CN115465871B - Method for preparing Silicalite-1 molecular sieve by using corn leaves - Google Patents
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Abstract
The application discloses a method for preparing Silicalite-1 molecular sieve by using corn leaves, which comprises the steps of firstly, washing and drying biomass corn leaves, secondly, processing biomass corn She Tanhua to obtain white powder, thirdly, washing and filtering the white powder, adding tetrapropylammonium hydroxide, alkali, water and seed crystal, mixing and stirring, fourthly, crystallizing the mixed solution to obtain a crystallized substance, and fifthly, washing, drying, roasting and solidifying the crystallized substance to obtain the zeolite molecular sieve; the application adopts SiO in biomass corn leaves 2 As a silicon source of the molecular sieve, the characteristics of biomass are effectively utilized, the method of biomass utilization technology is enriched, the damage to the environment in the existing silicon dioxide exploitation process is reduced, and a green synthetic route is provided for the problems of high-energy consumption and high-pollution silicon preparation technology and zeolite molecular sieve technology in industry.
Description
Technical Field
The application relates to the technical field of clean energy, in particular to a method for preparing Silicalite-1 molecular sieve by using corn leaves.
Background
The current society faces the problems of energy shortage, increasingly serious environmental damage and the like, biomass energy is taken as renewable green energy, a great deal of development and utilization are of great significance to industry and social life, and the preparation of the molecular sieve by taking biomass as a raw material is one of effective and feasible methods for converting biomass into a green molecular sieve synthetic route.
Corn is taken as biomass resource with annual output of 2.57 hundred million tons in China, the main components in corn leaves are cellulose, hemicellulose, lignin, silicon dioxide and inorganic metal ions, and the corn has huge application potential as biomass silicon source.
The corn leaves are used for coating in the form of silicon dioxide, so that scratch resistance, abrasion resistance, hardness, modulus, thermal stability, rheological property, hydrophobicity and the like can be obviously improved; the silicon element exists in the cell walls of leaves of the corn leaves and can weaken the transpiration together with the cuticle; for extracting these amorphous silica, inorganic acids such as sulfuric acid, hydrochloric acid and nitric acid are generally used for acid leaching to remove metal oxide impurities in corn leaves, and then calcination is used to separate organic matters in corn leaves, and strong acid is not suitable for mass use as an environmental pollutant, so the present application proposes a method for preparing Silicalite-1 molecular sieve from corn leaves to solve the problems in the prior art.
Disclosure of Invention
In view of the above problems, an object of the present application is to provide a method for preparing Silicalite-1 molecular sieve from corn leaves, which uses SiO in biomass corn leaves 2 As a silicon source of the molecular sieve, the characteristics of biomass are effectively utilized, the method of biomass utilization technology is enriched, the damage to the environment in the existing silicon dioxide exploitation process is reduced, and a green synthetic route is provided for the problems of high-energy consumption and high-pollution silicon preparation technology and zeolite molecular sieve technology in industry.
In order to achieve the purpose of the application, the application is realized by the following technical scheme: a method for preparing Silicalite-1 molecular sieve by using corn leaves, comprising the following steps:
step one, soaking biomass corn leaves with deionized water for 24 hours, repeatedly flushing the biomass corn leaves with water for 3-4 times until soil and other dirt on the surfaces of the biomass corn leaves are absent, and then placing the biomass corn leaves into a drying oven for drying treatment to obtain dry biomass corn leaves;
step two, putting 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;
step three, washing and filtering the obtained white powder to obtain pure white powder, and then carrying out strong stirring on tetrapropylammonium hydroxide, alkali, water and seed crystals to prepare uniform mixed solution;
transferring the obtained mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining for crystallization treatment to obtain a crystallized product;
and fifthly, washing the obtained crystallized product by deionized water until the crystallized product is nearly neutral, then placing the crystallized product in a drying box at 3-150 ℃ for drying treatment, placing the dried product in a muffle furnace at 400-700 ℃ for roasting for 4-20 hours, and solidifying the dried product to obtain the Silicalite-1 zeolite molecular sieve.
The further improvement is that: adding an acidic solution to remove metal ions when soaking biomass corn leaves, washing, and drying the washed biomass corn leaves in sunlight and then carrying out leaf drying treatment; during the drying treatment, biomass corn leaves are placed into a drying oven and kept dry for 4 hours under the ventilation condition of 60 ℃.
The further improvement is that: in the second step, the biomass corn leaves and the citric acid solution are subjected to azeotropy for 1h, then distilled water is used for flushing 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 Silicalite-1 zeolite molecular sieve ball milling to obtain Silicalite-1 crystals with the particle size of 100-300 nm.
The further improvement is that: the mixed solution after stirring in the third step is composed of TPAOH and SiO 2 、Na 2 O、H 2 O and Seed, where TPAOH, siO 2 、Na 2 O、H 2 The molar mass ratio of O to Seed is 0.2:1:0.01-0.1:20-50:0.005-0.05.
The further improvement is that: 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 the stirring rotation condition, and the pressure of crystallization reaction when water is heated is the pressure of the mixed liquid generated by heating components.
The further improvement is that: a molecular sieve prepared by a method for preparing Silicalite-1 molecular sieve by using corn leaves is applied to gas separation.
The beneficial effects of the application are as follows: the application adopts SiO in biomass corn leaves 2 As a silicon source of the molecular sieve, the characteristics of biomass are effectively utilized, the method of biomass utilization technology is enriched, the damage to the environment in the existing silicon dioxide exploitation process is reduced, and a green synthetic route is provided for the problems of high-energy consumption and high-pollution silicon preparation technology and zeolite molecular sieve technology in industry.
Drawings
FIG. 1 is a flow chart of a method according to embodiment 1 of the present application.
FIG. 2 is a morphology map of biomass Silicalite-1 of the present application.
FIG. 3 is an XRD pattern for biomass Silicalite-1 of the present application.
Detailed Description
The present application will be further described in detail with reference to the following examples, which are only for the purpose of illustrating the application and are not to be construed as limiting the scope of the application.
Example 1
According to the present embodiment, as shown in fig. 1, 2 and 3, there is provided a method for preparing Silicalite-1 molecular sieve from corn leaves, comprising the steps of:
step one, soaking biomass corn leaves with deionized water for 24 hours, repeatedly flushing the biomass corn leaves with water for 3-4 times until soil and other dirt are not on the surface of the biomass corn leaves, then placing the biomass corn leaves into a drying oven for drying treatment, placing the biomass corn leaves into the drying oven during the drying treatment, and keeping the biomass corn leaves dry for 4 hours under the ventilation condition of 60 ℃ to obtain dry biomass corn leaves;
when biomass corn leaves are soaked, an acidic solution is added to remove metal ions, and after washing, the washed biomass corn leaves are dried in the sun, and then subjected to leaf drying treatment.
Step two, putting biomass corn leaves into citric acid solution for azeotropy for 1h, then flushing the biomass corn leaves with distilled water for three times, repeating the steps for three times, obtaining a mixture after treatment, and preserving the mixture in a muffle furnace at 600-800 ℃ for 5h in air atmosphere to obtain white powder;
step three, washing and filtering the obtained white powder to obtain pure white powder, and then carrying out strong stirring on tetrapropylammonium hydroxide, alkali, water and seed crystals to prepare uniform mixed solution;
the mixed solution after stirring is composed of TPAOH and SiO 2 、Na 2 O、H 2 O and Seed, where TPAOH, siO 2 、Na 2 O、H 2 The molar mass ratio of O to Seed is 0.2:1:0.01-0.1:20-50:0.005-0.05;
wherein the seed crystal is Silicalite-1 crystal with the grain diameter of 100-300nm after ball milling of the Silicalite-1 zeolite molecular sieve.
Transferring the obtained mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining for crystallization treatment to obtain a crystallized product;
the crystallization treatment is static or dynamic crystallization treatment for 1-5 days at 100-200deg.C, 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 the stirring rotation condition, and the pressure of crystallization reaction when water is heated is the pressure of the mixed liquid generated by heating components.
And fifthly, washing the obtained crystallized product by deionized water until the crystallized product is nearly neutral, then placing the crystallized product in a drying box at 3-150 ℃ for drying treatment, placing the dried product in a muffle furnace at 400-700 ℃ for roasting for 4-20 hours, and solidifying the dried product to obtain the Silicalite-1 zeolite molecular sieve.
A molecular sieve prepared by a method for preparing Silicalite-1 molecular sieve by using 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 20h, repeatedly washing the corn leaves for 3-4 times to remove soil and other dirt attached to the surfaces of the corn leaves, putting the corn leaves into a drying oven, and keeping the temperature at 60 ℃ for ventilation drying for 4h.
Azeotropy of corn leaves and body citric acid solution for 1h, washing with distilled water for 3 times, repeating the above steps for 3 times, placing pretreated corn leaves into a muffle furnace, heating to 620 ℃ and preserving heat 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) was dissolved in 100gH 2 O was stirred uniformly to form solution A, then NaOH (1.25 g,0.031 mol) and TPAOH (9.15 g,0.042 mol) were dissolved in H 2 O (60 g,3.33 mol) is uniformly mixed to form a solution B, and then the solution B is slowly added with the A, wherein the molar mass ratio of each component is as follows: siO (SiO) 2 :TPAOH:Na 2 O:H 2 O＝1:0.56:0.19:111。
The resulting mixture was then transferred to a stainless steel reactor lined with polytetrafluoroethylene and statically crystallized at 175 ℃ for 1 day.
Quenching to room temperature after crystallization, washing to obtain a complete crystallization product, drying, roasting in a muffle furnace at 550 ℃ for 8 hours, and solidifying pore channels 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 20h, repeatedly washing the corn leaves for 3-4 times to remove soil and other dirt attached to the surfaces of the corn leaves, putting the corn leaves into a drying oven, and keeping the temperature at 60 ℃ for ventilation drying for 4h.
Azeotropy of corn leaves with bulk citric acid solution for 1h and rinsing 3 times with distilled water, repeating the above steps 3 times. The pretreated corn leaves are placed into a muffle furnace, the furnace temperature is increased to 620 ℃ and the temperature is kept for 6 hours, and white powder is obtained.
Washing and filtering the obtained white powder to obtain pure SiO 2 Product, 0.15g Silicalite-1 (0.15 wt%) seed was seeded with 4g biomass SiO at room temperature 2 The product (0.064 mol) was dissolved in 100gH 2 O was stirred uniformly to form solution A, and then NaOH (2 g, 0.05 mol) and TPAOH (3.9 g,0.019 mol) were dissolved in H 2 O (120 g,6.66 mol) is uniformly mixed in the solution B to form a solution B, and then the solution B is slowly added with the solution A, wherein the molar mass ratio of each component is as follows: siO (SiO) 2 :TPAOH:Na 2 O:H 2 O＝1:0.3:0.39:190。
The resulting mixture was then transferred to a stainless steel reactor lined with polytetrafluoroethylene and statically crystallized at 175 ℃ for 1 day.
Quenching to room temperature after crystallization, washing to obtain a complete crystallization product, drying, roasting in a muffle furnace at 550 ℃ for 8 hours, and solidifying pore channels 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 20h, repeatedly washing the corn leaves for 3-4 times to remove soil and other dirt attached to the surfaces of the corn leaves, putting the corn leaves into a drying oven, and keeping the temperature at 60 ℃ for ventilation drying for 4h.
Azeotropy of corn leaves and body citric acid solution for 1h, washing with distilled water for 3 times, repeating the above steps for 3 times, placing pretreated corn leaves into a muffle furnace, heating to 620 ℃ and preserving heat for 6h to obtain white powder.
Washing and filtering the obtained white powder to obtain pure SiO 2 Product 1g Silicalite-1 seed (1 wt%) was seeded with 5g biomass SiO at room temperature 2 The product (0.08 mol) was dissolved in 100gH 2 O was stirred uniformly to form solution A, then NaOH (1.25 g,0.031 mol) and TPAOH (13.73 g,0.068 mol) were dissolved in H 2 O (200 g,11.11 mol) is uniformly mixed in the solution B to form a solution B, and then the solution B is slowly added with the solution A, wherein the molar mass ratio of each component is as follows: siO (SiO) 2 :TPAOH:Na 2 O:H 2 O＝1:0.85:0.19:208。
The resulting mixture was then transferred to a stainless steel reactor lined with polytetrafluoroethylene and statically crystallized at 175 ℃ for 1 day.
Quenching to room temperature after crystallization, washing to obtain a complete crystallization product, drying, roasting in a muffle furnace at 550 ℃ for 8 hours, and solidifying pore channels 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 20h, repeatedly washing the corn leaves for 3-4 times to remove soil and other dirt attached to the surfaces of the corn leaves, putting the corn leaves into a drying oven, and keeping the temperature at 60 ℃ for ventilation drying for 4h.
Azeotropy of corn leaves with bulk citric acid solution for 1h and rinsing 3 times with distilled water, repeating the above steps 3 times. The pretreated corn leaves are placed into a muffle furnace, the furnace temperature is increased to 620 ℃ and the temperature is kept for 6 hours, and white powder is obtained.
Washing and filtering the obtained white powder to obtain pure SiO 2 Product, 2g Silicalite-1 seed (2 wt%) were seeded with 5g biomass SiO at room temperature 2 The product (0.08 mol) was dissolved in 100gH 2 Mixing evenly in OSolution A was formed and then NaOH (2.5 g,0.062 mol) and TPAOH (16.47 g,0.081 mol) were dissolved in H 2 O (300 g,16.67 mol) is uniformly mixed in the solution B to form a solution B, and then the solution B is slowly added with the solution A, wherein the molar mass ratio of the components is as follows: siO (SiO) 2 :TPAOH:Na 2 O:H 2 O＝1:1.01:0.39:278。
The resulting mixture was then transferred to a stainless steel reactor lined with polytetrafluoroethylene and statically crystallized at 175 ℃ for 1 day.
Quenching to room temperature after crystallization, washing to obtain a complete crystallization product, drying, roasting in a muffle furnace at 550 ℃ for 8 hours, and solidifying pore channels 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 20h, repeatedly washing the corn leaves for 3-4 times to remove soil and other dirt attached to the surfaces of the corn leaves, putting the corn leaves into a drying oven, and keeping the temperature at 60 ℃ for ventilation drying for 4h.
Azeotropy of corn leaves and body citric acid solution for 1h, washing with distilled water for 3 times, repeating the above steps for 3 times, placing pretreated corn leaves into a muffle furnace, heating to 620 ℃ and preserving heat for 6h to obtain white powder.
Washing and filtering the obtained white powder to obtain pure SiO 2 Product, 3g Silicalite-1 seed (3 wt%) and 5g biomass SiO at room temperature 2 The product (0.08 mol) was dissolved in 100gH 2 O was stirred uniformly to form solution A, then NaOH (2.5 g,0.062 mol) and TPAOH (32.94 g,0.162 mol) were dissolved in H 2 O (400 g,22.22 mol) is uniformly mixed in the solution B to form a solution B, and then the solution B is slowly added with the solution A, wherein the molar mass ratio of each component is as follows: siO (SiO) 2 :TPAOH:Na 2 O:H 2 O＝1:2.02:0.39:347。
The resulting mixture was then transferred to a stainless steel reactor lined with polytetrafluoroethylene and statically crystallized at 175 ℃ for 1 day.
Quenching to room temperature after crystallization, washing to obtain a complete crystallization product, drying, roasting in a muffle furnace at 550 ℃ for 8 hours, and solidifying pore channels to obtain the Silicalite-1 zeolite molecular sieve.
Example 7
The embodiment provides a molecular sieve test experiment prepared by a method for preparing Silicalite-1 molecular sieve by using corn leaves, and adsorption separation performance evaluation of the Silicalite-1 zeolite molecular sieve: in the form of CO 2 /N 2 、CO 2 /CH 4 The two double-component mixed gas (50 percent: 50 percent) is used as raw material gas to carry out penetration separation experiment on the Silicalite-1 zeolite molecular sieve.
The amount of the Silicalite-1 zeolite molecular sieve is 4.862g, the period from the start of adsorption of the mixed gas to the penetration of the weak adsorbate is defined as penetration time, also called common adsorption time, the period from the penetration of the weak adsorbate to the penetration of the strong adsorbate is called retention time, and generally, the shorter the penetration time is, the longer the retention time is, the better the adsorption separation effect of the material on the mixed gas is, and the adsorption separation effect is usually related to the selectivity and the adsorption quantity. The reaction results are shown in the following table 1, and the results prove that the Silicalite-1 zeolite molecular sieve of the application has higher gas adsorption capacity and gas adsorption selectivity and can effectively adsorb and separate CO 2 。
TABLE 1 Silicalite-1 adsorption selectivity coefficient (Si/j)
The biomass corn leaves in the application are not limited to the simple corn leaves, but can be other biomass resources.
The foregoing has shown and described the basic principles, principal features and advantages of the application. It will be understood by those skilled in the art that the present application is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present application, and various changes and modifications may be made without departing from the spirit and scope of the application, which is defined in the appended claims. The scope of the application is defined by the appended claims and equivalents thereof.
Claims (7)
1. A method for preparing Silicalite-1 molecular sieve by using corn leaves, which is characterized by comprising the following steps:
step one, soaking biomass corn leaves with deionized water for 24 hours, repeatedly flushing the biomass corn leaves with water for 3-4 times until soil and other dirt on the surfaces of the biomass corn leaves are absent, and then placing the biomass corn leaves into a drying oven for drying treatment to obtain dry biomass corn leaves;
step two, putting 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;
step three, washing and filtering the obtained white powder to obtain pure white powder, and then carrying out strong stirring on tetrapropylammonium hydroxide, alkali, water and seed crystals to prepare uniform mixed solution;
transferring the obtained mixed solution into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining for crystallization treatment to obtain a crystallized product;
and fifthly, washing the obtained crystallized product by deionized water until the crystallized product is nearly neutral, then placing the crystallized product in a drying box at 3-150 ℃ for drying treatment, placing the dried product in a muffle furnace at 400-700 ℃ for roasting for 4-20 hours, and solidifying the dried product to obtain the Silicalite-1 zeolite molecular sieve.
2. The method for preparing Silicalite-1 molecular sieve from corn leaves according to claim 1, wherein the method comprises the following steps: adding an acidic solution to remove metal ions when soaking biomass corn leaves, washing, and drying the washed biomass corn leaves in sunlight and then carrying out leaf drying treatment; during the drying treatment, biomass corn leaves are placed into a drying oven and kept dry for 4 hours under the ventilation condition of 60 ℃.
3. The method for preparing Silicalite-1 molecular sieve from corn leaves according to claim 1, wherein the method comprises the following steps: in the second step, the biomass corn leaves and the citric acid solution are subjected to azeotropy for 1h, then distilled water is used for flushing for three times, and the steps are repeated for three times.
4. The method for preparing Silicalite-1 molecular sieve from corn leaves according to claim 1, wherein the method comprises the following steps: and in the third step, the seed crystal is Silicalite-1 zeolite molecular sieve ball milling to obtain Silicalite-1 crystals with the particle size of 100-300 nm.
5. The method for preparing Silicalite-1 molecular sieve from corn leaves according to claim 1, wherein the method comprises the following steps: the mixed solution after stirring in the third step is composed of TPAOH and SiO 2 、Na 2 O、H 2 O and seed crystal, wherein TPAOH, siO 2 、Na 2 O、H 2 The molar mass ratio of O to the seed crystal is 0.2:1:0.01-0.1:20-50:0.005-0.05.
6. The method for preparing Silicalite-1 molecular sieve from corn leaves according to 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 the stirring rotation condition, and the pressure of crystallization reaction when water is heated is the pressure of the mixed liquid generated by heating components.
7. Use of a molecular sieve according to any one of claims 1-6 in gas separation, prepared by a process for preparing Silicalite-1 molecular sieve from corn leaves.
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| 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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| 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 |
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