Composite molecular sieve, desulfurization adsorbent and preparation method and application thereof

A composite molecular sieve and adsorbent technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, refined hydrocarbon oil, etc., can solve the problems of frequent regeneration of adsorbents, high energy consumption, and low sulfur adsorption capacity, and achieve good selection , high adsorption capacity and long service life

Active Publication Date: 2020-07-17
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Publication No. CN103182291A discloses a preparation method and application of a deep desulfurization adsorbent for pyrolysis C5 distillate oil. The desulfurization adsorbent used uses activated alumina as a carrier, impregnated with Zn, Cu, and Group ⅠA or ⅡA metal salts, and then dried When the adsorbent is used for desulfurization of cracked C5 distillate oil, C5 raw material oil with sulfur content lower than 1ppmw can be obtained, but the sulfur adsorption capacity is not high, the adsorbent regeneration is frequent, and the energy consumption is high

Method used

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  • Composite molecular sieve, desulfurization adsorbent and preparation method and application thereof
  • Composite molecular sieve, desulfurization adsorbent and preparation method and application thereof
  • Composite molecular sieve, desulfurization adsorbent and preparation method and application thereof

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Effect test

Embodiment 1

[0045] This embodiment provides a method for preparing a desulfurization adsorbent, the preparation process of which is as follows:

[0046] 1. Preparation of zinc in situ modified mordenite molecular sieve:

[0047] (1) Take 4.6g of Zn(NO 3 ) 2 ·6H 2 O is dissolved in the deionized water of 50ml, prepares zinc nitrate solution, stand-by;

[0048](2) Dissolve 12.0g of NaOH in 200ml of deionized water, then add 19.5g of NaAlO 2 , stirred until a clear solution is formed;

[0049] (3) Add 306.0g of silica sol (SiO 2 Content 30wt%), after stirring to form sol, then pour into zinc nitrate solution, stir evenly;

[0050] (4) Transfer the sol solution to a hydrothermal reaction kettle, and crystallize at 150° C. for 90 hours;

[0051] (5) After the crystallization is completed, the product is filtered, dried at 100°C for 10 hours, and then roasted at 500°C for 3 hours to obtain a zinc in-situ modified mordenite molecular sieve, calculated as zinc oxide, zinc The content is a...

Embodiment 2

[0112] This embodiment provides a method for preparing a desulfurization adsorbent, the preparation process of which is as follows:

[0113] 1. Preparation of zinc in situ modified ZSM-5 molecular sieve:

[0114] (1) Take 2.5g of ZnCl 2 Dissolve in 50ml of deionized water to prepare a zinc chloride solution for use;

[0115] (2) Dissolve 14.2g of NaOH in 400ml of deionized water, then add 12.5g of NaAlO 2 And the tetraethylammonium hydroxide solution (25wt%) of 25.0g, stir until forming clear solution;

[0116] (3) Add 294.0g of silica sol (SiO 2 Content 30wt%), after stirring to form sol liquid, then pour into zinc chloride solution, stir evenly;

[0117] (4) Transfer the sol solution to a hydrothermal reaction kettle, and crystallize at 180° C. for 40 hours;

[0118] (5) After the crystallization is completed, filter the product, dry it at 110°C for 10 hours, and then roast it at 500°C for 3 hours to obtain a zinc in-situ modified ZSM-5 molecular sieve, calculated as zi...

Embodiment 3

[0129] This embodiment provides a method for preparing a desulfurization adsorbent, the preparation process of which is as follows:

[0130] 1. Preparation of zinc in situ modified ZSM-5 molecular sieve:

[0131] (1) Take 4.2g of Zn(NO 3 ) 2 ·6H 2 O was dissolved in 40ml deionized water to prepare a zinc nitrate solution for use;

[0132] (2) Dissolve 14.2g of NaOH in 400ml of deionized water, then add 7.9g of NaAlO 2 And the tetraethylammonium hydroxide solution (25wt%) of 25.0g, stir until forming clear solution;

[0133] (3) Add 327.0g of silica sol (SiO 2 Content 30wt%), after stirring to form sol, then pour into zinc nitrate solution, stir evenly;

[0134] (4) Transfer the sol solution to a hydrothermal reaction kettle, and crystallize at 180° C. for 40 hours;

[0135] (5) After the crystallization is completed, filter the product, dry it at 110°C for 10 hours, and then roast it at 500°C for 3 hours to obtain a zinc in-situ modified ZSM-5 molecular sieve, calculate...

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Abstract

The invention provides a composite molecular sieve, a desulfurization adsorbent as well as a preparation method and application thereof. The preparation method of the composite molecular sieve comprises the following steps: adding a template agent for preparing a mesoporous molecular sieve into an alkaline solution, and stirring to obtain a clear solution; adding a metal zinc in-situ modified silicon-aluminum molecular sieve into the clear solution, and stirring to obtain a turbid liquid; adding a silicon source into the turbid liquid for stirring reaction, and filtering, drying and roasting after reaction to obtain the composite molecular sieve. The desulfurization adsorbent is prepared from the following raw materials in parts by weight: 30-70 parts of a composite molecular sieve, 1-10 parts of an IA group and / or IIA group metal oxygen-containing compound precursor and 30-60 parts of a binder. The desulfurization adsorbent disclosed by the invention is high in adsorption capacity, good in selectivity, high in desulfurization precision, capable of being recycled and long in service life; and C5 oil desulfurized by the desulfurization adsorbent can be directly used as a raw material for high-value utilization.

Description

technical field [0001] The invention belongs to the technical field of desulfurization adsorbents, and relates to a composite molecular sieve, a desulfurization adsorbent and a preparation method and application thereof, in particular to a method for deep removal of sulfur-containing compounds in C5 distillate oil by-product of naphtha cracking to produce ethylene the adsorbent. Background technique [0002] The cracked C5 fraction is a by-product of the ethylene cracking unit, generally 10% to 15% (mass fraction) of the ethylene output. With the continuous expansion of the scale of ethylene plants, more and more by-product C5 fractions are produced. The C5 fraction is mainly composed of isoprene, piperylene and cyclopentadiene. These dienes are produced through processes such as polymerization, hydrogenation, separation and cracking to produce synthetic rubber, petroleum resin, plastic and various The important raw material of fine chemical products is a precious resource...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/18B01J20/30C10G25/05C01B39/26C01B39/24C01B39/40C01B39/02
CPCB01J20/18C01B39/023C01B39/24C01B39/265C01B39/40C01P2002/72C01P2004/03C01P2004/84C01P2006/12C01P2006/14C10G25/05C10G2300/1037C10G2300/1044C10G2300/202
Inventor 周广林李芹王晓胜吴全贵周红军
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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