CN101891249A - Method for dissolving antimonous sulfide into stibious - Google Patents
Method for dissolving antimonous sulfide into stibious Download PDFInfo
- Publication number
- CN101891249A CN101891249A CN 201010259394 CN201010259394A CN101891249A CN 101891249 A CN101891249 A CN 101891249A CN 201010259394 CN201010259394 CN 201010259394 CN 201010259394 A CN201010259394 A CN 201010259394A CN 101891249 A CN101891249 A CN 101891249A
- Authority
- CN
- China
- Prior art keywords
- dissolving
- antimony
- antimonous sulfide
- solution
- dissolved
- 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.)
- Granted
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for dissolving antimonous sulfide, which utilizes the acidity and coordinating capability of hydrochloric acid and phosphoric acid to dissolve through a chemical dissolving method. In the method, a chemical product antimonous sulfide, the chemical purity of which is 97.0%, is utilized as a dissolving object, the content of antimonous sulfide can be measured after antimonous sulfide is dissolved under the optimum condition, and the measured result data can be used to illustrate the soluble completeness; the optimum condition of dissolving is as follows: adding 12ml of hydrochloric acid and 5ml of phosphoric acid; covering a watch glass, shaking the watch glass on an electric stove while slowly heating until the solution is boiling slightly, removing the watch glass, and maintaining slight boiling until the color of the solution is light yellow and transparent and is completely dissolved. Oxidation-reduction titration is used to measure the content of antimonous sulfide, therefore, the dissolved antimonous sulfide exists in the solution in the form of antimony (III), instead of in form of antimony (V). By using the dissolving method of antimonous sulfide in the invention, the measured result after a sample is dissolved reaches 96.82, which differs 0.18% to the actual value. In the method, the sample can be completely dissolved, and the solvent is non-toxic and safe and has low price, thereby meeting the requirements of environment protection and industrial production. The established dissolving method is also applied to dissolve antimonous sulfide in an antimonite and antimonous sulfide used as an additive in the industry and has wide application prospect.
Description
Technical field
The present invention relates to a kind of dissolving method of antimony trisulfide, more particularly say, relate to a kind of nontoxic, safe hydrochloric acid and phosphoric acid mixed-acid dissolution antimony trisulfide is antimonious method.When measuring the content of antimony trisulfide, normally use redox titration.Therefore, antimony trisulfide dissolving back should exist with the trivalent antimony form in solution, rather than quinquevalence antimony.
Background technology
Antimony trisulfide also claims antimony sulfide (Sb
2S
3), the black solid powder.Water insoluble, acetic acid can slowly be dissolved in the hot vitriol oil, are dissolved in dense HCl, alcohol, sulphur hydrogenation ammonium, potassium sulfide solution.Fusing point is 548 ℃, boiling point 1080-1090 ℃.Generate weisspiessglanz behind the pyrolytic decomposition.Sb (III) dissolves in dense HCl, and the compound that itself and chlorine form can be used general formula SbCl
x[(x-)+3]
+Describe.Chlorine can also generate the SbOCl insolubles with trivalent antimony when having excessive water to exist.In addition, antimony can be dissolved in the basic solution and (as be dissolved in Na
2S) etc.The oxidizing fire of material when antimony sulfide can prevent high temperature, the friction stability of maintenance material, the burn resistance energy of raising material; Can also reduce the decomposition rate of organic binder bond when high temperature, improve the work-ing life of material; The performance of the adjusting frictional coefficient that antimony sulfide is outstanding has made this material be used widely in the friction materials industry.Also be used in the fireworks and firecrackers medicament in recent years.In the prior art, the dissolving method of antimony trisulfide mainly contains five kinds: dense H
2SO
4-hydrazonium sulfate dissolution method (referring to GB 3255.1-1982. antimony trisulfide chemical analysis method-potassium bromate volumetric determination antimony and U.S. army mark MIL-A-159D 16 May 1972 ANTIMONY SULFIDE (FOR USE IN AMMUNITION)); Dense H
2SO
4-KHSO
4Dissolution method (to compile referring to Yan Guoqiang. factory's practical chemistry is analyzed handbook. the .1995 of China Machine Press (5): 470-472); Dense HCl-KCl dissolution method (is searched for referring to Baidu: comprehensive design topic-white antimony); Contrary chloroazotic acid-high chloro acid dissolution's antimony sulfide method and dense HCl-H
2O
2Dissolving antimony sulfide method (referring to Huang Yunxian, Sun Weizhen. the common elements chemical analysis method. Chemical Industry Press, 2007), in these two kinds of methods owing to used oxygenant HClO
4Or H
2O
2And make the most of dissolving of antimony become quinquevalence antimony.
Dense H
2SO
4-hydrazonium sulfate dissolution method is to add the dense H of people in Erlenmeyer flask
2SO
4, make the volatilization of most of sulphur under the temperature of closely boiling after, put to room temperature.Add hydrazonium sulfate heat-flash 5min, Sb
5+Be reduced to Sb
3+, move to the anxious heat in high temperature place again, make the white cigarette of sulfuric acid go out bottleneck, drive away residual hydrazonium sulfate and SO
2Deng reducing gas.This method is used hot dense H
2SO
4Danger close, the poisonous and wayward amount of driving out of at last of strong reductant hydrazonium sulfate, and also dissolving is not exclusively.Song Zhigang is arranged. survey particular problem and the terms of settlement that antimony ran in the antimony sulfide ore. big Golconda science and technology .1991, (1): introduce in the 1-6 document and add the black in a large number slag of nitric acid dissolve, improve solute effect.Dense H
2SO
4-KHSO
4Dissolution method is to use dense H
2SO
4With solid K HSO
4On electric furnace, heat and carry out, after making most of sulphur volatilization, cover watch-glass, continue the about 1h of dissolving.Consuming time, disadvantage is Sb
2S
3Dissolving not exclusively.These two kinds of methods are the most frequently used methods of present people.
Also add tartrate in the dense HCl-KCl dissolution method, by increasing Cl
-Amount form SbCl
x[(x-)+3]
+, but a large amount of hydrogen sulfide that produce still make solute effect poor.Have document (Ding Wei and. needle antimony is dissolved theoretical analysis [J] in hydrochloric acid soln. the Hunan non-ferrous metal, 1997, (01): 53-55) detailed analysis the solubility behavior of antimony trisulfide in hydrochloric acid because the existence of hydrogen sulfide and limited solubility.
At present, in numerous antimony trisulfide dissolving methods, be that main solvent is better with the vitriol oil, but compare that hydrochloric acid and phosphoric acid mixing acid are that solvent is safe in utilization, and dissolved is complete with the present invention.Use HCl, H by retrieval
3PO
4The mixed-acid dissolution antimony trisulfide is that antimonious method yet there are no report.
Summary of the invention
The dissolving method that the purpose of this invention is to provide a kind of antimony trisulfide, Hua Xue nontoxic, safe mixed-acid dissolution method particularly, this method is the dissolving object with chemical preparations antimony trisulfide (chemical pure, 97%), by chemical reaction, utilize the acidity and the Cl of hydrochloric acid
-Conformability and the PO of phosphoric acid
4 3-The character that forms coordination ion with metal ion is dissolved antimony trisulfide.Phosphoric acid is strong acid in the ternary, and is not volatile, is difficult for decomposing, and do not belong to oxidizing acid.Phosphate anion has very strong mating capability, can generate the title complex of solubility with many metal ions, as Fe
3+With PO
4 3-Can generate colourless solubility title complex [Fe (PO
4)
2]
3-[Fe (HPO
4)
2]
-, utilizing this character, phosphate anion commonly used cooperates with metal ion on the analytical chemistry, improves the stability of metal ion.In this dissolving method, the purpose that adds phosphoric acid makes PO exactly
4 3-With Sb
3+Generate colourless, stable solubility title complex [Sb (PO
4)
2]
3-[Sb (HPO
4)
2]
-, avoid driving away H
2SbCl in the S process
3Volatilization thereupon is to guarantee the accuracy of the last antimony content of being measured.This method is not only dissolved fully, and solvent is nontoxic, low price and safety, has satisfied the requirement on environmental protection and the industrial production.The dissolving method of being set up also can be used for the dissolving of antimony trisulfide in the white antimony and the dissolving that industrial antimony trisulfide uses as aspects such as additives, and boundless application prospect is arranged.
In order to realize the foregoing invention purpose, the present invention has adopted following technical scheme:
A kind of method of dissolving antimony trisulfide, wherein acidity and the coordination by solvent utilizes hydrochloric acid and phosphoric acid to dissolve for solvent.Be the dissolving object with chemical preparations antimony trisulfide (chemical pure, 97%), measure content after the dissolving fully the dissolved completeness is described.
Particularly, the method for dissolving antimony trisulfide of the present invention may further comprise the steps:
1, takes by weighing 0.05g～0.1g sample (being accurate to 0.0001g), place the 250mL Erlenmeyer flask;
2, add the dense HCl of 12mL, the dense H of 5mL
3PO
4, cover watch-glass;
3, shake the limit in adjustable low-temperature electric furnace top and be heated to slowly that solution is little to boil, remove watch-glass;
4, continue to keep little 4min～5min that boils, catch up with clean H
2S gas is used the Lead acetate paper inspection, and the test paper nondiscoloration is no H
2It is complete for dissolving that S, solution present little yellow transparent liquid.Above-mentioned numerical range can arbitrary combination, does not have inevitable corresponding relation.
Remarkable advantage of the present invention is, 1. with chemical preparations antimony trisulfide (chemical pure, 97%) is the dissolving object, the hydrochloric acid and the phosphoric acid of nontoxic, low price and safety are solvent, utilizing chemical reaction is acid-base reaction and complex reaction, dissolve being difficult for the antimonious antimony trisulfide of complete melt into, the method for another kind of dissolving antimony trisulfide is provided.2. this method is simple and easy to control, and carries out at a lower temperature, and is energy-conservation, do not have dangerous.3. dissolving is better than all methods of report at present fully.4. be widely used, method solubilized chemicals antimony trisulfide also can be used for the dissolving of antimony trisulfide in the white antimony and the dissolving that industrial antimony trisulfide uses as aspects such as additives, and boundless application prospect is arranged.
Embodiment
The present invention will be further described with embodiment below.
Main agents and instrument that the present invention uses comprise:
Hydrochloric acid (content 36.0～38.0%), analytical pure; Phosphoric acid (content is no less than 85.0%), analytical pure; Antimony trisulfide (content 97.0%), chemical pure; White antimony (antimony content is no less than 71.0%); Analytical balance: precision is 0.1mg; Adjustable electric furnace: 0～2000W; The 250mL Erlenmeyer flask; The 50mL beaker; Glass surface ware etc.
Embodiment 1
Take by weighing 0.05g antimony trisulfide sample, (being accurate to 0.0001g) places the 250mL Erlenmeyer flask, adds 12mL HCl and 5mL H
3PO
4, cover watch-glass, shake the limit in adjustable low-temperature electric furnace top and be heated to slowly that solution is little to boil, remove watch-glass, after continuing to keep little 4min that boils, use the Lead acetate paper inspection, the test paper nondiscoloration is no H
2S.Be dissolved as Sb
3+(existence form has: Sb
3+, SbCl
x[(x-)+3]
+, [Sb (PO
4)
2]
3-, [Sb (HPO
4)
2]
-).
Measure antimony trisulfide average content 96.83% through parallel 5 times.Absolute error 0.17%
Embodiment 2
Take by weighing 0.08g antimony trisulfide sample, (being accurate to 0.0001g) places the 250mL Erlenmeyer flask, adds 12mL HCl and 5mL H
3PO
4, cover watch-glass, shake the limit in adjustable low-temperature electric furnace top and be heated to slowly that solution is little to boil, remove watch-glass, after continuing to keep little 4.5min that boils, use the Lead acetate paper inspection, the test paper nondiscoloration is no H
2S.Be dissolved as Sb
3+(existence form has: Sb
3+, SbCl
x[(x-)+3]
+, [Sb (PO
4)
2]
3-, [Sb (HPO
4)
2]
-).
Through parallel 5 mensuration, the antimony trisulfide average content is 96.78%.Absolute error 0.22%
Embodiment 3
Take by weighing 0.10g antimony trisulfide sample, (being accurate to 0.0001g) places the 250mL Erlenmeyer flask, adds 12mL HCl and 5mL H
3PO
4, cover watch-glass, shake the limit in adjustable low-temperature electric furnace top and be heated to slowly that solution is little to boil, remove watch-glass, after continuing to keep little 5min that boils, use the Lead acetate paper inspection, the test paper nondiscoloration is no H
2S.Be dissolved as Sb
3+(existence form has: Sb
3+, SbCl
x[(x-)+3]
+, [Sb (PO
4)
2]
3-, [Sb (HPO
4)
2]
-).
Measure antimony trisulfide average content 96.62% through parallel 5 times.Absolute error 0.38%
Although above the specific embodiment of the present invention has been given to describe in detail and explanation; but should indicatedly be; we can carry out various equivalences to above-mentioned embodiment according to conception of the present invention and change and modification; when the function that it produced does not exceed spiritual that specification sheets contains yet, all should be within protection scope of the present invention.
Claims (6)
1. the dissolving method of an antimony trisulfide is characterized in that, utilizes the acidity and the coordination ability dissolving of hydrochloric acid and phosphoric acid by chemical dissolution method.
2. the method for claim 1 is characterized in that: be dissolving object, dissolving complete (solution presents little yellow transparent liquid) with chemical preparations antimony trisulfide (chemical pure, 97%) or white antimony.The existence form of its dissolving back antimony has increased [Sb (PO
4)
2]
3-[Sb (HPO
4)
2]
-
3. method as claimed in claim 1 or 2 may further comprise the steps:
1) takes by weighing 0.05g～0.1g sample (being accurate to 0.0001g), place the 250mL Erlenmeyer flask;
2) add the dense HCl of 12mL, the dense H of 5mL
3PO
4, cover watch-glass;
3) shake the limit in adjustable low-temperature electric furnace top and be heated to slowly that solution is little to boil, remove watch-glass;
4) continue to keep little 4min～5min that boils, catch up with clean H
2S gas is used the Lead acetate paper inspection, and the test paper nondiscoloration is no H
2It is complete for dissolving that S, solution present little yellow transparent liquid.
4. method as claimed in claim 3 wherein, takes by weighing 0.08g sample (being accurate to 0.0001g).
5. method as claimed in claim 3 wherein, continues to keep little 4.5min that boils.
6. method as claimed in claim 3, wherein, HCl (content 36.0～38.0%), analytical pure; H
3PO
4(content is no less than 85.0%), analytical pure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102593944A CN101891249B (en) | 2010-08-23 | 2010-08-23 | Method for dissolving antimonous sulfide into stibious |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102593944A CN101891249B (en) | 2010-08-23 | 2010-08-23 | Method for dissolving antimonous sulfide into stibious |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101891249A true CN101891249A (en) | 2010-11-24 |
| CN101891249B CN101891249B (en) | 2012-03-28 |
Family
ID=43100628
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102593944A Expired - Fee Related CN101891249B (en) | 2010-08-23 | 2010-08-23 | Method for dissolving antimonous sulfide into stibious |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101891249B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102072905A (en) * | 2010-08-24 | 2011-05-25 | 河北理工大学 | Analysis method of antimony trisulfide in mixed agent for firecracker |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1194237A (en) * | 1997-03-24 | 1998-09-30 | 张至德 | Wet process for preparing industrial pure antimony sulfide by removing load, arsenic, selenium, tin and mercury impurities in antimonic ore |
| JP2004307965A (en) * | 2003-04-09 | 2004-11-04 | Sumitomo Metal Mining Co Ltd | Method for removing arsenic and antimony by separation from slag fuming dust |
-
2010
- 2010-08-23 CN CN2010102593944A patent/CN101891249B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1194237A (en) * | 1997-03-24 | 1998-09-30 | 张至德 | Wet process for preparing industrial pure antimony sulfide by removing load, arsenic, selenium, tin and mercury impurities in antimonic ore |
| JP2004307965A (en) * | 2003-04-09 | 2004-11-04 | Sumitomo Metal Mining Co Ltd | Method for removing arsenic and antimony by separation from slag fuming dust |
Non-Patent Citations (1)
| Title |
|---|
| 《有色金属(选矿部分)》 20031231 张泽强 多金属硫化锑矿的综合回收 全文 1-6 , 第1期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102072905A (en) * | 2010-08-24 | 2011-05-25 | 河北理工大学 | Analysis method of antimony trisulfide in mixed agent for firecracker |
| CN102072905B (en) * | 2010-08-24 | 2012-09-19 | 河北理工大学 | Analysis method of antimony trisulfide in mixed agent for firecracker |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101891249B (en) | 2012-03-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mukherji | Analytical Chemistry of Zirconium and Hafnium: International Series of Monographs in Analytical Chemistry | |
| Lee et al. | Electrorefining of zirconium from zircaloy-4 cladding hulls in LiCl-KCl molten salts | |
| Mi et al. | A rhodamine–quinoline type molecular switch as a highly selective sequential sensor for Al 3+ and F− in aqueous solution | |
| Treitler et al. | How dangerous is too dangerous? A perspective on azide chemistry | |
| CN101891249B (en) | Method for dissolving antimonous sulfide into stibious | |
| Oxley et al. | Potential Biocides: Iodine‐Producing Pyrotechnics | |
| Geng et al. | Determination of total fluorine in coal by use of oxygen flask combustion method with catalyst | |
| Silvester et al. | The electrochemistry of simple inorganic molecules in room temperature ionic liquids | |
| Ansari et al. | Solvent effect on optical properties of hydrated lanthanide tris-acetylacetone | |
| Cho et al. | Electronic absorption spectra of U (III) ion in a LiCl–KCl eutectic melt at 450° C | |
| Reilly et al. | Trace element migration during UF4 bomb reduction: Implications to metal fuel production, worker health and safety, and nuclear forensics | |
| Raditzky et al. | Spectroscopic study of americium (III) complexes with nitrogen containing organic model ligands | |
| CN102072905B (en) | Analysis method of antimony trisulfide in mixed agent for firecracker | |
| CN102701893A (en) | Novel sulphur-free explosive for firecracker | |
| Linert et al. | Concerning the Problem of the Isokinetic Relationship. III. The Temperature-Dependance of the hammett Equation | |
| Taylor-Pashow et al. | Iodine Distribution During Evaporation of Hanford Waste Treatment Plant Direct Feed Low Activity Waste Effluent Management Facility Simulant | |
| CN102674288B (en) | Preparation method of boron-doped barium iron phosphate | |
| Polovov et al. | Vanadium speciation in fused alkali chlorides | |
| CN113640454B (en) | Rapid test method for calcium oxide content in limestone | |
| Petronio et al. | Complexation of scandium (III) with 8-quinolinol | |
| Selig | Ion-selective electrodes in organic elemental and functional group analysis: A review | |
| Asakura et al. | Extraction of hetero polyanions, P2W17O6110−, P2W18O626−, SiW11O398− by TBP | |
| CN101398404B (en) | Method for producing gas sensor for detecting novel refrigerant HC-600a | |
| CN102701179B (en) | Preparation method of Sc doped barium iron phosphate | |
| CN102674290B (en) | Preparation method of neodymium-doped barium iron phosphate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120328 Termination date: 20140823 |
|
| EXPY | Termination of patent right or utility model |