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A kind of method for preparing ts-1 molecular sieve

A TS-1, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, can solve the problems of high production cost, environmental pollution and high price of molecular sieve, and achieve the effect of shortening crystallization time, reducing production cost and low pollution

Inactive Publication Date: 2016-03-16
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a kind of method for preparing TS-1 molecular sieve, only use a small amount of template agent in the process of synthetic seed crystal, compare with other method for synthesizing TS-1 molecular sieve, template agent consumption is only 1 / 1 of other methods 20~1 / 50, which solves the problems of high production cost and environmental pollution of molecular sieves caused by the high price and high toxicity of organic templates

Method used

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  • A kind of method for preparing ts-1 molecular sieve
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Embodiment 1

[0027] Add tetrapropylammonium hydroxide and deionized water to butyl titanate, stir evenly to form A solution; stir ethyl orthosilicate and deionized water evenly to prepare B solution. Add solution B slowly to solution A under stirring, stir vigorously for 3 hours to make a mixed gel, the molar composition of the mixed gel is TiO 2 : SiO 2 =1:30~150,TPAOH:SiO 2 =0.25~0.40,H 2 O: SiO 2 =8~12. Transfer the mixed gel into a closed stainless steel reaction kettle with a polytetrafluoroethylene liner, crystallize at a temperature of 130-160°C for 3-24 hours, then cool to room temperature, and make a seed crystal to be prepared use.

[0028] Add isopropanol solution to butyl titanate to make solution A; weigh silica sol, NaOH and deionized water, stir well to make solution B; add solution A to solution B to make a molar ratio of TiO 2 : SiO 2 =1:30~150, Na 2 O: SiO 2 =2.0~3.5, H 2 O: SiO 2 =20~35, TiO 2 : IPA = 1:2 mixed gel, then add a certain amount of seed crystals ...

Embodiment 2

[0030] Add 0.195g of butyl titanate to 5.0g of tetrapropylammonium hydroxide and 0.267g of deionized water, stir evenly, and prepare A solution; weigh 3.691g of tetraethyl orthosilicate and slowly add to In solution A, stir vigorously for 3 hours to form a mixed gel, and the molar composition of the mixed gel is TiO 2 : SiO 2 =1:30,TPAOH:SiO 2 =0.357,H 2 O: SiO 2 =10.8. The above mixed gel was sealed in a stainless steel reactor with a polytetrafluoroethylene liner, crystallized at 140° C. for 9 hours, then taken out and cooled to room temperature to obtain seed crystals.

Embodiment 3

[0032] To 11.5g of silica sol (SiO 2 content is 40%), add 10g of water, weigh 0.75g of NaOH and 16.75g of deionized water, add it to the silica sol, stir evenly, and make A solution; weigh 0.85g of butyl titanate and add it to 2.32g of isopropanol, And drop into the A solution to make the molar ratio TiO 2 : SiO 2 =1:30, Na 2 O: SiO 2 =2.5,H 2 O: SiO 2 =25,TiO 2 : The mixed gel of IPA=1:2, add the seed crystal that accounts for mixed gel total amount 5% that is made by the method for embodiment 2 again, transfer to the stainless steel tank with polytetrafluoroethylene liner after stirring evenly In a closed reaction kettle, crystallize at 170°C for 24 hours, cool to room temperature, centrifuge the product, wash, dry, and roast to obtain TS-1 molecular sieve with a silicon-titanium ratio of 30 (molar ratio), denoted as TS-1 (30), its XRD spectrum and SEM photos are shown in figure 1 with figure 2 . figure 1 It shows that the synthesized TS-1(30) is a pure phase TS-1...

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Abstract

A method for preparing TS-1 molecular sieve relates to a synthesis method of TS-1 molecular sieve. The invention provides a low-cost, low-pollution method capable of changing the silicon-titanium ratio (30-150) of the TS-1 molecular sieve in a wide range. The method is as follows: step 1, preparing seed crystals; step 2, preparing Template-free mixed gel; step 3, adding the seed crystal prepared in step 1 to the gel described in step 2 to crystallize, cooling, centrifugal filtering, washing, drying, and roasting to obtain TS-1 molecular sieve. The method provided by the present invention only uses a small amount of template agent in the process of synthesizing the seed crystal. Compared with other methods for synthesizing TS-1 molecular sieve, the amount of template agent is only 1 / 20~1 / 50 of other methods, which solves the problem caused by organic The high price and high toxicity of the template agent lead to high production costs of molecular sieves and environmental pollution.

Description

technical field [0001] The invention relates to a synthesis method of TS-1 molecular sieve. Background technique [0002] The orthorhombic titanium silicalite TS-1 with MFI topology endows zeolite molecular sieves with catalytic oxidation reaction characteristics due to the introduction of titanium atoms. It is one of the most important molecular sieve catalytic materials and is widely used in various catalytic oxidation reactions. , including catalyzing the epoxidation of linear and branched alkenes and cyclic alkenes, catalyzing the hydroxylation of aromatic hydrocarbons, catalyzing the ammoxidation of cyclohexanone, catalytic oxidation of linear and cyclic alkanes, and the reaction of alcohols and amines wait. [0003] At present, the synthesis of TS-1 molecular sieves uses organic amine compounds as templates, which has a series of problems such as low yield, high cost, and pollution to the environment. Contents of the invention [0004] The object of the present inv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
Inventor 武光马方伟郑柄辉
Owner HEILONGJIANG UNIV
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