Dialkyl dicyclopentadienyl molybdenum complex as well as preparation method and application thereof

A technology of dialkyl dialkyl molybdenum and complexes, which is applied in the field of dialkyl dialkyl molybdenum complexes and their preparation, can solve the problems of limiting the application of MoS2, many uncontrollable parameters, and high deposition temperature, and achieves important scientific research value. , Broad industrial prospects, high yield effect

Pending Publication Date: 2020-10-16
苏州欣溪源新材料科技有限公司
View PDF5 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned traditional methods have problems such as high cost, difficult thickness control, high deposition temperature, and many uncontrollable parameters, which limit the development of MoS2. 2 Applications
Moreover, large-area single-crystal MoS 2 The preparation of atomic layer thin films is still the current constraint on MoS 2 The bottleneck of thin film application in high-performance electronic devices

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
  • Dialkyl dicyclopentadienyl molybdenum complex as well as preparation method and application thereof
  • Dialkyl dicyclopentadienyl molybdenum complex as well as preparation method and application thereof
  • Dialkyl dicyclopentadienyl molybdenum complex as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0050] The invention provides a preparation method of dialkylmolybdenocene complexes. The dichloromolybdenocene complexes are synthesized in one step by using a one-pot method of mixing, and then the dichloromolybdenocene complexes are mixed with alkyl Lithium reacted to prepare dialkyl molybdenum molybdenum complexes. The technical scheme is as follows:

[0051] A method for preparing dialkyl molybdenumocene complexes, comprising the following steps:

[0052] dissolving molybdenum pentachloride in the first solvent, and cooling for the first time to prepare the first solution;

[0053] dissolving lithium trialkylsilacyclopentadiene and sodium borohydride in a second solvent, and cooling for the second time to prepare a second solution;

[0054] Mix the first solution and the second solution, stir for 2h-4h, heat up to 55°C-75°C, react for 20h-28h, add alkane to the reaction product for extraction, filter, add chloroform to the filtrate, stir for 8h-12h, Preparation of two ...

Embodiment 1

[0099] This example provides a dialkyl molybdenumocene complex and its preparation method, which is carried out in a reaction vessel protected by a high-purity argon atmosphere, and the specific steps are as follows:

[0100] Step 1: Under an argon atmosphere, add 90 ml of cyclopentadienyl sodium in tetrahydrofuran to a 250 ml Schlenk bottle at a concentration of 2.0 moles per liter. Slowly add 20 g (0.18 mol) of trimethylchlorosilane dropwise while stirring to keep the temperature of the system at 0°C. After the dropwise addition, continue to keep the temperature in the bottle at 0°C and stir for 2 hours. Add ice water to the bottle to quench the reaction, extract with methyl tert-butyl ether, dry over anhydrous sodium sulfate, and vacuum the solvent to obtain trimethylsilcyclopentadiene, which is dissolved in 100 ml of n-hexane , cooled to 0°C, and 73 ml of n-butyllithium was added dropwise with a concentration of 2.5 moles per liter. After the dropwise addition, return to ...

Embodiment 2

[0105] This embodiment provides a dialkyl molybdenum molybdenum complex and its preparation method, the specific steps are as follows:

[0106] Step 1: Add 300 ml of tetrahydrofuran solution of sodium cyclopentadienyl to a 1000 ml Schlenk bottle under a nitrogen atmosphere at a concentration of 2.0 moles per liter. While stirring, 92 g (0.6 mol) of triethylchlorosilane was slowly added dropwise to keep the temperature of the system at 0°C. After the dropwise addition, the temperature in the bottle was kept at 0°C and stirred for 4 hours. Add ice water to the bottle to quench the reaction, extract with methyl tert-butyl ether, dry over anhydrous sodium sulfate, and vacuum the solvent to obtain triethylsilacyclopentadiene, which is dissolved in 400 ml of n-hexane , cooled to 0°C, and 306 ml of n-butyl lithium was added dropwise with a concentration of 2.5 moles per liter. After the dropwise addition, return to room temperature and react for 12 hours, filter and wash with n-hexa...

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

No PUM Login to view more

Abstract

The invention relates to a dialkyl dicyclopentadienyl molybdenum complex as well as a preparation method and application thereof. The preparation method comprises the following steps: dissolving molybdenum penta-chloride in a first solvent, cooling for the first time to prepare a first solution; dissolving trialkyl silicon cyclopentadiene lithium and sodium borohydride in a second solvent, coolingfor the second time to prepare a second solution; mixing the first solution and the second solution, stirring for 2-4 hours, heating to 55-75 DEG C, reacting for 20-18 hours, adding alkane into the reaction product, extracting, collecting the water phase, filtering, adding chloroform into the filtrate, stirring for 8-12 hours to prepare bis(trialkylsilylcyclopentadienyl) molybdenum dichloride; and reacting bis(trialkylsilylcyclopentadienyl) molybdenum dichloride with alkyl lithium. According to the preparation method, a dicyclopentadienyl molybdenum dichloride complex is synthesized in one step and then reacts with alkyl lithium to prepare the dialkyl dicyclopentadienyl molybdenum complex, so that the reaction steps are shortened, the production cost is reduced, the high yield is maintained, and the industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a dialkyl molybdenum molybdenum complex and a preparation method and application thereof. Background technique [0002] In recent years, with the upsurge of research on two-dimensional layered nanomaterials such as graphene, transition metal sulfides, a graphene-like material, have attracted extensive attention from researchers in many fields such as physics, chemistry, materials, and electronics. Among them, molybdenum disulfide (MoS 2 ) film is similar to graphene in structure and performance, and is different from graphene film with zero band gap. Molybdenum disulfide is a semiconductor material whose performance depends on the number of layers. When the number of layers changes from multilayer to single layer, its The indirect bandgap semiconductor of 1.2eV can be changed to the direct bandgap semiconductor of 1.9eV, which greatly increases the luminous efficiency....

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 Applications(China)
IPC IPC(8): C07F17/00C23C16/30C23C16/455
CPCC07F17/00C23C16/305C23C16/45525
Inventor 逄增波江德圣
Owner 苏州欣溪源新材料科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap