Patent classifications
C01G30/007
High purity tungsten pentachloride and production method thereof
Provided are high purity tungsten pentachloride, and a method for obtaining such high purity tungsten pentachloride at a high yield and in an efficient manner. Tungsten pentachloride in which a total content of metal impurities excluding Sb, Ti, and As is less than 10 wtppm is obtained by uniformly mixing one or more types of reducing agents selected from Sb, Ti, and As and tungsten hexachloride at a molar ratio of 1.0:2.0 to 1.0:5.0 (reducing agent/WCl.sub.6 ratio) in an inert atmosphere to obtain a mixture, heating and reducing the mixture for 1 to 100 hours in a temperature range in which a chloride of tungsten and the reducing agent becomes a liquid phase to obtain a reduced product, heating the reduced product for 1 to 100 hours at 100 Pa or less and in a temperature range of 90 to 130° C., and performing reduced-pressure distillation thereto to obtain a reduced-pressure distilled product, heating and sublimating the reduced-pressure distilled product for 1 to 100 hours at 100 Pa or less and in a temperature range of 130 to 170° C., and performing sublimation purification of achieving precipitation at 70 to 120° C.
METHOD FOR PRODUCING TRIFLUOROAMINE OXIDE
There is provided a method for producing trifluoroamine oxide. The method includes a step of preparing an intermediate product by simultaneously providing and reacting nitrogen trifluoride and nitrous oxide under the presence of a SbF.sub.5 reaction catalyst; and a step of producing trifluoroamine oxide by reacting the intermediate product with potassium fluoride. The step of reacting the intermediate product with potassium fluoride is performed under atmospheric pressure and room temperature.
FLUORINE REMOVAL FROM ANTIMONY FLUOROHALIDE CATALYST USING CHLOROCARBONS
A method of chlorinating a antimony fluorohalide catalyst is disclosed. In one embodiment the method comprises contacting an antimony fluorohalide catalyst that contains one or more fluorines with a regenerating agent chosen from 2-chloro-3,3,3-trifluoropropene (1233xf), 1,1,1,3-tetrachloropropane (250fb), 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb) and combinations of 1233xf, 250fb, and 244bb, under conditions effective to exchange at least one fluorine in the antimony fluorohalide catalyst with chlorine. The method can be used to regenerate spent antimony fluorohalide catalyst, for example regenerating SbCl.sub.5 from SbF.sub.5.
SOLUTION DEPOSITION OF METAL SALTS TO FORM METAL OXIDES
Certain disclosed embodiments concern an organic solution suitable for forming metal oxide films, particularly thins films, comprising a metal salt selected from a Sn salt, an Sb salt, a dopant, and combinations thereof. The salt often is a halide salt, such as SnCl.sub.2 or SbCl.sub.3. Certain disclosed compositions are preferably formed using substantially pure reagents and may include a dopant, such as a fluoride dopant. Described solutions may be used to form thin films, such as a thin film comprising SnO.sub.2, Sb:SnO.sub.2, F:SnO.sub.2, or (Sb,F):SnO.sub.2. Such thin films may have any desired thickness, such as a thickness of from 200 or 700 nm, and are extremely smooth, such as having an RMS surface roughness >3 nm, such as 3 nm to 10 nm, with certain embodiments having an RMS surface roughness <2 nm or <1 nm. Devices can be assembled comprising the thin films on a suitable substrate.
SOLUTION DEPOSITION OF METAL SALTS TO FORM METAL OXIDES
Certain disclosed embodiments concern an organic solution suitable for forming metal oxide films, particularly thins films, comprising a metal salt selected from a Sn salt, an Sb salt, a dopant, and combinations thereof. The salt often is a halide salt, such as SnCl.sub.2 or SbCl.sub.3. Certain disclosed compositions are preferably formed using substantially pure reagents and may include a dopant, such as a fluoride dopant. Described solutions may be used to form thin films, such as a thin film comprising SnO.sub.2, Sb:SnO.sub.2, F:SnO.sub.2, or (Sb,F):SnO.sub.2. Such thin films may have any desired thickness, such as a thickness of from 200 or 700 nm, and are extremely smooth, such as having an RMS surface roughness >3 nm, such as 3 nm to 10 nm, with certain embodiments having an RMS surface roughness <2 nm or <1 nm. Devices can be assembled comprising the thin films on a suitable substrate.
Fluorine removal from antimony fluorohalide catalyst using chlorocarbons
A method of chlorinating a antimony fluorohalide catalyst is disclosed. In one embodiment the method comprises contacting an antimony fluorohalide catalyst that contains one or more fluorines with a regenerating agent chosen from 2-chloro-3,3,3-trifluoropropene (1233xf), 1,1,1,3-tetrachloropropane (250fb), 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb) and combinations of 1233xf, 250fb, and 244bb, under conditions effective to exchange at least one fluorine in the antimony fluorohalide catalyst with chlorine. The method can be used to regenerate spent antimony fluorohalide catalyst, for example regenerating SbCl.sub.5 from SbF.sub.5.
HIGH PURITY TUNGSTEN PENTACHLORIDE AND PRODUCTION METHOD THEREOF
Provided are high purity tungsten pentachloride, and a method for obtaining such high purity tungsten pentachloride at a high yield and in an efficient manner. Tungsten pentachloride in which a total content of metal impurities excluding Sb, Ti, and As is less than 10 wtppm is obtained by uniformly mixing one or more types of reducing agents selected from Sb, Ti, and As and tungsten hexachloride at a molar ratio of 1.0:2.0 to 1.0:5.0 (reducing agent/WCl.sub.6 ratio) in an inert atmosphere to obtain a mixture, heating and reducing the mixture for 1 to 100 hours in a temperature range in which a chloride of tungsten and the reducing agent becomes a liquid phase to obtain a reduced product, heating the reduced product for 1 to 100 hours at 100 Pa or less and in a temperature range of 90 to 130 C., and performing reduced-pressure distillation thereto to obtain a reduced-pressure distilled product, heating and sublimating the reduced-pressure distilled product for 1 to 100 hours at 100 Pa or less and in a temperature range of 130 to 170 C., and performing sublimation purification of achieving precipitation at 70 to 120 C.
FLUORINE REMOVAL FROM ANTIMONY FLUOROHALIDE CATALYST USING CHLOROCARBONS
A method of chlorinating an antimony fluorohalide catalyst is disclosed. In one embodiment the method comprises contacting an antimony fluorohalide catalyst that contains one or more fluorines with a regenerating agent selected from 2-chloro-3,3,3-trifluoropropene (1233xf), 1,1,1,3-tetrachloropropane (250fb), 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb), and combinations of 1233xf, 250fb, and 244bb, under conditions effective to exchange at least one fluorine in the antimony fluorohalide catalyst with chlorine. The method can be used to regenerate spent antimony fluorohalide catalyst, for example regenerating SbCl.sub.5 from SbF.sub.5.
METHOD FOR PURIFYING ANTIMONY CHLORIDE SOLUTION THROUGH ARSENIC REMOVAL
The present disclosure belongs to the technical field of purification, and particularly relates to a method for purifying an antimony chloride solution through arsenic removal. The method includes: 1) adding copper-antimony alloy into a crude arsenic-containing antimony chloride solution to be treated in a protective atmosphere to obtain an antimony chloride solution containing low-concentration arsenic impurities after a reaction; and 2) performing distillation and concentration on the antimony chloride solution containing low-concentration arsenic impurities to obtain a high-purity antimony chloride solution. According to the present disclosure, the technical difficulty of removing impurity arsenic in a preparation process for high-purity antimony is solved, distillation is carried out under the condition of a low temperature, the operation is simple and low in energy consumption, and the technological process for preparation is simple, high in production efficiency, easy to realize, free of industrial pollution and therefore, suitable for industrialization.
SOLUTION DEPOSITION OF METAL SALTS TO FORM METAL OXIDES
Certain disclosed embodiments concern an organic solution suitable for forming metal oxide films, particularly thins films, comprising a metal salt selected from a Sn salt, an Sb salt, a dopant, and combinations thereof. The salt often is a halide salt, such as SnCl.sub.2 or SbCl.sub.3. Certain disclosed compositions are preferably formed using substantially pure reagents and may include a dopant, such as a fluoride dopant. Described solutions may be used to form thin films, such as a thin film comprising SnO.sub.2, Sb:SnO.sub.2, F:SnO.sub.2, or (Sb,F):SnO.sub.2. Such thin films may have any desired thickness, such as a thickness of from 200 or 700 nm, and are extremely smooth, such as having an RMS surface roughness>3 nm, such as 3 nm to 10 nm, with certain embodiments having an RMS surface roughness<2 nm or <1 nm. Devices can be assembled comprising the thin films on a suitable substrate.