Solid waste synthesis of ssz-16 zeolite molecular sieves and their adsorptive separation applications

Abstract

The application provides a solid waste synthesis SSZ-16 zeolite molecular sieve and adsorption separation application thereof, and relates to the technical field of zeolite molecular sieves. Water, an alkali source, an organic template agent, a silicon source and FCC solid waste are mixed to obtain an initial reaction gel; the initial reaction gel is subjected to hydrothermal crystallization to obtain an initial SSZ-16 zeolite molecular sieve; and the initial SSZ-16 zeolite molecular sieve is calcined to obtain an SSZ-16 zeolite molecular sieve. The application uses the FCC solid waste without any treatment as an aluminum source, additionally supplements a silicon source, an organic template agent and an alkali source, and for the first time utilizes the FCC solid waste to synthesize the SSZ-16 zeolite molecular sieve with an AFX topological structure through a hydrothermal method. Moreover, the synthesized SSZ-16 zeolite molecular sieve has excellent selective adsorption and separation performance of carbon dioxide, and has a broad prospect in application fields such as flue gas carbon dioxide capture and natural gas carbon dioxide removal.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of zeolite molecular sieve, and particularly relates to solid waste synthesis of SSZ-16 zeolite molecular sieve and adsorption separation application thereof. BACKGROUND

[0002] Fluid catalytic cracking (FCC) is the main preparation process of petroleum catalytic cracking. In the catalytic process, the heavy metal poisoning in the FCC catalyst and the high temperature and high pressure reaction conditions lead to the continuous decline of the activity of the FCC catalyst, and ultimately lead to the complete deactivation of the catalyst, so that the catalytic cracking reaction cannot proceed smoothly. The deactivated FCC catalyst is the FCC solid waste (FCC solid waste for short). The FCC catalyst accounts for about one-third of the global refinery catalyst market share. It is estimated that by 2025, 5.8 billion US dollars will be invested in the FCC catalyst. At present, the amount of FCC catalyst consumed in China each year is more than 200,000 tons. However, with the increasing demand for FCC catalysts around the world, the amount of deactivated FCC solid waste is also increasing. People often use landfill to dispose of FCC solid waste. However, FCC solid waste contains a large amount of toxic heavy metals such as V and Ni, which are very easy to leach into the soil and water resources by rainwater, posing a serious threat to the surrounding environment. In 2016, China published the latest National Hazardous Waste List, which classified FCC solid waste as HW50 hazardous waste. Therefore, developing a technology to recycle FCC solid waste not only protects the environment, but also to some extent reduces the economic losses caused by the deactivation of FCC catalysts.

[0003] There have been reports that FCC solid waste can be used as a raw material for preparing zeolite molecular sieve. Yang Zhichao et al. successfully synthesized SBA-15 zeolite molecular sieve with a combination of mesopores and micropores by using FCC solid waste as a single silicon source and aluminum source; Francesco Ferella et al. synthesized a mixture of NaA zeolite and NaX zeolite by using FCC solid waste after acid leaching of rare earth metal ions as a raw material; Zeel Kothari et al. synthesized pure phase FAU zeolite molecular sieve by using FCC solid waste as a raw material through a hydrothermal method. However, no one has reported the synthesis of SSZ-16 zeolite molecular sieve with AFX topology structure using FCC solid waste as a raw material. SUMMARY

[0004] Therefore, the purpose of the present application is to provide solid waste synthesis of SSZ-16 zeolite molecular sieve and adsorption separation application thereof. The present application successfully synthesizes SSZ-16 zeolite molecular sieve with AFX topology structure by using untreated FCC solid waste as an aluminum source through a hydrothermal method.

[0005] To achieve the above object, the present application provides the following technical solutions.

[0006] The present application provides a method for preparing SSZ-16 zeolite molecular sieve from FCC solid waste, comprising the following steps:

[0007] The water, alkali source, organic template agent, silicon source and FCC solid waste are mixed to obtain an initial reaction gel; the organic template agent is Et6-diquat-n dibromide and / or DABCO2-diquat-m dibromide, wherein n = 2-10, m = 2-10, and m and n are integers; the amounts of the water, alkali source, organic template agent, silicon source and FCC solid waste are such that the initial reaction gel satisfies the following molar ratio: organic template agent, SiO2, Al2O3, OH - and water = (0.1-10) :(5-100) :1:(3-40):(500-2000);

[0008] The initial reaction gel is subjected to hydrothermal crystallization to obtain an initial SSZ-16 zeolite molecular sieve;

[0009] The initial SSZ-16 zeolite molecular sieve is calcined to obtain the SSZ-16 zeolite molecular sieve.

[0010] Preferably, the FCC solid waste comprises the following mass percentage of oxides: Al2O3 40%-47%, SiO2 40%-43%, Na2O 0.90%-1.00%, Fe2O3 2.00%-2.50%, rare earth metal oxide 7%-10% and P2O5 2.6%-4%.

[0011] Preferably, the silicon source is one or more of silicic acid, water glass, silica sol, tetraethyl orthosilicate, sodium silicate and white carbon black.

[0012] Preferably, the alkali source is one or more of LiOH, NaOH, KOH and CsOH.

[0013] Preferably, the temperature of the hydrothermal crystallization is 100-250℃, and the time is 1-15d.

[0014] Preferably, the hydrothermal crystallization is static hydrothermal crystallization or dynamic hydrothermal crystallization, and the rotation speed of the dynamic hydrothermal crystallization is 5-100rpm.

[0015] Preferably, the temperature of the calcination is 400-800℃, and the time is 3-10h.

[0016] The present application provides the SSZ-16 zeolite molecular sieve prepared by the preparation method described above.

[0017] The application provides application of the SSZ-16 zeolite molecular sieve in selective adsorption and separation of carbon dioxide in a mixed gas.

[0018] Preferably, the mixed gas further comprises nitrogen.

[0019] The application provides a method for preparing SSZ-16 zeolite molecular sieve from FCC solid waste, comprising the following steps: mixing water, an alkali source, an organic template agent, a silicon source and FCC solid waste to obtain an initial reaction gel; the organic template agent is Et6-diquat-n dibromide and / or DABCO2-diquat-m dibromide, wherein n = 2-10, m = 2-10, and m and n are integers; the amount of the water, the alkali source, the organic template agent, the silicon source and the FCC solid waste satisfies the following molar ratio of the initial reaction gel: organic template agent, SiO2, Al2O3, OH - and water = (0.1-10) :(5-100) :1 :(3-40) :(500-2000); subjecting the initial reaction gel to hydrothermal crystallization to obtain an initial SSZ-16 zeolite molecular sieve; and subjecting the initial SSZ-16 zeolite molecular sieve to calcination to obtain the SSZ-16 zeolite molecular sieve. The application uses FCC solid waste without any treatment as an aluminum source, additionally supplements a silicon source, an organic template agent and an alkali source, and for the first time utilizes the FCC solid waste to synthesize SSZ-16 zeolite molecular sieve with AFX topology through a hydrothermal method. Moreover, the synthesized SSZ-16 zeolite molecular sieve has very high carbon dioxide selective adsorption and separation performance, has a broad prospect in application fields such as flue gas carbon dioxide capture and natural gas carbon dioxide removal, and realizes resource utilization of FCC solid waste. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 XRD patterns of S1, S2 and S3 samples prepared in Examples 1, 2 and 3 and SSZ-13 zeolite molecular sieve prepared in Comparative Example 1;

[0021] Figure 2 SEM patterns of S1, S2 and S3 samples prepared in Examples 1, 2 and 3 and SSZ-13 zeolite molecular sieve prepared in Comparative Example 1, Figure 2 (a)-(d) in the figure correspond to Example 1, Example 2, Example 3 and Comparative Example 1 in sequence;

[0022] Figure 3 CO2 and N2 adsorption isotherms of S1, S2 and S3 samples prepared in Examples 1, 2 and 3 and SSZ-13 zeolite molecular sieve prepared in Comparative Example 1 at 298 K. DETAILED DESCRIPTION

[0023] The application provides a method for preparing SSZ-16 zeolite molecular sieve from FCC solid waste, comprising the following steps:

[0024] water, an alkali source, an organic template agent, a silicon source and FCC solid waste are mixed to obtain an initial reaction gel; the organic template agent is Et6-diquat-n dibromide and / or DABCO2-diquat-m dibromide, wherein n = 2-10, m = 2-10, and m and n are integers; the water, the alkali source, the organic template agent, the silicon source and the FCC solid waste are in an amount such that the initial reaction gel satisfies the following molar ratio: organic template agent, SiO2, Al2O3, OH - and water = (0.1-10) :(5-100) :1 :(3-40) :(500-2000) ;

[0025] The initial reaction gel is subjected to hydrothermal crystallization to obtain an initial SSZ-16 zeolite molecular sieve;

[0026] The initial SSZ-16 zeolite molecular sieve is calcined to obtain the SSZ-16 zeolite molecular sieve.

[0027] In the application, the raw materials involved are all commercially available products well known in the art, unless otherwise specified.

[0028] The present application mixes water, alkali source, organic template agent, silicon source and FCC solid waste to obtain an initial reaction gel. In the present application, the FCC solid waste (i.e. deactivated FCC catalyst) is used as the total aluminum source, and no additional aluminum source is needed in the present application. In the present application, the FCC solid waste (characterized by ICP) preferably comprises the following mass percentage of oxides: Al2O3 40% to 47%, SiO2 40% to 43%, Na2O 0.90% to 1.00%, Fe2O3 2.00% to 2.50%, rare earth metal oxides 7% to 10%, and P2O5 2.6% to 4%; in the embodiments of the present application, the FCC solid waste specifically comprises the following mass percentage of oxides: Al2O3 44.71%, SiO2 40.57%, Na2O 0.97%, Fe2O3 2.05%, rare earth metal oxides 7.7%, and P2O5 4%. In the present application, the FCC solid waste does not need to be treated. In the present application, the water is preferably deionized water; and the alkali source is preferably one or more of LiOH, NaOH, KOH and CsOH. In the present application, the silicon source is preferably one or more of silicic acid, water glass, silica sol, tetraethyl orthosilicate, sodium silicate and white carbon black; the content of silicon dioxide in the water glass is preferably 10 to 40 wt%, more preferably 15 wt%; and the silica sol is preferably ammonium-type silica sol (silicon content 40 wt%, AS-40) or sodium-type silica sol (silicon content 40 wt%, HS-40).

[0029] In the present application, the organic template agent is Et6-diquat-n dibromide and / or DABCO2-diquat-m dibromide, wherein n = 2 to 10, m = 2 to 10, and both m and n are integers; in the embodiments of the present application, the n is preferably 4, and the m is preferably 4. The present application does not have special requirements for the source of the template agent, and a commercially available product or a preparation method well known to those skilled in the art can be used.

[0030] In the present application, when the template agent is Et6-diquat-n dibromide, the template agent is preferably prepared by the following method:

[0031] Triethylamine, 1, n-dibromo-n-alkane (n = 2 to 10, corresponding to the Chinese names ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, and decyl) and methanol are mixed in a molar ratio of 2:1:3, stirred at room temperature for 24 hours, washed with diethyl ether after the reaction is completed, and dried in a 50°C oven for 12 hours to obtain the organic template agent Et6-diquat-n dibromide (1, n-n-alkane dibromide, abbreviated as Et6-diquat-n, the structure is shown in formula I, n = 2 to 10, corresponding to the Chinese names ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, and decyl).

[0032] In the present application, when the template agent is DABCO2-diquat-m dibromide, the template agent is preferably prepared by the following method:

[0033] 1,4-diazidobicyclo[2.2.2]octane (DABCO) and 1, m-dibromo-n-malkane (m = 2-10, corresponding to the Chinese name of ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl) and methanol are mixed in a molar ratio of 2:1:3, stirred at room temperature for 24 hours, and after the reaction is completed, the solid product is washed with diethyl ether and placed in a 50°C oven for drying for 12 hours to obtain the organic template agent DABCO2-diquat-m dibromide (1, m-bis (1, 4-diazidobicyclo[2.2.2]octane) malkane dibromide, abbreviated as DABCO2-diquat-m, the structure shown in formula II, m = 2-10, corresponding to the Chinese name of ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl).

[0034]

[0035] In the present application, the amounts of water, alkali source, organic template agent, silicon source and FCC solid waste make the initial reaction gel satisfy the following molar ratio: organic template agent, SiO2, Al2O3, OH - and water = (0.1-10):(5-100):1:(3-40):(500-2000), preferably (2-8):(15-87):1:(16-40):(600-1700), more preferably (3-6):(20-78):1:(20-35):(600-1000). In the calculation of the molar ratio of the initial reaction gel, the silicon source and the alkali source are respectively converted into SiO2 and OH - , and the FCC solid waste is converted into Al2O3 and SiO2.

[0036] In the present application, the mixing method preferably comprises the following steps: adding water, alkali source and organic template agent into a beaker in sequence, stirring for 10 min to form a transparent solution; then adding the silicon source into the beaker and stirring until the silicon source is completely dissolved, and then adding the FCC solid waste into the beaker and stirring for 6 h.

[0037] After obtaining the initial reaction gel, the initial reaction gel is hydrothermally crystallized to obtain the initial SSZ-16 zeolite molecular sieve. In the present application, the temperature of the hydrothermal crystallization is preferably 100-250°C, more preferably 140-210°C, and further preferably 150-180°C, and the time of the hydrothermal crystallization is preferably 1-15 days, more preferably 1-13 days, and further preferably 3-10 days. In the present application, the hydrothermal crystallization is preferably carried out in a high-pressure reaction kettle; the hydrothermal crystallization is preferably static hydrothermal crystallization or dynamic hydrothermal crystallization, and the rotation speed of the dynamic hydrothermal crystallization is preferably 5-100 rpm, more preferably 10-60 rpm, and further preferably 30-50 rpm.

[0038] After the hydrothermal crystallization, the obtained system is preferably subjected to solid-liquid separation, and the obtained solid material is washed and dried to obtain the initial SSZ-16 zeolite molecular sieve. The present application does not have special limitations on the solid-liquid separation method, and a solid-liquid separation method well known in the art can be used, such as suction filtration or centrifugal separation. In the present application, the washing is preferably water washing, which is preferably carried out multiple times until the washing liquid is neutral. The present application does not have special limitations on the drying method, and a drying method well known to those skilled in the art can be used; in the embodiments of the present application, the drying method is preferably oven drying, the temperature of the oven drying is preferably 50-150°C, more preferably 70-130°C, and further preferably 80°C, and the time of the oven drying is preferably 12 h.

[0039] After obtaining the initial SSZ-16 zeolite molecular sieve, the initial SSZ-16 zeolite molecular sieve is calcined to obtain the SSZ-16 zeolite molecular sieve. In the present application, the temperature of the calcination is preferably 400-800°C, more preferably 550-700°C, and the time of the calcination is preferably 3-10 h, more preferably 6-8 h; the calcination can be carried out in an air atmosphere. The organic template is removed by the calcination.

[0040] The present application provides the SSZ-16 zeolite molecular sieve prepared by the preparation method described in the above technical solution.

[0041] The present application provides the application of the SSZ-16 zeolite molecular sieve described in the above technical solution in the selective adsorption and separation of carbon dioxide in a mixed gas, i.e., the SSZ-16 zeolite molecular sieve as a selective adsorbent for carbon dioxide. In the present application, the mixed gas also preferably includes nitrogen, and in the embodiments of the present application, the SSZ-16 zeolite molecular sieve is used as a selective adsorbent for carbon dioxide in a carbon dioxide and nitrogen mixed gas (CO2-N2).

[0042] Preferably, the SSZ-16 zeolite molecular sieve is activated before the application; the activation is particularly to activate the SSZ-16 zeolite molecular sieve under the condition of vacuum and 200-450°C. The present application does not have special limitation to the vacuum degree of the vacuum, and the vacuum degree well known in the art can be adopted; the time of the activation treatment is preferably 8-12h.

[0043] In order to further illustrate the present application, the solid waste for synthesizing SSZ-16 zeolite molecular sieve and its adsorption separation application provided by the present application are described in detail below in combination with examples, but they cannot be understood as limiting the protection scope of the present application.

[0044] The composition of the FCC solid waste used in each example (ICP test) is shown in Table 1:

[0045] Table 1 Composition of the FCC solid waste used in each example

[0046] FCC solid waste Al2O3 SiO2 Na2O Fe2O3 Rare earth oxides P2O5 <!-- 4 -->]] Mass fraction 44.71％ 40.57％ 0.97％ 2.05％ 7.70％ 4.0％

[0047] Example 1

[0048] The SSZ-16 zeolite molecular sieve is prepared from the FCC solid waste, and the method is as follows:

[0049] 1,4-diazidobicyclo[2.2.2]octane (DABCO) is mixed with 1,4-dibromobutane and methanol according to the molar ratio of 2:1:3, stirred at room temperature for 24 hours, and after the reaction is completed, the solid product is washed with diethyl ether, and after drying in a 50°C oven for 12 hours, the organic template DABCO2-diquat-4 dibromide (1,4-bis(1,4-diazidobicyclo[2.2.2]octane) butane dibromide, referred to as DABCO2-diquat-4) is obtained.

[0050] An electronic balance is used to weigh 27.63g of deionized water, 2.186g of sodium hydroxide, 3.859g of the organic template DABCO2-diquat-4, and sequentially added into a plastic beaker, and after stirring for 10 minutes, a transparent solution is formed; 4.873g of silicic acid is further added into the beaker, and stirred for 12 hours until the silicon source is completely dissolved; 0.5g of FCC solid waste (converted to Al2O3 and SiO2) is further added into the beaker, and stirred for 6 hours; finally, the gel in the plastic beaker is transferred into a reaction kettle, and placed into a 150°C rotary oven for hydrothermal crystallization for 3 days, with a rotation speed of 50rmp. After the hydrothermal treatment is completed, the washed product is dried in an oven after washing with deionized water until the washing liquid is neutral. Finally, it is placed in a muffle furnace and calcined at 550°C for 6 hours, and the final product is recorded as S1 sample.

[0051] The XRD pattern of the S1 sample obtained in Example 1 is as follows: Figure 1The XRD characterization shows that the sample S1 is SSZ-16 zeolite. Figure 1 The XRD characterization shows that the sample S1 is SSZ-16 zeolite.

[0052] The SEM image of the sample S1 obtained in Example 1 is shown in Fig. 1(a). Figure 2 The SEM image of the sample S1 obtained in Example 1 is shown in Fig. 1(a). Figure 2 The SEM image of the sample S1 obtained in Example 1 is shown in Fig. 1(a).

[0053] Example 2

[0054] The SSZ-16 zeolite was prepared from FCC solid waste as follows:

[0055] The SSZ-16 zeolite was prepared from FCC solid waste as follows:

[0056] The XRD characterization shows that the sample S1 is SSZ-16 zeolite. Figure 1 The XRD characterization shows that the sample S1 is SSZ-16 zeolite. Figure 1 The XRD characterization shows that the sample S1 is SSZ-16 zeolite.

[0057] The SEM image of the sample S2 obtained in Example 2 is shown in Fig. 2(b). Figure 2 The SEM image of the sample S2 obtained in Example 2 is shown in Fig. 2(b). Figure 2 The SEM image of the sample S2 obtained in Example 2 is shown in Fig. 2(b).

[0058] Example 3

[0059] The SSZ-16 zeolite was prepared from FCC solid waste as follows:

[0060] Triethylamine was mixed with 1,4-dibromon-butane and methanol in a molar ratio of 2:1:3, stirred at room temperature for 24 hours, and the solid product was washed with ether after the reaction was completed. The organic template Et6-diquat-4 dibromide (1,4-butane ethane dibromide, referred to as Et6-diquat-4) was obtained after drying in a 50°C oven for 12 hours.

[0061] The electronic balance was used to weigh 27.63 grams of deionized water, 2.186 grams of sodium hydroxide, and 3.666 grams of the organic template Et6-diquat-4 dibromide, and sequentially added to a plastic beaker. After stirring for 10 minutes, a transparent solution was formed. Then 3.749 grams of white carbon black was added to the beaker, and stirred for 12 hours until the silicon source was completely dissolved. Then 0.5 grams of FCC solid waste was added to the beaker, and stirred for 6 hours. Finally, the gel in the plastic beaker was transferred to a reaction kettle, and placed in a 150°C rotary oven for hydrothermal crystallization for 3 days at a rotation speed of 50 rpm. After hydrothermal treatment, the product was washed with deionized water until the washing liquid was neutral. The washed product was dried in an oven, and finally calcined in a muffle furnace at 550°C for 6 hours. The final product is recorded as the S3 sample.

[0062] The XRD pattern of the S3 sample obtained in Example 3 is shown in Figure 1 Fig. 1(c). Figure 1 The characterization by XRD showed that the SSZ-16 zeolite molecular sieve was successfully synthesized in Example 3 with white carbon black as a supplementary silicon source and Et6-diquat-4 dibromide as an organic template.

[0063] The SEM pattern of the S3 sample obtained in Example 3 is shown in Figure 2 Fig. 1(c). Figure 2 Fig. 1(c) shows that the sample still mainly exists in the form of spindle.

[0064] Comparative Example 1

[0065] The electronic balance was used to weigh 6.89 grams of deionized water, 1.2 grams of sodium hydroxide (alkali source), and 4.50 grams of N,N,N-trimethyl-1-adamantylammonium hydroxide aqueous solution (25wt%, organic template) and sequentially added to a plastic beaker. After stirring for 10 minutes, a transparent solution was formed. Then 2 grams of white carbon black (silicon source) was added to the beaker, and stirred for 24 hours until the silicon source was completely dissolved. Then 0.7 grams of FCC solid waste was added to the beaker, and stirred for 6 hours. The silicon source and alkali source were respectively calculated as SiO2 and OH - The silicon source and alkali source were respectively calculated as SiO2 and OH -The molar ratio of water to the product was 1.73:12.4:1:5.6:186. The gel in the plastic beaker was then transferred to a reaction vessel and placed in a static oven at 140°C for hydrothermal crystallization for 5 days. After hydrothermal treatment, the product was washed with deionized water until the washing solution was neutral. The washed product was then dried in an oven and finally calcined in a muffle furnace at 550°C for 6 hours.

[0066] The XRD pattern of the zeolite molecular sieve product obtained in Comparative Example 1 is shown below. Figure 1 As shown, via Figure 1 XRD characterization showed that Comparative Example 1 synthesized SSZ-13 zeolite molecular sieve.

[0067] The SEM image of the zeolite molecular sieve product obtained in Comparative Example 1 is shown below. Figure 2 As shown in (d). Figure 2 (d) indicates that the sample has a cubic morphology.

[0068] Application examples

[0069] The SSZ-16 zeolite molecular sieves prepared in Examples 1-3 and the SSZ-13 zeolite molecular sieve prepared in Comparative Example 1 were subjected to gas selective adsorption and separation tests. The samples, after calcination to remove the organic template agent, were activated under vacuum at 350°C for 10 hours. After cooling to room temperature, single-component gas isothermal adsorption-desorption tests were performed at a temperature of 298 K and a pressure of 0 to 1 bar.

[0070] Figure 3 The CO2 and N2 adsorption isotherms at 298 K are shown for the SSZ-16 zeolite molecular sieves prepared in Examples 1-3 and the SSZ-13 zeolite molecular sieve prepared in Comparative Example 1. The CO2 / N2 adsorption and separation performance of the SSZ-16 zeolite molecular sieves prepared in Examples 1-3 and the SSZ-13 zeolite molecular sieve prepared in Comparative Example 1 are listed in Table 2.

[0071] Table 2. Adsorption and separation performance of CO2 / N2 by zeolite molecular sieves

[0072]

[0073] From Table 2 and Figure 3As shown, the SSZ-16 zeolite molecular sieve prepared by taking FCC solid waste as an aluminum source, taking silicic acid or white carbon black as a silicon source, and taking DABCO2-diquat-4 as an organic template has a more excellent CO2 / N2 gas adsorption separation performance than the SSZ-13 zeolite molecular sieve prepared by taking FCC solid waste, and has a very high selective adsorption performance on carbon dioxide. However, the S3 sample prepared by taking FCC solid waste as an aluminum source, taking white carbon black as a silicon source, and taking Et6-diquat-4 dibromide as an organic template is slightly worse than the S2 sample prepared by taking FCC solid waste as an aluminum source, taking white carbon black as a silicon source, and taking DABCO2-diquat-4 as an organic template in terms of the CO2 / N2 gas adsorption separation performance.

[0074] The above description is only the preferred embodiments of the present application, and does not limit the present application in any form. It should be noted that, for ordinary skilled persons in the art, some improvements and refinements can be made without departing from the principles of the present application, and these improvements and refinements should also be considered as the protection scope of the present application.

Claims

1. A method for the preparation of SSZ-16 zeolite molecular sieve from FCC solid waste, characterized in that, The method comprises the following steps: Mixing water, alkali source, organic template agent, silicon source and FCC solid waste to obtain an initial reaction gel; the organic template agent is Et6-diquat-n dibromide and / or DABCO2-diquat-m dibromide, wherein n=2~10, m=2~10, and m and n are integers; the amount of water, alkali source, organic template agent, silicon source and FCC solid waste is such that the initial reaction gel satisfies the following molar ratio: organic template agent, SiO2, Al2O3, OH - and water=(0.1~10):(5~100):1:(3~40):(500~2000); The initial reaction gel is subjected to hydrothermal crystallization to obtain an initial SSZ-16 zeolite molecular sieve; the hydrothermal crystallization is performed at a temperature of 100-250 DEG C for 1-3 days; The initial SSZ-16 zeolite molecular sieve is calcined to obtain the SSZ-16 zeolite molecular sieve.

2. The method of claim 1, wherein, The FCC solid waste contains the following oxides in mass percentage: Al2O3 40-47%, SiO2 40-43%, Na2O 0.90-1.00%, Fe2O3 2.00-2.50%, rare earth metal oxide 7-10%, and P2O5 2.6-4%.

3. The method of claim 1, wherein, The silicon source is one or more of silicic acid, water glass, silica sol, tetraethyl orthosilicate, sodium silicate, and white carbon black.

4. The method of claim 1, wherein, The alkali source is one or more of LiOH, NaOH, KOH, and CsOH.

5. The method of claim 1, wherein, The hydrothermal crystallization is static hydrothermal crystallization or dynamic hydrothermal crystallization, and the rotation speed of the dynamic hydrothermal crystallization is 5-100 rpm.

6. The method of claim 1, wherein, The calcination is performed at a temperature of 400-800 DEG C for 3-10 h.

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