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Microsphere TS-1 catalyst and preparation method of microsphere TS-1 catalyst
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A technology of TS-1 and catalyst, applied in the field of microsphere TS-1 catalyst and its preparation, can solve the problem that there is no report of microsphere TS-1 catalyst with high catalytic activity, etc., and achieve the effect of easy industrial implementation and good mechanical strength
Inactive Publication Date: 2012-11-28
EAST CHINA NORMAL UNIV
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Problems solved by technology
[0008] There is no report on microspherical TS-1 catalyst with high catalytic activity
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Embodiment 1
[0027] In the first step, SiO in molar ratio silicon source 2 : Organic base template agent: TiO in titanium source 2 :H 2 O: crystallization aid is 1:0.2 : 0.033 :15 : 2.5×10 -3 , to prepare the reaction mixture solution; in the third step, the reaction mixture prepared in the second step was first crystallized at 80°C for 20 hours, then crystallized at 120°C for 5 hours, and finally crystallized at 170°C for 12 hours, and the crystallization was good The reaction mixture was filtered, washed, dried and calcined to obtain the microsphere TS-1 catalyst.
[0028] The scanning electron micrographs of the microsphere TS-1 catalyst are as follows: figure 1 , figure 2 As shown, the shape of the catalyst is spherical, and the particle diameter is about 10 μm. The XRD spectrum of the microsphere TS-1 catalyst is as follows image 3 As shown, the catalyst is pure phase TS-1 molecular sieve.
Embodiment 2
[0030] Implementation process is except following difference, and all the other are all the same with embodiment 1:
[0031] In the first step, SiO in molar ratio silicon source 2 : Organic base template agent: TiO in titanium source 2 :H 2 O: crystallization aid is 1:0.2 : 0.033 :15 : 1.5×10 -3 , Prepare the reaction mixture solution to obtain the microsphere TS-1 catalyst.
[0032] The SEM image of the microsphere TS-1 catalyst is similar to figure 1 , figure 2 , the shape of the catalyst is spherical, and the particle diameter is about 3 μm. The XRD pattern of microsphere TS-1 catalyst is similar to image 3 , the catalyst is pure phase TS-1 molecular sieve.
Embodiment 3
[0034] Implementation process is except following difference, and all the other are all the same with embodiment 1:
[0035] In the first step, SiO in molar ratio silicon source 2 : Organic base template agent: TiO in titanium source 2 :H 2 O: crystallization aid is 1:0.18 : 0.033 :20 : 3.5×10 -3 , to prepare the reaction mixture solution. In the third step, the reaction mixture prepared in the second step was first crystallized at 80°C for 10 hours, then crystallized at 110°C for 10 hours, and finally crystallized at 170°C for 20 hours to obtain microspheres TS-1 catalyst.
[0036] The SEM image of the microsphere TS-1 catalyst is similar to figure 1 , figure 2 , the shape of the catalyst is spherical, and the particle diameter is about 75 μm. The XRD pattern of microsphere TS-1 catalyst is similar to image 3 , the catalyst is pure phase TS-1 molecular sieve.
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Abstract
The invention discloses a microsphere TS-1 catalyst and a preparation method of the microsphere TS-1 catalyst, wherein the catalyst in the microspheric shape is a pure phase TS-1 molecular sieve with the dimension of 2 to 100 microns; the preparation method of the microsphere TS-1 catalyst comprises the steps of: based on the molar ratio of SiO2 in silicon source: organic base template agent: TiO2 in titanium source: H2O: crystallization auxiliary of 1: (0.05-0.4): (0.005:0.2): (10-30): (1.0*10-3 to 4.0*10-3), preparing reaction mixture solution, hydrolyzing and gelating the reaction mixture solution at the temperature from 50 to 60 DEG C for 0.5 to 1 hour, then transferring the reaction mixture colloidal sol to a high pressure reaction kettle for being crystallized at the temperature from 80 to 180 DEG C, filtering, washing, drying and calcining the crystallized reaction mixture to obtain the microsphere TS-1 catalyst. The catalyst of the invention in the microspheric shape has good mechanical strength, is easy to be separated from liquid phase substances in reaction system, and has the catalytic activity equivalent to that of TS-1 molecular sieve fine powder; besides the introduction of the crystallization auxiliary, the preparation method of the microsphere TS-1 catalyst is the same as the conventional TS-1 molecular sieve synthesis process, has no particular production equipment and process requirement, and is easy to realize industrial application.
Description
technical field [0001] The invention relates to a microsphere TS-1 catalyst and a preparation method thereof, belonging to the technical field of inorganic chemical synthesis. Background technique [0002] Titanium-silicon molecular sieve is the introduction of transition metal titanium atoms into the molecular sieve framework with a certain topology to form a porous crystalline material with catalytic oxidation activity. Using titanium silicate molecular sieve as catalyst and dilute H 2 o 2 It is a mild reaction system formed by an oxidant. It exhibits high activity and selectivity in organic oxidation reactions such as olefin epoxidation, aromatic hydrocarbon hydroxylation, ketone ammonia oximation, alkane oxidation, and alcohol oxidation. The by-product is only water. The environmentally friendly green chemical process has attracted widespread attention. TS-1 is a titanium-silicon molecular sieve with MFI topology, which was first reported in US 4,410,501 in 1983. [...
Claims
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