CN106044841A - Preparation method of chloroauric acid - Google Patents
Preparation method of chloroauric acid Download PDFInfo
- Publication number
- CN106044841A CN106044841A CN201610679335.XA CN201610679335A CN106044841A CN 106044841 A CN106044841 A CN 106044841A CN 201610679335 A CN201610679335 A CN 201610679335A CN 106044841 A CN106044841 A CN 106044841A
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- preparation
- hydrochloric acid
- reaction
- hydrogen peroxide
- gold chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G7/00—Compounds of gold
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a preparation method of chloroauric acid, including the steps of: performing a reaction to gold powder with a reactant mixture solution composed of hydrochloric acid and hydrogen peroxide, and separating the chloroauric acid from a product mixture solution generated in the reaction. In the preparation method, the gold powder is reacted with the reactant mixture solution composed of the hydrochloric acid and the hydrogen peroxide, wherein the hydrogen peroxide oxidizes the gold powder under an acid condition to generate water and the chloroauric acid, so that influence on purity of the chloroauric acid due to other impurities is avoided and product purity is ensured. In addition, the reaction side product, water, also can avoid environment pollution, so that the method is more environment-friendly.
Description
Technical field
The present invention relates to the technical field of gold chloride, particularly relate to the preparation method of a kind of gold chloride.
Background technology
Gold chloride, its molecular formula is HAuCl4, No. CAS: 16903-35-8.It is saffron crystallization, easily deliquescence, easily
It is dissolved in water.Decomposes is gold.Aqueous solution of chloraurate contains [the AuCl4]-ion of square plane, thus can prepare many
Containing plane square ion [AuX4]-salt (X=F, Cl, Br, I, CN, SCN, NO3) can be used for quasiconductor and integrated circuit
Lead frame partially plating gold, printed circuit board (PCB), electronic connector and other electric contacts gold-plated.Also red glass can be made
Glass.As analytical reagent, it is exclusively used in rubidium, the microanalysis of caesium and measures alkaloid composition etc..It is additionally operable to photographic material.Gold chloride
Salt, particularly sodium chloraurate NaAuCl4 is (by AuCl3React with NaCl and prepare), may replace poisonous hydrargyrum (II) salt as alkynes
The catalyst of hydrocarbon reaction.Meanwhile, gold chloride has important application as preparing nanometer grade gold aspect, general direct by reducing agent
The nanometer gold with fluorescent effect of reduction gold chloride, has important application in analytical chemistry.
In prior art, the preparation of gold chloride, using chloroazotic acid method more.The preparation process that chloroazotic acid is sent out is, by gold simple substance and chloroazotic acid
React after filtering, concentrating, add concentrated hydrochloric acid and denitrogenate compound, more concentrated gold chloride reagent crystallizes, grinds and obtain product, from ethanol
Solution is crystallized out anhydrous gold chloride (HAuCl4).Reaction equation: Au+HNO3+4HCl=HAuCl4+NO+2H2O.Chloroazotic acid method
Come with some shortcomings, as preparation process produces a large amount of red nitrogen oxides toxic gas, serious environment pollution.On the other hand, institute
The oxides of nitrogen gas and the unreacted nitric acid that produce are dissolved in reaction system with being difficult to avoid that, have impact on the pure of end product
Degree.
Summary of the invention
In view of this, the present invention provides the preparation method of a kind of gold chloride, the refined product obtained through this preparation method
Purity is higher, and more environmental protection.
The preparation method of a kind of gold chloride, reacts bronze and the reactant mixed solution being made up of hydrochloric acid and hydrogen peroxide,
Gold chloride is isolated again from the raw product mixture that described reaction obtains.
In above-mentioned preparation method, equation of its reaction is for for, 2Au+3H2O2+8HCl=2HAuCl4 +6H2O.In this reaction
In, Au is oxidized to Au3+Oxidizing electrode electromotive force be 1.52V, it is 1.763V that hydrogen peroxide is reduced into the oxidizing electrode electromotive force of water.
Although the oxidizing potential gap of the two is little, but due to Au3+5d, 6s, 6p unoccupied orbital, under chlorine anion effect occur dsp2
Hydridization, and become [AuCl with chlorine anion complexation4]-, it is possible to decrease the electrode potential that gold is oxidized, so Au is prior to chlorine anion quilt
Oxidation.
The present invention uses hydrogen peroxide as oxidant, it is reduced product is water, it is to avoid product exists gold chloride it
Outer impurity and affect the purity of gold chloride.
The temperature of above-mentioned reaction is preferably 80～100 DEG C, such as 80 DEG C, 82 DEG C, 85 DEG C, 90 DEG C, 95 DEG C, 98 DEG C, 99
DEG C or 100 DEG C etc..If temperature is too low, then the activation energy reacted is too low, reduces the conversion ratio of reaction；If the temperature of reaction is too high,
Then can cause product gold chloride decomposes.
At a temperature of this, the response time is 5～25min, such as 5min, 7min, 10min, 15min, 20min, 22min,
24min or 25min etc..
For obtaining higher conversion ratio, the consumption of hydrochloric acid is advisable with 6～10, such as 6,6.2,6.5,6.8,7,8,9,9.5,
9.8 or 10 etc., it is in terms of 1 by the material amount of bronze.The consumption of hydrogen peroxide can be 2.25～7.5, such as 2.25,2.5,3,4,5,
6,6.5,7,7.2,7.3,7.5 etc., it is in terms of 1 by the material amount of bronze.
Do not make the most harsh restriction as the concentration of hydrochloric acid, but the mass fraction of preferably hydrochloric acid is 30～37wt%, than
Such as 30wt%, 31wt%, 32wt%, 33wt%, 33.5wt%, 35wt%, 36wt%, 36.5wt% or 37wt% etc..Matter as hydrogen peroxide
Measuring mark, it is advisable with 15～35wt%, such as 15wt%, 16wt%, 18wt%, 20wt%, 25wt%, 30wt%, 32wt%, 34wt%
Or 35wt% etc..
Gold chloride is isolated specifically, first evaporate the mixing of described product from the product mixed liquor that described reaction obtains
Liquid is to concentrate, then crystallisation by cooling.Here, the temperature of evaporation is same as the temperature of reaction.The purpose of evaporation is so that product mixes
Closing the proud concentration of liquid, the terminal of evaporation is to occur that reddish black is thick with solution.The temperature of crystallisation by cooling can be at room temperature.
Certainly, in order to improve the purity of gold chloride product further, recrystallization etc. can be used again.No longer describe in detail in this.
As used herein, above-mentioned term:
" one ", " a kind of " and " described " are used interchangeably and refer to one or more.
"and/or" for represent the one or both of illustrated situation all it may happen that, such as, A and/or B includes (A
And B) and (A or B).
It addition, all numerical value that the scope stated by end points herein is comprised in the range of including this (such as, 1 to 10 bag
Include 1.4,1.9,2.33,5.75,9.98 etc.).
It addition, the statement of " at least one " herein include one and above all numbers (such as, at least 2, at least
4, at least 6, at least 8, at least 10, at least 25, at least 50, at least 100 etc.).
In the preparation method of the present invention, bronze and the reactant mixed solution being made up of hydrochloric acid and hydrogen peroxide are reacted, double
Oxygen water aoxidizes bronze in acid condition, generate water and gold chloride, it is to avoid the impact on gold chloride purity of other impurity, protects
Demonstrate,prove product purity.It addition, byproduct of reaction water it also avoid the pollution to environment, more environmental protection.
Detailed description of the invention
Technical scheme is further illustrated below in conjunction with embodiment.
Embodiment 1
Bronze is placed in many mouthfuls of beakers, so that methyl-silicone oil oil bath to be heated to 80 DEG C, adds the hydrochloric acid of 1/5th, start
Stirring.Being simultaneously added dropwise mass fraction with separatory funnel is 15wt% hydrogen peroxide (consumption is 2.25, is in terms of 1 by the material amount of bronze)
With remaining hydrochloric acid, the consumption of hydrochloric acid is 6 material amounts, is in terms of 1 by the material amount of bronze, and its mass fraction is the hydrochloric acid of 37wt%.
Reaction 25min terminates reaction.
Reaction starts to evaporate solution after being completely dissolved to bronze and is about original volume to reddish black thickness green pepper now liquor capacity
Field) time stop evaporation, cool down with cold water and stir, separating out crocus gold chloride crystal immediately, gained sample is dry with concentrated sulphuric acid
After bath, it is stored in the exsiccator filling silica gel.It is 98.1% that this example collects the yield of gold chloride, and purity is after tested
97.80%。
Embodiment 2
Bronze is placed in many mouthfuls of beakers, so that methyl-silicone oil oil bath to be heated to 100 DEG C, adds the hydrochloric acid of 1/5th, open
Dynamic stirring.Being simultaneously added dropwise mass fraction with separatory funnel is that (consumption is 2.25 to 35wt% hydrogen peroxide, with the material amount of bronze for 1
Meter) and remaining hydrochloric acid, the consumption of hydrochloric acid is 10 material amounts, is in terms of 1 by the material amount of bronze, and its mass fraction is 30wt%'s
Hydrochloric acid.Reaction 5min terminates reaction.
Reaction starts to evaporate solution after being completely dissolved to bronze and is about original volume to reddish black thickness green pepper now liquor capacity
Field) time stop evaporation, cool down with cold water and stir, separating out crocus gold chloride crystal immediately, gained sample is dry with concentrated sulphuric acid
After bath, it is stored in the exsiccator filling silica gel.It is 98.7% that this example collects the yield of gold chloride, and purity is after tested
98.15%。
Embodiment 3
Bronze is placed in many mouthfuls of beakers, so that methyl-silicone oil oil bath to be heated to 100 DEG C, adds the hydrochloric acid of 1/5th, open
Dynamic stirring.Being simultaneously added dropwise mass fraction with separatory funnel is 35wt% hydrogen peroxide (consumption is 7.5, is in terms of 1 by the material amount of bronze)
With remaining hydrochloric acid, the consumption of hydrochloric acid is 10 material amounts, is in terms of 1 by the material amount of bronze, and its mass fraction is the salt of 37wt%
Acid.Reaction 5min terminates reaction.
Reaction starts to evaporate solution after being completely dissolved to bronze and is about original volume to reddish black thickness green pepper now liquor capacity
Field) time stop evaporation, cool down with cold water and stir, separating out crocus gold chloride crystal immediately, gained sample is dry with concentrated sulphuric acid
After bath, it is stored in the exsiccator filling silica gel.It is 99.6% that this example collects the yield of gold chloride, and purity is after tested
98.26%。。
Embodiment 4
Bronze is placed in many mouthfuls of beakers, so that methyl-silicone oil oil bath to be heated to 90 DEG C, adds the hydrochloric acid of 1/5th, start
Stirring.Being simultaneously added dropwise mass fraction with separatory funnel is 35wt% hydrogen peroxide (consumption is 2.25, is in terms of 1 by the material amount of bronze)
With remaining hydrochloric acid, the consumption of hydrochloric acid is 6 material amounts, is in terms of 1 by the material amount of bronze, and its mass fraction is the hydrochloric acid of 37wt%.
Reaction 20min terminates reaction.
Reaction starts to evaporate solution after being completely dissolved to bronze and is about original volume to reddish black thickness green pepper now liquor capacity
Field) time stop evaporation, cool down with cold water and stir, separating out crocus gold chloride crystal immediately, gained sample is dry with concentrated sulphuric acid
After bath, it is stored in the exsiccator filling silica gel.It is 95.1% that this example collects the yield of gold chloride, and purity is after tested
98.32%。。
Embodiment 5
Bronze is placed in many mouthfuls of beakers, so that methyl-silicone oil oil bath to be heated to 90 DEG C, adds the hydrochloric acid of 1/5th, start
Stirring.It is simultaneously added dropwise mass fraction with separatory funnel to be 30wt% hydrogen peroxide (consumption is 5, is in terms of 1 by the material amount of bronze) and remain
Remaining hydrochloric acid, the consumption of hydrochloric acid is 8 material amounts, is in terms of 1 by the material amount of bronze, and its mass fraction is the hydrochloric acid of 33wt%.Reaction
20min terminates reaction.
Reaction starts to evaporate solution after being completely dissolved to bronze and is about original volume to reddish black thickness green pepper now liquor capacity
Field) time stop evaporation, cool down with cold water and stir, separating out crocus gold chloride crystal immediately, gained sample is dry with concentrated sulphuric acid
After bath, it is stored in the exsiccator filling silica gel.It is 99.5% that this example collects the yield of gold chloride, and purity is after tested
98.50%。
Owing to the numerical range of each technological parameter involved in the present invention can not all embody in the above-described embodiments,
As long as but the most envisioned any numerical value fallen in this numerical range above-mentioned of those skilled in the art all can implement this
Invention, the most also includes the combination in any of occurrence in the range of some numerical value.Herein, for the consideration of length, eliminate to
Going out the embodiment of occurrence in certain one or more numerical range, this disclosure being not to be construed as technical scheme is not filled
Point.
Applicant states, the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, i.e. do not mean that the present invention have to rely on above-mentioned in detail
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The equivalence of raw material each to product of the present invention is replaced and the interpolation of auxiliary element, concrete way choice etc., all falls within the present invention's
Within the scope of protection domain and disclosure.
Claims (8)
1. the preparation method of a gold chloride, it is characterised in that bronze and the reactant being made up of hydrochloric acid and hydrogen peroxide are mixed
Solution reaction, then isolate gold chloride from the raw product mixture that described reaction obtains.
Preparation method the most according to claim 1, it is characterised in that the temperature of described reaction is 80～100 DEG C.
Preparation method the most according to claim 1 and 2, it is characterised in that the response time is 5～25min.
Preparation method the most according to claim 1, it is characterised in that the consumption of described hydrochloric acid is 6～10, with the thing of bronze
Quality is 1 meter.
Preparation method the most according to claim 1, it is characterised in that the consumption of described hydrogen peroxide is 2.25～7.5, with gold
The material amount of powder is 1 meter.
Preparation method the most according to claim 1, it is characterised in that the mass fraction of described hydrochloric acid is 30～37wt%.
Preparation method the most according to claim 1, it is characterised in that the mass fraction of described hydrogen peroxide is 15～35wt%.
Preparation method the most according to claim 1, it is characterised in that divide from the product mixed liquor that described reaction obtains
Separate out gold chloride specifically, first evaporate described product mixed liquor to concentrate, then crystallisation by cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610679335.XA CN106044841A (en) | 2016-08-17 | 2016-08-17 | Preparation method of chloroauric acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610679335.XA CN106044841A (en) | 2016-08-17 | 2016-08-17 | Preparation method of chloroauric acid |
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| CN106044841A true CN106044841A (en) | 2016-10-26 |
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| CN201610679335.XA Pending CN106044841A (en) | 2016-08-17 | 2016-08-17 | Preparation method of chloroauric acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI626217B (en) * | 2017-01-24 | 2018-06-11 | 健鼎科技股份有限公司 | Method Of Making Inorganic Gold Compound |
| CN114261984A (en) * | 2020-09-25 | 2022-04-01 | 太仓沪试试剂有限公司 | A kind of preparation method of high activity and high purity chloroauric acid |
Citations (6)
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|---|---|---|---|---|
| CN1271781A (en) * | 1999-04-22 | 2000-11-01 | 中南工业大学 | Process for preparing gold by reduction of gold-contained chlorated liquid |
| CN101024864A (en) * | 2007-02-14 | 2007-08-29 | 苏州天地环境科技有限公司 | Method for recovering gold and copper from gold-plated printed circuit board waste material |
| CN103397186A (en) * | 2013-07-12 | 2013-11-20 | 湖南省同力电子废弃物回收拆解利用有限公司 | Regenerating method and process for recycling rare precious metals from electronic wastes |
| CN103667707A (en) * | 2013-12-04 | 2014-03-26 | 江苏融源再生资源科技有限公司 | Method of recovering gold and silver from a waste circuit board |
| CN104263961A (en) * | 2014-09-23 | 2015-01-07 | 铜仁市万山区盛和矿业有限责任公司 | Method for extracting gold from pyrite |
| CN104263962A (en) * | 2014-09-23 | 2015-01-07 | 铜仁市万山区盛和矿业有限责任公司 | Method for extracting gold from pyrrhotite |
-
2016
- 2016-08-17 CN CN201610679335.XA patent/CN106044841A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1271781A (en) * | 1999-04-22 | 2000-11-01 | 中南工业大学 | Process for preparing gold by reduction of gold-contained chlorated liquid |
| CN101024864A (en) * | 2007-02-14 | 2007-08-29 | 苏州天地环境科技有限公司 | Method for recovering gold and copper from gold-plated printed circuit board waste material |
| CN103397186A (en) * | 2013-07-12 | 2013-11-20 | 湖南省同力电子废弃物回收拆解利用有限公司 | Regenerating method and process for recycling rare precious metals from electronic wastes |
| CN103667707A (en) * | 2013-12-04 | 2014-03-26 | 江苏融源再生资源科技有限公司 | Method of recovering gold and silver from a waste circuit board |
| CN104263961A (en) * | 2014-09-23 | 2015-01-07 | 铜仁市万山区盛和矿业有限责任公司 | Method for extracting gold from pyrite |
| CN104263962A (en) * | 2014-09-23 | 2015-01-07 | 铜仁市万山区盛和矿业有限责任公司 | Method for extracting gold from pyrrhotite |
Non-Patent Citations (1)
| Title |
|---|
| 郑雅杰等: ""氯金酸的制备及其热解方法"", 《中国有色金属学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI626217B (en) * | 2017-01-24 | 2018-06-11 | 健鼎科技股份有限公司 | Method Of Making Inorganic Gold Compound |
| CN114261984A (en) * | 2020-09-25 | 2022-04-01 | 太仓沪试试剂有限公司 | A kind of preparation method of high activity and high purity chloroauric acid |
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