CN107115888A - A kind of preparation method and its usage of the catalyst of Cu SSZ 13 - Google Patents
A kind of preparation method and its usage of the catalyst of Cu SSZ 13 Download PDFInfo
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- CN107115888A CN107115888A CN201710396252.4A CN201710396252A CN107115888A CN 107115888 A CN107115888 A CN 107115888A CN 201710396252 A CN201710396252 A CN 201710396252A CN 107115888 A CN107115888 A CN 107115888A
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- 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
- B01J29/76—Iron group metals or copper
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
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- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/16—After treatment, characterised by the effect to be obtained to increase the Si/Al ratio; Dealumination
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Abstract
The invention provides a kind of preparation method and its usage of the catalyst of Cu SSZ 13.The preparation method comprises the following steps：1) raw material silicon source, silicon source, template, crystal seed are put into mortar and grind to form uniform mixture；2) crystallization in reactor is filled this blend into, the molecular sieve carriers of Na SSZ 13 are made in cooling washing dry roasting；3) prepare ammonium nitrate solution and add the molecular sieve carriers of Na SSZ 13, NH is made in filtration washing, drying after ion exchange4The molecular sieves of SSZ 13；4)) prepare copper nitrate solution and add NH4The molecular sieves of SSZ 13, filter, dry, are calcined after ion exchange, and the catalyst of Cu SSZ 13 is made.The catalyst of Cu SSZ 13 of the present invention has excellent NH3SCR catalytic activity, N2Selectivity, hydrothermal stability and anti-H2O and SO2Poisoning performance, the purification suitable for exhaust gas from diesel vehicle.
Description
Technical field
The present invention relates to catalyst technical field, and in particular to a kind of preparation method and its use of Cu-SSZ-13 catalyst
On the way.
Background technology
At present, with NH3For reducing agent Selective Catalytic Reduction of NO x (NH3- SCR), because its conversion rate of NOx is high, fuel-economy
Property the control of good, engine it is simple the advantages of be widely used among diesel car tail gas refining, catalyst is the technology
Core.Wherein V2O5-WO3(MoO3)/TiO2Industrial applications for many years, but there are still some drawbacks catalyst, such as grasp
Make N when narrower warm window, high temperature2Low, the active component V of selectivity has bio-toxicity, harm ecological environment and health etc..Its
Non- V catalyst such as oxide catalyst Ce-W, Fe-Ti that he develops and with ZSM-5, beta for carrier Cu bases or Fe base molecules
Sieve catalyst etc. is all different degrees of to have that temperature operating window is narrow, hydrothermal stability is poor and HC poisoning capabilities.
Therefore, exploitation has catalytic activity is high, temperature operating window is wide and possesses the catalyst of high hydrothermal stability to face huge
Challenge.
In recent years, Cu-SSZ-13 catalyst was received significant attention because of its high catalytic activity and high hydrothermal stability.Make at present
The conventional method of standby Cu-SSZ-13 catalyst is liquid-phase ion exchange, but this kind of method prepares SSZ-13 carriers and need to make
With expensive template N, N, N- front three fund steel alkane ammonium hydroxide, it is unfavorable for the large-scale promotion application of the catalyst.In order to
The production cost of catalyst is reduced, Cu-SSZ-13 is prepared with the cheap template such as Cu-TEPA complex compounds or Choline Chloride
Technology also receive significant attention, but the hydrothermal stability of the Cu-SSZ-13 catalyst thus prepared still needs to further raising.
Meanwhile, the crystallization process of all preparation methods is all completed under liquid phase environment, is not only produced in preparation process and has been given birth to sewage, produces
Rate is relatively low.Therefore, using new cheap template prepared under the conditions of anhydrous activity it is higher, hydrothermal stability is more preferable
Cu-SSZ-13 catalyst, for mobile source tail-gas is out of stock, environmental protection is respectively provided with very important meaning.
The content of the invention
In view of the shortcomings of the prior art, an object of the present invention is to provide a kind of preparation of Cu-SSZ-13 catalyst
Method, using solid-phase synthesis, obtained Cu-SSZ-13 catalyst has excellent NH3- SCR catalytic activity, N2Selectivity, water
Heat endurance and anti-H2O and SO2Poisoning performance.
For up to this purpose, the present invention uses following technical scheme：
A kind of preparation method of Cu-SSZ-13 catalyst, comprises the following steps：
1) raw material silicon source, silicon source, template, crystal seed are put into mortar, grind to form uniform mixture；
2) by step 1) uniform mixture be fitted into crystallization in reactor, Na- is made in cooling washing dry roasting
SSZ-13 molecular sieve carriers；
3) prepare ammonium nitrate solution, add step 2) made from Na-SSZ-13 molecular sieve carriers, filter after ion exchange
Washing, dry, obtained NH4- SSZ-13 molecular sieves；
4) prepare copper nitrate solution, add step 3) made from NH4- SSZ-13 molecular sieves, filter, do after ion exchange
Dry, roasting, is made Cu-SSZ-13 catalyst.
Step 1) in, the silicon source is sodium metasilicate, SiO2, source of aluminium is aluminum sulfate, and the template is N, N ,-diformazan
Base-N- ethylcyclohexyl ammonium bromides, the crystal seed is H-SSZ-13；
Preferably, the active principle of the raw material is with Na2O、SiO2、Al2O3, N, N ,-dimethyl-N-ethyl cyclohexyl bromide
Change ammonium, H-SSZ-13 meters, its consumption is as follows：The Na2The O and SiO2Mol ratio be (0.18~0.26):1, such as it is described
Na2The O and SiO2Mol ratio be 0.18:1、0.19:1、0.2:1、0.21:1、0.22:1、0.23:1、0.24:1、0.25:
1、0.26:1。
Preferably, the SiO2With the Al2O3Mol ratio be (18~24):1, such as described SiO2With the Al2O3
Mol ratio be 18:1、19:1、20:1、21:1、22:1、23:1、24:1.
Preferably, N, the N ,-dimethyl-N-ethyl cyclohexyl ammonium bromide and the SiO2Mol ratio for (0.1~
0.18):1, such as described N, N ,-dimethyl-N-ethyl cyclohexyl ammonium bromide and the SiO2Mol ratio be 0.1:1、0.11:
1、0.12:1、0.13:1、0.14:1、0.15:1、0.16:1、0.17:1、0.18:1。
Preferably, the mass percent that the H-SSZ-13 accounts for raw material gross weight is 1~10%, such as described H-SSZ-13 is accounted for
The mass percent of raw material gross weight is 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%.
Step 2) in, the temperature of the crystallization is 160~220 DEG C, such as 160 DEG C, 170 DEG C, 180 DEG C, 190 DEG C, 200
℃、210℃、220℃；The time of the crystallization be 3~8d (my god), such as 3d, 4d, 5d, 6d, 7d, 8d.
Step 2) in, the temperature of the cooling is 23~27 DEG C, such as 23 DEG C, 24 DEG C, 25 DEG C, 26 DEG C, 27 DEG C.
Preferably, the detailed process of the washing be washed with deionized to mixture for neutrality.
Preferably, the temperature of the drying is 100 DEG C, and the time of the drying is 12h.
Step 2) in, the temperature of the roasting is 500~800 DEG C, such as the temperature of described roasting is 500 DEG C, 550 DEG C,
600℃、650℃、700℃、750℃、800℃；The time of the roasting is 4~8h, such as time of described roasting is 4h,
5h、6h、7h、8h。
Step 3) in, the concentration of the ammonium nitrate solution is 0.5~1.5mol/L, such as 0.5mol/L, 0.7mol/L,
1.0mol/L、1.2mol/L、1.5mol/L。
Step 3) in, the consumption of Na-SSZ-13 molecular sieve carriers described in ammonium nitrate solution is 1g described in per 50mL.
Step 3) in, the temperature of the ion exchange is 70~85 DEG C, such as 70 DEG C, 71 DEG C, 72 DEG C, 73 DEG C, 74 DEG C, 75
℃、76℃、77℃、78℃、79℃、80℃、81℃、82℃、83℃、84℃、85℃。
Step 4) in, the concentration of the copper nitrate solution is 0.01~0.5mol/L, such as 0.01mol/L, 0.05mol/
L、0.1mol/L、0.15mol/L、0.2mol/L、0.25mol/L、0.3mol/L、0.35mol/L、0.4mol/L、0.45mol/
L、0.5mol/L。
Step 4) in, NH described in copper nitrate solution described in every 50~200mL4The consumption of-SSZ-13 molecular sieves is 1g.
Step 4) in, the temperature of the ion exchange is 23~27 DEG C, such as 23 DEG C, 24 DEG C, 25 DEG C, 26 DEG C, 27 DEG C.
Step 4) in, the temperature of the roasting is 500~800 DEG C, such as the temperature of described roasting is 500 DEG C, 550 DEG C,
600℃、650℃、700℃、750℃、800℃；The time of the roasting is 4~8h, such as time of described roasting is 4h,
5h、6h、7h、8h。
The second object of the present invention is to provide Cu-SSZ-13 catalyst made from a kind of above-mentioned preparation method.
The third object of the present invention is to provide a kind of purification method of exhaust gas from diesel vehicle, and the purification method is using above-mentioned
Cu-SSZ-13 catalyst.
Compared with prior art, beneficial effects of the present invention are：
(1) present invention has high catalytic activity by Cu-SSZ-13 catalyst made from solid-phase synthesis, especially exists
There are excellent catalytic activity, NO within the temperature range of 200-450 DEG CxConversion ratio more than 80%.
(2) present invention possesses excellent anti-high-speed ability by Cu-SSZ-13 catalyst made from solid-phase synthesis,
In the range of 250-450 DEG C, 800,000h-1Under remain in that higher NOxConversion ratio, NOxConversion ratio be more than 80%.
(3) present invention has excellent N by Cu-SSZ-13 catalyst made from solid-phase synthesis2Generation selectivity,
N in whole 150-550 DEG C of temperature range2Generation selectivity is more than 95%.
(4) preparation method method of the invention improves catalyst while Cu-SSZ-13 high activity of catalyst is obtained
Crystallinity and silica alumina ratio, silica alumina ratio is about 11, improves the hydrothermal stability of catalyst.
(5) Cu-SSZ-13 catalyst of the invention is protected after 800 DEG C of aging 16h still in the range of 225-450 DEG C
Hold more than 80% conversion ratio, be suitably applied the purification of exhaust gas from diesel vehicle.
(6) Cu-SSZ-13 catalyst of the invention is prepared using nontoxic component, and health and ecological environment will not be made
Into harm；Preparation method is simple to operation, no contaminated wastewater, yield ＞ 90%.
Brief description of the drawings
Fig. 1 Cu-SSZ-13 catalyst of difference Cu load capacity made from the solid-phase synthesis of the present invention and comparative example 1 one
Walk Cu made from synthetic method10.9The XRD spectrum schematic diagram of Na-SSZ-13 catalyst made from-SSZ-13 catalyst, embodiment 1；
The catalytic activity of Fig. 2 Cu-SSZ-13 catalyst of difference Cu load capacity made from the solid-phase synthesis of the present invention
Schematic diagram；
The Cu-SSZ-13 catalyst of Fig. 3 difference Cu load capacity made from the solid-phase synthesis of the present invention is to N2Selectivity
Schematic diagram；
Fig. 4 Cu-SSZ-13 catalyst of difference Cu load capacity made from the solid-phase synthesis of the present invention and comparative example 2-3
Catalytic activity after being handled through the Cu-SSZ-13 catalyst of difference Cu load capacity made from one-step synthesis through hydrothermal aging is shown
It is intended to；
Fig. 5 catalysis of Cu-SSZ-13 catalyst under different space velocities made from the solid-phase synthesis of the present invention is lived
The schematic diagram of property；
Fig. 6 Cu-SSZ-13 catalyst made from the solid-phase synthesis of the present invention is in H2O and SO2Urging in the presence of under conditions of
Change the schematic diagram of activity.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in understanding the present invention, is not construed as the concrete restriction to the present invention.
Embodiment 1
The preparation process of the Na-SSZ-13 molecular sieve carriers of the present embodiment is as follows：By 1.412g sodium metasilicate, 1.368g
Silica, 0.65g aluminum sulfate, 0.8g N, N ,-dimethyl-N-ethyl cyclohexyl ammonium bromide template and 0.05g crystalline substance
Kind H-SSZ-13, which is put into mortar, to be ground, and be put into reactor after grinding is uniform crystallizes 5 days at 180 DEG C, is then taken out
Filter washing, 100 DEG C of oven overnights are put into by filter cake, and 6h is finally calcined in 600 DEG C of air, and to obtain Na-SSZ-13 molecular sieve supported
Body.
Embodiment 2
The preparation process of the Cu-SSZ-13 catalyst of the present embodiment is as follows：By Na-SSZ-13 molecules made from embodiment 1
Sieve carrier and 1mol/L NH4NO3Solution stirs 5h at 80 DEG C, then again passes by filtering and washing, drying program and obtains NH4-
SSZ-13 powdered molecular sieves.By obtained NH4Cu (the NO of-SSZ-13 molecular sieves and 0.1mol/L3)2Solution is normal at room temperature
Temperature stirring 24h, then again passes by the programs such as filtering and washing, drying, roasting and obtains Cu-SSZ-13 powder catalysts.Will system
Catalyst tabletting, grind, sieve, taking 40-60 mesh standby.The catalyst of different Cu load capacity passes through Cu (NO3)2Solution
Ion exchange number of times is adjusted, and it is 1.7% Cu load capacity that the present embodiment obtains mass percent by 1 secondary ion exchange system
Cu1.7- SSZ-13 catalyst.
Embodiment 3
The preparation process of the Cu-SSZ-13 catalyst of the present embodiment is as follows：By Na-SSZ-13 molecules made from embodiment 1
Sieve carrier and 1mol/L NH4NO3Solution stirs 5h at 80 DEG C, then again passes by filtering and washing, drying program and obtains NH4-
SSZ-13 powdered molecular sieves.By obtained NH4-SSZ-13 molecular sieves and 0.1mol/L Cu (NO3)2Solution is normal at room temperature
Temperature stirring 24h, then again passes by the programs such as filtering and washing, drying, roasting and obtains Cu-SSZ-13 powder catalysts.Will system
Catalyst tabletting, grind, sieve, taking 40-60 mesh standby.The catalyst of different Cu load capacity passes through Cu (NO3)2Solution
Ion exchange number of times is adjusted, and it is 2.2% Cu load capacity that the present embodiment obtains mass percent by 2 secondary ion exchange systems
Cu2.2- SSZ-13 catalyst.
Embodiment 4
The preparation process of the Cu-SSZ-13 catalyst of the present embodiment is as follows：By Na-SSZ-13 molecules made from embodiment 1
Sieve carrier and 1mol/L NH4NO3Solution stirs 5h at 80 DEG C, then again passes by filtering and washing, drying program and obtains NH4-
SSZ-13 powdered molecular sieves.By obtained NH4-SSZ-13 molecular sieves and 0.1mol/L Cu (NO3)2Solution is normal at room temperature
Temperature stirring 24h, then again passes by the programs such as filtering and washing, drying, roasting and obtains Cu-SSZ-13 powder catalysts.Will system
Catalyst tabletting, grind, sieve, taking 40-60 mesh standby.The catalyst of different Cu load capacity passes through Cu (NO3)2Solution
Ion exchange number of times is adjusted, and it is 2.8% Cu load capacity that the present embodiment obtains mass percent by 3 secondary ion exchange systems
Cu2.8- SSZ-13 catalyst.
Comparative example 1
The Cu-SSZ-13 catalyst of this comparative example is made using one-step synthesis, and preparation process is as follows：First will
0.514gNaAlO2It is dissolved in 4.722g deionized waters, adds 1.149gCuSO4·H2O.Stir after 0.5h, be added dropwise
1.07gTEPA, adds after 1.1gNaOH, stirring 0.5h after being sufficiently stirred for, adds 3.33mL Ludox (31wt.%), stirring 2
~3h, is fitted into the steel bomb of polytetrafluoroethyllining lining, and reacts 4d at a temperature of 100 DEG C.After reaction terminates, by product
It is washed with deionized, and 12h is dried at 100 DEG C, 6h is calcined at 600 DEG C, obtains the Cu that mass percent is 10.9%
The Cu of load capacity10.9- SSZ-13 catalyst.
Comparative example 2
The Cu-SSZ-13 catalyst of this comparative example is made using one-step synthesis, and preparation process is as follows：First will
0.514gNaAlO2It is dissolved in 4.722g deionized waters, adds 1.149gCuSO4·H2O.Stir after 0.5h, be added dropwise
1.07gTEPA, adds after 1.1gNaOH, stirring 0.5h after being sufficiently stirred for, adds 3.33mL Ludox (31wt.%), stirring 2
~3h, is fitted into the steel bomb of polytetrafluoroethyllining lining, and reacts 4d at a temperature of 100 DEG C.After reaction terminates, by product
It is washed with deionized, and 12h is dried at 100 DEG C, obtains Cu-SSZ-13initialSample.By 1g Cu-SSZ-13initialPlus
Enter 100mL HNO3In (0.1mol/L) solution, 12h is exchanged under 80 DEG C of water bath conditions, it is 5.6% to obtain mass percent
The Cu of Cu load capacity5.6- SSZ-13 catalyst.
Comparative example 3
The Cu-SSZ-13 catalyst of this comparative example is made using one-step synthesis, and preparation process is as follows：First will
0.514gNaAlO2It is dissolved in 4.722g deionized waters, adds 1.149gCuSO4·H2O.Stir after 0.5h, be added dropwise
1.07gTEPA, adds after 1.1gNaOH, stirring 0.5h after being sufficiently stirred for, adds 3.33mL Ludox (31wt.%), stirring 2
~3h, is fitted into the steel bomb of polytetrafluoroethyllining lining, and reacts 4d at a temperature of 100 DEG C.After reaction terminates, by product
It is washed with deionized, and 12h is dried at 100 DEG C, obtains Cu-SSZ-13initialSample.By 1g Cu-SSZ-13initialPlus
Enter 100mL HNO3In (0.3mol/L) solution, 12h is exchanged under 80 DEG C of water bath conditions, it is 3.6% to obtain mass percent
The Cu of Cu load capacity3.6- SSZ-13 catalyst.
Embodiments of the invention 2-4 and catalyst made from comparative example 1-3 are used for the purification of exhaust gas from diesel vehicle, wherein,
The usage amount of catalyst is respectively 50mg, and the composition of reaction mixture gas is：[NO]=[NH3]=500ppm, [O2]=5%, N2Make
Balance Air, total gas flow rate is 500mL/min, and corresponding air speed is 200,000h-1, 400,000h-1, 800,000h-1, reaction temperature
150-550 DEG C of degree.NO and NH3And accessory substance N2O、NO2Determined using infrared-gas pond.
To the Cu-SSZ-13 of difference Cu load capacity made from Na-SSZ-13 catalyst made from embodiment 1, embodiment 2-4
Catalyst and Cu made from comparative example 110.9- SSZ-13 catalyst carries out XRD analysis, and XRD spectrum is as shown in Figure 1.Can be with from Fig. 1
Find out, relative to the Cu of the one-step synthesis synthesis of comparative example 110.9- SSZ-13 catalyst, Na-SSZ-13 molecules of the invention
Sieving carrier and obtained Cu-SSZ-13 catalyst has higher crystallinity.
Exhaust gas from diesel vehicle is used for the Cu-SSZ-13 catalyst of difference Cu load capacity made from embodiments of the invention 2-4
Purification, air speed be 400,000h-1Under conditions of its catalytic activity is compared, experimental result is as shown in Figure 2.By Fig. 2
As can be seen that the Cu-SSZ-13 molecular sieve catalysts prepared have wider temperature window, in 200-450 DEG C of temperature range
Interior conversion rate of NOx is more than 80%.
Exhaust gas from diesel vehicle is used for the Cu-SSZ-13 catalyst of difference Cu load capacity made from embodiments of the invention 2-4
Purification, air speed be 400,000h-1Under conditions of to it to N2Selectivity is compared, and experimental result is as shown in Figure 3.By scheming
3 as can be seen that the Cu-SSZ-13 catalyst of obtained difference Cu load capacity is to N2Selectivity is higher, more than 95%.
To the Cu-SSZ-13 catalyst of difference Cu load capacity made from embodiments of the invention 2-4 and comparative example 2-3 through one
The Cu-SSZ-13 catalyst for walking difference Cu load capacity made from synthetic method is handled through severe hydrothermal aging, i.e., by above-mentioned catalysis
Agent is passed through 16h in the air of the water containing 10wt% at a temperature of 800 DEG C, and the above-mentioned catalyst after processing then is used for into diesel vehicle
The purification of tail gas, has done comparing result as shown in Figure 4 to its catalytic activity.As seen from Figure 4, relative to comparative example 2-3, this
The Cu-SSZ-13 catalyst of difference Cu load capacity shows excellent hydrothermal stability made from the embodiment 2-4 of invention.
By Cu made from embodiment 32.2- SSZ-13 catalyst is surveyed under conditions of different air speeds to its catalytic activity
Examination, i.e. air speed are 200,000h-1、400,000h-1、800,000h-1, test result is as shown in Figure 5.As seen from Figure 5, i.e.,
Make in 800,000h-1Air speed under, Cu-SSZ-13 catalyst remains in that excellent made from solid-phase synthesis of the invention
Catalytic activity.
By Cu made from embodiment 32.2- SSZ-13 catalyst is containing H2O and SO2Under conditions of its catalytic activity is done
Test, test result is as shown in Figure 6.As seen from Figure 6, even in H2O and SO2In the presence of under conditions of, solid phase of the invention is closed
Excellent catalytic activity is remained in that into Cu-SSZ-13 catalyst made from method.
In summary, the present invention uses Cu-SSZ-13 catalyst made from solid-phase synthesis in whole temperature section 150-550
There is very high NO in the range of DEG CxActive, excellent N2Selectivity and hydrothermal stability, are highly suitable for exhaust gas from diesel vehicle
The catalytic purification of nitrogen oxides.
Applicant states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, do not mean that the present invention has to rely on above-mentioned detailed
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within the present invention's
Within the scope of protection domain and disclosure.
Claims (10)
1. a kind of preparation method of Cu-SSZ-13 catalyst, it is characterised in that comprise the following steps：
1) raw material silicon source, silicon source, template, crystal seed are put into mortar, grind to form uniform mixture；
2) by step 1) uniform mixture be fitted into crystallization in reactor, Na-SSZ-13 is made in cooling washing dry roasting
Molecular sieve carrier；
3) prepare ammonium nitrate solution, add step 2) made from Na-SSZ-13 molecular sieve carriers, after ion exchange cross diafiltration
Wash, dry, NH is made4- SSZ-13 molecular sieves；
4) prepare copper nitrate solution, add step 3) made from NH4- SSZ-13 molecular sieves, filter, dry, roast after ion exchange
Burn, Cu-SSZ-13 catalyst is made.
2. preparation method according to claim 1, it is characterised in that step 1) in, the silicon source is sodium metasilicate, SiO2, institute
Silicon source is stated for aluminum sulfate, the template is N, N, and-dimethyl-N-ethyl cyclohexyl ammonium bromide, the crystal seed is H-SSZ-13；
Preferably, the active principle of the raw material is with Na2O、SiO2、Al2O3, N, N ,-dimethyl-N-ethyl cyclohexyl ammonium bromide,
H-SSZ-13 is counted, and its consumption is as follows：The Na2The O and SiO2Mol ratio be (0.18~0.26):1；
Preferably, the SiO2With the Al2O3Mol ratio be (18~24):1；
Preferably, N, the N ,-dimethyl-N-ethyl cyclohexyl ammonium bromide and the SiO2Mol ratio be (0.1~0.18):
1；
Preferably, the mass percent that the H-SSZ-13 accounts for raw material gross weight is 1~10%.
3. preparation method according to claim 1 or 2, it is characterised in that step 2) in, the temperature of the crystallization is 160
~220 DEG C, the time of the crystallization is 3~8d.
4. the preparation method according to one of claim 1-3, it is characterised in that step 2) in, the temperature of the cooling is
23~27 DEG C；
Preferably, the detailed process of the washing be washed with deionized to mixture for neutrality；
Preferably, the temperature of the drying is 100 DEG C, and the time of the drying is 12h.
5. the preparation method according to one of claim 1-4, it is characterised in that step 2) in, the temperature of the roasting is
500~800 DEG C, the time of the roasting is 4~8h.
6. the preparation method according to one of claim 1-5, it is characterised in that step 3) in, the ammonium nitrate solution
Concentration is 0.5~1.5mol/L.
7. the preparation method according to one of claim 1-6, it is characterised in that step 3) in, ammonium nitrate described in per 50mL
The consumption of Na-SSZ-13 molecular sieve carriers described in solution is 1g；
Preferably, step 3) in, the temperature of the ion exchange is 70~85 DEG C；
Preferably, the detailed process of the washing be washed with deionized to mixture for neutrality；
Preferably, the temperature of the drying is 100 DEG C, and the time of the drying is 12h.
8. the preparation method according to one of claim 1-7, it is characterised in that step 4) in, the copper nitrate solution
Concentration is 0.01~0.5mol/L；
Preferably, step 4) in, NH described in copper nitrate solution described in every 50~200mL4The consumption of-SSZ-13 molecular sieves is 1g；
Preferably, step 4) in, the temperature of the ion exchange is 23~27 DEG C；
Preferably, step 4) in, the temperature of the roasting is 500~800 DEG C, and the time of the roasting is 4~8h.
9. the Cu-SSZ-13 catalyst that a kind of preparation method as described in one of claim 1-8 is prepared.
10. a kind of purification method of exhaust gas from diesel vehicle, it is characterised in that the purification method is using as claimed in claim 9
Cu-SSZ-13 catalyst.
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