CN104709917A - Method for synthesizing SSZ-13 molecular sieve through solid-phase grinding - Google Patents
Method for synthesizing SSZ-13 molecular sieve through solid-phase grinding Download PDFInfo
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Abstract
The invention relates to the field of molecular sieve preparation, and aims to provide a method for synthesizing an SSZ-13 molecular sieve through solid-phase grinding. The method for synthesizing the SSZ-13 molecular sieve through solid-phase grinding comprises the following steps: weighing a silicon source, an aluminum source, an alkali source and a template agent for crystallization reaction so as to obtain a crystallization reaction product after the reaction is completed, cooling and washing till being neutral, drying to obtain crude molecular sieve powder, and roasting the crude molecular sieve powder for 5 hours in air of 550 DEG C, thereby obtaining a final product SSZ-13 molecular sieve. The SSZ-13 molecular sieve with relatively good crystallinity degree is synthesized through solid-phase raw material grinding under a solvent-free condition, so that the use of solvent water is reduced to the maximum extent, the synthesis route only involves mixing synthesis steps of primary raw materials, the method is greatly simplified when being compared with a conventional method, the yield and the utilization rate of a single kettle are both relatively increased, the production cost is greatly lowered, the pollution to the environment is greatly reduced, and great industrial application prospect can be achieved.
Description
Technical field
The invention relates to the preparation field of molecular sieve, particularly a kind of method by solid-phase grinding synthesis SSZ-13 molecular sieve.
Background technology
Molecular sieve, due to features such as good shape selectivity, higher thermostability and the chemical stabilities in its regular structure, the adjustable sex change of skeleton composition, very high surface-area and loading capacity, positively charged ion interchangeability, duct, has now been widely used in catalysis industrial circle.A kind of new molecular sieve SSZ-13 of water heat transfer is passed through by Americanized scholar Zones S I.SSZ-13 has good thermostability, can be used as the carrier of sorbent material or catalyzer, such as air purifying preparation, auto-exhaust catalyst etc.SSZ-13 also has cationic exchange and acid adjustability simultaneously, thus to kinds of reaction, there is good catalytic performance, comprise the reaction of preparing light olefins from methanol (MTO), alkene and aromatic hydrocarbons structure, the catalytic cracking of hydrocarbon compound and hydrocracking etc.
The most frequently used method of current synthesis SSZ-13 molecular sieve is hydrothermal synthesis method, adopts N, N, N-trimethylammonium-1-adamantyl ammonium hydroxide to be template.The shortcoming of the method is that preparation process causes the waste of a large amount of solvent, and template synthesis step is complicated, expensive.On the other hand, solvent can cause still inner high voltage in heat-processed, and product yield is lower.
Summary of the invention
Main purpose of the present invention is to overcome deficiency of the prior art, provides a kind of novel method that can reduce production cost, reduce the synthesis SSZ-13 molecular sieve of waste discharge.For solving the problems of the technologies described above, solution of the present invention is:
A kind of method by solid-phase grinding synthesis SSZ-13 molecular sieve is provided, specifically comprises the steps:
(1) take silicon source, aluminium source, alkali source, template carry out ground and mixed, load in reactor after grinding evenly and carries out crystallization, the temperature of reaction of crystallization is 160 ~ 200 DEG C, and the reaction times is 3 ~ 10d;
Described silicon source is nine water water glass, solid silicone or white carbon black; Described aluminium source is aluminum sulfate octadecahydrate or sodium metaaluminate; Described alkali source is sodium hydroxide or nine water water glass (wherein nine water water glass both also existed as alkali source as silicon source); Described template is N, N-dimethyl-N'-ethylcyclohexyl brometo de amonio or N, N-dimethyl-N'-ethylcyclohexyl ammonium iodide; And when ensureing crystallization, Component molar proportioning meets, SiO
2: Al
2o
3: Na
2o: H
2o: R is 1:0.03 ~ 0.041:0.17 ~ 0.215:2.31:0.09 ~ 0.5 (H
2o comes from aquo compound, without the need to additionally adding water), wherein R refers to template;
(2) crystallization obtains crystallization product after completing, and at room temperature cools crystallization product, then uses deionized water wash crystallization product to neutral, at 100 DEG C of air dryings, obtains molecular screen primary powder;
(3) molecular screen primary powder will obtained in step (2), roasting 5 hours in 550 DEG C of air, namely obtains the finished product SSZ-13 molecular sieve.
In the present invention, described for the N as template, N-dimethyl-N'-ethylcyclohexyl brometo de amonio, concrete preparation method is: according to monobromethane and N, the mol ratio of N-dimethylcyclohexylamine is 0.5 ~ 5.0: 1, takes monobromethane and N, N-dimethylcyclohexylamine and dissolves in ethanol, then reflux in the temperature of 80 DEG C, stirring reaction 12h ~ 24h; After reaction terminates, in reaction product, add ether, produce white solid precipitation, by precipitation after filtration, obtain required template after drying treatment, be N, N-dimethyl-N'-ethylcyclohexyl brometo de amonio;
The monobromethane added in described preparation method replaces with iodoethane, then prepare for the N as template, N-dimethyl-N'-ethylcyclohexyl ammonium iodide.
Compared with prior art, the invention has the beneficial effects as follows:
1, the present invention is by the good SSZ-13 molecular sieve of synthetic crystallization degree under Solid raw materials grinding condition of no solvent, reduces the use of aqueous solvent to greatest extent; Present invention employs the N that price is lower, N-dimethyl-N'-ethylcyclohexyl brometo de amonio or N, N-dimethyl-N'-ethylcyclohexyl ammonium iodide, not only simplify SSZ-13 Zeolite synthesis step, and greatly reduce production cost, and decrease the discharge of refuse.
2, synthetic route of the present invention only relates to the mixing synthesis step of primary raw materials, and comparatively traditional method simplifies greatly, and productive rate and single still utilization ratio are all enhanced; Present invention greatly reduces production cost and the pollution to environment, have huge prospects for commercial application.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of product in the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of product in the present invention.
Fig. 3 is the scanning electron microscope (SEM) photograph of product in the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail:
The following examples can make professional and technical personnel's comprehend the present invention of this specialty, but do not limit the present invention in any way.
The preparation of embodiment 1 template
According to monobromethane and N, the mol ratio of N-dimethylcyclohexylamine is 2.6: 1, take 11.8g monobromethane and 5gN, N-dimethylcyclohexylamine is dissolved in 10ml ethanol, set temperature is 80 DEG C and refluxes, and stirs 12h, after reaction terminates, in reaction product, add the white solid precipitation that ether produces, after filtration, dry etc. obtain required template.
The preparation of embodiment 2 template
According to monobromethane and N, the mol ratio of N-dimethylcyclohexylamine is 0.5: 1, take 2.15g monobromethane and 5gN, N-dimethylcyclohexylamine is dissolved in 20ml ethanol, set temperature is 80 DEG C and refluxes, and stirs 18h, after reaction terminates, in reaction product, add the white solid precipitation that ether produces, after filtration, dry etc. obtain required template.
The preparation of embodiment 3 template
According to monobromethane and N, the mol ratio of N-dimethylcyclohexylamine is 5: 1, claim 21.5g monobromethane and 5gN, N-dimethylcyclohexylamine is dissolved in 20ml ethanol, set temperature is 80 DEG C and refluxes, and stirs 24h, after reaction terminates, in reaction product, add the white solid precipitation that ether produces, after filtration, dry etc. obtain required template.
In embodiment 1 to embodiment 3, monobromethane is replaced to the iodoethane of equimolar amount, carry out same operant response with N, N-dimethylcyclohexylamine, the N as template can be obtained, N-dimethyl-N'-ethylcyclohexyl ammonium iodide.
The preparation of embodiment 4 SSZ-13 sample
First by solid material: 1.50g Na
2siO
39H
2o, 0.61g Al
2(SO
4)
318H
2o, 1.35g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.03: 0.19: 2.31: 0.15.
Fig. 1 is the XRD characterization result of product, and product is typical SSZ-13 structure, and has good degree of crystallinity.
Fig. 2, Fig. 3 are the stereoscan photograph of product.
The preparation of embodiment 5 SSZ-13 sample
First by solid material: 1.50g Na
2siO
39H
2o, 0.61g Al
2(SO
4)
318H
2o, 1.35g white carbon black and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.03: 0.19: 2.31: 0.15.
The preparation of embodiment 6 SSZ-13 sample
First by solid material: 1.50g Na
2siO
39H
2o, 0.76g Al
2(SO
4)
318H
2o, 1.35g white carbon black and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.041: 0.19: 2.31: 0.15.
The preparation of embodiment 7 SSZ-13 sample
First by solid material: 1.50g Na
2siO
39H
2o, 0.187g sodium metaaluminate, mortar is poured into, ground and mixed 5 ~ 10min after 1.35g solid silicone and 1.00gN, N-dimethyl-N'-ethylcyclohexyl brometo de amonio weigh, load after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, with deionized water wash to neutral, after 100 DEG C of air dryings, obtain molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.03: 0.205: 2.31: 0.15.
The preparation of embodiment 8 SSZ-13 sample
First by solid material: 1.67g solid silicone, 0.61g Al
2(SO
4)
318H
2o, 0.044g sodium hydroxide and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.03: 0.215: 2.31: 0.15.
The preparation of embodiment 9 SSZ-13 sample
First by solid material: 1.70g Na
2siO
39H
2o, 0.65g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.035: 0.215: 2.31: 0.15.
The preparation of embodiment 10 SSZ-13 sample
First by solid material: 1.70g Na
2siO
39H
2o, 0.67g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.036: 0.215: 2.31: 0.15.
The preparation of embodiment 11 SSZ-13 sample
First by solid material: 1.70g Na
2siO
39H
2o, 0.70g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.038: 0.215: 2.31: 0.15.
The preparation of embodiment 12 SSZ-13 sample
First by solid material: 1.70g Na
2siO
39H
2o, 0.73g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.039: 0.215: 2.31: 0.15.
The preparation of embodiment 13 SSZ-13 sample
First by solid material: 1.70g Na
2siO
39H
2o, 0.76g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.041: 0.215: 2.31: 0.15.
The preparation of embodiment 14 SSZ-13 sample
First by solid material: 1.70g Na
2siO
39H
2o, 0.65g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.035: 0.215: 2.31: 0.15.
The preparation of embodiment 15 SSZ-13 sample
First by solid material: 1.58g Na
2siO
39H
2o, 0.65g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.035: 0.20: 2.31: 0.15.
The preparation of embodiment 16 SSZ-13 sample
First by solid material: 1.50g Na
2siO
39H
2o, 0.65g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 200 DEG C of crystallization 3d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.035: 0.19: 2.31: 0.15.
The preparation of embodiment 17 SSZ-13 sample
First by solid material: 1.42g Na
2siO
39H
2o, 0.65g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 160 DEG C of crystallization 10d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.035: 0.18: 2.31: 0.15.
The preparation of embodiment 18 SSZ-13 sample
First by solid material: 1.34g Na
2siO
39H
2o, 0.65g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 1.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.035: 0.17: 2.31: 0.15.
The preparation of embodiment 19 SSZ-13 sample
First by solid material: 1.58g Na
2siO
39H
2o, 0.65g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 3.33g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.035: 0.20: 2.31: 0.5.
The preparation of embodiment 20 SSZ-13 sample
First by solid material: 1.58g Na
2siO
39H
2o, 0.65g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 0.6g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl brometo de amonio weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 5d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.035: 0.20: 2.31: 0.09.
The preparation of embodiment 21 SSZ-13 sample
First by solid material: 1.58g Na
2siO
39H
2o, 0.65g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 7.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl ammonium iodide weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 3d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.035: 0.20: 2.31: 0.11.
The preparation of embodiment 22 SSZ-13 sample
First by solid material: 1.58g Na
2siO
39H
2o, 0.65g Al
2(SO
4)
318H
2o, 1.31g solid silicone and 14.00g N, mortar is poured into after N-dimethyl-N'-ethylcyclohexyl ammonium iodide weighs, ground and mixed 5 ~ 10min, loads after grinding evenly in reactor, in 180 DEG C of crystallization 10d, after crystallization completes, room temperature cools, and with deionized water wash to neutral, after 100 DEG C of air dryings, obtains molecular sieve powder.By molecular screen primary powder roasting 5 hours in 550 DEG C of air, obtain the finished product.The stoicheiometry of this system is as follows: SiO
2: Al
2o
3: Na
2o: H
2o: R is 1: 0.035: 0.20: 2.31: 0.21.
The above, it is only several case study on implementation of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with better case study on implementation, but and be not used to limit the present invention, any those skilled in the art, are not departing within the scope of technical solution of the present invention, when the structure and technology contents that can utilize above-mentioned announcement are made a little change or be modified to the equivalent case study on implementation of equivalent variations.But every content not departing from technical solution of the present invention, any simple modification done above case study on implementation according to technical spirit of the present invention, equivalent variations and modification, all still belong within the scope of technical solution of the present invention.
Claims (2)
1., by a method for solid-phase grinding synthesis SSZ-13 molecular sieve, it is characterized in that, specifically comprise the steps:
(1) take silicon source, aluminium source, alkali source, template carry out ground and mixed, load in reactor after grinding evenly and carries out crystallization, the temperature of reaction of crystallization is 160 ~ 200 DEG C, and the reaction times is 3 ~ 10d;
Described silicon source is nine water water glass, solid silicone or white carbon black; Described aluminium source is aluminum sulfate octadecahydrate or sodium metaaluminate; Described alkali source is sodium hydroxide or nine water water glass; Described template is N, N-dimethyl-N'-ethylcyclohexyl brometo de amonio or N, N-dimethyl-N'-ethylcyclohexyl ammonium iodide; And when ensureing crystallization, Component molar proportioning meets, SiO
2: Al
2o
3: Na
2o: H
2o: R is 1:0.03 ~ 0.041:0.17 ~ 0.215:2.31:0.09 ~ 0.5, and wherein R refers to template;
(2) crystallization obtains crystallization product after completing, and at room temperature cools crystallization product, then uses deionized water wash crystallization product to neutral, at 100 DEG C of air dryings, obtains molecular screen primary powder;
(3) molecular screen primary powder will obtained in step (2), roasting 5 hours in 550 DEG C of air, namely obtains the finished product SSZ-13 molecular sieve.
2. a kind of method by solid-phase grinding synthesis SSZ-13 molecular sieve according to claim 1, it is characterized in that, described for the N as template, N-dimethyl-N'-ethylcyclohexyl brometo de amonio, concrete preparation method is: be 0.5 ~ 5.0: 1 according to the mol ratio of monobromethane and N, N-dimethylcyclohexylamine, take monobromethane and N, N-dimethylcyclohexylamine dissolves in ethanol, then refluxes in the temperature of 80 DEG C, stirring reaction 12h ~ 24h; After reaction terminates, in reaction product, add ether, produce white solid precipitation, by precipitation after filtration, obtain required template after drying treatment, be N, N-dimethyl-N'-ethylcyclohexyl brometo de amonio;
The monobromethane added in described preparation method replaces with iodoethane, then prepare for the N as template, N-dimethyl-N'-ethylcyclohexyl ammonium iodide.
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| CN107115888A (en) * | 2017-05-27 | 2017-09-01 | 中国科学院生态环境研究中心 | A kind of preparation method and its usage of the catalyst of Cu SSZ 13 |
| CN107640776A (en) * | 2017-08-25 | 2018-01-30 | 中山大学惠州研究院 | A kind of preparation method with micro- meso-hole structure MFI molecular sieves |
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| CN110270368B (en) * | 2018-03-14 | 2020-09-04 | 北京化工大学 | Method for synthesizing carbon-chemical embedded catalyst material by solution-free method |
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| CN110860308B (en) * | 2019-10-18 | 2021-10-01 | 浙江大学 | Method for one-step alkali-free solid-phase synthesis of metal molecular sieve catalyst |
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