Method for synthesizing ZSM-5 molecular sieve through two-segment temperature change

A technology of ZSM-5 and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the temperature gradient of the synthesis system and the uneven distribution of gel components, and the crystallization of molecular sieve products In order to solve problems such as poor degree of stability and decreased equipment utilization rate, it can achieve the effects of narrow grain size distribution, good fluidity and improved efficiency.

Inactive Publication Date: 2012-10-24
吉林市品前化工技术开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the usual molecular sieve synthesis method, due to the low viscosity of the starting material, the stirring process can be started smoothly, but in the multi-stage variable temperature process, the reaction mixture that is aged by standing still tends to form a high viscosity after the aging is completed. Therefore, when the stirring is started, it is difficult to stir due to the large resistance, or the stirring equipment is overloaded and damaged; the insufficient stirring caused by this will easily cause the temperature gradient of the synthesis system and the uneven distribution of the gel components, resulting in The obtained molecular sieve product has poor crystallinity and uneven particle size
In addition, the high temperature section of the above method often still requires a higher crystallization temperature and a longer crystallization time, which will also result in a decrease in equipment utilization and an increase in energy consumption.

Method used

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  • Method for synthesizing ZSM-5 molecular sieve through two-segment temperature change
  • Method for synthesizing ZSM-5 molecular sieve through two-segment temperature change
  • Method for synthesizing ZSM-5 molecular sieve through two-segment temperature change

Examples

Experimental program
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Effect test

Embodiment 1

[0023]Mix 39.15 g of water glass (modulus 2.98) with 1.47 g of n-butylamine and 15 g of deionized water in a stainless steel synthesis kettle with a volume of 200 ml and stir evenly to prepare A solution; mix 0.72 g of aluminum sulfate and 2.27 g of sulfate (98%) and 24 g deionized water were stirred in a 50 ml beaker to prepare B solution. Slowly add solution B to solution A while stirring, then add 50 g of deionized water, stir for 0.5 h to obtain an initial reaction gel, add 200 mg of ZSM-5 seed crystals and seal. Under stirring, the temperature was first raised to 105°C for dynamic crystallization for 14 h, and then the temperature was raised to 125°C for dynamic crystallization for 26 h. After the product was cooled down, it was removed from the synthesis kettle, washed three times with deionized water, and dried at 120°C for 4 hours to obtain a ZSM-5 molecular sieve with a crystallinity of 100%. The product SiO 2 / Al 2 o 3 (mol ratio) was 69.

Embodiment 2

[0029] Mix 39.15 g of water glass (modulus 2.98) with 5.38 g of tetrapropylammonium bromide and 25 g of deionized water in a stainless steel synthesis kettle with a volume of 200 ml and stir evenly to prepare A solution; mix 0.72 g of aluminum sulfate, 2.27 g of sulfuric acid (98%) and 24 g of deionized water were stirred evenly in a 50 ml beaker to prepare B solution. Slowly add solution B to solution A while stirring, then add 40 g of deionized water, stir for 0.5 h to obtain an initial reaction gel, add 200 mg of finished ZSM-5 seed crystals and seal. Under stirring, the temperature was first raised to 110°C for dynamic crystallization for 10 h, and then the temperature was raised to 125°C for dynamic crystallization for 26 h. After the product was cooled down, it was removed from the synthesis kettle, washed three times with deionized water, and dried at 120°C for 4 hours to obtain a ZSM-5 molecular sieve with a crystallinity of 95%. The product SiO 2 / Al 2 o 3 (mol rat...

Embodiment 3

[0031] In a stainless steel synthesis kettle with a volume of 200 ml, 39.15 g of water glass (modulus 2.98) was mixed with 1.47 g of n-butylamine and 15 g of deionized water and stirred evenly to prepare A solution; 1.50 g of aluminum sulfate and 2.27 g of sulfuric acid ( 98%) and 24 g of deionized water were stirred in a 50 ml beaker to prepare B solution. While stirring, solution B was slowly added to solution A, and then 30 g of deionized water was added, and the initial reaction gel was obtained after stirring for 0.5 h. Add 250 mg of finished ZSM-5 seeds and seal. Under stirring, the temperature was first raised to 105 °C for dynamic crystallization for 12 h, and then the temperature was raised to 120 °C for dynamic crystallization for 32 h. After the product was cooled down, it was removed from the synthesis kettle, washed three times with deionized water, and dried at 120°C for 4 hours to obtain ZSM-5 molecular sieve, with a crystallinity of 99%, and the product SiO 2...

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Abstract

The invention relates to a method for synthesizing a ZSM-5 molecular sieve through a two-segment temperature-changing crystallizing process, which comprises the following steps of using a water-soluble liquid silicon source and a water-soluble liquid aluminum source as raw materials, wherein the molar ratios of the raw materials calculated by oxides are as follows: SiO2/Al2O3=50-70, Na2O/SiO2=0.05-5, H2O/SiO2=50-70, and a template agent/SiO2=0.05-0.4; mixing the silicon source and the template agent according to formula amounts with deionized water which is added by accounting for 15-33.3wt% of the total usage amount of the required water under a dynamic state of overall-process stirring to prepare an A solution, mixing the aluminum source and sulfuric acid according to the formula amounts with the water which is added by accounting for 24-44.4wt% of the total usage amount of the required water to prepare a B solution, slowly adding the B solution into the A solution, adding the residual water, adding ZSM-5 crystal seeds into initial gel which is obtained by stirring the mixture for 0.5-2 hours, crystallizing for 10-20 hours at the temperature of 80-110 DEG C, and then crystallizing for 10-40 hours after increasing the temperature to 115-130 DEG C.

Description

technical field [0001] The invention relates to the synthesis of molecular sieves, in particular to a method for synthesizing ZSM-5 molecular sieves through a two-stage variable temperature crystallization process. Background technique [0002] Mobile company first reported the synthesis of ZSM-5 in 1972. In its disclosed synthesis method (US3,702,886), tetraalkylammonium hydroxide (alkyl C number 2~5) is used as template, and the reaction mixture prepared by silicon source, aluminum source, water, alkali and template The ZSM-5 product was obtained after crystallization under hydrothermal conditions. Since then, people have improved the synthesis method of ZSM-5 molecular sieve through a lot of research. For example, a number of patents have disclosed methods for the synthesis of ZSM-5 using different types of organic templates, including primary amines (US4,151,189), diamines (US4,139,600, US4,495,166), polyamines (US4,495,166), 4,404,175), low-carbon alcohols (US 4,175,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
Inventor 王公慰谭娟王品江王健齐昕薛立新
Owner 吉林市品前化工技术开发有限公司
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