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

A diamine molybdenum molybdenum and complex technology, applied in chemical instruments and methods, metallocene, gaseous chemical plating, etc., can solve the problems of limiting the application of MoS2, many uncontrollable parameters, and high deposition temperature, and achieve important scientific research. Value, broad industrial prospects, high yield effect

Pending Publication Date: 2020-10-09
苏州欣溪源新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 A

Method used

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

Examples

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preparation example Construction

[0050] The invention provides a preparation method of diamine molybdenocene complexes. The dichloromolybdenocene complexes are synthesized in one step by mixing in one pot, and then the dichloromolybdenocene complexes are mixed with dioxane The reaction of diaminomolybdenum molybdenum complexes with lithium amide was prepared. The technical solution is as follows:

[0051] A kind of preparation method of diaminomolybdenum molybdenum compound, comprises the following steps:

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

[0053] dissolving the substituted lithium cyclopentadiene 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, 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, fil...

Embodiment 1

[0097] This example provides a diamine-based 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:

[0098] Step 1: Under an argon atmosphere, add 50 grams (0.367 mol) of pentamethylcyclopentadiene and 50 milliliters of n-hexane to a 500 milliliter Schlenk bottle, lower the temperature of the system to 0 ° C, and dropwise add 147 milliliters of n-butyl Lithium in n-hexane solution, the concentration of n-butyllithium is 2.5 moles per liter. After the dropwise addition, return to room temperature and react for 2 hours, filter, wash with n-hexane, and dry to obtain 41 g of lithium pentamethylcyclopentadiene, with a yield of 80%;

[0099] Step 2: Add 10 grams (0.037 mol) of molybdenum pentachloride, 25 milliliters of toluene and 125 milliliters of tetrahydrofuran into a 250 milliliter Schlenk bottle in sequence, stir to dissolve and then cool to -10°C to obt...

Embodiment 2

[0103] This embodiment provides a diamino molybdenum molybdenum complex and a preparation method thereof, the specific steps are as follows:

[0104] Step 1: Under a nitrogen atmosphere, add 80 grams (0.179 mol) of pentaphenylcyclopentadiene and 100 milliliters of n-hexane to a 500 milliliter Schlenk bottle, lower the temperature of the system to 0 ° C, and add 72 milliliters of n-butyllithium dropwise n-hexane solution, the concentration of n-butyllithium is 2.5 moles per liter. After the dropwise addition, return to room temperature and react for 2 hours, filter, wash with n-hexane, and dry to obtain 70 g of lithium pentamethylcyclopentadiene, with a yield of 86%;

[0105] Step 2: Add 22 grams (0.081 mol) of molybdenum pentachloride, 60 milliliters of toluene and 250 milliliters of tetrahydrofuran to a 500 milliliter Schlenk bottle, stir and dissolve, then cool to -10°C to obtain the first solution. Add 38 g (0.084 mol) of pentaphenylcyclopentadienyl lithium prepared in ste...

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Abstract

The invention relates to a diamino molybdenum dicyclopentadienyl complex as well as a preparation method and application thereof. The preparation method comprises the following steps of: dissolving molybdenum pentachloride in a first solvent, and performing cooling to prepare a first solution; dissolving substituted cyclopentadiene lithium and sodium borohydride in a second solvent, and performingcooling to prepare a second solution; mixing the first solution and the second solution, performing stirring for 2-4 hours, performing heating for 55-75 hours, performing a reaction for 20-18 hours,adding alkane into a reaction product, performing extraction, collecting a water phase, performing filtering, adding chloroform into a filtrate, and stirring for 8-12 hours to prepare bis (substitutedcyclopentadiene lithium) molybdenum dichloride; and making the bis (substituted cyclopentadiene lithium) molybdenum dichloride with dialkylamine lithium. According to the preparation method, the dichloro-molybdenum dicyclopentadienyl complex is synthesized in one step and then reacts with the lithium dialkylamine, so that the diamino-molybdenum dicyclopentadienyl complex can be prepared, so thatreaction steps are shortened, production cost is reduced, the higher yield is maintained, and the industrial production is better facilitated.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a diaminomolybdenum molybdenum complex and a preparation method and application thereof. Background technique [0002] Two-dimensional layered transition metal dichalcogenides (TMDs) with a graphene-like structure are widely considered to be promising candidates for future applications in electronic devices due to their unique properties such as high electron mobility, excellent optical absorption, and quantum Hall effect. One of the star materials with great potential. Among them, molybdenum sulfide (MoS 2 ) films are similar to graphene in structure and performance, but unlike graphene films with zero band gap, molybdenum disulfide has a tunable band gap. The band gap of bulk crystal molybdenum disulfide is 1.2eV, and the electronic transition mode is indirect transition, while the band gap of monolayer molybdenum disulfide can reach 1.8eV, and the electronic transi...

Claims

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Application Information

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IPC IPC(8): C07F17/00C23C16/18C23C16/455
CPCC07F17/00C23C16/18C23C16/45553
Inventor 逄增波江德圣
Owner 苏州欣溪源新材料科技有限公司
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