CN112537776A - Preparation method of Ti-ZSM-5 molecular sieve - Google Patents
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 36
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 15
- 230000008025 crystallization Effects 0.000 claims abstract description 15
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000010457 zeolite Substances 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 6
- 238000000967 suction filtration Methods 0.000 claims abstract description 6
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 5
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 description 16
- 239000000047 product Substances 0.000 description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B39/06—Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements, i.e. by direct or secondary synthesis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/89—Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B39/36—Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
- C01B39/38—Type ZSM-5
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention provides a preparation method of a Ti-ZSM-5 molecular sieve, which mainly comprises the following steps: placing an alkali source, a silicon source, a seed crystal and a titanium source in a mortar for mixing, uniformly grinding, transferring the mixture to a reaction kettle, and crystallizing for 0.08-5 d at the temperature of 100-220 ℃; and after crystallization, carrying out suction filtration and drying on the reaction product to finally prepare the Ti-ZSM-5 zeolite molecular sieve. The preparation method of the Ti-ZSM-5 molecular sieve has the advantages of simple process and low cost, and the obtained Ti-ZSM-5 molecular sieve has good heat resistance, can effectively purify harmful gases in automobile exhaust, and has good industrial production prospect and great economic value.
Description
Technical Field
The invention relates to the field of chemical synthesis technology and application thereof, in particular to a preparation method of a Ti-ZSM-5 molecular sieve.
Background
ZSM-5 zeolite is a widely studied high-silicon zeoliteHas two mutually crossed channel systems, the ten-membered ring channel parallel to the a-axis direction is Z-shaped, and the pore diameter is
The ten-membered ring channel parallel to the b-axis direction is linear, and the aperture is
ZSM-5 is a high-silicon molecular sieve rich in five-membered rings, and double five-membered rings (D5R) are generally considered as precursors for forming ZSM-5, and are connected through a shared edge to form a skeleton chain of the ZSM-5 molecular sieve, and the skeleton chain is further connected into a sheet to form a ZSM-5 skeleton structure. First synthesized in 1972 by the company Mobil, Argauer et al. ZSM-5 has a two-dimensional ten-membered ring channel with a space group of Pmna, orthorhombic system. The unit cell parameters are: α is 90.0 °, β is 90.0 °, γ is 90.0 °, Framework Density (FDSi) is an ideal unit cell composition of the ZSM-5 molecular sieve, and may be expressed as Nan(H2O)16AlnSi96-nO192Wherein the atomic number of Al is 0-27. The ZSM-5 zeolite molecular sieve has unique pore channel structure characteristics and higher thermal stability and hydrothermal stability, so that the zeolite molecular sieve is widely applied to the petrochemical fields of hydrocarbon shape-selective cracking, alkylation, isomerization, disproportionation, etherification, dewaxing and the like.
With the popularization of automobiles, the emission of automobile exhaust causes serious pollution to the environment, so that the treatment of harmful gases in the automobile exhaust is very necessary. The catalyst is the key of the purification effect, so the development of the high-efficiency catalyst is one of the best measures for controlling the automobile exhaust emission. With the improvement of catalyst preparation technology, two active centers of oxidation and reduction coexist on the same catalyst, and finally a three-way catalyst TWC (three-way catalyst) is developed. Wherein the catalyst coating comprises gamma-Al2O3The rare earth-transition metal composite oxide and the active components of noble metals such as Pt, Rh and Pd can oxidize and reduce three pollutants (carbon monoxide (CO), Hydrocarbon (HC) and oxynitride (NO) in the exhaust gas of the enginex) Simultaneous conversion into harmless water (H)2O), carbon dioxide (CO)2) And nitrogen (N)2) However, the three-way catalyst has the disadvantages of high cost and low high temperature resistance. Therefore, it is urgently needed to develop a synthetic method of a novel automobile exhaust catalyst which is simple in synthetic method, low in cost and applicable to industrial production so as to solve the problems in the prior art.
Disclosure of Invention
In order to solve the technical problems of high cost and low high temperature resistance of the automobile exhaust purification catalyst in the prior art, the invention provides a preparation method of a Ti-ZSM-5 molecular sieve, which comprises the following steps:
1) placing an alkali source, a silicon source, a seed crystal and a titanium source in a mortar for mixing, and uniformly grinding;
2) transferring the mixture obtained in the step 1) to a reaction kettle for crystallization;
3) and after crystallization, carrying out suction filtration and drying on the reaction product to finally prepare the Ti-ZSM-5 zeolite molecular sieve.
Further, in the above technical solution, the titanium source in step 1) is tetrabutyl titanate.
Further, in the above technical solution, the alkali source in step 1) is any one of potassium hydroxide and sodium hydroxide.
Further, in the above technical solution, the silicon source in step 1) is any one of solid silica gel or white carbon black.
Further, in the above technical solution, the seed crystal in step 1) is an all-silicon ZSM-5 zeolite seed crystal.
Further, in the above technical solution, the molar ratio of the added raw materials in step 1) is 1: 0.02-0.15: 25-125.
Further, in the above technical solution, the seed crystal addition amount in the step 1) is SiO21 to 10% by mass.
Further, in the technical scheme, the crystallization temperature in the step 2) is 100-220 ℃, and the crystallization time is 0.08-5 d.
Compared with the prior art, the invention has the beneficial technical effects that:
(1) the method for preparing the Ti-ZSM-5 zeolite molecular sieve avoids the use of expensive organic template in the prior art, simplifies the synthesis process and greatly reduces the synthesis cost of the molecular sieve;
(2) the molecular sieve prepared by the invention is a high-temperature resistant catalyst, has good stability at high temperature, can effectively treat harmful gas in automobile exhaust, and plays a positive role in environmental management;
(3) the synthetic raw materials adopted by the invention are low in price and easy to obtain, have a large-scale industrial production prospect, and have important significance in the field of actual chemical production.
Drawings
The invention is further illustrated in the following description with reference to the drawings.
FIG. 1 is an XRD pattern of a Ti-ZSM-5 molecular sieve obtained in example 1 of the present invention;
FIG. 2 is an SEM image of the Ti-ZSM-5 molecular sieve obtained in example 1 of the present invention;
FIG. 3 is a graph showing the catalytic effect of the Ti-ZSM-5 molecular sieve obtained in example 1 of the present invention.
Detailed Description
The invention provides a preparation method of a Ti-ZSM-5 molecular sieve, which comprises the following steps:
1) placing an alkali source, a silicon source, a seed crystal and a titanium source in a mortar for mixing, and uniformly grinding;
2) transferring the mixture obtained in the step 1) to a reaction kettle for crystallization;
3) and after crystallization, carrying out suction filtration and drying on the reaction product to finally prepare the Ti-ZSM-5 zeolite molecular sieve.
In one embodiment, in the above technical solution, the titanium source in step 1) is tetrabutyl titanate.
In one embodiment, in the above technical solution, the alkali source in step 1) is any one of potassium hydroxide or sodium hydroxide.
In an embodiment, in the above technical scheme, the silicon source in step 1) is any one of solid silica gel and white carbon black.
In one embodiment, in the above technical scheme, the seed crystal in the step 1) is an all-silicon ZSM-5 zeolite seed crystal.
In one embodiment, in the above technical solution, the molar ratio of the added raw materials in step 1) is 1: 0.02-0.15: 25-125.
In one embodiment, in the above technical solution, the seed crystal addition amount in the step 1) is SiO2110% of the mass.
In one embodiment, in the above technical solution, the crystallization temperature in step 2) is 100 to 220 ℃, and the crystallization time is 0.08 to 5 days.
The preparation method of the Ti-ZSM-5 molecular sieve of the present invention is further illustrated with reference to the following examples.
Example 1
A preparation method of a Ti-ZSM-5 molecular sieve automobile exhaust catalyst comprises the following steps:
firstly, placing 16.70g of white carbon black, 1.54g of NaOH and 0.33g of all-silicon ZSM-5 zeolite seed crystal (2%) in a mortar for grinding for 2min, then dripping 3.75g of tetrabutyl titanate into the mixture, and uniformly grinding to obtain a reaction raw material; and finally, adding the reaction raw materials into a polytetrafluoroethylene stainless steel reaction kettle, crystallizing at 180 ℃ for 2 days to obtain complete crystallization, and performing suction filtration and drying on the product to obtain a product No. 1. The molar ratio of the reaction raw materials is as follows: SiO 22:Na2O:TiO2＝1:0.07:0.04。
The XRD spectrum of this example is shown in fig. 1, and it can be seen from the scanning electron micrograph that the synthesized product is in the form of a block, which is typical of the ZSM-5 zeolite molecular sieve.
Example 2
A preparation method of a Ti-ZSM-5 molecular sieve automobile exhaust catalyst comprises the following steps:
placing 17.27g of white carbon black, 1.59g of NaOH and 0.34g of all-silicon ZSM-5 zeolite seed crystal (2%) in a mortar for grinding for 2min, then dropwise adding 0.97g of tetrabutyl titanate into the mixture, and uniformly grinding to obtain a reaction raw material;and finally, adding the reaction raw materials into a polytetrafluoroethylene stainless steel reaction kettle, crystallizing at 180 ℃ for 2 days to obtain complete crystallization, and performing suction filtration and drying on the product to obtain a product No. 2. The molar ratio of the reaction raw materials is as follows: SiO 22:Na2O:TiO2＝1:0.07:0.01。
XRD and SEM analysis of the 2# Ti-ZSM-5 zeolite molecular sieve shows that the X-ray diffraction pattern is the same as that in attached figure 1 and the scanning electron microscope is similar to that in attached figure 2.
The Ti-ZSM-5 molecular sieve automobile prepared in the example 1 is used as an automobile exhaust catalyst, the conversion rates of CO and NO in automobile exhaust are examined, and the test is carried out in a fixed bed reactor. The measurement method is as follows:
adding the Ti-ZSM-5 molecular sieve automobile exhaust catalyst into a fixed bed reactor, introducing CO and NO into the fixed bed reactor by using argon as carrier gas, heating the fixed bed reactor at the heating rate of 2 ℃/min, and finally heating to 620 ℃. The conversion rates of CO and NO are tested, and the curve of the change relationship of the conversion rates of CO and NO with the temperature is shown in figure 3. It can be seen from fig. 3 that the catalytic reaction starts to occur at 300 c and the highest catalytic efficiency is reached at 620 c. Finally, the conversion rate of NO in the automobile exhaust reaches 92 percent, the conversion rate of CO reaches 84 percent,
therefore, the catalyst prepared by the method can perform CO catalysis and NO reduction reactions at higher temperature. The temperature is more consistent with the actual environment temperature for treating the automobile exhaust. The product related to the invention has potential practical application value.
The above embodiments are only for further illustration of the present invention and are not intended to limit the present invention, and all equivalent implementations of the present invention should be included in the scope of the claims of the present invention. The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (8)
1. A preparation method of a Ti-ZSM-5 molecular sieve is characterized by comprising the following steps:
1) placing an alkali source, a silicon source, a seed crystal and a titanium source in a mortar for mixing, and uniformly grinding;
2) transferring the mixture obtained in the step 1) to a reaction kettle for crystallization;
3) and after crystallization, carrying out suction filtration and drying on the reaction product to finally prepare the Ti-ZSM-5 zeolite molecular sieve.
2. The method of claim 1, wherein the titanium source in step 1) is tetrabutyl titanate.
3. The method for preparing the Ti-ZSM-5 molecular sieve of claim 1, wherein the alkali source in step 1) is one or both of potassium hydroxide and sodium hydroxide.
4. The method for preparing the Ti-ZSM-5 molecular sieve of claim 1, wherein the silicon source in step 1) is one or both of solid silica gel and white carbon black.
5. The method of claim 1, wherein the seeds in step 1) are all-silica ZSM-5 zeolite seeds.
6. The method for preparing the Ti-ZSM-5 molecular sieve according to claim 1, wherein the molar ratio of the raw materials added in the step 1) is 1: 0.02-0.15: 25-125.
7. The preparation method of the Ti-ZSM-5 molecular sieve of claim 1, wherein the seed crystal is added in step 1) in an amount of 1-10% by mass of the silicon source.
8. The method for preparing the Ti-ZSM-5 molecular sieve of claim 1, wherein the crystallization temperature in step 2) is 100-220 ℃ and the crystallization time is 0.08-5 d.
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|---|---|---|---|---|
| CN103553068A (en) * | 2013-11-14 | 2014-02-05 | 黑龙江大学 | Method for preparing TS-1 molecular sieve |
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2020
- 2020-12-23 CN CN202011537561.7A patent/CN112537776A/en active Pending
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| Title |
|---|
| LONGFENG ZHU ET AL.: "Solvent-free synthesis of titanosilicate zeolites", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
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