CN102020318B - Method for preparing molybdenum pentachloride - Google Patents
Method for preparing molybdenum pentachloride Download PDFInfo
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- CN102020318B CN102020318B CN2010106060807A CN201010606080A CN102020318B CN 102020318 B CN102020318 B CN 102020318B CN 2010106060807 A CN2010106060807 A CN 2010106060807A CN 201010606080 A CN201010606080 A CN 201010606080A CN 102020318 B CN102020318 B CN 102020318B
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Abstract
The invention relates to a method for preparing molybdenum pentachloride, which belongs to the technical filed of inorganic chemistry. The method comprises the following steps of: firstly blending molybdenum trioxide and dehydrated carbon tetrachloride in mass ratio of 1:4-1:6 in a round-bottom stainless steel reaction bulb, and closing a valve for sealing after the reaction bulb is degassed; then completely immerging the reaction bulb into an oil bath pan and heating to 150 DEG-240 DEG, keeping the temperature for 1-12 hours, and taking out the reaction bulb after cooling; and at the moment, with the change of a reaction solution color from original colorlessness to brownish red and the precipitation of black acicular crystals, opening the valve of the reaction bulb to discharge reaction gas, pouring the reaction solution into an evaporator, and evaporating to remove the carbon tetrachloride to obtain black molybdenum pentachloride crystals. The method has the advantages of simple and easily-controlled technology, high production efficiency, lower raw material price, simple production condition, low production cost, single product phase structure and high purity, and because the reaction is carried out in a sealed system, less pollution is generated.
Description
Technical field
The invention belongs to technical field of inorganic, particularly a kind of method for preparing molybdenum pentachloride.
Technical background
Molybdenum pentachloride is an important catalyst in the organic chemical industry field.Like it is the chlorination of aromatic nucleus and the partially or completely chlorating effective catalyst of phthalic acid acid anhydrides; Can be used for the synthetic polypentanamer of catalysis, the existence of its composition, purity, content and trace impurity all has considerable influence to polyreaction; It obtains (benzene) phenol molybdenum compound with the compound reaction of (benzene) phenol, and it is Yu Geshi reagent react generation diarsine and diarsine compound also.
Molybdenum pentachloride also is used to realize the vapour deposition of molybdenum.High-purity molybdenum that the molybdenum pentachloride thermolysis obtains can be deposited on metal and the nonmetallic surface, obtains the even adherent hard coat of skim, characteristic such as that molybdenum coating has is corrosion-resistant, high temperature resistance.Can reduce the molybdenum powder of producing fines with dry hydrogen control gaseous state molybdenum pentachloride, this molybdenum powder has been used for producing scolder, Monel metal, scolder.
Molybdenum pentachloride also is metal-organic important source material such as preparation hexacarbonylmolybdenum, and hexacarbonylmolybdenum has a wide range of applications at organic synthesis, metal molybdenum and aspects such as compound film material, coating material thereof.
The method for preparing at present molybdenum pentachloride mainly adopts metal molybdenum and chlorine to make (more than 800 ℃) through pyroreaction.Use metal molybdenum (powder or bar) to be raw material, cost is higher; High through the pyroreaction production energy consumption; Chlorine has than high toxicity and severe corrosive simultaneously, is difficult to be guaranteed owing to revealing the security that causes in process of production, and can causes environmental pollution.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing molybdenum pentachloride; Improve the existing deficiency that adopts in metal molybdenum and the chlorine reaction technology of preparing; Realized that technology is simple, production safety, cheap, production efficiency is high, and the molybdenum pentachloride phase composition of preparation is single, purity is high.
Technical scheme of the present invention is: at first the tetracol phenixin with molybdic oxide and dehydration mixed in round bottom stainless steel reaction bottle with mass ratio in 1: 4～1: 6, valve-off sealing after reaction flask is outgased.Then reaction flask all being submerged is heated to 150～240 ℃ in the oil bath pan, keeps 1～12 hour, and take out the cooling back.This moment, reaction soln was by the colourless red-brown that becomes of beginning, and had the black needle-like crystal to separate out.Open the reaction flask valve and emit reactant gases, reaction soln is poured in the vaporizer, remove tetracol phenixin through evaporation and promptly get the molybdenum pentachloride black crystals.Entire reaction course is carried out in encloses container (reaction flask).
The chemical equation of above-mentioned reaction can be expressed as:
2MoO
3+6CCl
4＝2MoCl
5+6COCl
2+Cl
2
The tetracol phenixin that uses among the present invention is a reaction raw materials, also is solvent, carries out processed before requiring to use.
Reaction principle of the present invention is: in enclosed system; The tetracol phenixin gasification of being heated; Form certain system pressure, (belong to redox reaction, molybdic oxide is an oxygenant to the chlorination reaction of molybdic oxide and tetracol phenixin generation gas-solid interface with this understanding; Tetracol phenixin is a reductive agent), finally form the pentachloride salt of molybdenum.
Outstanding advantage of the present invention is: (1) technology is simple and easy to control, and production efficiency is high; (2) cost of material is lower, and working condition is simple, and production cost is low; (3) because reaction is in enclosed system, to carry out, pollute little; (4) the product phase structure is single, and purity is high.
Description of drawings
The molybdenum pentachloride crystalline Phase Structure Analysis spectrogram of Fig. 1 for adopting the inventive method to make.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention, but embodiment does not limit the present invention, and do not address part and be applicable to prior art in the invention.
Embodiment 1
With molybdic oxide 10g, the tetracol phenixin 37.5ml of dehydration (mass ratio 1: 6) puts into round bottom stainless steel reaction bottle and mixes, valve-off sealing after reaction flask is outgased.Then reaction flask all being submerged is heated to 150 ℃ in the oil bath pan, keeps 12 hours, and take out the cooling back.This moment, reaction soln was by the colourless red-brown that becomes of beginning, and had the black needle-like crystal to separate out.Open the reaction flask valve and emit reactant gases, reaction soln is poured in the vaporizer, remove tetracol phenixin through evaporation and promptly get black crystals, the Phase Structure Analysis of carrying out through X-ray diffraction confirms that this black crystals is molybdenum pentachloride (seeing accompanying drawing 1).The product 8.2g that weighs, yield 43%.
Embodiment 2
With molybdic oxide 10g, the tetracol phenixin 30ml of dehydration (mass ratio 1: 5) puts into round bottom stainless steel reaction bottle and mixes, valve-off sealing after reaction flask is outgased.Then reaction flask all being submerged is heated to 240 ℃ in the oil bath pan, keeps 1 hour, and take out the cooling back.This moment, reaction soln was by the colourless red-brown that becomes of beginning, and had the black needle-like crystal to separate out.Open the reaction flask valve and emit reactant gases, reaction soln is poured in the vaporizer, remove tetracol phenixin through evaporation and promptly get molybdenum pentachloride black crystals 11.8g, product yield 62%.Phase Structure Analysis result is with embodiment 1.
Embodiment 3
With molybdic oxide 10g, the tetracol phenixin 25ml of dehydration (mass ratio 1: 4) puts into round bottom stainless steel reaction bottle and mixes, valve-off sealing after reaction flask is outgased.Then reaction flask all being submerged is heated to 180 ℃ in the oil bath pan, keeps 8 hours, and take out the cooling back.This moment, reaction soln was by the colourless red-brown that becomes of beginning, and had the black needle-like crystal to separate out.Open the reaction flask valve and emit reactant gases, reaction soln is poured in the vaporizer, remove tetracol phenixin through evaporation and promptly get molybdenum pentachloride black crystals 14.8g, product yield 78%.Phase Structure Analysis result is with embodiment 1.
Embodiment 4
With molybdic oxide 10g, the tetracol phenixin 30ml of dehydration (mass ratio 1: 5) puts into round bottom stainless steel reaction bottle and mixes, valve-off sealing after reaction flask is outgased.Then reaction flask all being submerged is heated to 220 ℃ in the oil bath pan, keeps 5 hours, and take out the cooling back.This moment, reaction soln was by the colourless red-brown that becomes of beginning, and had the black needle-like crystal to separate out.Open the reaction flask valve and emit reactant gases, reaction soln is poured in the vaporizer, remove tetracol phenixin through evaporation and promptly get molybdenum pentachloride black crystals 16.2g, product yield 85%.Phase Structure Analysis result is with embodiment 1.
Claims (1)
1. a method for preparing molybdenum pentachloride is characterized in that, process step is: at first the tetracol phenixin with molybdic oxide and dehydration mixed in round bottom stainless steel reaction bottle with mass ratio in 1: 4～1: 6, valve-off sealing after reaction flask is outgased; Then reaction flask all being submerged is heated to 150～240 ℃ in the oil bath pan, keeps 1～12 hour, and take out the cooling back; Open the reaction flask valve, emit the gas that reaction produces, reaction soln is poured in the vaporizer, remove tetracol phenixin, obtain the molybdenum pentachloride black crystals through evaporation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106060807A CN102020318B (en) | 2010-12-15 | 2010-12-15 | Method for preparing molybdenum pentachloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106060807A CN102020318B (en) | 2010-12-15 | 2010-12-15 | Method for preparing molybdenum pentachloride |
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| Publication Number | Publication Date |
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| CN102020318A CN102020318A (en) | 2011-04-20 |
| CN102020318B true CN102020318B (en) | 2012-11-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010106060807A Expired - Fee Related CN102020318B (en) | 2010-12-15 | 2010-12-15 | Method for preparing molybdenum pentachloride |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB391988A (en) * | 1932-05-27 | 1933-05-11 | Robert Arthur Acton Taylor | Improvements in catalysts for the hydrogenation of organic materials |
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2010
- 2010-12-15 CN CN2010106060807A patent/CN102020318B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB391988A (en) * | 1932-05-27 | 1933-05-11 | Robert Arthur Acton Taylor | Improvements in catalysts for the hydrogenation of organic materials |
Non-Patent Citations (1)
| Title |
|---|
| 天津化工研究设计院编，乐志强等 主编.18.29五氯化钼.《无机精细化学品手册》.化学工业出版社,2001,801. * |
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| CN102020318A (en) | 2011-04-20 |
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