CN102978414B - Method for precipitating gold from cyanogen-containing gold-plated waste liquid - Google Patents
Method for precipitating gold from cyanogen-containing gold-plated waste liquid Download PDFInfo
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- CN102978414B CN102978414B CN201210496357.4A CN201210496357A CN102978414B CN 102978414 B CN102978414 B CN 102978414B CN 201210496357 A CN201210496357 A CN 201210496357A CN 102978414 B CN102978414 B CN 102978414B
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Abstract
The invention provides a method for precipitating gold from a cyanogen-containing gold-plated waste liquid. The method comprises the following steps of: (1) adding the cyanogen-containing gold-plated waste liquid containing 1-500mg/L gold ions into a container, adjusting the pH to 12 with 10wt% NaOH, adding NaClO to adjust the redox potential to 350mv, and reacting for 30 minutes; adding 10wt% H2SO4 to adjust the pH to 7.5, adding NaClO to adjust the redox potential to 650mv, and reacting for 30 minutes so that the cyanogen concentration in the waste liquid is damaged to less than 1mg/L; and (2) adding a gold precipitator into the cyanogen-containing gold-plated waste liquid with damaged cyanogen, stirring for reaction and filtering. The method provided by the invention can be used for protecting environment, precipitating gold and improving the utilization rate of resources.
Description
Technical field
The invention belongs to technical field of chemical engineering, being specifically related to a kind of from containing the method precipitating gold the gold-plated waste liquid of cyanogen.
Background technology
Printed circuit board (Printed Circuit Board, be called for short PCB) need in production process to carry out gold-plated, prussiate plating is because its plating quality is good, erosion resistance is high, bath stability, and the advantages such as operating temperature range is wide, are not also replaced by cyanideless electro-plating at present completely.In prussiate electroplating effluent, cyano group (CN-) enters environment and can cause severe contamination, and usually containing 10-300mg/L gold, directly can enter environment and can cause the wasting of resources in waste liquid.
In order to fully utilize containing the gold-plated waste liquid resource of cyanogen, enrichment general at present, precipitation technology mainly contain: Zn powder substitution method is (as non-patent literature the research of gold recovering " from the electroplating effluent ", China's goods and materials regeneration, 1997.06.8-9.), active carbon adsorption and electrolytic process (as patent documentation CN 101705507A) etc.Zn powder substitution method temperature of reaction is high, complex treatment process, and for containing the weak effect in the gold-plated waste liquid of cyanogen, golden deposition rate is low, and in precipitation process, produce new chemical substance, increases wastewater treatment burden.Active carbon adsorption active regeneration difficulty, the absorption of waste liquid gold not exclusively.Gold in electrolytic process waste liquid can only drop to 5mg/L usually.
Summary of the invention
The object of the present invention is to provide a kind of method will precipitated completely containing the gold in the gold-plated waste liquid of cyanogen.
The method of the present invention that can realize above-mentioned purpose is a kind of from containing the method precipitating gold the gold-plated waste liquid of cyanogen, it is characterized in that, comprises the steps:
(1) cyanogen is destroyed
Add in a reservoir gold ion content be 1-500mg/L containing the gold-plated waste liquid of cyanogen, regulate pH to be 12 with the NaOH that mass concentration is 10%, add NaClO and regulate redox potential to be 350mv, reaction 30min, then add the H that mass concentration is 10%
2sO
4regulate pH to be 7.5, add NaClO and regulate redox potential to be 650mv, reaction 30min, makes the cyanogen concentration in waste liquid be destroyed to being less than 1mg/L;
(2) precipitation gold
Containing in the gold-plated waste liquid of cyanogen after being destroyed to cyanogen adds golden precipitation agent, stirring reaction, filters.
In above-mentioned steps (1), as container, the enamel reaction still that preferred non-corrosibility is strong.
In above-mentioned steps (2), described golden precipitation agent can be Sodium dimethyldithiocarbamate 40min or Thiocarb, can use solid, also can use its aqueous solution.
The add-on (in Sodium dimethyldithiocarbamate 40min or Thiocarb) of gold precipitation agent is generally 10-30000 times containing gold ion content in the gold-plated waste liquid of cyanogen, and doubly, more preferably 50-18000 doubly for preferred 20-20000.
The feed postition of gold precipitation agent can add for solid-state, also can be that the aqueous solution of 10-40% adds with mass concentration.
The reaction times of precipitation gold is generally 15-120min, preferred 15-60min, more preferably 15-30min, and the temperature of reaction of precipitation gold is generally room temperature-90 DEG C.
Use method process of the present invention containing the gold-plated waste liquid of cyanogen, the gold in waste liquid can be captured with sedimentary state completely, thus improves resource utilization.And method treatment process of the present invention is simple, waste liquid can qualified discharge after NaClO oxide treatment, alleviates environmental pollution.
Embodiment
The present invention is described in detail below in conjunction with embodiment; but the following examples are only the present invention's preferably embodiment; protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Embodiment 1
In 1000ml beaker, add cyanogen content is 108.0mg/L, gold content be 5.449mg/L containing cyanogen electroplating waste liquid 400ml, drip the NaOH adjustment pH to 12 that mass concentration is 10%, drip mass concentration be 11% NaClO regulate redox-potential (ORP) be 350mv, carry out the first step oxidation, reaction times 30min; Dripping mass concentration is the H of 10%
2sO
4regulate pH to be 7.5, drip NaClO and regulate ORP to be 650mv, carry out second step oxidation, reaction times 30min.Detect cyanogen in waste liquid with silver nitrate titration method, in waste liquid, cyanogen is less than 1mg/L.
Add the Sodium dimethyldithiocarbamate 40min aqueous solution 82.0g that the mass concentration prepared in advance is 40% in waste liquid after being at room temperature destroyed to cyanogen, stir 30min, filter.By atomic absorption spectrophotometry (WFX-110B type atomic absorption spectrophotometer, Beijing Rayleigh Analytical Instrument Co., Ltd produces), gold ion in filtrate is detected, do not detect gold ion.In filtrate, add NaClO solution adjustment ORP is 50mv, filters, filtrate qualified discharge.
Embodiment 2
Substitute Sodium dimethyldithiocarbamate 40min with Thiocarb, other destroys cyanogen, golden deposition condition completely with embodiment 1.Gold ion in filtrate is detected, does not detect gold ion.In filtrate, add NaClO solution adjustment ORP is 50mv, filters, filtrate qualified discharge.
Embodiment 3
With 32.8g Sodium dimethyldithiocarbamate 40min solid substitute its solution of 40% join cyanogen be destroyed after waste liquid in, other working method is completely with embodiment 1.Gold ion in filtrate is detected, does not detect gold ion.In filtrate, add NaClO solution adjustment ORP is 50mv, filters, filtrate qualified discharge.
Embodiment 4
With 32.8g Thiocarb solid substitute its solution of 40% join cyanogen be destroyed after waste liquid in, other working method is completely with embodiment 2.Gold ion in filtrate is detected, does not detect gold ion.In filtrate, add NaClO solution adjustment ORP is 50mv, filters, filtrate qualified discharge.
Embodiment 5
Carry out gold precipitation after waste liquid after being destroyed by cyanogen is heated to 90 DEG C, other working method is completely with embodiment 1.Gold ion in filtrate is detected, does not detect gold ion.In filtrate, add NaClO solution adjustment ORP is 50mv, filters, filtrate qualified discharge.
Embodiment 6
Stir 15min after adding golden precipitation agent, other working method is completely with embodiment 1.Detect gold ion in filtrate, gold ion content is 0.987mg/L.In filtrate, add NaClO solution adjustment ORP is 50mv, filters, filtrate qualified discharge.
Claims (9)
1., from containing the method precipitating gold the gold-plated waste liquid of cyanogen, it is characterized in that, comprise the steps:
(1) cyanogen is destroyed
Add in a reservoir gold ion content be 1-500mg/L containing the gold-plated waste liquid of cyanogen, regulate pH to be 12 with the NaOH that mass concentration is 10%, add NaClO and regulate redox potential to be 350mv, reaction 30min, then add the H that mass concentration is 10%
2sO
4regulate pH to be 7.5, add NaClO and regulate redox potential to be 650mv, reaction 30min, makes the cyanogen concentration in waste liquid be destroyed to being less than 1mg/L;
(2) precipitation gold
Containing in the gold-plated waste liquid of cyanogen after being destroyed to cyanogen adds excessive golden precipitation agent, stirring reaction, filters;
(3) in filtrate, add NaClO solution adjustment ORP is 50mv, filters;
Described golden precipitation agent is Sodium dimethyldithiocarbamate 40min or Thiocarb.
2. method according to claim 1, is characterized in that, the add-on of golden precipitation agent is 10-30000 times containing gold ion content in the gold-plated waste liquid of cyanogen.
3. method according to claim 2, is characterized in that, the add-on of golden precipitation agent is 20-20000 times containing gold ion content in the gold-plated waste liquid of cyanogen.
4. method according to claim 2, is characterized in that, the add-on of golden precipitation agent is 50-18000 times containing gold ion content in the gold-plated waste liquid of cyanogen.
5. method according to claim 1, is characterized in that, the feed postition of golden precipitation agent is solid-stately add or be that the aqueous solution of 10-40% adds with mass concentration.
6. method according to claim 1, is characterized in that, the reaction times of precipitation gold is 15-120min.
7. method according to claim 6, is characterized in that, the reaction times of precipitation gold is 15-60min.
8. method according to claim 6, is characterized in that, the reaction times of precipitation gold is 15-30min.
9. method according to claim 1, is characterized in that, the temperature of reaction of precipitation gold is room temperature-90 DEG C.
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CN106702158B (en) * | 2015-07-13 | 2019-01-01 | 灵宝欣宏金属科技有限公司 | Electrolysis method manufactures the regeneration method of waste produced by citric acid gold potassium and/or gold potassium cyanide |
CN108374090B (en) * | 2018-03-28 | 2019-07-12 | 广东致卓环保科技有限公司 | A kind of gold refinement method applied to the gold-plated waste liquid of sulfurous acid system |
CN113832343B (en) * | 2021-09-07 | 2023-04-18 | 昆明理工大学 | Method for recovering gold in thiosulfate gold leaching system by precipitation method |
CN113802008A (en) * | 2021-09-16 | 2021-12-17 | 兰州大学 | Method for treating waste liquid containing platinum group noble metal |
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CN85106777A (en) * | 1985-09-07 | 1987-03-25 | 中国有色金属工业总公司昆明贵金属研究所 | The recovery of iridium and method of purification |
CN1068600A (en) * | 1991-07-11 | 1993-02-03 | 上海贵稀金属提炼厂 | The novel gold dissolving liquid of gold coated article and molten golden method |
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CN101736159A (en) * | 2009-09-02 | 2010-06-16 | 紫金矿业集团股份有限公司 | Method for recovering gold from alkaline waste water |
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US4678584A (en) * | 1985-06-20 | 1987-07-07 | Cx/Oxytech, Inc. | Method of removing heavy metal from wastewater streams |
JPS63121625A (en) * | 1986-11-10 | 1988-05-25 | Kurita Water Ind Ltd | Method for recovering gold and silver from waste water |
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Patent Citations (6)
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CN85106670A (en) * | 1985-08-31 | 1987-03-11 | 中国有色金属工业总公司昆明贵金属研究所 | Extract precious metal with the CONTROLLED POTENTIAL method from the anode sludge |
CN85106777A (en) * | 1985-09-07 | 1987-03-25 | 中国有色金属工业总公司昆明贵金属研究所 | The recovery of iridium and method of purification |
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CN101736159A (en) * | 2009-09-02 | 2010-06-16 | 紫金矿业集团股份有限公司 | Method for recovering gold from alkaline waste water |
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CN101928840A (en) * | 2010-08-02 | 2010-12-29 | 惠州市奥美特环境科技有限公司 | Method for recovering gold and silver from waste circuit boards |
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