[2]The invention relates to a method for dissolving a lateral, more particularly said, relates to a non-toxic, the security of the mixed acid of hydrochloric acid and phosphate three lateral three price stibium antimony-based method. In determining the content of the three sulfur when the lateral, usually with oxidation-reduction titration. Therefore, after dissolving three lateral should be in solution form to three price stibium , instead of a pentavalent antimony.
[4]Three sulfur antimony sulfide also called lateral (Sb2 S3), black solid powder. Insoluble in water, acetic acid, can slowly soluble in hot concentrated sulfuric acid, soluble in concentrated HCl, alcohol, proposed sulfur, vulcanization potassium solution. Melting point is 548 the [...] , boiling point the 1080-1090 [...]. High-temperature decomposition generated after the antimony oxide. Sb (III) can be dissolved in concentrated HCl, the chlorine can be expressed by general formula of the compound formed SbClx [(x-) + 3]+ to describe. when chlorine excessive presence of water can also be and trivalent antimony generating SbOCl insolubles. Furthermore, antimony be soluble in alkaline solution (such as soluble in Na2 S), and the like. Antimony sulfide can prevent oxidation and combustion of the high temperature of the material, maintaining friction stability of the material, anti-burning performance of the material is improved; also can reduce the organic binder in the decomposition rate at the time of high temperature, the service life of the material is improved; antimony sulfide projecting the performance of the adjustment of the friction coefficient of the material in the friction material is used widely in industry. In recent years are also used in the fireworks in medicine. In the prior art, three lateral dissolution method is mainly to five: loong H2 SO4- [...] solution of sulfuric acid (refer to GB 3255.1-1982. Three lateral-potassium bromate method of chemical analysis method for determining capacity MIL-A-159D antimony and the United States military standard 16 May 1972 SULFIDE ANTIMONY ( AMMUNITION IN USE FOR)); loong H2 SO4-KHSO4 dissolution method (refer to yan Guostrong arranges. Factory utility chemical analysis manual. Mechanical industrial press. 1995 (5): 470-472); loong HCl-KCl dissolution method (refer to Baidu search: entitled comprehensive design-Stibnite); reverse aqua regia-perchloricacid dissolved sulfide stibium law and concentrated HCl-H2 O2stibium law dissolved sulfide (refer to huang Yunxian , sun Weizhen. Chemical analysis method for the common elements. Chemical industry press, 2007), the two kind of method due to the use of an oxidizer HClO4 or H2 O2 the antimony most of the dissolved as a pentavalent antimony.
[5]Loong H2 SO4-the sulfuric acid decomposition [...]in the bottle adds the human loong H2 SO4, nearly boils the temperature of most of the sulfur volatilizes, the, discharge to the room temperature. Adding sulfuric acid heat [...] 5 min, the Sb5+ reduced to Sb3+, heat processed to move from, the bottle white smoke out of the sulfuric acid, removing residual [...] and SO2 reductibility such as gas. This method uses the heat-concentrated H2 SO4 is very dangerous, toxic and strong reducing agent [...] final expels the quantity is not easy to control, and is not completely dissolved. With song Zhigang. Sulfurizes measures the stibium frnace encountered in the specific problems and solutions. paoshan technology. 1991, (1): 1-6 introduced in the literature adding nitric acid to dissolve a large amount of black slag, improving dissolution effect. Loong H2 SO4-KHSO4 dissolution method is to use concentrated H2 SO4 and solid KHSO4 to be heated in the electric furnace, until the most of the sulfur to volatilize, discloses a speed increaser on the cover, to continue to dissolve about 1h. Time-consuming, is the biggest drawback of Sb2 S3 is not dissolved completely. The two kind of method is currently the most commonly used method.
[6]Loong HCl-KCl tartaric acid is also added in the melting method, by increasing the Cl- form the amount of SbClx [(x-) + 3]+, but still generating a large amount of hydrogen sulfide dissolved effect is poor. A literature (ding Wei and. Three antimony sulfide in the hydrochloric acid dissolved in the solution [J] theoretical analysis. Honam non-ferrous metal, 1997, (01): 53-55) a detailed analysis of the three lateral dissolved in the hydrochloric acid to conduct, due to the limited solubility of the existence of hydrogen sulfide.
[7]At present, in many three sulfur dissolving method in a lateral, to better concentrated sulfuric acid as the main solvent, compared with the present invention, however, hydrochloric acid and phosphoric acid mixed acid as the solvent it is safe to use, but also dissolved completely. The search HCl, H3 PO4 mixed acid dissolving three lateral three price stibium antimony-based method also not see a report.
[8]Content of the invention
[9]The purpose of this invention is to provide a method for dissolving a lateral, in particular chemical non-toxic, the security of the mixed acid dissolving method, the method using chemical products with a lateral three sulfur antimony (chemically pure, 97%), in order to dissolve the object, through chemical reaction, with hydrochloric acid and Cl- and compliance of the phosphate PO43- complex ions formed with the metal ion of the three lateral nature of antimony dissolved. Phosphoric acid as ternary in strong acid, non-volatile, is difficult to decompose, does not belong to the oxidizing acid. Phosphate ions have very strong mating capability, can work with many metal ion generating soluble complex, such as Fe3+ and PO43- can produce colorless soluble complex [Fe (PO4)2]3- and [Fe (HPO4)2]-, use of this nature, analytical chemistry of the commonly-used phosphoric acid ion with the metal ion, improve the stability of the metal ions. This dissolving method, the purpose of the phosphoric acid is added is to make PO43- and Sb3+ generating colorless, stable soluble complex [Sb (PO4)2]3- and [Sb (HPO4)2]-, avoid shooed H2 S process SbCl3 thereupon volatile, in order to guarantee the final determination of the accuracy of the antimony content. The method not only completely dissolved, and the solvent is non-toxic, inexpensive and safe, meet the environmental protection and industrial production requirements. The establishment of the dissolution method can also be used for lateral three sulfur antimony Stibnite in the dissolution of a lateral industrial three sulfur and antimony as the dissolution of the additives, there is a very broad application prospect.
[10]In order to realize the purpose of the above-mentioned invention, the present invention adopts the following technical scheme:
[11]A dissolving three sulfur antimony method of lateral, wherein the acid of the solvent and coordinating use of hydrochloric acid and phosphoric acid as the solvent to dissolve. Three lateral chemical products to antimony (chemically pure, 97%), in order to dissolve the object, measured after completely dissolved dissolved completely degree to illustrate content.
[12]In particular, the invention of the method of the three lateral, comprising the following steps:
[13]1, weighing 0.05g -0.1g sample (accurate to 0.0001g), placed in 250 ml conical flask;
[14]2, by adding 12 ml of concentrated HCl, 5 ml concentrated H3 PO4, discloses a speed increaser on the cover;
[15]3, the upper side of the adjustable low-temperature electric furnace is rocked until the solution- micro boils slow heating, the watch glass is removed;
[16]4, to continue to the 4 min -5 min, to catch net H2 S gas, a lead acetate test for inspection, without so as to not test H2 S, solution presents pale yellow transparent liquid is completely dissolved. The above-mentioned numerical range can be combined arbitrarily, not necessarily the corresponding relations.
[17]The prominent advantage of this invention lies in that, in order to (1) three lateral chemical products (chemically pure, 97%), in order to dissolve the object, non-toxic, inexpensive and safe hydrochloric acid and phosphoric acid as solvent, using a chemical reaction, in particular, acid-base reaction and reaction, is not easy to completely to be dissolved into the trivalent antimony dissolved three lateral, provides another lateral dissolving three sulfur antimony method. (2) the method is simple and easy to control, and under the low temperature, energy-saving, without danger. (3) completely dissolved, all of the reports is superior to the present method. (4) the application is wide, can be dissolved chemical preparation method for a lateral three sulfur antimony Stibnite in can also be used for dissolution of the three lateral industrial and three lateral use antimony as the dissolution of additives, there is a very broad application prospect.
[19]In the embodiment of the present invention for further description.
[20]Main reagent used in this invention the apparatus comprises:
[21]Hydrochloric acid (content 36.0-38.0%), analytical pure; phosphoric acid (content not less than 85.0%), analytical pure; three sulfur antimony (content 97.0%)with a lateral, chemically pure; Stibnite (not less than antimony content 71.0%); analytical balance: accuracy of 0.1 mg; adjustable electric furnace: 0-2000W; 250 ml conical flask; 50 ml beaker; such as the watch glass is glass.
[23]Weighing 0.05g three sulfur antimony a lateral sample, (accurate to 0.0001g), placed in 250 ml conical flask, by adding 12 ml HCl and 5 ml H3 PO4, discloses a speed increaser on the cover, the upper side of the adjustable low-temperature electric furnace is rocked until the solution- micro boils slow heating, to remove the watch glass is, to continue to the 4 min later, a lead acetate test for inspection, without so as to not test H2 S. Is dissolved to Sb3+ (existing form may have: Sb3+, SbClx [(x-) + 3]+, [Sb (PO4)2]3-, [Sb (HPO4)2]-).
[24]The parallel 5 time average content of three lateral 96.83%. Absolute error 0.17%
[26]Weighing 0.08g three sulfur antimony a lateral sample, (accurate to 0.0001g), placed in 250 ml conical flask, by adding 12 ml HCl and 5 ml H3 PO4, discloses a speed increaser on the cover, the upper side of the adjustable low-temperature electric furnace is rocked until the solution- micro boils slow heating, to remove the watch glass is, to continue to the 4.5 min later, a lead acetate test for inspection, without so as to not test H2 S. Is dissolved to Sb3+ (existing form may have: Sb3+, SbClx [(x-) + 3]+, [Sb (PO4)2]3-, [Sb (HPO4)2]-).
[27]The parallel 5 time, three lateral the average content of the antimony 96.78%. Absolute error 0.22%
[29]Weighing 0.10g three sulfur antimony a lateral sample, (accurate to 0.0001g), placed in 250 ml conical flask, by adding 12 ml HCl and 5 ml H3 PO4, discloses a speed increaser on the cover, the upper side of the adjustable low-temperature electric furnace is rocked until the solution- micro boils slow heating, to remove the watch glass is, to continue to the 5 min later, a lead acetate test for inspection, without so as to not test H2 S. Is dissolved to Sb3+ (existing form may have: Sb3+, SbClx [(x-) + 3]+, [Sb (PO4)2]3-, [Sb (HPO4)2]-).
[30]The parallel 5 time, the average content of three lateral 96.62%. Absolute error 0.38%
[31]Although the above specific embodiments of the present invention to give a detailed description and explanation, however, it should be specified that, we can according to the invention to the above-mentioned embodiment of the concept of various equivalent changes and modification, function of the generated still does not exceed the spirit of the covered by the specification, should be in the scope of protection of this invention.
