CN103940694A - Method for measuring solubility of molybdenum powder - Google Patents
Method for measuring solubility of molybdenum powder Download PDFInfo
- Publication number
- CN103940694A CN103940694A CN201410150488.6A CN201410150488A CN103940694A CN 103940694 A CN103940694 A CN 103940694A CN 201410150488 A CN201410150488 A CN 201410150488A CN 103940694 A CN103940694 A CN 103940694A
- Authority
- CN
- China
- Prior art keywords
- molybdenum powder
- time
- molybdenum
- residual
- hydrogen peroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Catalysts (AREA)
Abstract
The invention discloses a method for measuring solubility of molybdenum powder. The method comprises the six steps of mixing and dissolving, shaking, carrying out suction filtration, drying, weighing and calculating. According to the method, a common hydrogen peroxide solution is taken as a solvent, the solubility of the molybdenum powder can be accurately measured, the testing cost is low, the operation is simple, the measurement result is accurate and reliable, and the solubility of the molybdenum powder can be accurately reflected and powerful data support is provided for subsequent preparation of a molybdenum-based catalyst by using the molybdenum powder.
Description
Technical field
The invention belongs to material properties test technical field, be specifically related to a kind of deliquescent method of molybdenum powder of measuring.
Background technology
Molybdenum is a kind of rare insoluble metal, and the sulfur tolerance of molybdenum uniqueness makes to have irreplaceable effect in its hydrofining, CO sulphur-resistant conversion and low-carbon alcohols building-up process in catalyst field.Its oxide or composite oxides are good catalyst of lower carbon number hydrocarbons selective oxidation, its good coordination property can be brought into play the advantage of complex compound catalyst in selective oxidation of olefins and asymmetric oxidation process, as the Synthesis of Propylene Oxide taking organic-molybdenum salt as catalyzer, unifining process taking the sulfide of molybdenum as active component etc.Therefore, molybdenum is in the existing quite long history of applied research of catalytic field, and catalyst with base of molybdenum plays an important role in chemical process.
In the time preparing catalysts containing molybdenum, generally all adopting compound and the oxide of the molybdenums such as molybdenum trioxide, ammonium molybdate, molybdenum sulfide is for many years raw material.In recent years, along with the increase of chemical industry to catalyst activity and stability requirement, it is that raw material is prepared highly active catalysts containing molybdenum that domestic and international Some Enterprises starts to adopt pure molybdenum powder.In the preparation process of this kind of catalysts containing molybdenum, first need molybdenum powder to utilize organic solvent to dissolve, and the dissolubility of molybdenum powder in organic solvent will directly have influence on serviceable life of production cost and production equipment of catalyzer.
For the different catalyzer of preparation, its organic solvent using is not quite similar, and this has brought difficulty to judgement molybdenum powder dissolubility.And, the conventionally test index of molybdenum powder is as granularity, pine ratio, specific surface area etc., dissolving with molybdenum powder in organic solvent does not have inevitable contacting, therefore, find the deliquescent method of a kind of direct test molybdenum powder in organic solvent, Kaolinite Preparation of Catalyst is had to good directive significance with preparation and the selecting of catalyzer industry molybdenum powder of molybdenum powder.
Summary of the invention
The object of the present invention is to provide a kind of deliquescent method of molybdenum powder of measuring, can measure exactly the dissolubility of molybdenum powder in hydrogen peroxide solution, for the follow-up catalyst with base of molybdenum of preparing provides important data.
The technical solution adopted in the present invention is: measure the deliquescent method of molybdenum powder, comprise the steps:
The first step, mixed dissolution
Get respectively hydrogen peroxide solution and molybdenum powder, in test tube, mix as the ratio of 2.4～2.6:1 taking the mol ratio of hydrogen peroxide solution and molybdenum powder, obtain mixed solution;
Second step, rocks
The mixed solution that the first step is made is placed on shaking table, and mixed solution is rocked for the first time, open test tube plug after rocking for the first time to exit, and then stoppered test tube is filled in row and rocked for the second time;
The 3rd step, suction filtration
Carry out suction filtration by being placed in bottle,suction through the mixed solution of second step processing, after suction filtration, the residual molybdenum powder particle that do not dissolve is adsorbed on the filter paper in bottle,suction;
The 4th step, dry
There is the filter paper of residual molybdenum powder particles to be placed in vacuum drying chamber the absorption of the 3rd step and be dried processing;
The 5th step, weighs
Molybdenum powder residual on filter paper through the 4th step processing is weighed, obtain the quality of residual molybdenum powder;
The 6th step, calculates
The quality of the molybdenum powder weighing according to the 5th step, and adopt following formula to calculate the solubleness of molybdenum powder in hydrogen peroxide;
Wherein S is solubleness;
M
1for the quality of the molybdenum powder obtained in the first step;
M
2while being the 5th step, weigh the quality of the residual molybdenum powder obtaining.
Feature of the present invention is also,
In the first step, the concentration of hydrogen peroxide solution is 2%～4%.
In second step, the frequency of shaking table is 40～70 revs/min.
The time of rocking for the first time in second step is 15～25 minutes; The time of rocking is for the second time 35～45 minutes.
The aperture of the filter paper using in bottle,suction in the 3rd step is 2～10 μ m.
In the 4th step, the temperature setting of vacuum drying chamber is set to 60～80 DEG C, and the dry time of processing is 1.8～2.2 hours.
The invention has the beneficial effects as follows: the present invention measures the deliquescent method of molybdenum powder, adopt comparatively common hydrogen peroxide solution as solvent, can measure exactly the dissolubility of molybdenum powder, the method testing cost is low, simple to operate, measurement result is accurately credible, reflects exactly the dissolubility of molybdenum powder, provides strong Data support for following adopted molybdenum powder carries out producing of catalyst with base of molybdenum.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Because the molybdenum powder of different production batch has different physics and chemistry characteristics, as granularity, pine is compared etc., show dissolubility aspect, the molybdenum powder of different production batch also has different solubleness, and therefore we choose the molybdenum powder of three different batches, measure its corresponding solubleness, illustrate that with this present invention measures the feasibility of the deliquescent method of molybdenum powder, the molybdenum powder of three different batches represents with A type molybdenum powder, Type B molybdenum powder and C type molybdenum powder respectively.
Embodiment 1
Measure the deliquescent method of molybdenum powder, comprise the steps:
The first step, mixed dissolution
Get respectively concentration and be 4% hydrogen peroxide solution 10mL and A type molybdenum powder and mix, wherein the mol ratio of hydrogen peroxide solution and A type molybdenum powder is 2.4:1, obtains mixed solution;
Second step, rocks
The mixed solution that the first step is made is placed on shaking table, and the frequency of shaking table is 40 revs/min, and mixed solution is rocked for the first time, after rocking 25 minutes, open test tube plug and exit, and then stoppered test tube fill in row rock for the second time, the time of rocking is for the second time 35 minutes;
The 3rd step, suction filtration
Carry out suction filtration by being placed in bottle,suction through the mixed solution of second step processing, when suction filtration, the aperture of filter paper used is 2 μ m, and after suction filtration, residual not dissolving A type molybdenum powder particle is adsorbed on filter paper;
The 4th step, dry
Have the filter paper of residual A type molybdenum powder particle to be placed in vacuum drying chamber the 3rd step absorption and be dried processing, the temperature of vacuum drying chamber is 60 DEG C, dry processing 1.8 hours;
The 5th step, weighs
A type molybdenum powder residual on filter paper through the 4th step processing is weighed, obtain the quality of residual A type molybdenum powder;
The 6th step, calculates
The quality of the residual A type molybdenum powder weighing according to the 5th step, and adopt following formula to calculate the solubleness of A type molybdenum powder in hydrogen peroxide;
Wherein S is solubleness;
M
1for the quality of the A type molybdenum powder obtained in the first step;
M
2while being the 5th step, weigh the quality of the residual A type molybdenum powder obtaining.
Be 99.59% through the solubleness that calculates A type molybdenum powder.
Checking dissolubility: above-mentioned A type molybdenum powder is dissolved in the preparation process of petroleum refining hydrofining catalysts containing molybdenum, and gained solubleness is 99.50%, the solubleness of the A type molybdenum powder recording with the present embodiment is 99.59% basically identical.
Embodiment 2
Measure the deliquescent method of molybdenum powder, comprise the steps:
The first step, mixed dissolution
Get respectively concentration and be 2% hydrogen peroxide solution 10mL and Type B molybdenum powder and mix, wherein the mol ratio of hydrogen peroxide solution and Type B molybdenum powder is 2.6:1, obtains mixed solution;
Second step, rocks
The mixed solution that the first step is made is placed on shaking table, and the frequency of shaking table is 70 revs/min, and mixed solution is rocked for the first time, after rocking 15 minutes, open test tube plug and exit, and then stoppered test tube fill in row rock for the second time, the time of rocking is for the second time 45 minutes;
The 3rd step, suction filtration
Carry out suction filtration by being placed in bottle,suction through the mixed solution of second step processing, when suction filtration, the aperture of filter paper used is 10 μ m, and after suction filtration, residual not dissolving Type B molybdenum powder particle is adsorbed on filter paper;
The 4th step, dry
Have the filter paper of residual A type molybdenum powder particle to be placed in vacuum drying chamber the 3rd step absorption and be dried processing, the temperature of vacuum drying chamber is 80 DEG C, dry processing 2.2 hours;
The 5th step, weighs
Type B molybdenum powder residual on filter paper through the 4th step processing is weighed, obtain the quality of residual Type B molybdenum powder;
The 6th step, calculates
The quality of the residual Type B molybdenum powder weighing according to the 5th step, and adopt following formula to calculate the solubleness of Type B molybdenum powder in hydrogen peroxide;
Wherein S is solubleness;
M
1for the quality of the Type B molybdenum powder obtained in the first step;
M
2while being the 5th step, weigh the quality of the residual Type B molybdenum powder obtaining.
Be 93.15% through the solubleness that calculates Type B molybdenum powder.
Checking dissolubility: above-mentioned Type B molybdenum powder is dissolved in the preparation process of petroleum refining CO sulphur-resistant conversion catalysts containing molybdenum, and gained solubleness is 93.10%, the solubleness of the Type B molybdenum powder recording with the present embodiment is 93.15% basically identical.
Embodiment 3
Measure the deliquescent method of molybdenum powder, comprise the steps:
The first step, mixed dissolution
Get respectively concentration and be 3% hydrogen peroxide solution 10mL and C type molybdenum powder and mix, wherein the mol ratio of hydrogen peroxide solution and C type molybdenum powder is 2.5:1, obtains mixed solution;
Second step, rocks
The mixed solution that the first step is made is placed on shaking table, and the frequency of shaking table is 55 revs/min, and mixed solution is rocked for the first time, after rocking 20 minutes, open test tube plug and exit, and then stoppered test tube fill in row rock for the second time, the time of rocking is for the second time 40 minutes;
The 3rd step, suction filtration
Carry out suction filtration by being placed in bottle,suction through the mixed solution of second step processing, when suction filtration, the aperture of filter paper used is 6 μ m, and after suction filtration, residual not dissolving C type molybdenum powder particle is adsorbed on filter paper;
The 4th step, dry
Have the filter paper of residual C type molybdenum powder particle to be placed in vacuum drying chamber the 3rd step absorption and be dried processing, the temperature of vacuum drying chamber is 70 DEG C, dry processing 2 hours;
The 5th step, weighs
C type molybdenum powder residual on filter paper through the 4th step processing is weighed, obtain the quality of residual C type molybdenum powder;
The 6th step, calculates
The quality of the residual C type molybdenum powder weighing according to the 5th step, and adopt following formula to calculate the solubleness of C type molybdenum powder in hydrogen peroxide;
Wherein S is solubleness;
M
1for the quality of the C type molybdenum powder obtained in the first step;
M
2while being the 5th step, weigh the quality of the residual C type molybdenum powder obtaining.
Be 95.24% through the solubleness that calculates C type molybdenum powder.
Checking dissolubility: above-mentioned C type molybdenum powder is dissolved in the preparation process of petroleum refining CO sulphur-resistant conversion catalysts containing molybdenum, and gained solubleness is 95.28%, the solubleness of the C type molybdenum powder recording with the present embodiment is 95.24% basically identical.
By the way, the present invention measures the deliquescent method of molybdenum powder, adopt comparatively common hydrogen peroxide solution as solvent, can measure exactly the dissolubility of molybdenum powder, the method testing cost is low, simple to operate, and measurement result is accurately credible, reflect exactly the dissolubility of molybdenum powder, provide strong Data support for following adopted molybdenum powder carries out producing of catalyst with base of molybdenum.
Claims (6)
1. measure the deliquescent method of molybdenum powder, it is characterized in that, comprise the steps:
The first step, mixed dissolution
Get respectively hydrogen peroxide solution and molybdenum powder, in test tube, mix as the ratio of 2.4～2.6:1 taking the mol ratio of hydrogen peroxide solution and molybdenum powder, obtain mixed solution;
Second step, rocks
The mixed solution that the first step is made is placed on shaking table, and mixed solution is rocked for the first time, open test tube plug after rocking for the first time to exit, and then stoppered test tube is filled in row and rocked for the second time;
The 3rd step, suction filtration
Carry out suction filtration by being placed in bottle,suction through the mixed solution of second step processing, after suction filtration, the residual molybdenum powder particle that do not dissolve is adsorbed on the filter paper in bottle,suction;
The 4th step, dry
There is the filter paper of residual molybdenum powder particles to be placed in vacuum drying chamber the absorption of the 3rd step and be dried processing;
The 5th step, weighs
Molybdenum powder residual on filter paper through the 4th step processing is weighed, obtain the quality of residual molybdenum powder;
The 6th step, calculates
The quality of the molybdenum powder weighing according to the 5th step, and adopt following formula to calculate the solubleness of molybdenum powder in hydrogen peroxide;
Wherein S is solubleness;
M
1for the quality of the molybdenum powder obtained in the first step;
M
2while being the 5th step, weigh the quality of the residual molybdenum powder obtaining.
2. the deliquescent method of mensuration molybdenum powder as claimed in claim 1, is characterized in that, the concentration of hydrogen peroxide solution described in the first step is 2%～4%.
3. the deliquescent method of mensuration molybdenum powder as claimed in claim 1, is characterized in that, the frequency of the shaking table described in second step is 40～70 revs/min.
4. the deliquescent method of mensuration molybdenum powder as claimed in claim 1, is characterized in that, the time of rocking for the first time described in second step is 15～25 minutes; The time of rocking is for the second time 35～45 minutes.
5. the deliquescent method of mensuration molybdenum powder as claimed in claim 1, is characterized in that, the aperture of the filter paper using in the bottle,suction described in the 3rd step is 2～10 μ m.
6. the deliquescent method of mensuration molybdenum powder as claimed in claim 1, is characterized in that, the temperature setting of the vacuum drying chamber described in the 4th step is set to 60～80 DEG C, and the dry time of processing is 1.8～2.2 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410150488.6A CN103940694A (en) | 2014-04-15 | 2014-04-15 | Method for measuring solubility of molybdenum powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410150488.6A CN103940694A (en) | 2014-04-15 | 2014-04-15 | Method for measuring solubility of molybdenum powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103940694A true CN103940694A (en) | 2014-07-23 |
Family
ID=51188457
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410150488.6A Pending CN103940694A (en) | 2014-04-15 | 2014-04-15 | Method for measuring solubility of molybdenum powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103940694A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101907550A (en) * | 2010-08-11 | 2010-12-08 | 肇庆理士电源技术有限公司 | Method for measuring degree of oxidation of lead powder |
| CN102262031A (en) * | 2011-04-22 | 2011-11-30 | 中国制浆造纸研究院 | Method for determining practical solubility of calcium sulfate for paper fillers |
| CN102507367A (en) * | 2011-11-15 | 2012-06-20 | 中国航空工业集团公司北京航空材料研究院 | Detection method for non-metal foreign substances in high speed steel powder |
| US20130245158A1 (en) * | 2012-03-19 | 2013-09-19 | Kemira Oyj | Methods of measuring a characteristic of a creping adhesive film and methods of modifying the creping adhesive film |
-
2014
- 2014-04-15 CN CN201410150488.6A patent/CN103940694A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101907550A (en) * | 2010-08-11 | 2010-12-08 | 肇庆理士电源技术有限公司 | Method for measuring degree of oxidation of lead powder |
| CN102262031A (en) * | 2011-04-22 | 2011-11-30 | 中国制浆造纸研究院 | Method for determining practical solubility of calcium sulfate for paper fillers |
| CN102507367A (en) * | 2011-11-15 | 2012-06-20 | 中国航空工业集团公司北京航空材料研究院 | Detection method for non-metal foreign substances in high speed steel powder |
| US20130245158A1 (en) * | 2012-03-19 | 2013-09-19 | Kemira Oyj | Methods of measuring a characteristic of a creping adhesive film and methods of modifying the creping adhesive film |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Bonke et al. | In situ electron paramagnetic resonance spectroscopy for catalysis | |
| Liu et al. | Transfer channel of photoinduced holes on a TiO2 surface as revealed by solid-state nuclear magnetic resonance and electron spin resonance spectroscopy | |
| Ma et al. | Atomically dispersed copper sites in a metal–organic framework for reduction of nitrogen dioxide | |
| Brozek et al. | Dynamic DMF binding in MOF-5 enables the formation of metastable cobalt-substituted MOF-5 analogues | |
| Finke et al. | Trisubstituted heteropolytungstates as soluble metal oxide analogs. III. Synthesis, characterization, phosphorus-31, silicon-29, vanadium-51, and 1-and 2-D tungsten-183 NMR, deprotonation, and proton mobility studies of organic solvent solute forms of HxSiW9V3O40x-7 and HxP2W15V3O62x-9 | |
| Gibson et al. | Complexation Equilibria Involving Salts in Non‐Aqueous Solvents: Ion Pairing and Activity Considerations | |
| Kochubey et al. | Combined X-ray absorption near-edge structure and X-ray photoelectron study of the electrocatalytically active cobalt (I) cage complexes and the clathrochelate cobalt (II)-and cobalt (III)-containing precursors and analogs | |
| Yamamoto et al. | Structural analysis of iron and manganese species in iron-and manganese-promoted sulfated zirconia | |
| Krawietz et al. | Alkali metal oxides, peroxides, and superoxides: a multinuclear MAS NMR study | |
| Lerf et al. | Nuclear Quadrupole Interaction and Time‐Resolved Perturbed γ‐γ‐Angular Correlation Spectroscopy: Applications in Chemistry, Materials Science, and Biophysical Chemistry. New Analytical Methods (31) | |
| Brown et al. | Electronic Structures of Formic Acid (HCOOH) and Formate (HCOO–) in Aqueous Solutions | |
| Hemmann et al. | Comparison of acidic site quantification methods for a series of nanoscopic aluminum hydroxide fluorides | |
| Mani et al. | A high‐throughput composite catalyst based on nickel carbon cubes for the hydrogenation of 5‐hydroxymethylfurfural to 2, 5‐dimethylfuran | |
| Foster et al. | Identifying reaction intermediates and catalytic active sites through in situ characterization techniques | |
| CN108152444B (en) | Method for detecting content of free nitric acid in bismuth nitrate solution | |
| CN101408515B (en) | Method for measuring zirconium in steel | |
| Seshadri et al. | Studies of molybdena-alumina catalysts: I. The formation of Mo (V) in reduced MoO3-Al2O3 systems and the determination of its absolute concentration by ESR techniques | |
| Rossetti et al. | EXAFS− XANES evidence of in situ cesium reduction in Cs− Ru/C catalysts for ammonia synthesis | |
| Kim et al. | A Crystallographic Study of the Decomposition of NO in Fully Indium Exchanged Zeolite Y. In+, In3+, and In3+–NO3–Complexes with Facially Coordinating Nitrate Ions Are in Supercages. Distorted Cubic In4O44+ Clusters Fill Sodalite Cavities | |
| CN105067758A (en) | Method for measuring content of carbonyl oxygen-containing functional groups on surface of carbon black | |
| Rolison et al. | Power of aerogel platforms to explore mesoscale transport in catalysis | |
| CN101526478B (en) | Method for detecting bullion content of metal carrier catalytic converter | |
| CN103940694A (en) | Method for measuring solubility of molybdenum powder | |
| CN104200025B (en) | A kind of method of quantitative analysis zeolitic imidazolate framework material lewis acidity | |
| CN111307888B (en) | Method for detecting content of primary hydroxyl in block polyether polyol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140723 |