CN102774872A - Preparation method of granular chloroauric acid - Google Patents
Preparation method of granular chloroauric acid Download PDFInfo
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- CN102774872A CN102774872A CN2012102973961A CN201210297396A CN102774872A CN 102774872 A CN102774872 A CN 102774872A CN 2012102973961 A CN2012102973961 A CN 2012102973961A CN 201210297396 A CN201210297396 A CN 201210297396A CN 102774872 A CN102774872 A CN 102774872A
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Abstract
The invention relates to a preparation method of granular chloroauric acid. The preparation method comprises the steps of: dissolving gold by aqua regia; removing the rest nitric acid and nitrogen compound by using hydrochloric acid; and filtering, concentrating and pelleting to obtain the finished product. In the technical process, gold-containing mother liquor is not generated, and the product yield reaches up to 98%; and the prepared finished product is granulous, small in specific surface area, difficult in moisture absorption and dissolution and convenient to store and weigh for use, thus being widely applied to electronic industry and manufacturing of a semiconductor device.
Description
Technical field
The invention belongs to the fine chemical product production field, relate to the preparation of hydrochloro-auric acid, especially a kind of preparation method of granular hydrochloro-auric acid.
Background technology
Common hydrochloro-auric acid product is tiny needle crystal now, and its preparation method is: gold is with aqua regia dissolution after except that nitric acid and nitrogen compound, and filtration, condensing crystal, fractional crystallization, the mother liquor after the crystallization are waited until when preparing next time and used.Yield of this technology is about about 60%.Because tiny crystalloid hydrochloro-auric acid is exposed in the air very easily the moisture absorption and dissolves, packing with use very inconvenience of weighing, preserve improper meeting and dissolve into liquid.
Through retrieval, do not find the publication document of the granular hydrochloro-auric acid of preparation as yet.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of granular hydrochloro-auric acid.
A kind of preparation method of granular hydrochloro-auric acid, preparing method's step is:
⑴ dissolving: in beaker, put into gold ingot, add chloroazotic acid and heating and make the gold ingot dissolving, the solution heating is concentrated, gold ingot is 1.0～1.5 with the liquor capacity ratio;
⑵ denitrogenate: obtain adding in the solution concentrated hydrochloric acid to step ⑴, heating evaporation makes liquor capacity be concentrated into the capacity of step ⑴; Add the concentrated hydrochloric acid with capacity again, the reheat evaporation makes liquor capacity be concentrated into the capacity of step ⑴; This process is wanted triplicate, obtains chlorauric acid solution;
⑶ filter: with G4 glass funnel suction strainer, filtrating is transferred in the polytetrafluoroethylene beaker with chlorauric acid solution, and funnel and suction lottle are taken out with hydrochloric acid and washed repetition 3 times, and washing lotion merges in the filtrating in the polytetrafluoroethylene beaker;
⑷ concentrate: polytetrafluoroethylene beaker is transferred to evaporation concentration in 70～80 ℃ the water-bath together with liquid wherein, be concentrated to solution proportion is 2.25～2.45 always;
⑸ granulation: will concentrate the hydrochloro-auric acid drop to polyethylene board, and put into the moisture eliminator internal cooling rapidly, the hydrochloro-auric acid grain that will solidify after the cooling strips down from polyethylene board, gets granular hydrochloro-auric acid finished product.
And the gold ingot purity of said step ⑴ is >=99.99%, and preparation chloroazotic acid used hydrochloric acid and nitric acid is the commercially available article of analytical pure chemical reagent, the consumption of chloroazotic acid so that ingot all dissolve.
And the hydrochloric acid of at every turn denitrogenating in the process step among the said step ⑵ to be added and the volume ratio of solution are 2.3～3.5.
The technical scheme that the present invention adopts is:
Positively effect of the present invention and advantage are:
1, the present invention earlier use aqua regia dissolution with gold, removes remaining nitric acid and nitrogen compound with concentrated hydrochloric acid then, through filter, concentrated, granulation obtains granulous hydrochloro-auric acid product; Prepared granulous hydrochloro-auric acid product; Specific surface area is little, is difficult for the moisture absorption, makes things convenient for packing and use; Productive rate also will increase substantially simultaneously, reach 98%.
2, do not produce in the technological process of the present invention and contain golden mother liquor, one feeding product yield is high, has reduced funds tied up, has improved economic benefit, is widely used in electronic semiconductor components manufacturing and gold-plated and gold compound preparation.
Embodiment
Below in conjunction with specific embodiment the present invention is done further explain; Following embodiment is illustrative, is not determinate,
Can not limit protection scope of the present invention with following enforcement.
A kind of preparation method of granular hydrochloro-auric acid the steps include:
⑴ dissolving: in beaker, put 100 gram gold ingots, add 800 milliliters of chloroazotic acid (being mixed by 3 volume hydrochloric acid and 1 volume nitric acid), heating makes the gold dissolving, can add chloroazotic acid in case of necessity and make the gold dissolving fully; It is 100～150 milliliters that the solution heating is concentrated into volume, and ingot is 1.0～1.5 with the liquor capacity ratio.
⑵ denitrogenate: obtain adding 350 milliliters of concentrated hydrochloric acids in the solution to step ⑴, heating evaporation makes liquor capacity be concentrated into 100～150 milliliters; Add 350 milliliters of concentrated hydrochloric acids again, the reheat evaporation makes liquor capacity be concentrated into 100～150 milliliters; This process will repeat 3 times, obtains chlorauric acid solution.
⑶ filter: with G4 glass funnel suction strainer, filtrating is transferred in the polytetrafluoroethylene beaker with chlorauric acid solution, and funnel and suction lottle are taken out with 50 milliliters of hydrochloric acid and washed repetition 3 times, and washing lotion merges in the filtrating in the polytetrafluoroethylene beaker.
⑷ concentrate: polytetrafluoroethylene beaker is transferred to evaporation concentration in 70～80 ℃ the water-bath together with liquid wherein, be concentrated to solution proportion is 2.25～2.45 always.
⑸ granulation: the hydrochloro-auric acid drop that will concentrate is put into the moisture eliminator internal cooling rapidly to polyethylene board, and the hydrochloro-auric acid grain that will solidify after the cooling strips down from polyethylene board, and weighing and bagging gets finished product.Output 205.5 grams, productive rate 98.3%.
Gold is purity >=99.99% (4N) in the present embodiment, and hydrochloric acid and nitric acid are the analytical pure chemical reagent.
Below be finished product index and analytical results:
Above analytical data shows that the granular hydrochloro-auric acid preparation method of the present invention processes the granular finished product of hydrochloro-auric acid and can reach technical requirement.
Principles of Chemical Engineering of the present invention are: use aqua regia dissolution gold, with hydrochloric acid and remaining nitric acid and nitrogen compound reaction, generate the evaporable material its evaporation is removed again; Remove by filter insoluble impurities, be concentrated into hydrochloro-auric acid and become molten state, cooling makes its completely solidified not produce mother liquor, improves the product yield; Use tetrafluoroethylene as last spissated container, can reduce to greatest extent that container adheres to and the finished product loss that causes.
Claims (3)
1. the preparation method of a granular hydrochloro-auric acid, it is characterized in that: preparing method's step is:
⑴ dissolving: in beaker, put into gold ingot, add chloroazotic acid and heating and make the gold ingot dissolving, the solution heating is concentrated, gold ingot is 1.0～1.5 with the liquor capacity ratio;
⑵ denitrogenate: obtain adding in the solution concentrated hydrochloric acid to step ⑴, heating evaporation makes liquor capacity be concentrated into the capacity of step ⑴; Add the concentrated hydrochloric acid with capacity again, the reheat evaporation makes liquor capacity be concentrated into the capacity of step ⑴; This process is wanted triplicate, obtains chlorauric acid solution;
⑶ filter: with G4 glass funnel suction strainer, filtrating is transferred in the polytetrafluoroethylene beaker with chlorauric acid solution, and funnel and suction lottle are taken out with hydrochloric acid and washed repetition 3 times, and washing lotion merges in the filtrating in the polytetrafluoroethylene beaker;
⑷ concentrate: polytetrafluoroethylene beaker is transferred to evaporation concentration in 70～80 ℃ the water-bath together with liquid wherein, be concentrated to solution proportion is 2.25～2.45 always;
⑸ granulation: will concentrate the hydrochloro-auric acid drop to polyethylene board, and put into the moisture eliminator internal cooling rapidly, the hydrochloro-auric acid grain that will solidify after the cooling strips down from polyethylene board, gets granular hydrochloro-auric acid finished product.
2. the preparation method of granular hydrochloro-auric acid according to claim 1; It is characterized in that: the gold ingot purity of said step ⑴ is >=99.99%; Preparation chloroazotic acid used hydrochloric acid and nitric acid is the commercially available article of analytical pure chemical reagent, the consumption of chloroazotic acid so that ingot all dissolve.
3. the preparation method of granular hydrochloro-auric acid according to claim 1 is characterized in that: the hydrochloric acid of at every turn denitrogenating in the process step among the said step ⑵ to be added and the volume ratio of solution are 2.3～3.5.
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| CN2012102973961A CN102774872A (en) | 2012-08-21 | 2012-08-21 | Preparation method of granular chloroauric acid |
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| CN2012102973961A CN102774872A (en) | 2012-08-21 | 2012-08-21 | Preparation method of granular chloroauric acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106191461A (en) * | 2015-05-05 | 2016-12-07 | 沈阳有色金属研究院 | A kind of preparation method of high activity high-purity chloro auric acid |
| TWI626217B (en) * | 2017-01-24 | 2018-06-11 | 健鼎科技股份有限公司 | Method Of Making Inorganic Gold Compound |
| US10046976B1 (en) | 2017-01-25 | 2018-08-14 | Tripod Technology Corporation | Method of making inorganic gold compound |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060570A (en) * | 2010-12-28 | 2011-05-18 | 醴陵市彩虹颜料有限公司 | High-temperature underglaze gold ruby pigment and preparation method thereof |
| CN101549891B (en) * | 2008-04-03 | 2011-07-06 | 天津市风船化学试剂科技有限公司 | Method for preparing granular platinic chloride |
-
2012
- 2012-08-21 CN CN2012102973961A patent/CN102774872A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101549891B (en) * | 2008-04-03 | 2011-07-06 | 天津市风船化学试剂科技有限公司 | Method for preparing granular platinic chloride |
| CN102060570A (en) * | 2010-12-28 | 2011-05-18 | 醴陵市彩虹颜料有限公司 | High-temperature underglaze gold ruby pigment and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106191461A (en) * | 2015-05-05 | 2016-12-07 | 沈阳有色金属研究院 | A kind of preparation method of high activity high-purity chloro auric acid |
| TWI626217B (en) * | 2017-01-24 | 2018-06-11 | 健鼎科技股份有限公司 | Method Of Making Inorganic Gold Compound |
| US10046976B1 (en) | 2017-01-25 | 2018-08-14 | Tripod Technology Corporation | Method of making inorganic gold compound |
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Application publication date: 20121114 |