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Molecular sieves with shape-selective properties and their direct synthesis

A molecular sieve and performance technology, applied in molecular sieve catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problems of high production cost, cumbersome process operation, and many preparation steps, and achieve high energy saving and emission reduction efficiency, and a wide range of operations. , the effect of high selectivity

Active Publication Date: 2018-11-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Generally speaking, an amorphous silicon oxide layer will form on the surface of ZSM-5 molecular sieve after being treated with a silicon-containing organic solution. A series of ZSM-5 with different surface structures can be obtained by changing the organic silicon treatment conditions and processes, but the process is cumbersome and the production high cost
In the synthesis process of core-shell molecular sieves, different surface structures can induce the growth of shell structures with different coverages, but the core-shell molecular sieves synthesized by this method need to be synthesized step by step, that is, the core-phase molecular sieves are synthesized first, and the silicalite is adhered to the core-shell molecular sieves. -1 and then secondary growth to obtain core-shell molecular sieves, the preparation steps are numerous, and the repeatability of industrial operations is poor
[0011] It can be seen from the above that the technology of aromatic hydrocarbon alkylation has made some progress in recent years, but the shape-selective modification methods used often have problems such as many preparation steps and poor repeatability of industrial operations.

Method used

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  • Molecular sieves with shape-selective properties and their direct synthesis
  • Molecular sieves with shape-selective properties and their direct synthesis
  • Molecular sieves with shape-selective properties and their direct synthesis

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Experimental program
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Effect test

Embodiment 1

[0057] Water, tetraethyl orthosilicate, aluminum isopropoxide, sodium hydroxide and tetrapropylammonium bromide are composed of moles of each component (in terms of oxides) Na 2 O / SiO 2 =0.66, (TPA) 2 O / SiO 2 =15, SiO 2 / Al 2 o 3 =350,H 2 O / SiO 2 =290 Prepare solution A (water+tetrapropylammonium bromide+sodium hydroxide), solution B1 (water+aluminum isopropoxide) and solution B2 (water+tetraethylorthosilicate).

[0058] First put solution A in a closed container with stirring, and after stirring for 0.5 hours, slowly add solution B1, stir evenly after adding, add solution B2 slowly, and control the pH value between 12-13. After stirring evenly, gradually raise the temperature to 100°C and keep it for 12 hours for aging, then put it into a crystallization kettle, slowly raise the temperature to 150°C for crystallization, and keep it for 30 hours. After the end, quenched, filtered the solid product, washed with deionized water, dried at 120°C, and calcined at 550°C for ...

Embodiment 2

[0062] Water, tetraethyl orthosilicate, aluminum isopropoxide, potassium hydroxide and tetrapropylammonium bromide are composed of moles of each component (in terms of oxides) K 2 O / SiO 2 =0.66, (TPA) 2 O / Al 2 o 3 = 21, SiO 2 / Al 2 o 3 =150,H 2 O / SiO 2 =690 Prepare solution A (water+tetrapropylammonium bromide+sodium hydroxide), solution B1 (water+aluminum isopropoxide) and solution B2 (water+tetraethylorthosilicate).

[0063] First, put solution A in a stirrer, and after stirring for 0.5 hours, slowly add solution B1, stir evenly after adding, add solution B2 slowly, and control the pH value to be greater than 9. Heat to 70°C, stir and age for 5 hours, then put into the crystallization kettle, crystallize at 180°C for 24 hours, take out the crystallization kettle, quench in water, filter the solid product, wash with deionized water, dry at 120°C, and roast at 550°C for 5 hours , to obtain the molecular sieve SS-2 with an overall silicon-aluminum ratio of 120 and an M...

Embodiment 3

[0069] Water, activated clay, aluminum isopropoxide, sodium hydroxide and ammonium fluoride are composed of moles of each component (calculated as oxides) Na 2 O / SiO 2 =0.66, NH 4 F / SiO 2 = 0.12, SiO 2 / Al 2 o 3 =80,H 2 O / SiO 2 =400 Prepare solution A (water+ammonium fluoride+sodium hydroxide), solution B1 (water+aluminum isopropoxide) and solution B2 (water+activated clay).

[0070] First put solution A in a stirrer, and after stirring for 0.5 hours, slowly add solution B1, stir evenly after adding, add solution B2 slowly, and control the pH value to 11. Heat to 100°C, stir and age for 12 hours, put it into the crystallization kettle, raise the temperature to 170°C and crystallize for 36 hours, take out the crystallization kettle, quench in water, filter the solid product, wash with deionized water, dry at 120°C, and roast at 550°C for 5 hours , to obtain the molecular sieve SS-3 with an overall silicon-aluminum ratio of 75 and an MFI structure. Characterized by XPS,...

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Abstract

The invention relates to a molecular sieve with shape-selective performance and a direct synthesis method thereof. The content of aluminum on the outer surface of the molecular sieve is lower than that of bulk phase aluminum; in the room-temperature static absorption test of the molecular sieve, pX / mX is larger than 8, wherein pX is p-xylene, and mX is m-xylene. The molecular sieve can be applied to the shape-selective catalytic reaction of toluene and / or benzene and alkylating reagents.

Description

technical field [0001] The invention relates to a molecular sieve with shape-selective performance and a direct synthesis method thereof. Background technique [0002] As one of the most important basic organic chemical raw materials, the demand for p-xylene has shown a strong growth trend in the past five years. Due to the rapid development of the downstream main product PTA industry, the market demand for PX will continue to rise rapidly in the next few years. It is expected that the average annual growth rate of demand will be 24.9%, and the annual consumption growth rate will reach 22.4%. By 2010, China's PTA plant consumption of PX will reach 5.4-6.1 million tons, and the construction of production capacity is far behind the growth of demand. The gap between China's PX demand and production will further expand. [0003] Aromatic alkylation is a catalytic reaction in which aromatic compounds react with an alkylating agent to produce p-xylene. At present, the most studi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02C01B39/04B01J29/40C07C2/88C07C15/08
CPCY02P20/52
Inventor 邹薇孔德金周亚新管卉李旭光
Owner CHINA PETROLEUM & CHEM CORP