CN106927477B - A kind of preparation method of mesoporous Y type molecular sieve - Google Patents
A kind of preparation method of mesoporous Y type molecular sieve Download PDFInfo
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Abstract
A kind of preparation method of mesoporous Y type molecular sieve, it is characterized in that this method be by Y type molecular sieve in the mixed liquor of glycerol and cellulose after 150~220 DEG C of 0.5~5h of processing, 0.5~2h is contacted at normal temperatures and pressures with a kind of inorganic directing agent, then mixture is placed in closed reactor at 80~120 DEG C and handles 2~20h and recycles products therefrom；Wherein, the mass ratio of Y type molecular sieve and glycerol, cellulose is 1:(1~20): the mass ratio of (0.01~3), Y type molecular sieve and inorganic directing agent is 1:(0.1~10).In the mesoporous Y type molecular sieve that this method obtains, mesopore volume up to total pore volume 40~60%.
Description
Technical field
The present invention relates to a kind of preparation methods of mesoporous Y type molecular sieve.
Background technique
Y type molecular sieve (HY, REY, USY) is since the sixties in last century of use for the first time, just always catalytic cracking (FCC)
The chief active constituent element of catalyst.However, the polycyclic compound content in FCC feedstock is significant with the aggravation of crude oil heaviness
Increase, the diffusivity in zeolite cavity is but remarkably decreased.In order to overcome the defect of general microporous molecular sieve, reduce molecule
It sieve crystallite dimension and is introduced into molecular sieve crystal and mesoporous can be effectively improved its diffusion.Compared to traditional micropore
Molecular sieve, the transgranular external diffusion of mesopore molecular sieve are had excellent performance, and show unique catalytic activity in high molecular catalysis reaction,
And catalyst inactivation can be delayed, reduce coke yield (Perez-Ramirez J, et al.Chemical Society
Reviews2008；37:2530-42).
Up to the present, the important method that meso-hole structure is introduced in conventional Y type molecular sieve is the side of soda acid modification
Method.
In view of the protective effect that aluminium atom in routine (silica alumina ratio~5) NaY molecular sieve is strong to silicon atom, directly to routine
NaY directly to carry out alkali process be that cannot obtain (Martinez, the et al.Catalysis containing mesoporous Y type molecular sieve
Science&Technology 2012；2:987-994；Verboekend,et al.Advanced Functional
Materials 2012；22:916-928).So existing obtain mesoporous Y type by being handled conventional NaY molecular sieve
The method of molecular sieve, it usually needs exchange multiple processes in conjunction with acid processing and alkali process and ammonium and be carried out continuously processing.?
Disclosed in CN102333728A it is a kind of mesoporous method is introduced in conventional Y type molecular sieve, by advanced to Y type molecular sieve
Row acid processing improves its silica alumina ratio, carries out alkali process again then to prepare mesoporous Y type molecular sieve, is not passed through water steaming before acid processing
Vapour, alkali process process add CTAB, and product is mainly characterized by 2~8nm of aperture, crystallinity 72% or so.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of mesoporous Y type molecular sieve.
The preparation method of mesoporous Y type molecular sieve provided by the invention, it is characterised in that this method is by Y type molecular sieve sweet
In the mixed liquor of oil and cellulose after 150~220 DEG C of 0.5~5h of processing, contacted at normal temperatures and pressures with a kind of inorganic directing agent
0.5~2h, then mixture is placed in closed reactor at 80~120 DEG C and handles 2~20h and recycles products therefrom；Wherein, Y
The mass ratio of type molecular sieve and glycerol, cellulose is 1:(1~20): (0.01~3), preferably 1:(3~15): (0.05~1), more
It is preferred that 1:(5~10): the mass ratio of (0.1~0.5), Y type molecular sieve and inorganic directing agent is 1:(0.1~10), preferably 1:
(0.5~8), more preferable 1:(1~5).
The Y type molecular sieve is selected from NaY molecular sieve, and mole silica alumina ratio of silica and aluminium oxide is 4.5~6.
The preparation of the inorganic directing agent is according to 1Al2O3: (1~30) SiO2: (10~30) Na2O:(200~450)
H2The molar ratio of O, preferably 1Al2O3: (5~25) SiO2: (12~25) Na2O:(230~400) H2The molar ratio of O, more preferably
1Al2O3: (10~20) SiO2: (15~20) Na2O:(260~360) H2The molar ratio of O mixes silicon source, silicon source and water, then
Room temperature~80 DEG C at a temperature of, it is small that 0.2~40 is aged at a temperature of preferably 25~70 DEG C, at a temperature of more preferable 30~60 DEG C
When, it preferably 5~35 hours, obtains within more preferable 8~30 hours.
The silicon source is one or more of waterglass, silica solution, silica gel, Alusil and white carbon black, preferably water glass
Glass, silica solution, silica gel and Alusil, more preferable waterglass and silica solution.
The silicon source is the one or more of aluminum sulfate, activated alumina, aluminium isopropoxide, aluminate or Aluminum sol, excellent
Select aluminum sulfate, aluminium isopropoxide, aluminate and Aluminum sol, more preferable aluminum sulfate and Aluminum sol.
The cellulose preferably carboxymethyl cellulose and/or carboxyethyl cellulose, wherein the more preferable degree of polymerization be 100~
The carboxymethyl cellulose that 2000 carboxymethyl cellulose, the most preferably degree of polymerization are 300~1000, have it is preferably water-soluble and
Glycerol dissolubility is conducive to dissolve dispersion in glycerol and water solution mixed system.
The processing, condition are to carry out 5~15 hours for 90~110 DEG C in closed reactor.Described recovery product
Process is well known to those skilled in the art, no longer numerous herein to state, and typically refers to the process of dry roasting.
The method of the present invention, handling any type of NaY can obtain having significant, concentration mesoporous pore size point
The Y type molecular sieve of cloth solves the problems, such as relatively to have difficult labour in conventional NaY type molecular sieve raw transgranular mesoporous.Its mesopore volume is reachable
The 40~60% of total pore volume.
Molecular sieve obtained by this method shows as the FAU crystal structure of pure phase, and no stray crystal forms (XRD spectra).
The low temperature nitrogen adsorption-desorption curve of molecular sieve obtained by this method shows the IV that thermoisopleth belongs in IUPAC classification
Type, in P/P0In the case where 0.8-1.0, adsorbance is sharply increased, and is formd biggish mesoporous；It is calculated according to BJH model
The pore size distribution curve arrived shows that the aperture peak of molecular sieve is distributed between 10~25nm, wherein in 15nm or so peak intensity up to most
Big value.
The method of the present invention is since glycerol treated mother liquor is without being separated by filtration, and recoverable, cellulose are also made
For a kind of biomaterial of environmental protection, be conducive to environmental protection.
The Y type molecular sieve that the method for the present invention is prepared can be used for catalyst and catalyst carrier.The Y type molecular sieve has
Multi-stage porous topological structure, for petroleum distillate isomerization-visbreaking, be hydrocracked, the process such as catalytic cracking.
Detailed description of the invention
Fig. 1 is the XRD spectra for the mesoporous Y type molecular sieve that the present invention obtains.
Fig. 2 is the low temperature nitrogen adsorption-desorption curve for the mesoporous Y type molecular sieve that the present invention obtains.
Fig. 3 is the BJH pore size distribution curve figure for the mesoporous Y type molecular sieve that the present invention obtains.
Fig. 4 is the BJH pore size distribution curve figure of comparative example sieve sample.
Specific embodiment
Below by embodiment, the invention will be further described, but content not thereby limiting the invention.
In embodiments, product crystal structure is determined with X-ray diffraction (XRD), the spectrogram that 2 angles θ of record are 5 to 35 °.
Product specific surface and pore structure parameter are obtained by low temperature nitrogen adsorption desorption measurement.
Routine NaY is produced by Sinopec Shandong catalyst plant in embodiment and comparative example, crystallinity 88%, silica alumina ratio
It is 5.2.
Embodiment 1
According to 1Al2O3: 15SiO2: 16.5Na2O:320H29.4g waterglass (modulus 3.3) is added to by the molar ratio of O
In 6.9g sodium aluminate solution, stirring and dissolving obtains directed agents after being then aged 5 hours at 45 DEG C.
NaY type molecular sieve is handled into 3h, Y type in the carboxyethyl cellulose mixed liquor that 170 DEG C of glycerol and the degree of polymerization are 200
The mass mixing ratio of molecular sieve and glycerol, carboxyethyl cellulose is 1:20:0.05, then by gained mixed liquor and inorganic guiding
The mass mixing ratio of agent normal temperature and pressure mixing 1h, Y type molecular sieve and inorganic directing agent be 1:0.5, after in closed reactor
8h is handled at 90 DEG C, by mixture filtering, is washed with water, and 5 hours dry in 100 DEG C, then by it in 550 DEG C of roasting temperatures
5 hours, sieve sample is obtained, is denoted as GL-1.
Fig. 1 is the XRD spectra of GL-1.Fig. 1 shows that gained Y type molecular sieve shows as the FAU crystal structure of pure phase, no stray crystal
It is formed.
Fig. 2 is the low temperature nitrogen adsorption-desorption curve of GL-1.Fig. 2 shows the IV that this thermoisopleth belongs in IUPAC classification
Type, as shown in the figure, P/P0In the case of 0.8-1.0, adsorbance is sharply increased, and is formd inside gained Y type molecular sieve biggish
It is mesoporous.
Fig. 3 is the BJH pore size distribution curve figure of sample, and the aperture peak of molecular sieve is distributed between 10~25nm, wherein in
15nm or so peak intensity reaches maximum value.
Structural parameters are shown in Table 1.
Comparative example 1
This comparative example illustrates the result that NaY molecular sieve is handled in glycerol plain without added fiber.
According to 1Al2O3: 15SiO2: 16.5Na2O:320H29.4g waterglass (modulus 3.3) is added to by the molar ratio of O
In 6.9g sodium aluminate solution, stirring and dissolving obtains directed agents after being then aged 5 hours at 45 DEG C.
NaY type molecular sieve is handled into 3h in 170 DEG C of glycerol, Y type molecular sieve and qualities of glycerin mixed proportion are 1:20, so
Afterwards by gained mixed liquor and inorganic directing agent normal temperature and pressure mixing 1h, the mass mixing ratio of Y type molecular sieve and inorganic directing agent
For 1:0.5, after handle 8h at 90 DEG C in closed reactor, by mixture filtering, be washed with water, and in 100 DEG C dry 5 small
When, then by its in 550 DEG C roasting temperature 5 hours, obtain sieve sample, be denoted as DB-1.
Sample BET pore structure parameter such as table 1 obtained by DB-1, BJH pore size distribution curve such as figure are shown in Fig. 4.
Embodiment 2
According to 1Al2O3: 15SiO2: 16.5Na2O:320H29.4g waterglass (modulus 3.3) is added to by the molar ratio of O
In 6.9g sodium aluminate solution, stirring and dissolving obtains directed agents after being then aged 5 hours at 45 DEG C.
NaY type molecular sieve is handled into 3h, Y type in the carboxyethyl cellulose mixed liquor that 170 DEG C of glycerol and the degree of polymerization are 500
The mass mixing ratio of molecular sieve and glycerol, carboxyethyl cellulose is 1:20:0.05, then by gained mixed liquor and inorganic guiding
The mass mixing ratio of agent normal temperature and pressure mixing 1h, Y type molecular sieve and inorganic directing agent be 1:0.5, after in closed reactor
8h is handled at 90 DEG C, by mixture filtering, is washed with water, and 5 hours dry in 100 DEG C, then by it in 550 DEG C of roasting temperatures
5 hours, sieve sample is obtained, is denoted as GL-2.
XRD spectra is with the feature of Fig. 1, and for low temperature nitrogen adsorption-desorption curve with the feature of Fig. 2, BJH pore size distribution curve is same
The feature of Fig. 3.
Structural parameters are shown in Table 1.
Embodiment 3
According to 1Al2O3: 15SiO2: 16.5Na2O:320H29.4g waterglass (modulus 3.3) is added to by the molar ratio of O
In 6.9g sodium aluminate solution, stirring and dissolving obtains directed agents after being then aged 5 hours at 45 DEG C.
NaY type molecular sieve is handled into 3h, Y in the carboxyethyl cellulose mixed liquor that 170 DEG C of glycerol and the degree of polymerization are 1500
Type molecular sieve and glycerol, carboxyethyl cellulose mass mixing ratio be 1:20:0.05, then by gained mixed liquor and inorganic lead
To agent normal temperature and pressure mixing 1h, the mass mixing ratio of Y type molecular sieve and inorganic directing agent is 1:0.2, after in closed reactor
In handle 8h at 90 DEG C, by mixture filtering, be washed with water, and 5 hours dry in 100 DEG C, then it is roasted at a temperature of 550 DEG C
It burns 5 hours, obtains sieve sample, be denoted as GL-3.
XRD spectra is with the feature of Fig. 1, and for low temperature nitrogen adsorption-desorption curve with the feature of Fig. 2, BJH pore size distribution curve is same
The feature of Fig. 3.
Structural parameters are shown in Table 1.
Embodiment 4
According to 1Al2O3: 25SiO2: 18Na2O:320H215.7g waterglass (modulus 3.3) is added to by the molar ratio of O
In 6.9g sodium aluminate solution, stirring and dissolving obtains directed agents after being then aged 5 hours at 45 DEG C.
NaY type molecular sieve is handled into 3h, Y in the carboxyethyl cellulose mixed liquor that 170 DEG C of glycerol and the degree of polymerization are 2000
The mass mixing ratio of type molecular sieve and glycerol, carboxyethyl cellulose is 1:20:3, then by gained mixed liquor and inorganic guiding
The mass mixing ratio of agent normal temperature and pressure mixing 1h, Y type molecular sieve and inorganic directing agent be 1:10, after 90 in closed reactor
8h is handled at DEG C, by mixture filtering, is washed with water, and 5 hours dry in 100 DEG C, then by it in 550 DEG C of roasting temperatures 5
Hour, sieve sample is obtained, GL-4 is denoted as.
XRD spectra is with the feature of Fig. 1, and for low temperature nitrogen adsorption-desorption curve with the feature of Fig. 2, BJH pore size distribution curve is same
The feature of Fig. 3.
Structural parameters are shown in Table 1.
Embodiment 5
With embodiment 2, the difference is that cellulose be added is the carboxymethyl cellulose that the degree of polymerization is 500.According to
1Al2O3: 15SiO2: 16.5Na2O:320H2It is molten to be added to 6.9g sodium metaaluminate by the molar ratio of O for 9.4g waterglass (modulus 3.3)
In liquid, stirring and dissolving obtains directed agents after being then aged 5 hours at 45 DEG C.
NaY type molecular sieve is handled into 3h, Y type in the carboxymethyl cellulose mixed liquor that 170 DEG C of glycerol and the degree of polymerization are 500
The mass mixing ratio of molecular sieve and glycerol, carboxymethyl cellulose is 1:20:0.05, then by gained mixed liquor and inorganic guiding
The mass mixing ratio of agent normal temperature and pressure mixing 1h, Y type molecular sieve and inorganic directing agent be 1:0.5, after in closed reactor
8h is handled at 90 DEG C, by mixture filtering, is washed with water, and 5 hours dry in 100 DEG C, then by it in 550 DEG C of roasting temperatures
5 hours, sieve sample is obtained, is denoted as GL-5.
XRD spectra is with the feature of Fig. 1, and for low temperature nitrogen adsorption-desorption curve with the feature of Fig. 2, BJH pore size distribution curve is same
The feature of Fig. 3.
Structural parameters are shown in Table 1.
Embodiment 6
With embodiment 3, the difference is that cellulose be added is the carboxymethyl cellulose that the degree of polymerization is 1500.According to
1Al2O3: 15SiO2: 16.5Na2O:320H2It is molten to be added to 6.9g sodium metaaluminate by the molar ratio of O for 9.4g waterglass (modulus 3.3)
In liquid, stirring and dissolving obtains directed agents after being then aged 5 hours at 45 DEG C.
NaY type molecular sieve is handled into 3h, Y in the carboxymethyl cellulose mixed liquor that 170 DEG C of glycerol and the degree of polymerization are 1500
Type molecular sieve and glycerol, carboxymethyl cellulose mass mixing ratio be 1:20:0.05, then by gained mixed liquor and inorganic lead
To agent normal temperature and pressure mixing 1h, the mass mixing ratio of Y type molecular sieve and inorganic directing agent is 1:0.2, after in closed reactor
In handle 8h at 90 DEG C, by mixture filtering, be washed with water, and 5 hours dry in 100 DEG C, then it is roasted at a temperature of 550 DEG C
It burns 5 hours, obtains sieve sample, be denoted as GL-6.
XRD spectra is with the feature of Fig. 1, and for low temperature nitrogen adsorption-desorption curve with the feature of Fig. 2, BJH pore size distribution curve is same
The feature of Fig. 3.
Structural parameters are shown in Table 1.
Embodiment 7
According to 1Al2O3: 15SiO2: 16Na2O:400H28.2g NaOH is added to 58ml deionized water by the molar ratio of O
In, solution is stirred to clarify, 3.0g sodium metaaluminate is added in above-mentioned solution, 35.8g waterglass (modulus is then added
2.5), room temperature continues stirring to whole dissolutions, obtains directed agents after being then aged 20 hours at 30 DEG C.
NaY type molecular sieve is handled into 2h, Y type in the carboxymethyl cellulose mixed liquor that 200 DEG C of glycerol and the degree of polymerization are 200
The mass mixing ratio of molecular sieve and glycerol, carboxymethyl cellulose is 1:5:0.3, then by gained mixed liquor and inorganic directing agent
Mix 1h under normal temperature and pressure, the mass mixing ratio of Y type molecular sieve and inorganic directing agent is 1:0.5, after in closed reactor
In handle 12h at 100 DEG C, by mixture filtering, be washed with water, and 5 hours dry in 100 DEG C, then by it at a temperature of 550 DEG C
Roasting 5 hours, obtains sieve sample, is denoted as GL-7.
Feature of the XRD spectra of GL-7 with Fig. 1, feature of the low temperature nitrogen adsorption-desorption curve with Fig. 2, BJH pore-size distribution
Feature of the curve with Fig. 3.
Structural parameters are shown in Table 1.
Table 1
Seen from table 1, the present invention has an apparent modified effect to conventional NaY, in the mesoporous Y type molecular sieve of gained, mesoporous hole
Hold and mesoporous Kong Rong/total Kong Kongrong ratio dramatically increases, while also remaining good molecular sieve crystallinity.
Claims (8)
1. a kind of preparation method of mesoporous Y type molecular sieve, it is characterised in that this method is by Y type molecular sieve in glycerol and cellulose
Mixed liquor in after 150~220 DEG C of 0.5~5h of processing, contact 0.5~2h at normal temperatures and pressures with a kind of inorganic directing agent, then
Mixture is placed in closed reactor at 80~120 DEG C and handles 2~20h and recycles products therefrom；Wherein, Y type molecular sieve with
Glycerol, cellulose mass ratio be 1:(1~20): the mass ratio of (0.01~3), Y type molecular sieve and inorganic directing agent is 1:
(0.1~10)；Described cellulose is selected from carboxymethyl cellulose and/or carboxyethyl cellulose；The inorganic directing agent be by
1Al2O3: (1~30) SiO2: (10~30) Na2O:(200~450) H2Temperature of the mixture of the molar ratio of O in room temperature~80 DEG C
What lower ageing obtained for 0.2~40 hour.
2. according to the method for claim 1 wherein the mass ratio of Y type molecular sieve and glycerol, cellulose is 1:(3~15):
The mass ratio of (0.05~1), Y type molecular sieve and inorganic directing agent is 1:(0.5~8).
3. according to method for claim 2, wherein the mass ratio of Y type molecular sieve and glycerol, cellulose is 1:(5~10): (0.1
~0.5), the mass ratio of Y type molecular sieve and inorganic directing agent is 1:(1~5).
4. be selected from NaY molecular sieve according to the method for claim 1 wherein, described Y type molecular sieve, silica and aluminium oxide
Mole silica alumina ratio is 4.5~6.
5. described silicon source is one in waterglass, silica solution, silica gel, Alusil and white carbon black according to method of claim 1
Kind is a variety of.
6. described silicon source is that aluminum sulfate, activated alumina, aluminium isopropoxide, aluminate and aluminium are molten according to method of claim 1
Glue it is one or more.
7. according to the method for claim 1 wherein described cellulose is the carboxymethyl cellulose that the degree of polymerization is 100~2000.
8. according to method for claim 7, wherein the described degree of polymerization is 300~1000.
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| CN103003202A (en) * | 2010-05-14 | 2013-03-27 | 墨西哥石油研究院 | Process for altering the physico-chemical properties of faujasite Y-type zeolites |
| CN104760973A (en) * | 2015-03-31 | 2015-07-08 | 中国石油大学(北京) | Y-type molecular sieve with ultra-high mesoporous content and preparation method of Y-type molecular sieve |
| CN104891523A (en) * | 2014-03-07 | 2015-09-09 | 中国石油天然气股份有限公司 | Preparation method of mesoporous Y-type molecular sieve |
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| CN103003202A (en) * | 2010-05-14 | 2013-03-27 | 墨西哥石油研究院 | Process for altering the physico-chemical properties of faujasite Y-type zeolites |
| CN104891523A (en) * | 2014-03-07 | 2015-09-09 | 中国石油天然气股份有限公司 | Preparation method of mesoporous Y-type molecular sieve |
| CN104760973A (en) * | 2015-03-31 | 2015-07-08 | 中国石油大学(北京) | Y-type molecular sieve with ultra-high mesoporous content and preparation method of Y-type molecular sieve |
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