Supercharge Your Innovation With Domain-Expert AI Agents!

A kind of preparation method of ZSM-11 molecular sieve containing phosphorus in crystal

A technology of ZSM-11 and molecular sieves, which is applied in the field of preparation of ZSM-11 molecular sieves, can solve the problems of few synthesis research reports, easy formation of miscellaneous crystals or mixed crystals, and harsh synthesis requirements

Active Publication Date: 2019-01-08
CHINA PETROLEUM & CHEM CORP +1
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] ZSM-11 is easy to form miscellaneous crystals or mixed crystals during the synthesis process, so the requirements for synthesis are relatively strict, and there are few reports on its synthesis.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of ZSM-11 molecular sieve containing phosphorus in crystal
  • A kind of preparation method of ZSM-11 molecular sieve containing phosphorus in crystal
  • A kind of preparation method of ZSM-11 molecular sieve containing phosphorus in crystal

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0021] The preparation method of the phosphorus-containing ZSM-11 molecular sieve provided by the present invention comprises the following steps:

[0022] (1) Mix tetrabutylphosphorus hydroxide and aluminum source evenly, tetrabutylphosphorus hydroxide in the mixture and Al in the aluminum source 2 o 3 The molar ratio is 0.1 to 40:1, and the mixture is treated in a closed reactor at 50 to 300°C for at least 0.1h to obtain an intermediate product, and the aluminum source is selected from aluminum sources that do not contain alkali metal ions;

[0023] (2) Mix the intermediate product in step (1) with silicon source and deionized water evenly, and in the resulting mixture, SiO 2 / Al 2 o 3 =25~1000、H 2 O / SiO 2 =2~20;

[0024] (3) The mixture obtained in step (2) is subjected to hydrothermal crystallization at 50-250° C. for 10-200 hours in a closed reaction kettle, and the ZSM-11 molecular sieve containing phosphorus is recovered.

[0025] In the method of the present inv...

Embodiment 1

[0037] Take by weighing 0.67g pseudo-boehmite (Changling Catalyst Factory, Al 2 o 3 content is 70%), it is mixed with 30.0g tetrabutyl phosphorus hydroxide (Sinopharm Group Chemical Reagent Co., Ltd., analytically pure, TBPOH content 40%), the mixture molar ratio TBPOH / Al 2 o 3 =8.0, put it in a crystallization kettle containing a polytetrafluoroethylene liner, react with 140°C for 2h and cool to room temperature, after that, mix it with 20.0g silica gel (Qingdao Ocean Chemical Co., Ltd., SiO 2 Content 99.1%) and 21.0g water are mixed evenly, and the molar ratio of the mixture is SiO 2 / Al 2 o 3 =80,H 2 O / SiO 2 = 6.5. The mixture was hydrothermally crystallized at 150° C. for 48 h in an autoclave. After the crystallization was completed, the sample in the kettle was centrifuged, dried at 110°C for 20 hours, and calcined at 550°C for 3 hours to obtain a molecular sieve sample, numbered ZP-1.

[0038] The XRD spectrum of molecular sieve sample ZP-1 is shown in figure 1...

Embodiment 2

[0044] Weigh 0.8g pseudo-boehmite (Beijing Chemical Plant, analytically pure, Al 2 o 3 content is 70%), it is mixed with 21.0g tetrabutyl phosphorus hydroxide (Sinopharm Group Chemical Reagent Co., Ltd., analytically pure, TBPOH content 40%), the mixture molar ratio TBPOH / Al 2 o 3 =5.0, put it in a crystallization kettle containing a polytetrafluoroethylene lining, react with 150°C for 2h and cool to room temperature, after that, mix it with 20.0g silica gel (Qingdao Ocean Chemical Co., Ltd., SiO 2 Content 99.1%) and 12.0g water are mixed evenly, and the molar ratio of the mixture is SiO 2 / Al 2 o 3 =50,H 2 O / SiO 2 =7. The mixture was hydrothermally crystallized at 150° C. for 72 h in an autoclave. After the crystallization was completed, the sample in the kettle was centrifuged, dried at 110°C for 20 hours, and calcined at 550°C for 3 hours to obtain a molecular sieve sample, numbered ZP-2.

[0045] The XRD spectrum of the molecular sieve sample ZP-2 has figure 1 Th...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
crystallinityaaaaaaaaaa
crystallinityaaaaaaaaaa
crystallinityaaaaaaaaaa
Login to View More

Abstract

The invention provides a preparation method of intracrystalline phosphorus-containing ZSM-11 molecular sieve. The method comprises the following steps: uniformly mixing and processing tetrabutylphosphonium hydroxide and an aluminum source to obtain an intermediate, uniformly mixing the intermediate with a silicon source and deionized water, and carrying out hydrothermal crystallization recovery to obtain the intracrystalline phosphorus-containing ZSM-11 molecular sieve. The method is an alkali-free metal synthesis system, and does not need crystal seeds, and allows the intracrystalline phosphorus-containing ZSM-11 molecular sieve with pure phase, high crystallization degree and the crystal size of 200-500 nm to be obtained.

Description

technical field [0001] The invention relates to a method for preparing phosphorus-containing ZSM-11 molecular sieves, more specifically to a method for preparing phosphorus-containing ZSM-11 molecular sieves without introducing crystal seeds. Background technique [0002] ZSM-11 molecular sieve is a new structural molecular sieve (USP3709979) developed by Mobil Corporation in the 1970s, which consists of two-dimensional straight channels (0.51nm×0.55nm) in the shape of an oval ten-membered ring. At present, ZSM-11 molecular sieve has been used as a catalytic active component in many petrochemical catalysts, such as hydrocracking and catalytic dewaxing catalysts. [0003] During the synthesis process of ZSM-11, miscellaneous crystals or mixed crystals are easily formed, so the requirements for synthesis are relatively strict, and there are few reports on its synthesis. There are very few reports on the synthesis of phosphides introduced into ZSM-11 molecular sieves. [0004...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/36
Inventor 张欣王萍王殿中罗一斌欧阳颖徐广通舒兴田
Owner CHINA PETROLEUM & CHEM CORP
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com