CN119899939A - A washing and drying device and an ultra-high purity gold production process based thereon - Google Patents
A washing and drying device and an ultra-high purity gold production process based thereon Download PDFInfo
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- CN119899939A CN119899939A CN202510406225.5A CN202510406225A CN119899939A CN 119899939 A CN119899939 A CN 119899939A CN 202510406225 A CN202510406225 A CN 202510406225A CN 119899939 A CN119899939 A CN 119899939A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B17/00—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement
- F26B17/18—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement with movement performed by rotating helical blades or other rotary conveyors which may be heated moving materials in stationary chambers, e.g. troughs
- F26B17/22—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement with movement performed by rotating helical blades or other rotary conveyors which may be heated moving materials in stationary chambers, e.g. troughs the axis of rotation being vertical or steeply inclined
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
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- C22B3/02—Apparatus therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/065—Nitric acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/001—Drying-air generating units, e.g. movable, independent of drying enclosure
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/004—Nozzle assemblies; Air knives; Air distributors; Blow boxes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/08—Drying solid materials or objects by processes not involving the application of heat by centrifugal treatment
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Abstract
本发明涉及一种洗涤烘干设备及基于其的超高纯黄金生产工艺，包括：洗烘罐；搅拌机构，包含转动安装的搅拌杆，搅拌杆呈管状结构且固定安装有搅拌叶片；分隔导料斗，固定安装在洗烘罐上，分隔导料斗的斗口与搅拌杆的外侧壁间距设置；液料循环机构，包含同轴套设在搅拌杆的顶部的均散环管，均散环管连通回流管且其下方均布连接设置有喷头；物料回流机构，包含同轴套设在搅拌杆内的驱动杆，驱动杆上安装有呈螺旋向上设置的绞龙叶片；分散烘干机构，包含固接在所述搅拌杆上的布散盘，搅拌杆上位于布设有导料管。本发明有效提高除杂率的黄金纯度，并且利用低品位合质金原料生产6N超高纯黄金。
The present invention relates to a washing and drying device and an ultra-high purity gold production process based thereon, comprising: a washing and drying tank; a stirring mechanism, comprising a rotatably mounted stirring rod, the stirring rod being a tubular structure and fixedly mounted with stirring blades; a partitioning guide hopper, fixedly mounted on the washing and drying tank, the hopper mouth of the partitioning guide hopper being spaced apart from the outer wall of the stirring rod; a liquid material circulation mechanism, comprising a uniform dispersion ring tube coaxially sleeved on the top of the stirring rod, the uniform dispersion ring tube being connected to a reflux pipe and having nozzles uniformly connected thereunder; a material reflux mechanism, comprising a driving rod coaxially sleeved in the stirring rod, the driving rod being mounted with auger blades spirally arranged upward; a dispersion drying mechanism, comprising a dispersing disc fixedly connected to the stirring rod, and a material guide pipe being arranged on the stirring rod. The present invention effectively improves the purity of gold with impurity removal rate, and produces 6N ultra-high purity gold using low-grade alloy gold raw materials.
Description
Technical Field
The invention relates to the technical field of gold production and purification, in particular to washing and drying equipment and an ultra-high purity gold production process based on the washing and drying equipment, and particularly relates to a 6N ultra-high purity gold production process by low-grade alloy.
Background
The purity of gold determines the performance and the use scene, and the general high-purity gold is applied to the fields of finance, industry, medical treatment, aerospace, scientific research, jewelry and the like, while the 6N high-purity gold is widely applied to miniature electronic elements, satellite element gold plating layers, quantum computation due to the extremely high purity and excellent unique performance. Therefore, in order to increase the purity of gold during the preparation process, impurities in gold must be removed.
The purification method of gold in the prior art mainly comprises Wang Shuifa, an electrolytic method, a pyrogenic method, a solvent extraction method, an ion exchange method and a microbiological method. The methods are all thousands of times, and impurities are removed in a corresponding mode, so that the impurity removal rate is improved. However, the existing method has an important defect that the purity of gold prepared by purifying gold raw materials with lower requirements can only reach below 4N, and gold raw materials used for preparing more than 5N or even 6N have higher requirements.
Therefore, the washing and drying equipment for further washing and drying by using the detergent is designed to effectively improve the impurity removal rate and further improve the purity of gold, and the defects that the traditional high-purity gold production method is poor in raw material adaptability, the impurity silver in gold is difficult to separate, the low-grade raw material cannot be used for producing high-purity gold, and the product cannot reach high-purity grade are overcome, and the washing and drying equipment for producing 6N ultra-high-purity gold by using the low-grade alloy raw material and the ultra-high-purity gold production process based on the washing and drying equipment are the research purpose of the invention.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides washing and drying equipment and an ultra-high-purity gold production process based on the washing and drying equipment, and the washing and drying equipment and the ultra-high-purity gold production process based on the washing and drying equipment can effectively solve the technical problems in the prior art.
The technical scheme of the invention is as follows:
A washing and drying apparatus comprising:
the washing and drying tank is characterized in that a corresponding sealing cover is fixedly arranged at the upper part of the washing and drying tank, a feeding pipe and a liquid inlet pipe are respectively arranged on the sealing cover, a corresponding discharging pipe is arranged at the bottom of the washing and drying tank, a corresponding liquid outlet pipe and a corresponding hot gas inlet pipe are respectively arranged at the side edge of the bottom of the washing and drying tank, and the liquid outlet pipe and the hot gas inlet pipe are both arranged above the sediment;
the stirring mechanism comprises a stirring rod which is driven by a corresponding first driving motor to rotate and is arranged at the lower side of the sealing cover, and the stirring rod is of a tubular structure and is fixedly provided with corresponding stirring blades;
A separation guide hopper is fixedly arranged on the inner side wall of the washing and drying tank below the stirring blade at the bottommost side, the separation guide hopper and the stirring rod are coaxially arranged, and a hopper opening of the separation guide hopper and the outer side wall of the stirring rod are arranged at intervals;
The liquid material circulating mechanism comprises a uniform-dispersion ring pipe coaxially sleeved at the top of the stirring rod, the uniform-dispersion ring pipe is communicated with the return pipe, and spray heads under the open slots are uniformly distributed and connected below the uniform-dispersion ring pipe;
The material backflow mechanism comprises a driving rod coaxially sleeved in the stirring rod and a second driving motor fixedly connected to the top of the sealing cover and opposite to the first driving motor in rotation direction, the driving rod is driven by the second driving motor, and auger blades which are spirally upwards arranged are arranged on the driving rod;
The dispersing and drying mechanism comprises a distributing disc fixedly connected to the top of the stirring rod and arranged below the distributing ring pipe, a plurality of penetrating holes penetrating through the distributing disc are uniformly distributed on the distributing disc, corresponding material guiding pipes are obliquely and uniformly distributed at the upper end of the distributing disc on the stirring rod, when the second driving motor is started, the driving rod and the auger blades are driven to rotate so as to convey gold mud deposited at the bottom of the washing and drying tank upwards and flow onto the distributing disc along with the material guiding pipes, and when the second driving motor reversely rotates, the stirring rod and the distributing disc are driven to rotate, and materials are uniformly dispersed and downwards conducted under the action of centrifugal force.
The washing and drying tank is supported and mounted by corresponding support legs, a corresponding closing cover is arranged on the feed pipe in an openable and closable manner, corresponding valves are fixedly arranged on the liquid inlet pipe, the discharge pipe, the hot gas inlet pipe, the liquid return pipe and the liquid discharge pipe, and the liquid outlet pipe and the hot gas inlet pipe are arranged below the separation guide hopper.
The bottom side of the sealing cover is downwards fixedly connected with a corresponding mounting pipe or mounting ring plate at a position corresponding to the stirring rod, the stirring rod is rotationally sleeved on the mounting pipe or the mounting ring plate through a corresponding bearing, and the stirring rod is in transmission connection with the output shaft end of the first driving motor through a gear meshing transmission mode or a belt transmission mode.
The ultra-high purity gold production process based on the washing and drying equipment comprises the following specific steps of:
s1, analyzing raw material gold, namely sampling and analyzing gold, silver, moisture and impurity elements;
s2, carrying out vacuum gasification separation, namely realizing separation of gold and silver by a physical method at one time under a high vacuum condition;
S3, separating gold from the aqua regia, namely preparing the aqua regia by using concentrated nitric acid and concentrated hydrochloric acid, wherein the aqua regia can dissolve gold, gold is dissolved in the dissolving reaction process, and meanwhile, impurity silver reacts with chloride ions to form silver chloride precipitate, so that the deep separation of gold and silver by a chemical method is realized again;
S4, filtering and settling the gold-containing noble liquid, namely filtering and purifying the gold-containing noble liquid through a titanium sintering filter element and a pressurizing and filtering mode, and then enabling the gold-containing noble liquid to enter a natural settling tank for standing and settling;
S5, extracting, namely extracting the gold-containing noble liquid by adopting a composite extractant, wherein gold and the extractant exist in a form of complex ions and are dissolved in an organic phase in the extracting process to form a load organic phase;
s6, back extraction, namely reducing gold ions in the loaded organic phase into gold atoms by a reducing agent by adopting a reduction back extraction method, and controlling the reaction temperature and time to produce ultra-high purity gold mud;
and S7, washing and drying, namely cleaning the gold mud by using the combined detergent and the washing and drying equipment to remove impurity content, and drying the gold mud to obtain the ultra-high purity gold mud.
The raw material gold used in the step S1 is low-grade alloy, and contains 60-99% of gold, 5-50% of silver and 0.1-10% of copper.
The vacuum degree of vacuum gasification separation in the step S2 is 1-100 Pa, the gasification temperature is 1400-1600 ℃, the heat preservation time is 3-10 h, and the silver vapor condensation temperature is 100-300 ℃.
The aqua regia gold in the step S3 is prepared by adopting concentrated nitric acid with the concentration of 95-98% and concentrated hydrochloric acid with the concentration of 33-36%, wherein the ratio of the concentrated nitric acid to the concentrated hydrochloric acid is 1:3, the dissolution reaction time of the aqua regia gold is 2-4 h, the reaction temperature is 50-100 ℃, and the cooling temperature after the reaction is 10-30 ℃.
The filtering device for filtering and settling the gold-containing noble liquid in the step S4 is a closed container with a titanium material shell, a plurality of titanium sintering filter cores are arranged in the container, the filtering pressure is 0.5-1.0 MPa, and the filtering device is kept stand through a natural settling tank after filtering, and the settling time is 8-16 h.
The extraction in the step S5 adopts a composite extractant to carry out liquid-liquid extraction of gold-containing noble liquid, wherein an extraction system mainly comprises multistage extraction, multistage washing and back extraction processes, the extraction speed is controlled by adopting frequency conversion, the extraction frequency is 15-40 Hz, the volume ratio O/A is 1:1.5-3.0, the number of stages of an extraction stage is 3-8, the number of stages of a washing stage is 3-5, the washing stage adopts washing agent for washing, and the addition concentration of the washing agent is 0.3-0.65 mol/L.
The reduction back extraction temperature of the step S6 is 50-90 ℃, the reduction back extraction time is 1.5-3 h, the washing and drying of the step S7 are carried out by using a combined detergent to clean the gold mud, wherein the washing temperature is 80-100 ℃, and the drying temperature is 200-450 ℃.
The invention has the advantages that:
1) On the basis of independent stirring, washing and drying, the invention combines the stirring, washing and drying into washing and drying integrated equipment, thereby realizing the double effects of washing and drying. The washing and drying tank is divided into an upper part and a lower part which can be communicated by utilizing a separation guide hopper, the detergent and sediment can be guided to the lower part of the washing and drying tank along with the separation guide hopper which gradually contracts in the process of stirring and washing the mixed detergent for effective separation, the detergent guided to the lower part of the washing and drying tank is pumped back to the upper part of the washing and drying tank through a liquid material circulating mechanism for continuous reaction with materials, and the detergent and the materials are dispersed into the materials in a centrifugal state through a dispersing disc which rotates along with a stirring rod, so that the sufficient contact reaction of the detergent and the materials is ensured, the utilization rate of the detergent is further improved, and the washing and impurity removal rate is further improved.
2) The precipitate is guided from the separating guide hopper with gradually shrinking mouth to the lower part of the washing and drying tank, and meanwhile, the gold mud with insufficient washing part can be mixed, so that the invention further improves the washing and impurity removing efficiency by coaxially arranging the driving rod which rotates reversely in the stirring rod with a tubular structure and installing the spiral upward auger blade on the driving rod, further conveying the material and the precipitate which are guided and filtered to the lower part of the washing and drying tank again and guiding the material and the precipitate into the dispersing disc through the guide pipe, and carrying out centrifugal dispersing and mixing contact with the reflowed detergent again.
3) After traditional washing, the materials are required to be transferred into a corresponding filtering container for filtering and then dried by a drying device, so that the materials are sticky in the device, and the recovery rate of finished products is reduced. Therefore, after washing is completed, sediment and washing liquid are directly guided to the lower part of the washing and drying tank through the gradually-shrinking separation guide hopper, a relatively independent space is formed in the washing and drying tank, the influence of the stirring process of the upper part is avoided, the solid-liquid separation of the next step is not required to be continued after the stirring process is completely completed, the washing and drying processing efficiency is effectively improved, and rapid solid-liquid layering is further effectively realized. The upper liquid of separation passes through the liquid material pump and draws together, and lower floor's precipitate upwards conveys and carries out centrifugal dispersion through pivoted dispersion disk through the auger blade of material reflux mechanism, carries out hot gas conveying through the steam pipe that advances, and the rethread separates the guide hopper and forms upwards open dispersion, fully contacts with the precipitate of dispersion and dries, ensures to improve drying efficiency.
4) On the basis of ensuring the washing impurity removal rate of gold mud and improving the efficiency, silver can be further removed by vacuum gasification separation, the saturated vapor of silver is larger and is concentrated on the top layer of vacuum gasification separation equipment in a gaseous state by utilizing the saturated vapor pressure difference of each element in alloy, the silver is collected and then enters a silver purification and recovery process, and gold is concentrated on the bottom layer of the vacuum gasification separation equipment in a solid state by virtue of smaller saturated vapor than silver and enters an ultra-high purity gold production process, and the gold and silver physical separation is realized once under high vacuum condition by adopting a high-temperature melting physical method, so that more silver slag is prevented from being generated to wrap gold in the gold separation process of the rear aqua regia, and the direct yield of gold is reduced; gold is dissolved by separating gold from aqua regia, gold is dissolved in the dissolving reaction process, meanwhile, impurity silver reacts with chloride ion to form silver chloride precipitate, the deep separation of gold and silver by a chemical method is realized again, the sedimentation of gold-containing noble liquid is realized by the pressurized filtration and natural sedimentation of a titanium sintering filter element, the gold and silver-containing noble liquid is mainly formed by multistage extraction, multistage washing and back extraction processes through liquid-liquid extraction, gold and an extractant exist in a complex ion form in an organic phase in the extraction process to form a loaded organic phase, the gold ion in the loaded organic phase is reduced into gold atoms by a reducing back extraction method by adopting a reducing agent, the reaction temperature and time are controlled to produce ultra-pure gold mud, finally, the gold mud is cleaned by using a combined detergent, the ultra-pure gold mud is dried, the impurity content requirement of the ultra-pure gold mud is further removed, the gold content in the gold mud is up to 99.9999%, and the direct yield of 6N ultra-pure gold is 99%. The method can effectively overcome the defects that the traditional high-purity gold production method has poor raw material adaptability, the impurity silver in gold is difficult to separate, the low-grade raw material cannot be used for producing high-purity gold, and the product cannot reach high purity, and the low-grade alloy raw material is used for producing 6N ultra-high-purity gold.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a schematic cross-sectional view of fig. 1.
FIG. 3 is a schematic view of the installation of the diffuser collar and the diffuser plate.
Fig. 4 is a flow chart of the production process in the present invention.
In the drawing, a washing and drying tank 1, a feeding pipe 101, a liquid inlet pipe 102, a discharging pipe 103, a liquid outlet pipe 104, a hot gas inlet pipe 105, a heat exchange jacket 106, a sealing cover 2, a stirring mechanism 3, a first driving motor 301, a stirring rod 302, stirring blades 303, a material guiding pipe 304, a separation material guiding hopper 4, a liquid material circulating mechanism 5, a material liquid pump 501, a uniform dispersion ring pipe 502, a spray head 503, a material reflux mechanism 6, a driving rod 601, a second driving motor 602, a packing auger blade 603, a dispersion drying mechanism 7 and a cloth dispersion plate 701.
Detailed Description
For the convenience of understanding by those skilled in the art, the structure of the present invention will now be described in further detail with reference to the accompanying drawings:
Embodiment one:
Referring to fig. 1 to 3, a washing and drying apparatus includes:
The washing and drying tank 1 is fixedly provided with a corresponding sealing cover 2 at the upper part, the sealing cover 2 is respectively provided with a feeding pipe 101 and a feeding pipe 102, the bottom of the washing and drying tank 1 is provided with a corresponding discharging pipe 103, the side edge of the bottom of the washing and drying tank 1 is respectively provided with a corresponding liquid outlet pipe 104 and a corresponding hot gas feeding pipe 105, and the liquid outlet pipe 104 and the hot gas feeding pipe 105 are both arranged above the sediment;
The stirring mechanism 3 comprises a stirring rod 302 which is rotatably arranged at the lower side of the sealing cover 2 and driven by a corresponding first driving motor 301, and the stirring rod 302 is in a tubular structure and is fixedly provided with a corresponding stirring blade 303;
A separation guide hopper 4 fixedly installed on the inner side wall of the washing and drying tank 1 below the stirring blade 303 at the bottommost side, wherein the separation guide hopper 4 is coaxially arranged with the stirring rod 302, and a hopper opening of the separation guide hopper is arranged at a distance from the outer side wall of the stirring rod 302;
the liquid material circulation mechanism 5, the liquid outlet pipe 104 is connected with a corresponding liquid outlet pipe and a corresponding return pipe in parallel through a corresponding liquid material pump 501, the liquid material circulation mechanism 5 comprises a uniform dispersion ring pipe 502 coaxially sleeved at the top of the stirring rod 302, the uniform dispersion ring pipe 502 is communicated with the return pipe, and spray heads 503 under open slots are uniformly distributed and connected below the uniform dispersion ring pipe;
The material reflux mechanism 6 comprises a driving rod 601 coaxially sleeved in the stirring rod 302 and a second driving motor 602 fixedly connected to the top of the sealing cover 2 and having a rotation direction opposite to that of the first driving motor 301, the driving rod 601 is driven by the second driving motor 602, and an auger blade 603 which is spirally upwards arranged is arranged on the driving rod 601;
The dispersing and drying mechanism 7 comprises a dispersing disc 701 fixedly connected to the top of the stirring rod 302 and arranged below the dispersing ring pipe 502, a plurality of penetrating holes penetrating through the dispersing disc 701 are uniformly distributed on the dispersing disc 701, corresponding material guide pipes 304 are obliquely and uniformly distributed at the upper end of the dispersing disc 701 on the stirring rod 302, when the second driving motor 602 is started, the driving rod 601 and the auger blades 603 are driven to rotate so as to convey gold mud deposited at the bottom of the washing and drying tank 1 upwards and flow onto the dispersing disc 701 along with the material guide pipes 304, and when the first driving motor 301 reversely rotates, the stirring rod 302 and the dispersing disc 701 are driven to rotate, and the materials are uniformly dispersed and downwards conducted under the action of centrifugal force.
On the basis of independent stirring, washing and drying, the invention combines the stirring, washing and drying into washing and drying integrated equipment, thereby realizing the double effects of washing and drying. The washing and drying tank 1 is divided into an upper part and a lower part which can be communicated by the separation guide hopper 4, the detergent and sediment can be guided to the lower part of the washing and drying tank 1 along with the separation guide hopper 4 which gradually contracts in the process of stirring and washing the mixed detergent to be effectively separated, the detergent guided to the lower part of the washing and drying tank 1 is pumped back to the upper part of the washing and drying tank to continuously react with materials by the liquid material circulating mechanism 5, and the detergent and the materials are dispersed into the materials in a centrifugal state by the dispersing disc which rotates along with the stirring rod 302, so that the sufficient contact reaction of the detergent and the materials is ensured, the utilization rate of the detergent is further improved, and the washing and impurity removing rate is improved.
The precipitate is guided from the separating guide hopper 4 with gradually shrinking openings to the lower part of the washing and drying tank 1, and meanwhile, the gold mud with insufficient washing part can be possibly mixed, therefore, the invention further improves the washing and impurity removing efficiency by coaxially arranging the driving rod 601 which rotates reversely in the stirring rod 302 with a tubular structure, arranging the spiral upward auger blade 603 on the driving rod 601, further conveying the material and the precipitate which are guided and filtered to the lower part of the washing and drying tank 1 again and guiding the material and the precipitate into the dispersing disc through the guide pipe 304, and carrying out centrifugal dispersing and mixing contact again along with the reflowed detergent.
After traditional washing, the materials are required to be transferred into a corresponding filtering container for filtering and then dried by a drying device, so that the materials are sticky in the device, and the recovery rate of finished products is reduced. Therefore, after washing is completed, sediment and washing liquid are directly guided to the lower part of the washing and drying tank 1 through the gradually-shrinking separation guide hopper 4, and a relatively independent space is formed in the washing and drying tank 1, so that the influence of the stirring process of the upper part is avoided, the next solid-liquid separation is not required to be continued after the stirring process is completed completely, the washing and drying processing efficiency is effectively improved, and further, the rapid solid-liquid layering is effectively realized. The upper liquid of separation passes through the liquid material pump and draws together, and lower floor's precipitate upwards conveys and carries out centrifugal dispersion through pivoted dispersion disk through auger blade 603 of material reflow mechanism 6, carries out hot gas conveying through hot gas inlet tube 105, and the rethread separates guide hopper 4 and forms upwards open dispersion, fully contacts with the precipitate of dispersion and dries, ensures to improve drying efficiency.
The washing and drying tank 1 is supported and mounted by corresponding support legs, a corresponding closing cover is arranged on the feeding pipe 101 in an openable and closable manner, corresponding valves are fixedly arranged on the liquid inlet pipe 102, the discharging pipe 103, the hot gas inlet pipe 105, the liquid return pipe and the liquid discharge pipe, and the liquid outlet pipe 104 and the hot gas inlet pipe 105 are arranged below the separation guide hopper 4.
The bottom side of the sealing cover 2 is fixedly connected with a corresponding mounting pipe or mounting ring plate downwards at a position corresponding to the stirring rod 302, the stirring rod 302 is rotatably sleeved on the mounting pipe or the mounting ring plate through a corresponding bearing, and the stirring rod 302 is connected to the output shaft end of the first driving motor 301 in a transmission mode of gear engagement or a belt transmission mode.
Embodiment two:
Referring to fig. 4, an ultra-high purity gold production process based on the washing and drying device comprises the following specific steps:
s1, analyzing raw material gold, namely sampling and analyzing gold, silver, moisture and impurity elements;
s2, carrying out vacuum gasification separation, namely realizing separation of gold and silver by a physical method at one time under a high vacuum condition;
S3, separating gold from the aqua regia, namely preparing the aqua regia by using concentrated nitric acid and concentrated hydrochloric acid, wherein the aqua regia can dissolve gold, gold is dissolved in the dissolving reaction process, and meanwhile, impurity silver reacts with chloride ions to form silver chloride precipitate, so that the deep separation of gold and silver by a chemical method is realized again;
S4, filtering and settling the gold-containing noble liquid, namely filtering and purifying the gold-containing noble liquid through a titanium sintering filter element and a pressurizing and filtering mode, and then enabling the gold-containing noble liquid to enter a natural settling tank for standing and settling;
S5, extracting, namely extracting the gold-containing noble liquid by adopting a composite extractant, wherein gold and the extractant exist in a form of complex ions and are dissolved in an organic phase in the extracting process to form a load organic phase;
s6, back extraction, namely reducing gold ions in the loaded organic phase into gold atoms by a reducing agent by adopting a reduction back extraction method, and controlling the reaction temperature and time to produce ultra-high purity gold mud;
and S7, washing and drying, namely cleaning the gold mud by using the combined detergent and the washing and drying equipment to remove impurity content, and drying the gold mud to obtain the ultra-high purity gold mud.
The raw material gold used in the step S1 is low-grade alloy, and contains 60-99% of gold, 5-50% of silver and 0.1-10% of copper.
The vacuum degree of vacuum gasification separation in the step S2 is 1-100 Pa, the gasification temperature is 1400-1600 ℃, the heat preservation time is 3-10 h, and the silver vapor condensation temperature is 100-300 ℃.
The aqua regia gold in the step S3 is prepared by adopting concentrated nitric acid with the concentration of 95-98% and concentrated hydrochloric acid with the concentration of 33-36%, wherein the ratio of the concentrated nitric acid to the concentrated hydrochloric acid is 1:3, the dissolution reaction time of the aqua regia gold is 2-4 h, the reaction temperature is 50-100 ℃, and the cooling temperature after the reaction is 10-30 ℃.
The filtering device for filtering and settling the gold-containing noble liquid in the step S4 is a closed container with a titanium material shell, a plurality of titanium sintering filter cores are arranged in the container, the filtering pressure is 0.5-1.0 MPa, and the filtering device is kept stand through a natural settling tank after filtering, and the settling time is 8-16 h.
The extraction in the step S5 adopts a composite extractant to carry out liquid-liquid extraction of gold-containing noble liquid, wherein an extraction system mainly comprises multistage extraction, multistage washing and back extraction processes, the extraction speed is controlled by adopting frequency conversion, the extraction frequency is 15-40 Hz, the volume ratio O/A is 1:1.5-3.0, the number of stages of an extraction stage is 3-8, the number of stages of a washing stage is 3-5, the washing stage adopts washing agent for washing, and the addition concentration of the washing agent is 0.3-0.65 mol/L.
The reduction back extraction temperature of the step S6 is 50-90 ℃, the reduction back extraction time is 1.5-3 h, the washing and drying of the step S7 are carried out by using a combined detergent to clean the gold mud, wherein the washing temperature is 80-100 ℃, and the drying temperature is 200-450 ℃.
On the basis of ensuring the washing impurity removal rate of gold mud and improving the efficiency, silver can be further removed by vacuum gasification separation, the saturated vapor of silver is larger and is concentrated on the top layer of vacuum gasification separation equipment in a gaseous state by utilizing the saturated vapor pressure difference of each element in alloy, the silver is collected and then enters a silver purification and recovery process, and gold is concentrated on the bottom layer of the vacuum gasification separation equipment in a solid state by virtue of smaller saturated vapor than silver and enters an ultra-high purity gold production process, and the gold and silver physical separation is realized once under high vacuum condition by adopting a high-temperature melting physical method, so that more silver slag is prevented from being generated to wrap gold in the gold separation process of the rear aqua regia, and the direct yield of gold is reduced; gold is dissolved by separating gold from aqua regia, gold is dissolved in the dissolving reaction process, meanwhile, impurity silver reacts with chloride ion to form silver chloride precipitate, the deep separation of gold and silver by a chemical method is realized again, the sedimentation of gold-containing noble liquid is realized by the pressurized filtration and natural sedimentation of a titanium sintering filter element, the gold and silver-containing noble liquid is mainly formed by multistage extraction, multistage washing and back extraction processes through liquid-liquid extraction, gold and an extractant exist in a complex ion form in an organic phase in the extraction process to form a loaded organic phase, the gold ion in the loaded organic phase is reduced into gold atoms by a reducing back extraction method by adopting a reducing agent, the reaction temperature and time are controlled to produce ultra-pure gold mud, finally, the gold mud is cleaned by using a combined detergent, the ultra-pure gold mud is dried, the impurity content requirement of the ultra-pure gold mud is further removed, the gold content in the gold mud is up to 99.9999%, and the direct yield of 6N ultra-pure gold is 99%. The method can effectively overcome the defects that the traditional high-purity gold production method has poor raw material adaptability, the impurity silver in gold is difficult to separate, the low-grade raw material cannot be used for producing high-purity gold, and the product cannot reach high purity, and the low-grade alloy raw material is used for producing 6N ultra-high-purity gold.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A washing and drying apparatus, comprising:
The washing and drying tank (1) is fixedly provided with a corresponding sealing cover (2) at the upper part, the sealing cover (2) is respectively provided with a feeding pipe (101) and a liquid inlet pipe (102), the bottom of the washing and drying tank (1) is provided with a corresponding discharging pipe (103), the side edge of the bottom of the washing and drying tank is respectively provided with a corresponding liquid outlet pipe (104) and a hot gas inlet pipe (105), and the liquid outlet pipe (104) and the hot gas inlet pipe (105) are both arranged above the sediment;
The stirring mechanism (3) comprises a stirring rod (302) which is rotatably arranged at the lower side of the sealing cover (2) by a corresponding first driving motor (301), wherein the stirring rod (302) is in a tubular structure and is fixedly provided with corresponding stirring blades (303);
a separation guide hopper (4) which is fixedly arranged on the inner side wall of the washing and drying tank (1) below the stirring blade (303) at the bottommost side, wherein the separation guide hopper (4) and the stirring rod (302) are coaxially arranged, and the hopper opening of the separation guide hopper is arranged at a distance from the outer side wall of the stirring rod (302);
The liquid material circulating mechanism (5), the liquid outlet pipe (104) is connected with a corresponding liquid outlet pipe and a corresponding return pipe in parallel through a corresponding liquid pump (501), the liquid material circulating mechanism (5) comprises a uniform dispersion ring pipe (502) coaxially sleeved at the top of the stirring rod (302), the uniform dispersion ring pipe (502) is communicated with the return pipe, and spray heads (503) below the uniform dispersion ring pipe are uniformly distributed and connected with the return pipe;
The material backflow mechanism (6) comprises a driving rod (601) coaxially sleeved in the stirring rod (302) and a second driving motor (602) fixedly connected to the top of the sealing cover (2) and opposite to the first driving motor (301) in rotation direction, the driving rod (601) is driven by the second driving motor (602), and an auger blade (603) which is spirally upwards arranged is arranged on the driving rod (601);
The dispersing and drying mechanism (7) comprises a distributing disc (701) fixedly connected to the top of the stirring rod (302) and arranged below the distributing ring tube (502), a plurality of penetrating holes penetrating through the distributing disc (701) are uniformly distributed on the distributing disc (701), corresponding material guide pipes (304) are obliquely and uniformly distributed at the upper end of the distributing disc (701) on the stirring rod (302), when the second driving motor (602) is started, the driving rod (601) and the auger blades (603) are driven to rotate so as to convey gold mud deposited at the bottom of the washing and drying tank (1) upwards and flow onto the distributing disc (701) along with the material guide pipes (304), and when the first driving motor (301) reversely rotates, the stirring rod (302) and the distributing disc (701) are driven to rotate, and the materials are uniformly dispersed and downwards conducted under the action of centrifugal force.
2. The washing and drying device according to claim 1, wherein a corresponding heat exchange jacket (106) is arranged on the outer side of the washing and drying tank (1) in an outward interlayer at intervals, a corresponding medium inlet pipe and a corresponding medium outlet pipe are respectively arranged on the upper side and the lower side of the heat exchange jacket (106) in a opposite mode, the medium inlet pipe is connected to an external heat exchange liquid source outwards through a corresponding liquid suction pump, the washing and drying tank (1) is supported and installed through corresponding support legs, a corresponding closing cover is arranged on the feeding pipe (101) in an openable and closable mode, corresponding valves are fixedly arranged on the liquid inlet pipe (102), the discharging pipe (103), the hot gas inlet pipe (105), the liquid return pipe and the liquid discharge pipe, and the liquid outlet pipe (104) and the hot gas inlet pipe (105) are arranged below the separation guide hopper (4).
3. The washing and drying equipment according to claim 1, wherein the bottom side of the sealing cover (2) is fixedly connected with a corresponding mounting pipe or a mounting ring plate downwards at a position corresponding to the stirring rod (302), the stirring rod (302) is rotatably sleeved on the mounting pipe or the mounting ring plate through a corresponding bearing, and the stirring rod (302) is in transmission connection with the output shaft end of the first driving motor (301) through a gear engagement transmission mode or a belt transmission mode.
4. An ultra-high purity gold production process based on a washing and drying device according to any one of the preceding claims 1-3, characterized by comprising the following specific steps:
s1, analyzing raw material gold, namely sampling and analyzing gold, silver, moisture and impurity elements;
s2, carrying out vacuum gasification separation, namely realizing separation of gold and silver by a physical method at one time under a high vacuum condition;
S3, separating gold from the aqua regia, namely preparing the aqua regia by using concentrated nitric acid and concentrated hydrochloric acid, wherein the aqua regia can dissolve gold, gold is dissolved in the dissolving reaction process, and meanwhile, impurity silver reacts with chloride ions to form silver chloride precipitate, so that the deep separation of gold and silver by a chemical method is realized again;
S4, filtering and settling the gold-containing noble liquid, namely filtering and purifying the gold-containing noble liquid through a titanium sintering filter element and a pressurizing and filtering mode, and then enabling the gold-containing noble liquid to enter a natural settling tank for standing and settling;
S5, extracting, namely extracting the gold-containing noble liquid by adopting a composite extractant, wherein gold and the extractant exist in a form of complex ions and are dissolved in an organic phase in the extracting process to form a load organic phase;
s6, back extraction, namely reducing gold ions in the loaded organic phase into gold atoms by a reducing agent by adopting a reduction back extraction method, and controlling the reaction temperature and time to produce ultra-high purity gold mud;
S7, washing and drying, namely cleaning the gold mud by using a combined detergent and the washing and drying equipment according to any one of claims 1-3 to remove impurity content, and drying the gold mud to obtain ultra-high purity gold mud.
5. The process for producing ultra-high purity gold according to claim 4, wherein the raw material gold used in step S1 is low-grade alloy containing 60 to 99% gold, 5 to 50% silver, and 0.1 to 10% copper.
6. The ultra-high purity gold production process according to claim 4, wherein the vacuum degree of vacuum gasification separation in the step S2 is 1-100 Pa, the gasification temperature is 1400-1600 ℃, the heat preservation time is 3-10 h, and the silver vapor condensation temperature is 100-300 ℃.
7. The process for producing ultra-high purity gold according to claim 4, wherein the aqua regia in step S3 is prepared by using concentrated nitric acid with a concentration of 95-98%, concentrated hydrochloric acid with a concentration of 33-36%, a ratio of the concentrated nitric acid to the concentrated hydrochloric acid is 1:3, a dissolution reaction time of the aqua regia is 2-4 h, a reaction temperature is 50-100 ℃, and a cooling temperature after the reaction is 10-30 ℃.
8. The ultra-high purity gold production process according to claim 4, wherein the filtering device used for filtering and settling the gold-containing noble liquid in the step S4 is a closed container with a titanium material shell, a plurality of titanium sintering filter cores are arranged in the container, the filtering pressure is 0.5-1.0 MPa, and the filtering device is placed in a natural settling tank for settling time of 8-16 h after filtering.
9. The ultra-high purity gold production process according to claim 4, wherein the extraction in step S5 is performed by using a composite extractant to perform liquid-liquid extraction of gold-containing noble liquid, wherein the extraction system mainly comprises multistage extraction, multistage washing and back extraction processes, the extraction speed is controlled by adopting variable frequency, the extraction variable frequency is 15-40 hz, the volume ratio O/a is 1:1.5-3.0, the number of stages of the extraction stage is 3-8, the number of stages of the washing stage is 3-5, the washing stage is washed by using a detergent, and the addition concentration of the detergent is 0.3-0.65 mol/L.
10. The ultra-high purity gold production process according to claim 4, wherein the reduction and stripping temperature in the step S6 is 50-90 ℃, the reduction and stripping time is 1.5-3 hours, and the washing and drying in the step S7 uses a combined detergent to clean gold mud, wherein the washing temperature is 80-100 ℃, and the drying temperature is 200-450 ℃.
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