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Method for modifying mesoporous-rich USY (Ultra-Stable Y) molecular sieve in combined manner

A molecular sieve, rich mesopore technology, applied in the direction of crystalline aluminosilicate zeolite, favhedral crystalline aluminosilicate zeolite, etc., can solve the problems of unfavorable industrialization, harsh modification conditions, and high EDTA price.

Inactive Publication Date: 2014-12-24
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But using SiCl 4 , EDTA and (NH 4 ) 2 SiF 6 The modification conditions are relatively harsh, and EDTA is expensive, which is not conducive to the realization of industrialization

Method used

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  • Method for modifying mesoporous-rich USY (Ultra-Stable Y) molecular sieve in combined manner
  • Method for modifying mesoporous-rich USY (Ultra-Stable Y) molecular sieve in combined manner
  • Method for modifying mesoporous-rich USY (Ultra-Stable Y) molecular sieve in combined manner

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0025] Weigh 12g of a fixed amount of industrial USY and pour it into a 250ml three-necked flask (plastic); according to the design ratio of the orthogonal test (orthogonal test, see Table 1), measure a certain concentration and a certain amount of citric acid and ammonium fluoride Salt solution; at room temperature, use a 250ml three-necked flask as a reactor, install and stir, and set a certain water bath temperature to start the reaction; after the water temperature reaches the set temperature, record the time. After reacting at constant temperature for a certain period of time, wash and filter until the surface of the sample is neutral; put it in an oven at 110°C, dry at constant temperature for 16 hours, and grind to obtain a modified sample. Through the visual analysis of the orthogonal test, the optimal modification conditions for the industrial USY adopted are citric acid concentration 0.4mol / L, MAP concentration 0.2mol / L, volume ratio 0.5, reaction time 8h, reaction te...

example 2

[0027] Prepare the required 0.4mol / L citric acid solution and 0.2mol / L ammonium fluoride salt solution; enlarge the modification scale by 4 times, weigh 48g of industrial USY and pour it into a 1L autoclave; according to the optimal condition ratio , Measure 160ml of citric acid solution and 320ml of ammonium fluoride solution respectively, install and stir, install the kettle, and set the temperature of the inner kettle to 90°C; when the temperature of the inner kettle reaches the set temperature, record the time. After 8 hours of constant temperature reaction, wash and filter until the surface of the sample is neutral; put it in an oven at 110°C, dry it at a constant temperature for 16 hours, and grind to obtain a modified sample in a large kettle.

Embodiment 3

[0033] This example is the determination of the specific surface area, pore volume and skeleton information of the above-mentioned modified USY, see Table 2 and Table 3.

[0034] Table 1 USY modified orthogonal test table

[0035]

[0036]

[0037] Table 2 Specific surface area and pore distribution of modified USY molecular sieves

[0038]

[0039] Table 3 Crystal structure parameters of modified USY molecular sieves

[0040]

[0041] Combining modified USY can achieve better results than individual organic acid and inorganic salt modification. The modified USY molecular sieve sample has a high micropore retention rate, a large increase in specific surface area, and an increase in the proportion of secondary pores (>0.20cm 3 / g), and at the same time maintain a high degree of crystallinity (>75%), the ratio of silicon to aluminum increases, and the unit cell constant decreases.

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Abstract

The invention relates to a method for modifying a USY (Ultra-Stable Y) molecular sieve. The method is characterized in that organic acid and an inorganic salt dealuminizing reagent are simultaneously added in a modifying process for organic acid-inorganic salt combined modification, and optimum process conditions, namely optimum concentration, volume ratio, reaction time, reaction temperature and the like, of an organic acid and an inorganic salt solution are determined by virtue of an orthogonal test. Compared with an industrial USY molecular sieve, the USY molecular sieve obtained by adopting the method disclosed by the invention is obviously increased in secondary pore content, can be kept at higher crystallinity and is enhanced in silica-alumina ratio, reduced in lattice constant and suitable for high-medium oil type hydrocracking catalyst carriers.

Description

technical field [0001] The invention relates to a combined modification method of a mesoporous-rich ultrastable Y molecular sieve. This method is to dealuminate the industrial USY by adding organic acid and inorganic salt at the same time, which can maintain high crystallinity while forming more secondary pores, increase the silicon-aluminum ratio, and reduce the unit cell constant. technical background [0002] At present, the demand for high-quality middle distillate products (diesel, civil fuel oil, jet fuel and kerosene) in domestic and foreign oil markets has been increasing. The Cambridge Energy Research Association (CERA) predicts that if the global refinery configuration remains unchanged in 2007 and the conversion capacity increases in proportion to 2007, there will be a shortage of 3 million bbl / d of middle distillates by 2020. Hydrocracking is an important secondary processing technology in the oil refining industry. It can directly produce high-quality middle di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/24
Inventor 阎子峰刘欣梅昌兴文张志华秦丽红戴宝琴高雄厚张忠东
Owner PETROCHINA CO LTD
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