaves as the raw material according to claim 1, wherein the method comprises the following steps: in the third step, the seed crystal is Silicalite-1 zeolite molecular sieve, and the Silicalite-1 crystal with the particle size of 100-300nm is obtained after ball milling.
5. The method for preparing the Silicalite-1 molecular sieve by using the corn leaves as the raw material according to claim 1, wherein the method comprises the following steps: the mixed solution after stirring in the third step consists of TPAOH and SiO 2 、Na 2 O、H 2 O and Seed, wherein TPAOH, siO 2 、Na 2 O、H 2 The molar mass ratio of O to Seed is 0.01-0.1.
6. The method for preparing the Silicalite-1 molecular sieve by using the corn leaves as claimed in claim 1, wherein the method comprises the following steps: in the step four, static or dynamic crystallization treatment is carried out for 1-5 days at the temperature of 100-200 ℃ during crystallization treatment, wherein the static crystallization treatment time is 1-2 days; the dynamic crystallization treatment time is 2-5 days, the dynamic purification treatment comprises crystallization under stirring and rotating conditions, and the pressure of crystallization reaction when water is heated is the self pressure of the components in the mixed solution generated by heat.
7. The use of the molecular sieve prepared by the method of any one of claims 1-6 for preparing Silicalite-1 molecular sieve from corn leaves in gas separation.
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Publication number Priority date Publication date Assignee Title
US5985238A (en) * 1995-06-07 1999-11-16 Pq Corporation Process for preparing ferrierite
CN101163546A (en) * 2005-04-22 2008-04-16 巴斯福股份公司 Process for preparing a nanosized zeolitic material
CN102320619A (en) * 2011-10-06 2012-01-18 大连理工大学 Synthesis method of titanium silicalite TS-1
CN107934986A (en) * 2017-11-23 2018-04-20 武汉凯迪工程技术研究总院有限公司 Biomass ash resource utilization method
CN114031094A (en) * 2021-12-06 2022-02-11 格润科技(大连)有限责任公司 Nano MFI/MOR eutectic molecular sieve and synthesis method of nano Ti-MFI/MOR eutectic molecular sieve

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5985238A (en) * 1995-06-07 1999-11-16 Pq Corporation Process for preparing ferrierite
CN101163546A (en) * 2005-04-22 2008-04-16 巴斯福股份公司 Process for preparing a nanosized zeolitic material
CN102320619A (en) * 2011-10-06 2012-01-18 大连理工大学 Synthesis method of titanium silicalite TS-1
CN107934986A (en) * 2017-11-23 2018-04-20 武汉凯迪工程技术研究总院有限公司 Biomass ash resource utilization method
CN114031094A (en) * 2021-12-06 2022-02-11 格润科技(大连)有限责任公司 Nano MFI/MOR eutectic molecular sieve and synthesis method of nano Ti-MFI/MOR eutectic molecular sieve

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