Tungsten complex and preparation method and application thereof

A technology of complexes and adducts, applied in chemical instruments and methods, bulk chemical production, organic chemistry, etc., can solve the problems of high cost, limited application, and many uncontrollable parameters, and achieve high saturated vapor pressure and no Potential safety hazards, the effect of ensuring safety

Active Publication Date: 2020-06-05
苏州欣溪源新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, problems such as high cost and many uncontrollable parameters limit the WS 2 Applications
At the same time, large-area single crystal WS 2 The...

Method used

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  • Tungsten complex and preparation method and application thereof
  • Tungsten complex and preparation method and application thereof

Examples

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Embodiment 1

[0026] This embodiment relates to a preparation method of a tungsten complex, carried out in a reaction vessel protected by a high-purity argon atmosphere, comprising the following steps:

[0027] Step 1: Add 15 grams of tungsten hexachloride and 50 milliliters of dichloromethane to a 250 milliliter Schlenk bottle in sequence, and slowly add 34 milliliters of cyclopentene dropwise while stirring, keep the temperature of the system at 45°C, and reflux for 30 minutes Afterwards, vacuum suction filtration, add 20 milliliters of ethylene glycol dimethyl ether to the filtrate, continue to react for 30 minutes, vacuum suction filtration, the filter residue is washed three times with 10 milliliters of methyl tert-butyl ether and vacuum-dried to obtain tungsten tetrachloride 13 grams of glycol dimethyl ether adduct, yield 85%;

[0028] Step 2: Add 14 g of cyclopentadienyllithium, 600 ml of methyl tert-butyl ether and 40 g of tungsten tetrachloride ethylene glycol dimethyl ether prepar...

Embodiment 2

[0032] This embodiment relates to a preparation method of a tungsten complex, carried out in a reaction vessel protected by a high-purity argon atmosphere, comprising the following steps:

[0033] Step 1: Add 120 grams of tungsten hexachloride and 400 milliliters of dichloromethane to a 2-liter Schlenk bottle; slowly add 300 milliliters of cyclopentene dropwise while stirring to keep the temperature of the system at 50 ° C, and reflux for 2 hours , return to room temperature, vacuum filter, add 160 milliliters of ethylene glycol dimethyl ether to the filtrate, continue to react for 2 hours, vacuum filter, filter residue is vacuum-dried after washing three times with 100 milliliters of methyl tert-butyl ether, obtain tetrachloro 110 grams of tungsten chloride ethylene glycol dimethyl ether adduct, yield 90%;

[0034] Step 2: Add 14 g of cyclopentadienyllithium, 600 ml of methyl tert-butyl ether and 40 g of tungsten tetrachloride ethylene glycol dimethyl ether prepared by the me...

Embodiment 3

[0037] Different from Example 1, this example only replaces 22 grams of lithium dimethylamide in step 3 of Example 1 with 34 grams of lithium diethylamide, and finally obtains the product bis(diethylamino) The yield of bis(cyclopentadienyl)tungsten is 86%, and the saturated vapor pressure at 69°C is 1.2mmHg. The product was detected by nuclear magnetic resonance, and the results were as follows, 1 HNMR (CDCl 3 ): 4.15, 3.60, 1.12ppm.

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Abstract

The invention discloses a tungsten complex as well as a preparation method and application thereof and belongs to the technical field of organic chemistry. The preparation method of the tungsten complex comprises the following steps: 1) mixing tungsten hexachloride and dichloromethane, dropwise adding cyclopentene, heating, carrying out reflux reaction, filtering, adding ethylene glycol dimethyl ether into afiltrate, filtering after the reaction, washing a filter residue with methyl tert-butyl ether, and carrying out vacuum drying to obtain a product A; 2) mixing the product A with cyclopentadienyl lithium and methyl tert-butyl ether, reacting overnight, filtering, reacting an obtained solid with ethylene glycol dimethyl ether, filtering again, washing asolid product with tetrahydrofuran,ethanol and methyl tert-butyl ether, and drying in vacuum to obtain a product B; and 3) mixing the product B with methyl tert-butyl ether, adding lithium dialkylamide in batches while stirring, reacting overnight at room temperature, pumping out the solvent, adding an alkane solvent, extracting, filtering, and pumping out the alkane solvent to obtain bis (dialkylamino) bis (cyclopentadienyl) tungsten. The tungsten complex prepared by the invention can be used for preparing tungsten sulfide films.

Description

technical field [0001] The invention relates to a technique in the field of organic chemistry, in particular to a tungsten complex and its preparation method and application. Background technique [0002] Two-dimensional transition metal chalcogenides are widely regarded as star materials with great potential for future electronic device applications because of their graphene-like structures. Among them, tungsten sulfide (WS 2 ) has wide application prospects in solar cells, semiconductor industries, especially in the field of solid lubrication because of its solid lubrication and bipolar electron transport properties. [0003] Many preparations of WS have been reported 2 Thin film methods, including ion beam sputtering, pulsed laser deposition (PLD), chemical vapor deposition (CVD), etc. However, problems such as high cost and many uncontrollable parameters limit the WS 2 Applications. At the same time, large-area single crystal WS 2 The fabrication of atomic layer th...

Claims

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Application Information

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IPC IPC(8): C07F17/00C23C16/30C23C16/455
CPCC07F17/00C23C16/305C23C16/45553Y02P20/52
Inventor 逄增波
Owner 苏州欣溪源新材料科技有限公司
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