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Method for preparing titanium-silicon molecular sieve and method for preparing cyclohexane oxime by using molecular sieve

A technology of silicon molecular sieve and molecular sieve, which is applied in the field of large particle size titanium-silicon molecular sieve preparation, can solve the problems of increasing the amount of catalyst and insufficient reactivity

Active Publication Date: 2011-08-17
CHINA PETROCHEM DEVMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patents No. 5500199, No. 6106803 and No. 6524984 teach the use of inorganic adhesives to aggregate small particle catalysts and then spray-dry and granulate them. Although this method can increase the size of catalyst particles, it has the disadvantage that the active groups of the catalyst are covered by the adhesive. And the lack of reactivity caused by the dilution of the active group and the need to increase the amount of catalyst to maintain the same catalytic effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0015] Firstly, a 500 ml round bottom flask was nitrogen blanketed in a vacuum system, 1.98 g of tetra-n-butyl titanate was added into the nitrogen blanketed round bottom flask, and the temperature was cooled to 5°C. Next, 20 grams of anhydrous isopropanol was injected into the above-mentioned nitrogen-covered round-bottomed flask with a syringe, and stirring was started simultaneously. After the temperature was balanced, 30 g of tetraethylsilicate was added dropwise into a nitrogen-sealed round-bottom flask with an isobaric feeding system, and stirred for 1 hour after the dropwise addition was completed. Take 28 grams (40%) of tetra-n-propylammonium hydroxide aqueous solution and add it dropwise into a nitrogen-covered round-bottom flask with an isobaric feeding system, and stir for 1 hour after the dropwise addition is completed. After the system was brought back to room temperature, it was stirred for 1 hour, and finally alcohol was removed at 80° C. for 2 hours, and water ...

Embodiment 1

[0019] Take 0.8 grams of uncalcined titanium-silicon molecular sieve TS-1, disperse it in 40 milliliters of water with stirring, add 3.5 milliliters of 0.5% by weight anionic flocculant (sodium acrylate and acrylammonium copolymer, average molecular weight is 15,000,000 to 20,000,000) aqueous solution, after being stirred for 1 hour, 1.5 g of tetramethylsilicate was added, and stirred for another 1 hour to form a suspension of aggregated particles.

[0020] The above-mentioned suspension of aggregated particles was mixed with 100 grams of the titanium-silicon template synthetic gel of Preparation Example 1 and stirred for 1 hour, and then the mixed solution was sealed in a Teflon-lined stainless steel pressure tank, and heated in water at 170° C. for 120 hours. After separating the solid from the liquid, the solid part was washed with pure water until neutral, dried at 100° C. and calcined at 500° C. for 24 hours to obtain titanium-silicon molecular sieve sample 1. (average pa...

Embodiment 2

[0022] Take 0.7 grams of uncalcined titanium-silicon molecular sieve TS-1, disperse it in 40 milliliters of water with stirring, add 1.5 milliliters of 0.5% by weight anionic flocculant (sodium acrylate and acrylammonium copolymer, average molecular weight is 15,000,000 to 20,000,000) aqueous solution, after stirring for 1 hour, add 0.43 g of ES-40, and then stir for 1 hour to form a suspension of aggregated particles.

[0023] The above-mentioned suspension of aggregated particles was mixed with 100 grams of the titanium-silicon template synthetic gel of Preparation Example 1 and stirred for 1 hour, and then the mixed solution was sealed in a Teflon-lined stainless steel pressure tank, and heated in water at 170° C. for 120 hours. After separating the solid from the liquid, the solid part was washed with pure water until neutral, dried at 100° C. and calcined at 500° C. for 24 hours to obtain titanium-silicon molecular sieve sample 2. (average particle size is 8.9 microns, me...

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Abstract

The invention provides a method for preparing a titanium-silicon molecular sieve with large particle diameter. The method comprises the following steps of: preparing dispersion liquid of a first-level crystalline particle molecular sieve; adding a flocculating agent and a coagulant aid into the dispersion liquid, and gathering the particles so as to form gathered particle solution; mixing the gathered particle solution and titanium-silicon template synthetic cement; and performing a hydrothermal process. The titanium-silicon molecular sieve prepared by the method has an average particle diameter of more than 5 microns; and when serving as a contact agent for preparing cyclohexane oxime, the titanium-silicon molecular sieve has high conversion rate and selection rate, and has the advantage of easiness for filtering and recycling.

Description

technical field [0001] The invention relates to a method for preparing a titanium-silicon molecular sieve, in particular to a method for preparing a large-diameter titanium-silicon molecular sieve. Background technique [0002] Crystalline titanium-silicon molecular sieve is a crystal form with MFI structure by introducing titanium atoms into the network structure of silica, also known as TS-1 molecular sieve. The molecular sieve is widely used as a catalyst in the oxidation reaction using hydrogen peroxide as an oxidant, and its preparation method has been disclosed in the US Patent No. 4410501. However, the molecular sieve particles produced by this method are about 0.2 microns. However, the 0.2-micron catalyst faces great challenges in chemical process applications (such as the use of cyclohexanone, ammonia, hydrogen peroxide and other reactants to prepare cyclohexanone oxime with titanium-silicon molecular sieves as catalysts). Therefore, subsequent inventors have devo...

Claims

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Application Information

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IPC IPC(8): C01B39/08B01J29/89C07C251/44C07C249/04
Inventor 姚秉铎谢正发赵士尧梁扬闵
Owner CHINA PETROCHEM DEVMENT
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