CN106745032A - The method that the mesopore molecular sieves of Al MCM 41 are directly synthesized by kaolin or Hanggin 2# soil - Google Patents
The method that the mesopore molecular sieves of Al MCM 41 are directly synthesized by kaolin or Hanggin 2# soil Download PDFInfo
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- 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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Abstract
Method the present invention relates to be directly synthesized the mesopore molecular sieves of Al MCM 41 by kaolin or Hanggin 2# soil.Specific steps mainly include：(1) 4mol/L aqueous sulfuric acids acid activation lamellar clay raw ore obtains acid-treated clay；(2) after acid-treated clay is mixed 1 hour with the alkaline solution of certain density cetyl trimethylammonium bromide in 70 DEG C of water-baths, pH value of solution=10 are adjusted, is further continued for stirring 1 hour；(3) in hydrothermal reaction kettle, 110 DEG C stand crystallization 12 hours to gained mixture；(4) product is dried through washing, and the post processing such as roasting obtains final product the mesopore molecular sieves of Al MCM 41.The inventive method avoids using the highly energy-consuming pretreatment procedures such as high-temperature roasting, high speed ball milling or high temperature alkali fuse, and template usage amount is greatly reduced, and can also obtain Patent alum accessory substance.Therefore the method is simple and easy to do, cost has been saved.
Description
Technical field
The present invention relates to a kind of low energy consumption by kaolin or Hanggin 2#The layered clay minerals such as soil are directly synthesized Al-MCM-
The method of 41 mesopore molecular sieves, belongs to field of inorganic nonmetallic material.
Background technology
1992, Mobil (Mobil) company research staff used structure self-assembling technique, with cetyl trimethyl bromination
Ammonium (CTABr) is template, synthesis first obtains that duct is uniform, MCM-41 mesopore molecular sieves of six side's ordered arrangements (Nature,
1992,359,710-712).The declaration of ordered mesoporous molecular sieve epoch is arrived.MCM-41 mesopore molecular sieves because its catalysis, absorption,
The extensive use in field such as isolate and purify, and enjoy researcher to pay close attention to.It is Material synthesis MCM-41 with organic or inorganic silica reagent
The report of mesopore molecular sieve emerges in an endless stream.Also there is many hetero atoms (such as Al3+, Fe3+, Ga3+Deng) doping MCM-41 mesopore molecular sieve
By synthesis (Chem.Rev., 1997,97,2373-2419) in succession.But there is expensive starting materials, complex technical process etc. in these methods
Defect.Therefore, lot of domestic and international researcher has turned one's attention to and has synthesized MCM-41 mesopore molecular sieves using natural clay mineral
Research work.Wherein kaolin is because of the advantage of its global rich reserves, and correlative study is extremely more.But generally existing in these work
Problem mainly have：(1) the acidifying soil after raw ore or acidified removal of impurities can not be used directly as silicon and aluminum source, it is necessary to must be to it
Carry out the pre-treatment step rears such as 500 DEG C of high temperature above roastings, high speed ball milling or high temperature alkali fuses and can be used for synthesising mesoporous molecular sieve
(Appl.Clay Sci.,2015,107,182-187；J.Colloid Interface Sci.,2012,369,216-222；
CN102602954A), not only energy resource consumption is considerable, and product yield is low；(2) when aluminium content is higher, silicon source must additionally be added
(Appl.Clay Sci., 2007,35,155-161), increases synthesis cost.
The content of the invention
It is an object of the invention to provide one kind with layered clay mineral be unique silicon and aluminum source, only acidified pre-treatment, and nothing
Need the highly energy-consuming steps such as high-temperature roasting, high speed ball milling or high temperature alkali fuse, the side of quick Hydrothermal Synthesiss Al-MCM-41 mesopore molecular sieves
Method.The method is by conditions such as accurate Control architecture agent concentration, synthesis temperature and synthesis pH value and overcomes existing technological deficiency.
Lamellar clay raw ore of the present invention can be Coaseries kaolin 1 (Ordos of Inner Mongolia Jungar Banner,
Mainly contain kaolinite, 80 mesh sieves point, primary chemical composition (wt%)：SiO243.99, Al2O339.51), Coaseries kaolin 2 is (interior
Mongolian Huhehaote City Qingshuihe County, mainly containing kaolinite, boehmite, 80 mesh sieves point, primary chemical composition (wt%)：
SiO235.17, Al2O347.05, TiO2Or Hanggin 2 1.75)#Native (Ordos of Inner Mongolia Hangjin Banner, mainly containing concave convex rod
Stone, illite, chlorite, 200 mesh sieves point, primary chemical composition (wt%)：SiO251.57, Al2O322.72, Fe2O38.19,
CaO 5.83, MgO 5.61, K2O 4.02) in one kind.
Main technological steps of the invention are as follows：
S1. one of above-mentioned lamellar clay is pressed into 1g with 4mol/L sulfuric acid:10mL ratios mix, boiling reflux 2 hours, natural
Cooling, is once washed to neutrality, and suction filtration, 60 DEG C of dryings obtain acid-treated clay in 6 hours；
S2. 0.2mol/L sodium hydrate aqueous solutions 100mL constant temperature in 70 DEG C of water-baths is taken；
S3. cetyl trimethylammonium bromide (CTABr) is added in the solution of step 2, stirring makes it all dissolve, control
CTABr processed is 1 with the amount ratio of the material of water:1350；
S4. 4g step 1 gained acid-treated clays are added in the solution of step 3, continues to stir 1 hour；
S5. 1mol/L sulfuric acid is added dropwise in the solution of step 4, pH value of solution=10 are adjusted, continues to stir 1 hour；
S6. step 5 gained mixture is moved into having a hydrothermal reaction kettle of polytetrafluoroethyllining lining, 110 DEG C of standing crystallization
12 hours；
S7. by step 6 products therefrom suction filtration, and with being once washed to neutrality, after the drying 6 hours of 60 DEG C of solid product,
Roasting obtains final product Al-MCM-41 mesopore molecular sieves in 4 hours in 550 DEG C of air atmospheres.
The major advantage of synthetic method involved in the present invention has：(1) 4mol/L sulfuric acid used by step 1 is through hot suction filtration solid-liquid
After separation not only can crystallisation by cooling separate out Patent alum accessory substance, and reclaim sulfuric acid it is reusable in acidifying raw ore；(2) keep away
Exempt to use the highly energy-consuming pretreatment procedures such as high-temperature roasting, high speed ball milling or high temperature alkali fuse, not only shorten generated time, hence it is evident that drop
Low process energy consumption, and product yield is more than 95%；(3) bar such as accurate Control architecture agent concentration, synthesis temperature and synthesis pH value
Part, to realize and be directly synthesized Al-MCM-41 mesopore molecular sieves by acidifying lamellar clay under low template agent concentration, significantly reduces mould
The usage amount of plate agent CTABr, has saved synthesis cost.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail；It should be understood that the following example is solely for the purpose of illustration
Technical solution of the invention, rather than the scope of the present invention is limited by any way.
Embodiment 1
Al-MCM-41 mesopore molecular sieves are synthesized by Coaseries kaolin 1：Coaseries kaolin 1 and 4mol/L sulfuric acid are pressed into 1g:
10mL ratios mix, and boiling reflux 2 hours, natural cooling is once washed to neutrality, and suction filtration, 60 DEG C of dryings must be acidified height in 6 hours
Ridge soil 1.Take 0.2mol/L sodium hydrate aqueous solutions 100mL constant temperature in 70 DEG C of water-baths；CTABr 1.5g are added, stirring makes its complete
Dissolve in portion；4g acidifying kaolin 1 is added, continues to stir 1 hour；1mol/L sulfuric acid is added dropwise, pH value of solution=10 are adjusted, continues to stir
Mix 1 hour.The immigration of gained mixture has in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, and 110 DEG C stand crystallization 12 hours.It is natural
After cooling, by products therefrom suction filtration, and with being once washed to neutrality；After the drying 6 hours of 60 DEG C of solid product, in 550 DEG C of air
Roasting obtains final product Al-MCM-41 mesopore molecular sieves in 4 hours in atmosphere.Product yield and characterization result are shown in Table 1.
Embodiment 2
It is 2-in-1 into Al-MCM-41 mesopore molecular sieves by Coaseries kaolin：Coaseries kaolin 2 and 4mol/L sulfuric acid are pressed into 1g:
10mL ratios mix, and boiling reflux 2 hours, natural cooling is once washed to neutrality, and suction filtration, 60 DEG C of dryings must be acidified height in 6 hours
Ridge soil 2.Take 0.2mol/L sodium hydrate aqueous solutions 100mL constant temperature in 70 DEG C of water-baths；CTABr 1.5g are added, stirring makes its complete
Dissolve in portion；4g acidifying kaolin 2 is added, continues to stir 1 hour；1mol/L sulfuric acid is added dropwise, pH value of solution=10 are adjusted, continues to stir
Mix 1 hour.The immigration of gained mixture has in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, and 110 DEG C stand crystallization 12 hours.It is natural
After cooling, by products therefrom suction filtration, and with being once washed to neutrality；After the drying 6 hours of 60 DEG C of solid product, in 550 DEG C of air
Roasting obtains final product Al-MCM-41 mesopore molecular sieves in 4 hours in atmosphere.Product yield and characterization result are shown in Table 1.
Embodiment 3
By Hanggin 2#Soil synthesis Al-MCM-41 mesopore molecular sieves：By Hanggin 2#Soil presses 1g with 4mol/L sulfuric acid:10mL ratios
Mixing, boiling reflux 2 hours, natural cooling is once washed to neutrality, and suction filtration, 60 DEG C of dryings must be acidified Hanggin 2 in 6 hours#Soil
(atlapulgite).Take 0.2mol/L sodium hydrate aqueous solutions 100mL constant temperature in 70 DEG C of water-baths；Add CTABr 1.5g, stirring
It is set all to dissolve；4g atlapulgites are added, continues to stir 1 hour；1mol/L sulfuric acid is added dropwise, pH value of solution=10 are adjusted, after
Continuous stirring 1 hour.The immigration of gained mixture has in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, and 110 DEG C stand crystallization 12 hours.
After natural cooling, by products therefrom suction filtration, and with being once washed to neutrality；After the drying 6 hours of 60 DEG C of solid product, at 550 DEG C
Roasting obtains final product Al-MCM-41 mesopore molecular sieves in 4 hours in air atmosphere.Product yield and characterization result are shown in Table 1.
Embodiment 4
It is 2-in-1 into Al-MCM-41 mesopore molecular sieves (sulfuric acid reuse experiment) by Coaseries kaolin：By Coaseries kaolin 2 with return
Receive sulfuric acid and press 1g:15mL ratios mix, and boiling reflux 2 hours, natural cooling is once washed to neutrality, suction filtration, 60 DEG C of dryings 6
Hour obtains reuse acidifying kaolin 2.Take 0.2mol/L sodium hydrate aqueous solutions 100mL constant temperature in 70 DEG C of water-baths；Add CTABr
1.5g, stirring makes it all dissolve；4g reuses acidifying kaolin 2 is added, continues to stir 1 hour；1mol/L sulfuric acid is added dropwise, adjusts
Section pH value of solution=10, continue to stir 1 hour.The immigration of gained mixture has in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, 110 DEG C
Stand crystallization 12 hours.After natural cooling, by products therefrom suction filtration, and with being once washed to neutrality；60 DEG C of dryings 6 of solid product
After hour, roasting obtains final product Al-MCM-41 mesopore molecular sieves in 4 hours in 550 DEG C of air atmospheres.Product yield and characterization result are shown in
Table 1.
Table 1 synthesizes Al-MCM-41 mesopore molecular sieves yield and characterization result
Claims (4)
1. the method for Al-MCM-41 mesopore molecular sieves being directly synthesized by kaolin or Hanggin 2# soil, it is characterised in that：The method with
Low consumption cetyl trimethylammonium bromide is template, by accurate Control architecture agent concentration, synthesis temperature and synthesis pH value
Condition, without the highly energy-consuming pre-treatment steps such as high-temperature roasting, high speed ball milling or high temperature alkali fuse, quick Hydrothermal Synthesiss Al-MCM-41
Mesopore molecular sieve；The method comprises the following steps that,
Lamellar clay and 4mol/L sulfuric acid are pressed 1g by S1:10mL ratios mix, boiling reflux 2 hours, and natural cooling is once washed
To neutral, suction filtration, 60 DEG C of dryings obtain acid-treated clay in 6 hours；
S2 takes 0.2mol/L sodium hydrate aqueous solutions 100mL constant temperature in 70 DEG C of water-baths；
S3 adds cetyl trimethylammonium bromide in the solution of step S2, and stirring makes it all dissolve, controls CTABr and water
Material amount ratio be 1:1350；
S4 adds 4g step 1 gained acid-treated clays in the solution of step S3, continues to stir 1 hour；
S5 is added dropwise 1mol/L sulfuric acid in the solution of step S4, adjusts pH value of solution=10, continues to stir 1 hour；
S6 has step S5 gained mixture immigrations in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, and 110 DEG C of standing crystallization 12 are small
When；
S7 by step S6 products therefrom suction filtrations, and with neutrality is once washed to, after the drying 6 hours of 60 DEG C of solid product, at 550 DEG C
Roasting obtains final product Al-MCM-41 mesopore molecular sieves in 4 hours in air atmosphere.
2. the method that Al-MCM-41 mesopore molecular sieves are directly synthesized by kaolin or Hanggin 2# soil according to claim 1,
It is characterized in that：Silicon and aluminum source used is entirely Coaseries kaolin I, Coaseries kaolin II or Hanggin 2#One kind in soil, without volume
Outer other silicon and aluminum sources of addition；Coaseries kaolin I mainly contains kaolinite, 80 mesh sieves point；Coaseries kaolin II is mainly containing kaolinite, soft
Diaspore, 80 mesh sieves point；Hanggin 2#It is native mainly to contain attapulgite, illite, chlorite, 200 mesh sieves point.
3. the method that Al-MCM-41 mesopore molecular sieves are directly synthesized by kaolin or Hanggin 2# soil according to claim 1,
It is characterized in that：This method can obtain Patent alum accessory substance.
4. the method that Al-MCM-41 mesopore molecular sieves are directly synthesized by kaolin or Hanggin 2# soil according to claim 1,
It is characterized in that：In accurate Control architecture agent concentration, CTABr is 1 with the amount ratio of the material of water:1350, synthesis temperature is 70 DEG C
And synthesis pH value=10.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272057A (en) * | 2018-03-14 | 2019-09-24 | 中南大学 | A method of ordered mesoporous material Al-MCM-41 is prepared using rectorite |
| CN114713266A (en) * | 2022-05-05 | 2022-07-08 | 内蒙古师范大学 | Ammonium modified silicon oxide loaded boron oxide for propane oxidative dehydrogenation and preparation method thereof |
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| CN102198947A (en) * | 2010-03-26 | 2011-09-28 | 北京化工大学 | Preparation method for synthesizing hetero atom composite molecular sieve with natural kaolin |
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| CN1654330A (en) * | 2005-01-24 | 2005-08-17 | 复旦大学 | Method for preparing aluminium-containing MCM-41 inter-aperture molecular screen using metakaolin as raw material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272057A (en) * | 2018-03-14 | 2019-09-24 | 中南大学 | A method of ordered mesoporous material Al-MCM-41 is prepared using rectorite |
| CN114713266A (en) * | 2022-05-05 | 2022-07-08 | 内蒙古师范大学 | Ammonium modified silicon oxide loaded boron oxide for propane oxidative dehydrogenation and preparation method thereof |
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Effective date of registration: 20230411 Address after: 010300 Industrial Park, Dalu new area, Jungar banner, Ordos City, Inner Mongolia Autonomous Region Patentee after: SYNFUELS CHINA INNER MONGOLIA Co.,Ltd. Address before: 010022 No. 81, Wuda Road, Saihan District, the Inner Mongolia Autonomous Region, Hohhot Patentee before: INNER MONGOLIA NORMAL University |