CN106745034A - A kind of method of molecular sieves of double template one-step synthesis SSZ 13 and its application - Google Patents
A kind of method of molecular sieves of double template one-step synthesis SSZ 13 and its application Download PDFInfo
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/04—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
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- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
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Abstract
The invention provides a kind of method of the molecular sieves of double template one-step synthesis SSZ 13, this method uses N, and N, N trimethyl adamantane ammonium (TMADa+) and Choline Chloride are used as double template, the molecular sieves of SSZ 13 of high-crystallinity, pure phase, and the Cu in load are obtained2+Afterwards, the selective reduction ability and high hydrothermal stability of excellent NO are shown.The method can be greatly decreased expensive template N, the use of N, N trimethyl adamantane ammonium, so as to reduce the production cost of the molecular sieves of SSZ 13, it is a kind of method that part costliness template is substituted using cheap template, and product can be applied to diesel vehicle post processing (NH3SCR) NO in system catalystxElimination process.
Description
Technical field
The invention belongs to chemical industry and field of Environment Protection, it is related to the preparation of SSZ-13 molecular sieves, it is specifically a kind of to use cheap mould
Plate agent come substitute part costliness template method, to reduce the production cost of SSZ-13 molecular sieves, and product can be applied to bavin
NOx eliminates process in oily car post processing (NH3-SCR) system catalyst.
Background technology
SSZ-13 molecular sieves have chabasie (CHA) structure, and the structure is by double the six of AABBCCAA mode stacked arrangements
Yuan of rings are connected to become a kind of four-membered ring and constitute.It has three-dimensional octatomic ring pore structure, and pore size is 0.38nm × 0.38nm,
It is a kind of small pore molecular sieve.SSZ-13 molecular sieves have excellent hydrothermal stability, specific surface area higher and more surface
Ion-exchange sites (2014.33 (02) .368-373 of synthesis and application progress chemical industry progress of Yang Bo, SSZ-13 molecular sieve), because
This, is widely used in exhaust gas from diesel vehicle treatment (NH3-SCR), methanol-to-olefins (MTO) and CO2Adsorbing separation in.
1985, Zones made public for the first time the synthesis of SSZ-13 molecular sieves, and it utilizes N, N, N- trimethyl adamantane ammonium
(TMADa+) it is template (US NO.4,544,538), the SSZ-13 molecular sieves of high-purity has successfully been synthesized by hydro-thermal method.
But the complicated synthesis step of the template and fancy price, make SSZ-13 molecular sieves production have it is very huge into
This.2006, Miller etc. was template (US NO.60/882) using benzyltrimethylammon.um (BTMA+), adds a small amount of SSZ-
13 crystal seeds have synthesized SSZ-13 molecular sieves.The equally use benzyl group trimethyl ammonium such as Takura (Chemistry Letters,
2008,37 (9)：908-909.) using FAU types molecular sieve as silicon source and silicon source, by the Hydrothermal Synthesiss of certain hour, obtain
SSZ-13 molecular sieves.2011, Zones had also been proposed and substitutes N, N, N- trimethyl using benzyltrimethylammon.um (BTMA+) part
Adamantane ammonium (TMADa+), the double template constituted using BTMA++TMADa+ synthesizes SSZ-13 molecular sieves (US, 8007763B2)
So as to reach the purpose of reduces cost.However, the toxicity of benzyl group trimethyl ammonium still makes it be not widely deployed for SSZ-13
In the production of molecular sieve.2013, Zhang et al. by the use of cheap Choline Chloride as template, with sodium metaaluminate as silicon source,
Ludox is silicon source, successfully synthesized with high-crystallinity SSZ-13 molecular sieves (Environ.Sci.Technol.2014,
48,13909-13916) NO conversion ratios higher and preferable anti-propane and SO, and in NH3-SCR applications are shown2Poisoning
Ability.
The content of the invention
Task of the invention is to provide a kind of method of double template one-step synthesis SSZ-13 molecular sieves.
Another task of the invention is to provide a kind of preparation method and applications of Cu-SSZ-13 molecular sieve catalysts.
Realize the technical scheme is that：
The method of the double template one-step synthesis SSZ-13 molecular sieves that the present invention is provided, comprises the following steps：
(1) will be added in deionized water as the raw material NaOH of sodium source at room temperature, and stirring is completely dissolved to it；
(2) just it is added in above-mentioned solution as the raw material sodium metaaluminate of silicon source, is stirred until homogeneous；
(3) organic formwork agent N, N, N- trimethyl -1- amantadines and Choline Chloride are sequentially added, and it is small to continue stirring 2
When；
(4) add and stirred to forming homogeneous colloidal sol as the raw material Ludox of silicon source；
(5) complete colloidal sol will be stirred to be placed in hydrothermal reaction kettle, crystallization 4-5 days at 165 DEG C；
(6) after colloidal sol being cooled into room temperature, through centrifugal filtration, deionized water washing, dry, calcined at 500~600 DEG C
5 hours, obtain SSZ-13 molecular sieves.
In the method for above-mentioned double template one-step synthesis SSZ-13 molecular sieves, reaction mass sodium source in terms of Na2O, silicon source
In terms of Al2O3, silicon source in terms of SiO2, solvent in terms of H2O, template N, N, N- trimethyl adamantane ammonium is in terms of R1, template chlorine
Change choline in terms of R2, each reaction mass is 0.2~1.0Na2O according to mol ratio:0.2~0.5Al2O3:10SiO2:120~
250H2O:0.1~1.0R1:0.1~1.0R2 is fed intake, and wherein R1 is template N, N, N- trimethyl adamantane ammonium, and R2 is
Template Choline Chloride.
The preparation method of Cu-SSZ-13 molecular sieve catalysts that the present invention is provided is：By the bimodulus described in present patent application
SSZ-13 molecular sieves obtained in the method for plate agent one-step synthesis SSZ-13 molecular sieves, with 0.5~1.5mol/L under the conditions of 70 DEG C
CuSO4Solion is exchanged 12 hours, after centrifugal filtration, deionized water washing, drying, is calcined 4 hours at 600 DEG C, is obtained
To Cu-SSZ-13 molecular sieve catalysts.
The Cu-SSZ-13 molecular sieve catalysts that the inventive method is prepared can be used for the purification of exhaust gas from diesel vehicle NO.
The invention discloses a kind of new synthetic method, using N, N, N- trimethyl adamantane ammonium (TMADa+) and chlorination courage
Alkali has obtained the SSZ-13 molecular sieves of high-crystallinity, pure phase as double template.And after Cu2+ in load, show
The selective reduction ability and high hydrothermal stability of excellent NO.The method can be greatly decreased expensive template N, N, N- tri-
The use of methyl adamantane ammonium, is that one kind is replaced using cheap template so as to reduce the production cost of SSZ-13 molecular sieves
The method of the expensive template in generation part, and product can be applied to NOx eliminations in diesel vehicle post processing (NH3-SCR) system catalyst
Process.With N, N, N- trimethyl adamantane ammonium and Choline Chloride are as double template, NaOH as sodium source, inclined aluminium for the present invention
Sour sodium synthesizes the preparation method of SSZ-13 molecular sieves as silicon source, Ludox as silicon source, deionized water as solvent.In this hair
In bright method, cheap template Choline Chloride instead of part costliness template N, N, N- trimethyl -1- amantadines, drop significantly
The low production cost of SSZ-13 molecular sieves.The SSZ-13 molecular sieves prepared using the inventive method, with high-crystallinity, high-purity
Degree, the advantage of high yield, and specific surface area higher, and Si/Al ratio is adjustable within the specific limits.Prepared by the inventive method
The Cu-SSZ-13 molecular sieves obtained after the molecular sieve carried upper Cu2+ of SSZ-13, can be used for exhaust gas from diesel vehicle NO purifications, even if in height
Still there is excellent NO conversion ratios and reaction temperature window wider under air speed.Additionally, the Cu-SSZ-13 molecules that the present invention is provided
Sieve illustrates that it has long lifespan, NO high conversion rates by after high temperature hydrothermal aging, can still keep the stabilization of framework of molecular sieve
Advantage.
Brief description of the drawings
Fig. 1 is the XRD that embodiment 1-3 obtains powder SSZ-13 molecular sieves；
Fig. 2 is the N2 adsorption desorption figures that embodiment 1 obtains powder SSZ-13 molecular sieves；
Fig. 3 is that embodiment 1 obtains that catalyst Cu-SSZ-13 is fresh, 800 DEG C of hydrothermal aging samples XRD, and Fig. 3 shows,
Sample structure after hydrothermal aging is kept, and framework of molecular sieve keeps complete, illustrates that the catalyst has outstanding hydro-thermal
Stability；
Fig. 4 is the NH3-SCR catalytic effect evaluation figures that embodiment 1 obtains catalyst Cu-SSZ-13, and Fig. 4 shows, Cu-
Fresh, the hydrothermal aging superior activity of SSZ-13 catalyst, the conversion ratio of NO is all very high, and temperature window is wider, illustrates that this is urged
Agent has excellent fresh, aging catalysis activity
Specific embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by specific embodiment.
Embodiment 1
(1) 0.8g NaOH is added in 40g deionized waters at room temperature, and 2h is stirred at room temperature, Zhi Daoqing
Sodium oxide molybdena is completely dissolved；
(2) 0.5g sodium metaaluminates (content is 80%) are subsequently adding, are stirred until homogeneous；
(3) 0.2g N, N, N- trimethyl -1- amantadines (content is 25%) and 0.85g chlorinations are respectively added slowly to again
Choline, continues to be stirred until homogeneous；
(4) 15g Ludox (content is 30%) is continuously added, stirring forms homogeneous colloidal sol；
(5) colloidal sol is put into the hydrothermal reaction kettle of polytetrafluoroethylliner liner, crystallization 4 days at 155 DEG C；
(6) after the completion of crystallization, colloidal sol is cooled to room temperature, after centrifugal filtration, deionized water washing, drying, and 600
Calcined 5 hours at DEG C, obtain SSZ-13 molecular sieves, be designated as sample 1；
(7) it is small that SSZ-13 molecular sieves obtained by carry out ion exchange 12 under the conditions of 70 DEG C with 0.5mol/L CuSO4 solution
When, and after centrifugal filtration, deionized water washing, drying, calcined 4 hours at 600 DEG C, obtain Cu-SSZ-13 molecular sieves and urge
Agent.
Tested by bet, the bet specific surface areas of gained SSZ-13 molecular sieves are 660.30m2/g.Tested by ICP, institute
The Si/Al ratio for obtaining SSZ-13 molecular sieves is 20.05.
The hydrothermal aging of catalyst is adopted with the following method：
Integral catalyzer is put into aging equipment, 800 DEG C is risen to by 10 DEG C/min heating rates, and be passed through air and
10% vapor, maintains 12 hours in the temperature
The evaluation of catalyst is adopted with the following method：
2g Cu-SSZ-13 catalyst fineses are mixed with 5g water, slurries are prepared, cordierite honeycomb ceramic matrix is coated on
Sample, catalyst coated weight is about 250gL-1, and in 100 DEG C of dryings 2 hours, 500 DEG C were calcined 2 hours sample, as prepare
Monoblock type Cu-SSZ-13 catalyst, puts it into fixed bed activity rating device, and simulated flue gas composition is 1000ppm NO,
1100ppm NH3,5%O2 and 10%H2O, reaction velocity are 30,000h-1.
Fig. 3 shows that the sample structure after hydrothermal aging is kept, and framework of molecular sieve keeps complete, illustrates the catalysis
Agent has outstanding hydrothermal stability.Fig. 4 shows that fresh, the hydrothermal aging superior activity of Cu-SSZ-13 catalyst, NO's turns
Rate is all very high, and temperature window is wider, illustrates that the catalyst has excellent fresh, aging catalysis activity
Embodiment 2
(1) 0.7g NaOH is added in 40g deionized waters at room temperature, and 2h is stirred at room temperature, Zhi Daoqing
Sodium oxide molybdena is completely dissolved；
(2) 0.6g sodium metaaluminates (content is 80%) are subsequently adding, are stirred until homogeneous；
(3) 0.4g N, N, N- trimethyl -1- amantadines (content is 25%) and 0.45g chlorinations are respectively added slowly to again
Choline, continues to be stirred until homogeneous；
(4) it is further continued for adding 12g Ludox (content is 30%), stirring forms homogeneous colloidal sol；
(5) colloidal sol is put into the hydrothermal reaction kettle of polytetrafluoroethylliner liner, crystallization 4 days at 155 DEG C；
(6) after the completion of crystallization, colloidal sol is cooled to room temperature, after centrifugal filtration, deionized water washing, drying, at 600 DEG C
Lower calcining 5 hours, obtains SSZ-13 molecular sieves, is designated as sample 2；
Tested by bet, the bet specific surface areas of gained SSZ-13 molecular sieves are 620.30m2/g.Tested by ICP, institute
The Si/Al ratio for obtaining SSZ-13 molecular sieves is 13.05.
Embodiment 3
(1) 0.7g NaOH is added in 40g deionized waters at room temperature, and 2h is stirred at room temperature, Zhi Daoqing
Sodium oxide molybdena is completely dissolved；
(2) 0.6g sodium metaaluminates (content is 80%) are subsequently adding, are stirred until homogeneous；
(3) 0.6g N, N, N- trimethyl -1- amantadines (content is 25%) and 0.15g Choline Chlorides are slow added into,
Continue to be stirred until homogeneous；
(4) it is further continued for adding 15g Ludox (content is 30%), stirring forms homogeneous colloidal sol；
(5) colloidal sol is put into the hydrothermal reaction kettle of polytetrafluoroethylliner liner, crystallization 4 days at 155 DEG C；
(6) after the completion of crystallization, colloidal sol is cooled to room temperature, after centrifugal filtration, deionized water washing, drying, at 600 DEG C
Lower calcining 5 hours, obtains SSZ-13 molecular sieves, is designated as sample 3；
Tested by bet, the bet specific surface areas of gained SSZ-13 molecular sieves are 610.30m2/g.Tested by ICP, institute
The Si/Al ratio for obtaining SSZ-13 molecular sieves is 8.05.
Tested by three groups of embodiments to more than, it is found that three groups of samples are respectively provided with specific surface area higher, and Si/Al
It is more adjustable than in the range of 8~20.05.
Applicant's statement, the foregoing is only embodiments of the invention, but the invention is not limited in above-mentioned method detailed,
Do not mean that the present invention has to rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field it will be clearly understood that
Any improvement in the present invention, the addition to the equivalence replacement and auxiliary element of each raw material of product of the present invention, the choosing of concrete mode
Select, within the scope of all falling within protection scope of the present invention and disclosing.
Claims (4)
1. a kind of method of double template one-step synthesis SSZ-13 molecular sieves, comprises the following steps:
(1) will be added in deionized water as the raw material NaOH of sodium source at room temperature, and stirring is completely dissolved to it；
(2) will be added in above-mentioned solution as the raw material sodium metaaluminate of silicon source, be stirred until homogeneous；
(3) organic formwork agent N, N, N- trimethyl -1- amantadines and Choline Chloride are sequentially added, and continues stirring 2 hours；
(4) add and stirred to forming homogeneous colloidal sol as the raw material Ludox of silicon source；
(5) complete colloidal sol will be stirred to be placed in hydrothermal reaction kettle, crystallization 4-5 days at 165 DEG C；
(6) after colloidal sol being cooled into room temperature, through centrifugal filtration, deionized water washing, dry, 5 are calcined at 500~600 DEG C small
When, obtain SSZ-13 molecular sieves.
2. a kind of preparation method of Cu-SSZ-13 molecular sieve catalysts, it is characterised in that by the SSZ- obtained by claim 1
13 molecular sieves are exchanged 12 hours under the conditions of 70 DEG C with 0.5~1.5mol/L CuSO4 solions, through centrifugal filtration, deionization
After water washing, drying, calcined 4 hours at 600 DEG C, obtain Cu-SSZ-13 molecular sieve catalysts.
3. method according to claim 1 and 2, it is characterised in that in terms of Na2O, silicon source is with Al2O3 for reaction mass sodium source
Meter, silicon source in terms of SiO2, solvent in terms of H2O, template N, N, N- trimethyl adamantane ammonium in terms of R1, template Choline Chloride with
R2 is counted, and each reaction mass is 0.2~1.0Na2O according to mol ratio:0.2~0.5Al2O3:10SiO2:120~250H2O:0.1
~1.0R1:0.1~1.0R2 is fed intake, and wherein R1 is template N, N, N- trimethyl adamantane ammonium, and R2 is template chlorination
Choline.
4. the Cu-SSZ-13 molecular sieve catalysts that claim 2 methods described is prepared are in exhaust gas from diesel vehicle NO purifications
Using.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107804855A (en) * | 2017-10-31 | 2018-03-16 | 阜阳欣奕华材料科技有限公司 | A kind of preparation method, the preparation method of SCR catalyst of the hydrogen type molecular sieves of SSZ 13 |
| CN108160105A (en) * | 2017-12-12 | 2018-06-15 | 南开大学 | Redox molecule sieve catalyst and its synthetic method are catalyzed for methane selectively |
| CN108190907A (en) * | 2018-02-06 | 2018-06-22 | 四川润和催化新材料股份有限公司 | A kind of SSZ-13 molecular sieves and preparation method thereof |
| CZ307576B6 (en) * | 2017-12-21 | 2018-12-19 | Unipetrol výzkumně vzdělávací centrum, a.s. | A method of producing SSZ-13 zeolite |
| CN109110777A (en) * | 2017-06-22 | 2019-01-01 | 中国科学院宁波材料技术与工程研究所 | A kind of synthetic method of SSZ-13 molecular sieve |
| CN109201109A (en) * | 2018-07-30 | 2019-01-15 | 中国石油大学(北京) | A kind of methanol-to-olefin catalyst and preparation method thereof |
| CN110562994A (en) * | 2019-09-27 | 2019-12-13 | 浙江天地环保科技有限公司 | method for synthesizing SSZ-13 molecular sieve by converting mixed template agent dry glue and application thereof |
| CZ308130B6 (en) * | 2018-11-27 | 2020-01-15 | Unipetrol výzkumně vzdělávací centrum, a.s. | Process for producing zeolite SSZ-13 with mechanochemical activation |
| CN112473730A (en) * | 2020-12-14 | 2021-03-12 | 大连海事大学 | Copper-based CHA-type silicon-aluminum molecular sieve catalyst and preparation method thereof |
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| CN109110777A (en) * | 2017-06-22 | 2019-01-01 | 中国科学院宁波材料技术与工程研究所 | A kind of synthetic method of SSZ-13 molecular sieve |
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| CN109201109A (en) * | 2018-07-30 | 2019-01-15 | 中国石油大学(北京) | A kind of methanol-to-olefin catalyst and preparation method thereof |
| CZ308130B6 (en) * | 2018-11-27 | 2020-01-15 | Unipetrol výzkumně vzdělávací centrum, a.s. | Process for producing zeolite SSZ-13 with mechanochemical activation |
| US20220097033A1 (en) * | 2018-12-19 | 2022-03-31 | Basf Se | Cha type zeolitic materials and methods for their preparation |
| CN110562994A (en) * | 2019-09-27 | 2019-12-13 | 浙江天地环保科技有限公司 | method for synthesizing SSZ-13 molecular sieve by converting mixed template agent dry glue and application thereof |
| CN113387369A (en) * | 2020-03-12 | 2021-09-14 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | Preparation method of Cu-SSZ-13 molecular sieve |
| US20220162081A1 (en) * | 2020-11-20 | 2022-05-26 | LiFeng Wang | Chabazite zeolite synthesis with combined organic templates |
| CN112473730A (en) * | 2020-12-14 | 2021-03-12 | 大连海事大学 | Copper-based CHA-type silicon-aluminum molecular sieve catalyst and preparation method thereof |
| CN112473730B (en) * | 2020-12-14 | 2024-01-19 | 大连海事大学 | Copper-based CHA type silicon-aluminum molecular sieve catalyst and preparation method thereof |
| CN116393164A (en) * | 2023-03-30 | 2023-07-07 | 华中科技大学 | Auxiliary metal modified Fe-SSZ-13 molecular sieve, preparation and application as denitration catalyst |
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