Method for preparing zeolite molecular sieve through quick crystallization of dry glue

A technology of zeolite molecular sieve and molecular sieve, applied in chemical instruments and methods, crystalline aluminosilicate zeolite, octahedral crystalline aluminum silicate zeolite, etc., can solve problems such as low crystallinity and impure crystal phase, and achieve crystallization time Short, short crystallization cycle, and the effect of shortening the production cycle

Active Publication Date: 2019-08-23
TAIYUAN DACHENG ENVIRONMENTAL ENERGY CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above technologies are the results of small laboratory experiments. For its industrial scale-up, it is necessary to solve the problems of crystal phase impurity, low crystallinity, and autoclave design during the scale-up process.

Method used

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  • Method for preparing zeolite molecular sieve through quick crystallization of dry glue
  • Method for preparing zeolite molecular sieve through quick crystallization of dry glue
  • Method for preparing zeolite molecular sieve through quick crystallization of dry glue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Get 1 ton of NaY crystallization mother liquor produced when catalyst factory is produced, wherein NaY 2 O mass fraction is 4.2%, SiO 2 The mass fraction is 20%; according to the proportion of the directing agent is 1Al 2 o 3 : 8SiO 2 : 0.01F - Add the following raw materials: pseudo-boehmite (65.5wt%, Aluminum Corporation of China Shanxi Aluminum Plant) 64.88kg, NH 4 F (96wt%, Tianjin Kemiou Reagent Co., Ltd.) 0.16kg was crystallized in a crystallization kettle at 90°C for 2 hours to obtain a directing agent for use.

[0037] The following raw materials are added to the guide agent: sodium hydroxide (chemically pure, content ≥96.0%) 36.98kg, white carbon black (industrial grade, content ≥97.0%), Shanxi Tongde Chemical Co., Ltd. company) 51.54kg. Finally, dry glue powder was made after flash drying at 90°C.

[0038] With the prepared dry rubber powder, in the solid phase continuous reactor (such as figure 1 ) Add 1000kg of deionized water to the bottom of the ke...

Embodiment 2

[0046] Get 1 ton of NaY crystallization mother liquor produced when catalyst factory is produced, wherein NaY 2 O mass fraction is 4.2%, SiO 2 The mass fraction is 30%; according to the ratio of the directing agent is 1Al 2 o 3 : 5SiO 2 : 0.1F - Add the following raw materials: pseudoboehmite (Al 2 o 3 The content is 65.5wt%, Aluminum Corporation of China Shanxi Aluminum Plant) 155kg, NH 4 3.85kg of F (96wt%, Tianjin Kemiou Reagent Co., Ltd.) was crystallized in a crystallization kettle at 90°C for 10 hours to obtain a directing agent for use.

[0047] Adding raw materials to the guide agent: Sodium hydroxide (chemically pure, content ≥96.0% Tianjin Kemiou Chemical Reagent Development Center) 602kg, white carbon black (industrial grade, content ≥97.0%, Shanxi Tongde Chemical Co., Ltd.) 927kg. The prepared gel was finally dried at 90°C to make dry gel powder.

[0048] With the prepared dry rubber powder, in the solid phase continuous reactor (such as figure 1 ) Add 50...

Embodiment 3

[0054] Another batch of NaY type molecular sieve crystallization mother liquor 1 ton produced when getting catalyst factory production, wherein NaY 2 The mass fraction of O is 5.4%: SiO 2 The mass fraction is 25%; according to the ratio of the directing agent is 1Al 2 o 3 : 4SiO 2 : 0.05F - Add the following raw materials: pseudoboehmite (Al 2 o 3 The content of NaF is 65.5wt%, Aluminum Corporation of China (Shanxi Aluminum Factory) 162kg, NaF (98wt%, Tianjin Jinke Fine Chemical Research Institute) 2.28kg, crystallized in the crystallization kettle at 90°C for 5h to obtain the directing agent.

[0055] Add raw materials to the guiding agent: sodium hydroxide (chemically pure, content ≥ 96.0% Tianjin Kemiou Chemical Reagent Development Center) 213kg, silica sol (25wt%, Qingdao Ocean Chemical Co., Ltd.) 2750kg. Finally, it is dried at 90°C to make dry rubber powder.

[0056] The dry rubber powder was crystallized at 100°C for 10 hours in a water vapor atmosphere in a spec...

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Abstract

The invention discloses a method for preparing a zeolite molecular sieve through quick crystallization of dry glue, and relates to the field of molecular sieve solid phase synthesis. The method specifically comprises the following steps: adding an aluminum source and a fluoride into a silicon-aluminum type molecular sieve mother solution for crystallizing to obtain a silicon-aluminum type molecular sieve guiding agent; adding an alkali source, a silicon source, a template agent R and deionized water into the silicon-aluminum type molecular sieve guiding agent, uniformly carrying out mixing, and then carrying out drying to obtain dry glue powder; and crystallizing the dry glue powder in a steam atmosphere in a continuous crystallization kettle to obtain the zeolite molecular sieve, whereinthe crystallization time is 2-10 hours. The guiding agent disclosed by the invention is obtained by secondary crystallization, and is high in activity and strong in guiding action, so that the usage amount of the template agent can be reduced, crystallinity can be improved, generation of hybrid crystal phases formed by solid-phase synthesis is avoided, and the crystallization period is shortened.The continuous crystallization kettle can be used for continuous production without need of cooling and pressure relief, so that the required crystallization time is short, and efficiency and yield are high. The prepared zeolite molecular sieve is good in stability, high in crystallinity and high in silicon-aluminum ratio.

Description

technical field [0001] The invention relates to the technical field of solid-phase synthesis of zeolite molecular sieves, in particular to a method for preparing zeolite molecular sieves by rapid crystallization of dry glue. Background technique [0002] At present, most technologies for the synthesis of molecular sieves by solid-phase method are still in the stage of laboratory research and development. The main technical problems in the industrial production of solid-phase method include the design of industrial reactors, low crystallinity, and impure crystal phase. [0003] The patent US3492090 adds self-made silica-alumina sol to the gel, and through a series of processes such as aging, the crystallization time can be greatly shortened. This method is collectively called the sol-directing agent method, but industrial practice has proved that the preparation of the sol-directing agent is not sensitive to temperature. The requirements are relatively strict, and it is easy ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48C01B39/24
CPCC01B39/24C01B39/48C01P2002/72C01P2004/03
Inventor 窦涛谭富江
Owner TAIYUAN DACHENG ENVIRONMENTAL ENERGY CHEM TECH
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