Fine grain strong acid type molecular sieve and method for synthesizing same

A synthesis method and molecular sieve technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve problems such as product loss, affecting product yield, and difficulty in the filtration process, so as to simplify the production process and shorten the production process. The effect of synthesis cycle and high selectivity

Active Publication Date: 2007-09-26
天津南化催化剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, in actual production, due to the fine grain size of the molecular sieve, the filtration process of separating it from the water phase is difficult, which can easily cause product loss and affect the product yield.

Method used

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  • Fine grain strong acid type molecular sieve and method for synthesizing same
  • Fine grain strong acid type molecular sieve and method for synthesizing same
  • Fine grain strong acid type molecular sieve and method for synthesizing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 20.3 kg of water glass (SiO 2 : 27.2% Na 2 O: 6.1%) and 22 kilograms of deionized water are mixed evenly, and the solution formulated by 1.5 kilograms of aluminum sulfate, 40 kilograms of deionized water and 0.16 kilograms of sulfuric acid is added under stirring, and ultrasonic pretreatment is carried out for 1 hour, and the treatment temperature is controlled at room temperature to 70°C. Then the autoclave was sealed and kept at a constant temperature of 170° C. for 20 hours. The reaction mixture was cooled, and then the molecular sieves were washed and concentrated by filtration with a ceramic filter element, and then ion exchange was performed with 1 mol / L nitric acid at room temperature for 6 hours. Finally, after fully washing until the solution is neutral, it is dried at 120° C. for 4 hours to obtain product A. It can be clearly seen that the product is a ZSM-5 molecular sieve through its X-ray diffraction pattern (Fig. 1). Analysis of its SiO by other 2 / Al...

Embodiment 2

[0029] 22.0 kg of water glass (SiO 2 : 27.2% Na 2O: 6.1%) was mixed evenly with 28 kilograms of deionized water, and a solution prepared by 2.3 kilograms of aluminum sulfate, 40 kilograms of deionized water and 2.6 kilograms of phosphoric acid was added under stirring, and ultrasonic pretreatment was carried out for 5 hours, and the treatment temperature was controlled at room temperature to 70°C. Then, the autoclave was sealed and kept at a constant temperature of 180° C. for 10 hours. The reaction mixture was cooled, and then the molecular sieve was washed and concentrated by filtration with a ceramic filter element, followed by ion exchange with 1 mol / L hydrochloric acid at 60° C. for 4 hours. Finally, after fully washing until the solution is neutral, it is dried at 110° C. for 5 hours to obtain product B. It can be clearly seen that the product is a ZSM-5 molecular sieve through its X-ray diffraction pattern (Fig. 3). Analysis of its SiO by other 2 / Al 2 o 3 =25, t...

Embodiment 3

[0031] 18.9 kg of water glass (SiO 2 : 27.2% Na 2 O: 6.1%) mixes evenly with 20 kilograms of deionized water, adds the solution prepared by 1.2 kilograms of aluminum sulfate, 20 kilograms of deionized water and 0.77 kilograms of sulfuric acid under stirring, mixes 35 kilograms of filtrates (solid matter) in other examples content of about 4%), ultrasonic pretreatment was carried out for 3 hours, and the treatment temperature was controlled at room temperature to 70°C. Then, the autoclave was sealed and kept at a constant temperature of 190° C. for 5 hours. The reaction mixture was cooled, and then the molecular sieves were washed and concentrated by filtration with a ceramic filter element, followed by ion exchange with 1 mol / L sulfuric acid at 70° C. for 3 hours. Finally, after fully washing until the solution is neutral, it is dried at 130° C. for 4 hours to obtain product C. It can be clearly seen that the product is a ZSM-5 molecular sieve through its X-ray diffraction ...

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Abstract

The invention discloses a synthetic method of fine grain strong acid type ZSM-5 molecular sieve, which comprises the following steps: fetching silica dioxide and aluminum oxide; allocating mole ratio at 15-100, junior particle diameter at 0.01-0.5 mu m and surface area at 300-550m2 / g; making silica source, aluminium source and inorganic acid as raw material; fore-treating through supersonic wave; hydrothermal blooming; filtering; exchanging; washing; filtering and drying under exciting seed or non-exciting seed condition; getting the product. The molecular sieve possess higher active, which can product cyclohexanol effectively.

Description

1. Technical field [0001] The invention relates to a small-grain strong-acid ZSM-5 molecular sieve and a synthesis method thereof. More particularly, it relates to a ZSM-5 molecular sieve catalyst used for hydration of cyclohexene to produce cyclohexanol and a synthesis method thereof. 2. Background technology [0002] With the development of nylon 6, nylon 66 and other industries worldwide, the demand for cyclohexanol (ketone) continues to grow. At present, the production of cyclohexanol (ketone) has three methods: cyclohexane oxidation, cyclohexene hydration, and cyclohexane biomimetic catalysis. Among them, the production cost of the cyclohexane oxidation method is 20% higher than that of the cyclohexene hydration method, and the production cost of the cyclohexane biomimetic catalysis method is reported to be still below the level of the cyclohexene hydration method. It has an industrial level, and another key to the cyclohexene hydration method is the cyclohexene hydra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38B01J29/06
Inventor 曹刚邹连生姜继锁景国耀梁巍吴华文刘国梁朱卫东李识寒
Owner 天津南化催化剂有限公司
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