CN107794377A - Au plasma enrichment method in a kind of soil - Google Patents
Au plasma enrichment method in a kind of soil Download PDFInfo
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- CN107794377A CN107794377A CN201710965710.1A CN201710965710A CN107794377A CN 107794377 A CN107794377 A CN 107794377A CN 201710965710 A CN201710965710 A CN 201710965710A CN 107794377 A CN107794377 A CN 107794377A
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- foamed plastics
- container
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- candle ash
- candle
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
-
- 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
-
- 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
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1608—Leaching with acyclic or carbocyclic agents
- C22B3/1616—Leaching with acyclic or carbocyclic agents of a single type
-
- 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
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses Au plasma enrichment method in a kind of soil, comprise the following steps：S1：Sample is weighed, calcination, is transferred to after cooling in container；S2：1 is added in step S1 container:The Fe of 1 chloroazotic acid and 95 120g/L3+Solution, chloroazotic acid and Fe3+The volume ratio of solution is 45 60:1, the 3h of ebuillition of heated 1.5；Heating evaporation is concentrated into acidity 5% 10%, is diluted with water into an extract solution, standby；S3：Foamed plastics is added in a step S2 extract solution, shakes 45 90min；S4：Foamed plastics is taken out, is cleaned up with water, is dried；S5：Foamed plastics in step S4 is put into container, adds the thiourea solution that concentration is 10 12g/L in a reservoir, places a limiter in a reservoir so that by the position restriction of foamed plastics below the liquid level of thiourea solution；Covered in the opening of container, container is heated to 30 60min in boiling water bath；Constant volume obtains concentrated extracting solution after taking out foamed plastics while hot.With improving extracted amount so as to improving the effect of test accuracy.
Description
Technical field
The present invention relates to heavy metal-polluted soil Treatment process field, Au plasma enrichment method in more particularly to a kind of soil.
Background technology
Heavy metal pollution of soil is one of more serious environmental problem in the whole world.Usual heavy metal in soil total amount is higher, and its is right
Environment is potentially hazardous bigger.At present, the recovery technique on heavy metal pollution, still rest on based on phytoremediation, it is auxiliary
With chemistry, microorganism and Agro-ecology measure technological phase on, it is expected the biological effectiveness for reaching increase heavy metal, promote
The growth and absorption of plant, so as to improve the overall efficiency of phytoremediation.Using phytoremediation as leading " system engineering " still not
It is ripe, remain limitation in technology.Therefore, it is necessary to be monitored to the content of beary metal in soil, it is necessary to enter to its content
Row detection, the first step seek to the gold in soil carrying out enrichment extraction, and wherein steel foams method is the most frequently used Extraction and enrichment
One of method, steel foams method generally comprise the steps：Soil pattern is immersed in chloroazotic acid first and extracts gold, then uses foam
Plastics adsorb gold ion from extract solution, are finally extracted from foamed plastics gold ion with thiocarbamide, complete Au plasma
And enrichment.
The principle of thiourea gold extraction is as follows：1) (thiocarbamide also known as vulcanizes urea element (H2NCSNH2), in aqueous can be with transition
The stable complex cation of metal ion generation, the formula of reaction can be write as：Men++x(Thio)→[Me(Thio)x]n+Thio in formula
For thiocarbamide；N is chemical valence；X is ligancy.Thiocarbamide as a kind of strong acidic site body, can by the nonbonding electron pair of nitrogen-atoms or
Sulphur atom is combined with metalloform-selective.Au (I)-thiocarbamide complex cation (Au (Thio)2+) cationic property with it is corresponding
Cyanogen complex anion (Au (CN)2-) property is entirely different.Although the former stability is more slightly worse than the latter, Hg (Thio) is removed4 2+Than
Au(Thio)2+It is stable outer, other metals (such as Ag+、Cu2+、Cd2+、Pb2+、Zn2+、Fe2+、Bi3+) thiourea complex be all not so good as Au
(Thio)2+It is stable, therefore thiocarbamide is to Au+With preferable selectivity.Thiocarbamide is unstable in alkaline solution, easily decomposes generation vulcanization
Thing and cyanamide, cyanamide hydrolysis then generate urea.Thiocarbamide has reducing property in an acidic solution, is easily oxidized two sulphur of generation
Carbonamidine (is abbreviated as RSSR), and two sulphur carbonamidines further aoxidize, are decomposed into cyanamide and elementary sulfur, and reaction examination is：2SC
(NH2)2=(SCN2H3)2+2H++2e；(SCN2H3)2=SC (NH2)2+H2Thiocarbamide in NCN+S solution increases with acidity of medium
And tend towards stability.As the pH ＜ 1.75 of medium, the thiocarbamide of high concentration easily aoxidizes, therefore the appropriate to the occasion acid using dilute thiocarbamide of gold lixiviation
Property solution.
Foamed plastics is usually the liquid level for floating on thiourea solution in leaching process, causes some foamed plastics and thiocarbamide
Solution time of contact is short, and thiourea solution is relatively difficult to the inside into foamed plastics, and extraction is not complete enough.
The content of the invention
It is an object of the invention to provide Au plasma enrichment method in a kind of soil, existing Extraction and enrichment side is which solved
Method extraction is incomplete, the problem of influenceing test accuracy, has and improves extracted amount so as to improve the effect of test accuracy.
The present invention above-mentioned technical purpose technical scheme is that：
Au plasma enrichment method in a kind of soil, it is characterized in that, comprise the following steps：
S1：Sample is weighed, calcination, is transferred to after cooling in container；
S2：1 is added in step S1 container:The Fe of 1 chloroazotic acid and 95-120g/L3+Solution, chloroazotic acid and Fe3+The volume ratio of solution
For 45-60:1, ebuillition of heated 1.5-3h；Heating evaporation is concentrated into acidity in 5%-10%, is diluted with water into an extract solution, standby
With；
S3：Foamed plastics is added in a step S2 extract solution, places the first limiter in a reservoir so as to by foam plastic
The position restriction of material is boiled below the liquid level of an extract solution and shakes 45-90min；
S4：Foamed plastics is taken out, is cleaned up with water, is dried；
S5：Foamed plastics in step S4 is put into container, adds the thiourea solution that concentration is 10-12g/L in a reservoir,
The second limiter is placed in container so that by the position restriction of foamed plastics below the liquid level of thiourea solution；In the opening of container
Place is covered, and container is heated into 30-60min in boiling water bath；Constant volume obtains concentrated extracting solution after taking out foamed plastics while hot.
More preferably：First limiter includes fixed part, stop part and for connecting portion and the company of stop part
Socket part, fixed part are overlapped in the opening of container, and stop part is provided with small opening, and the size of small opening is less than foamed plastics.
Using such scheme, the first limiter is easy to use and is advantageous to foamed plastics being limited in the liquid of an extract solution
Below face, be advantageous to improve the contact area of foamed plastics and an extract solution, improve adsorption efficiency.
More preferably：Second limiter includes fixed cup and the press section in fixed cup, and fixed cup upper end is taken
The opening of container is connected to, spring, spring and any one in fixed cup or press section are provided between press section and fixed cup
It is fixed；The bottom of fixed cup is provided with small opening, and gap is provided between press section and the bottom of fixed cup, and the size in gap, which is at least, steeps
The size of foam plastics.
Using such scheme, foamed plastics is defined to the gap location between press section and fixed cup in the second limiter,
One side foamed plastics can be soaked in thiourea solution, improve the contact area of foamed plastics and thiourea solution, improve absorption
Efficiency；On the other hand, by pressing press section, can crushed foam plastics, make thiourea solution in the space of foamed plastics not
Break off a friendship and swap out into so as to improve the contacting efficiency of thiocarbamide molecule and the gold ion in foamed plastics, raising extraction efficiency.
More preferably：Press section is set for cup-shaped, and outer wall and the fixed cup internal wall transitions of press section coordinate；Press section
Bottom be provided with small opening, the size of small opening is less than foamed plastics.
Using such scheme, the possibility of space volatilization of the solvent between press section and fixed cup is reduced, keeps thiocarbamide molten
The liquid level stabilizing of liquid, prevent foamed plastics from reducing and being exposed outside liquid level with liquid level.
More preferably：Comprise the following steps：
S1：Sample is weighed, calcination, is transferred to after cooling in container；
S2：1 is added in step S1 container:The Fe of 1 chloroazotic acid and 95-120g/L3+Solution, chloroazotic acid and Fe3+The volume ratio of solution
For 50:1, ebuillition of heated 1.5-3h；Heating evaporation is concentrated into acidity in 5%-10%, is diluted with water into an extract solution, standby；
S3：Foamed plastics is added in a step S2 extract solution, the first limiter is put into container, foamed plastics is hindered
Gear boils below the liquid level of an extract solution and shakes 45-90min；
S4：Foamed plastics is taken out, is cleaned up with water, is dried；
S5：The thiourea solution that concentration is 10-12g/L is added in a reservoir, and fixed cup is put into container first, places into step
Press section, is then placed in fixed cup by the foamed plastics in S4, and the bottom of press section contacts with thiourea solution, so as to by foam
The position restriction of plastics is below the liquid level of thiourea solution；By pressing press section crushed foam plastics repeatedly in extraction process；
Covered in the opening of container, container is heated into 30-60min in boiling water bath；Constant volume obtains after taking out foamed plastics while hot
To concentrated extracting solution.
More preferably：In step S1, the technique of calcination is from normal temperature in Muffle furnace with 5 DEG C/min programming rate
650 DEG C are warming up to, is incubated 1.5h, Temperature fall.
More preferably：In step S3, the addition mass ratio of foamed plastics and an extract solution is 2-5：1000.
More preferably：Foamed plastics is the modified foamed plastics of candle ash, is prepared as follows to obtain：
A1：The preparation of candle ash：The glass cleaned up is placed in accumulation candle ash above the candle flame being burning；When wax
Candle ash accumulate to after certain thickness candle ash is collected it is standby；
A2：Candle ash is cooled down after calcination 1-2h under the conditions of 500-600 DEG C standby；
A3：Candle ash in step A2 and PPG, diisocyanate, water, catalyst, organic foam stabilizer are added
In the container for entering to scribble releasing agent, foamed after mixing under agitation in 60-70 DEG C of baking oven, foamed time 20-
25min；In parts by weight, the content of each component is as follows：Candle ash：1.6-6.4 part；PPG：20-25 parts；Two is different
Cyanate：45-60 parts；Water：3.0-3.4 part；Catalyst：1.5-2.5 part；Organic foam stabilizer：0.5-0.65 parts；
A4：The demoulding, cleans up rear drying to obtain candle ash with ethanol, isopropanol, liquid detergent and water after foam is cut and changes
Property foamed plastics.
It is foamed plastics is modified with candle ash, it is possible to increase foamed plastics is to gold ion in soil using such scheme
Absorption property because candle ash be a kind of material with loose structure, there is stronger absorption property, change by candle ash
Property after foamed plastics porosity improve, so as to improve the absorption property to gold ion.
More preferably：Step A2 calcination technique is：200 DEG C are warming up to 5 DEG C/min programming rate, insulation
30min, continue to be warming up to 500-600 DEG C with 5 DEG C/min programming rate, be incubated 1-2h, naturally cool to room temperature.
More preferably：In step A3, candle ash mixes with PPG first, and ultrasonic wave added disperses, then with its
He mixes component.
In summary, the invention has the advantages that：1st, the use of the first limiter and the second limiter is to improving
The extraction efficiency of gold ion has critical effect, on the one hand, foamed plastics is limited in an extract solution by the first limiter
Liquid level below, the contact area of increase foamed plastics and an extract solution, raising adsorption efficiency；Second limiter is by foam plastic
Material is limited in below the liquid level of thiourea solution and constantly crushed foam plastics are completed in bubble and in solution during experiment
Fluid exchange, so that the gold ion in bubble fully be extracted, improve extraction efficiency；2nd, by foamed plastics candle ash
It is modified, it is possible to increase foamed plastics is to the absorption property of gold ion in soil, because candle ash is that a kind of have loose structure
Material, there is stronger absorption property, improved by the modified foamed plastics porosity of candle ash, so as to improve to gold from
The absorption property of son.
Brief description of the drawings
Fig. 1 is that the first limiter of embodiment 15 and container are used cooperatively view；
Fig. 2 is that the second limiter of embodiment 15 and container are used cooperatively view；
Fig. 3 be embodiment 15 Fig. 2 in A portions partial enlarged drawing.
In figure, 1, container；2nd, the first limiter；21st, fixed part；22nd, stop part；23rd, connecting portion；3rd, small opening；4th, second
Limiter；41st, fixed cup；411st, flange；42nd, press section；43rd, spring；44th, gap.
Embodiment
The present invention is described in further detail below.
This specific embodiment is only explanation of the invention, and it is not limitation of the present invention, people in the art
Member can make the modification of no creative contribution to the present embodiment as needed after this specification is read, but as long as at this
All protected in the protection domain of invention by Patent Law.
Embodiment 1：A kind of preparation method of the modified foamed plastics of candle ash, comprises the following steps：
A1：The preparation of candle ash：The glass cleaned up is placed in accumulation candle ash above the candle flame being burning；When wax
Candle ash accumulate to after certain thickness with scraper candle ash is scraped it is standby；
A2：Candle ash is placed in crucible, 200 DEG C is warming up to 5 DEG C/min programming rate, is incubated 30min, continue with 5 DEG C/
Min programming rate is warming up to 550 DEG C, is incubated 1.5h, naturally cools to room temperature, standby；
A3：Raw material is weighed according to following parts by weight：Candle ash in step A2：4.8 part；PPG：22 parts；Two isocyanic acids
Ester：50 parts；Water：3.2 part；Catalyst：2.0 part；Organic foam stabilizer：0.6 part；Wherein, PPG uses polyethers
Triol 330N, diisocyanate use toluene di-isocyanate(TDI), and catalyst is dibutyl tin laurate, and silicon foams are stable
Agent is polyether silicone oil；First by candle ash and PPG mix after ultrasonic disperse, then with diisocyanate, water, catalyst,
Organic foam stabilizer adds in the container for scribbling releasing agent together, is sent out after mixing under agitation in 65 DEG C of baking oven
Bubble, foamed time 22min；
A4：The demoulding, after being cleaned by ultrasonic totally with ethanol, isopropanol, liquid detergent and water respectively after foam is cut, it is put into 60 DEG C
The modified foamed plastics of drying to obtain candle ash, is cut into 3cm*1.5cm*1.5cm fritters, is designated as P1 in baking oven.
Embodiment 2：A kind of preparation method of the modified foamed plastics of candle ash, comprises the following steps：
A1：The preparation of candle ash：The glass cleaned up is placed in accumulation candle ash above the candle flame being burning；When wax
Candle ash accumulate to after certain thickness with scraper candle ash is scraped it is standby；
A2：Candle ash is placed in crucible, 200 DEG C is warming up to 5 DEG C/min programming rate, is incubated 30min, continue with 5 DEG C/
Min programming rate is warming up to 550 DEG C, is incubated 1h, naturally cools to room temperature, standby；
A3：Raw material is weighed according to following parts by weight：Candle ash in step A2：4.8 part；PPG：22 parts；Two isocyanic acids
Ester：50 parts；Water：3.2 part；Catalyst：2.0 part；Organic foam stabilizer：0.6 part；Wherein, PPG uses polyethers
Triol 330N, diisocyanate use toluene di-isocyanate(TDI), and catalyst is dibutyl tin laurate, and silicon foams are stable
Agent is polyether silicone oil；First by candle ash and PPG mix after ultrasonic disperse, then with diisocyanate, water, catalyst,
Organic foam stabilizer adds in the container for scribbling releasing agent together, is sent out after mixing under agitation in 65 DEG C of baking oven
Bubble, foamed time 22min；
A4：The demoulding, after being cleaned by ultrasonic totally with ethanol, isopropanol, liquid detergent and water respectively after foam is cut, it is put into 60 DEG C
The modified foamed plastics of drying to obtain candle ash, is cut into 3cm*1.5cm*1.5cm fritters, is designated as P2 in baking oven.
Embodiment 3：A kind of preparation method of the modified foamed plastics of candle ash, comprises the following steps：
A1：The preparation of candle ash：The glass cleaned up is placed in accumulation candle ash above the candle flame being burning；When wax
Candle ash accumulate to after certain thickness with scraper candle ash is scraped it is standby；
A2：Candle ash is placed in crucible, 200 DEG C is warming up to 5 DEG C/min programming rate, is incubated 30min, continue with 5 DEG C/
Min programming rate is warming up to 550 DEG C, is incubated 2h, naturally cools to room temperature, standby；
A3：Raw material is weighed according to following parts by weight：Candle ash in step A2：4.8 part；PPG：22 parts；Two isocyanic acids
Ester：50 parts；Water：3.2 part；Catalyst：2.0 part；Organic foam stabilizer：0.6 part；Wherein, PPG uses polyethers
Triol 330N, diisocyanate use toluene di-isocyanate(TDI), and catalyst is dibutyl tin laurate, and silicon foams are stable
Agent is polyether silicone oil；First by candle ash and PPG mix after ultrasonic disperse, then with diisocyanate, water, catalyst,
Organic foam stabilizer adds in the container for scribbling releasing agent together, is sent out after mixing under agitation in 65 DEG C of baking oven
Bubble, foamed time 22min；
A4：The demoulding, after being cleaned by ultrasonic totally with ethanol, isopropanol, liquid detergent and water respectively after foam is cut, it is put into 60 DEG C
The modified foamed plastics of drying to obtain candle ash, is cut into 3cm*1.5cm*1.5cm fritters, is designated as P3 in baking oven.
Embodiment 4：A kind of preparation method of the modified foamed plastics of candle ash, comprises the following steps：
A1：The preparation of candle ash：The glass cleaned up is placed in accumulation candle ash above the candle flame being burning；When wax
Candle ash accumulate to after certain thickness with scraper candle ash is scraped it is standby；
A2：Candle ash is placed in crucible, 200 DEG C is warming up to 5 DEG C/min programming rate, is incubated 30min, continue with 5 DEG C/
Min programming rate is warming up to 500 DEG C, is incubated 1.5h, naturally cools to room temperature, standby；
A3：Raw material is weighed according to following parts by weight：Candle ash in step A2：4.8 part；PPG：22 parts；Two isocyanic acids
Ester：50 parts；Water：3.2 part；Catalyst：2.0 part；Organic foam stabilizer：0.6 part；Wherein, PPG uses polyethers
Triol 330N, diisocyanate use toluene di-isocyanate(TDI), and catalyst is dibutyl tin laurate, and silicon foams are stable
Agent is polyether silicone oil；First by candle ash and PPG mix after ultrasonic disperse, then with diisocyanate, water, catalyst,
Organic foam stabilizer adds in the container for scribbling releasing agent together, is sent out after mixing under agitation in 65 DEG C of baking oven
Bubble, foamed time 22min；
A4：The demoulding, after being cleaned by ultrasonic totally with ethanol, isopropanol, liquid detergent and water respectively after foam is cut, it is put into 60 DEG C
The modified foamed plastics of drying to obtain candle ash, is cut into 3cm*1.5cm*1.5cm fritters, is designated as P4 in baking oven.
Embodiment 5：A kind of preparation method of the modified foamed plastics of candle ash, comprises the following steps：
A1：The preparation of candle ash：The glass cleaned up is placed in accumulation candle ash above the candle flame being burning；When wax
Candle ash accumulate to after certain thickness with scraper candle ash is scraped it is standby；
A2：Candle ash is placed in crucible, 200 DEG C is warming up to 5 DEG C/min programming rate, is incubated 30min, continue with 5 DEG C/
Min programming rate is warming up to 600 DEG C, is incubated 1.5h, naturally cools to room temperature, standby；
A3：Raw material is weighed according to following parts by weight：Candle ash in step A2：4.8 part；PPG：22 parts；Two isocyanic acids
Ester：50 parts；Water：3.2 part；Catalyst：2.0 part；Organic foam stabilizer：0.6 part；Wherein, PPG uses polyethers
Triol 330N, diisocyanate use toluene di-isocyanate(TDI), and catalyst is dibutyl tin laurate, and silicon foams are stable
Agent is polyether silicone oil；First by candle ash and PPG mix after ultrasonic disperse, then with diisocyanate, water, catalyst,
Organic foam stabilizer adds in the container for scribbling releasing agent together, is sent out after mixing under agitation in 65 DEG C of baking oven
Bubble, foamed time 22min；
A4：The demoulding, after being cleaned by ultrasonic totally with ethanol, isopropanol, liquid detergent and water respectively after foam is cut, it is put into 60 DEG C
The modified foamed plastics of drying to obtain candle ash, is cut into 3cm*1.5cm*1.5cm fritters, is designated as P5 in baking oven.
Embodiment 6：A kind of preparation method of the modified foamed plastics of candle ash, comprises the following steps：
A1：The preparation of candle ash：The glass cleaned up is placed in accumulation candle ash above the candle flame being burning；When wax
Candle ash accumulate to after certain thickness with scraper candle ash is scraped it is standby；
A2：Candle ash is placed in crucible, 200 DEG C is warming up to 5 DEG C/min programming rate, is incubated 30min, continue with 5 DEG C/
Min programming rate is warming up to 550 DEG C, is incubated 1.5h, naturally cools to room temperature, standby；
A3：Raw material is weighed according to following parts by weight：Candle ash in step A2：4.8 part；PPG：22 parts；Two isocyanic acids
Ester：50 parts；Water：3.2 part；Catalyst：2.0 part；Organic foam stabilizer：0.6 part；Wherein, PPG uses polyethers
Triol 330N, diisocyanate use toluene di-isocyanate(TDI), and catalyst is dibutyl tin laurate, and silicon foams are stable
Agent is polyether silicone oil；First by candle ash and PPG mix after ultrasonic disperse, then with diisocyanate, water, catalyst,
Organic foam stabilizer adds in the container for scribbling releasing agent together, is sent out after mixing under agitation in 60 DEG C of baking oven
Bubble, foamed time 25min；
A4：The demoulding, after being cleaned by ultrasonic totally with ethanol, isopropanol, liquid detergent and water respectively after foam is cut, it is put into 60 DEG C
The modified foamed plastics of drying to obtain candle ash, is cut into 3cm*1.5cm*1.5cm fritters, is designated as P6 in baking oven.
Embodiment 7：A kind of preparation method of the modified foamed plastics of candle ash, comprises the following steps：
A1：The preparation of candle ash：The glass cleaned up is placed in accumulation candle ash above the candle flame being burning；When wax
Candle ash accumulate to after certain thickness with scraper candle ash is scraped it is standby；
A2：Candle ash is placed in crucible, 200 DEG C is warming up to 5 DEG C/min programming rate, is incubated 30min, continue with 5 DEG C/
Min programming rate is warming up to 550 DEG C, is incubated 1.5h, naturally cools to room temperature, standby；
A3：Raw material is weighed according to following parts by weight：Candle ash in step A2：4.8 part；PPG：22 parts；Two isocyanic acids
Ester：50 parts；Water：3.2 part；Catalyst：2.0 part；Organic foam stabilizer：0.6 part；Wherein, PPG uses polyethers
Triol 330N, diisocyanate use toluene di-isocyanate(TDI), and catalyst is dibutyl tin laurate, and silicon foams are stable
Agent is polyether silicone oil；First by candle ash and PPG mix after ultrasonic disperse, then with diisocyanate, water, catalyst,
Organic foam stabilizer adds in the container for scribbling releasing agent together, is sent out after mixing under agitation in 70 DEG C of baking oven
Bubble, foamed time 20min；
A4：The demoulding, after being cleaned by ultrasonic totally with ethanol, isopropanol, liquid detergent and water respectively after foam is cut, it is put into 60 DEG C
The modified foamed plastics of drying to obtain candle ash, is cut into 3cm*1.5cm*1.5cm fritters, is designated as P7 in baking oven.
Embodiment 8-12：A kind of preparation method of the modified foamed plastics of candle ash, with differing only in for embodiment 1, step
In rapid A3, candle ash is different with the content of PPG, diisocyanate, water, catalyst, organic foam stabilizer, presses
According to parts by weight meter, the content of each component is as shown in table 1；Wherein, PPG uses polyether triol 330N, and diisocyanate is adopted
With toluene di-isocyanate(TDI), catalyst is dibutyl tin laurate, and organic foam stabilizer is polyether silicone oil；It is prepared
Foamed plastics be respectively labeled as P8, P9, P10, P11, P12.
The component and content table of foamed plastics in the embodiment 1 of table 1, embodiment 8-12
Embodiment 13：A kind of preparation method of the modified foamed plastics of candle ash, comprises the following steps：
A11：The preparation of candle ash：The glass cleaned up is placed in accumulation candle ash above the candle flame being burning；When
Candle ash accumulate to after certain thickness with scraper candle ash is scraped it is standby；
A21：Raw material is weighed according to following parts by weight：Candle ash in step A11：4.8 part；PPG：22 parts；Two isocyanides
Acid esters：50 parts；Water：3.2 part；Catalyst：2.0 part；Organic foam stabilizer：0.6 part；Wherein, PPG is using poly-
Ether triol 330N, diisocyanate use toluene di-isocyanate(TDI), and catalyst is dibutyl tin laurate, and silicon foams are steady
It is polyether silicone oil to determine agent；First by candle ash and PPG mix after ultrasonic disperse, then with diisocyanate, water, catalysis
Agent, organic foam stabilizer add in the container for scribbling releasing agent together, enter after mixing under agitation in 65 DEG C of baking oven
Row foaming, foamed time 22min；
A31：The demoulding, after being cleaned by ultrasonic totally with ethanol, isopropanol, liquid detergent and water respectively after foam is cut, it is put into 60 DEG C
Baking oven in the modified foamed plastics of drying to obtain candle ash, be cut into 3cm*1.5cm*1.5cm fritters, be designated as P13.
Embodiment 14：A kind of preparation method of the modified foamed plastics of candle ash, comprises the following steps：
A12：PPG, diisocyanate, water, catalyst, organic foam stabilizer are added to the appearance for scribbling releasing agent
In device, foamed after mixing under agitation in 65 DEG C of baking oven, foamed time 22min；In parts by weight, each component
Content it is as follows：PPG：22 parts；Diisocyanate：50 parts；Water：3.2 part；Catalyst：2.0 part；Silicon foams are steady
Determine agent：0.6 part；Wherein, PPG uses polyether triol 330N, and diisocyanate uses toluene di-isocyanate(TDI), catalysis
Agent is dibutyl tin laurate, and organic foam stabilizer is polyether silicone oil；
A22：The demoulding, after being cleaned by ultrasonic totally with ethanol, isopropanol, liquid detergent and water respectively after foam is cut, it is put into 60 DEG C
Baking oven in the modified foamed plastics of drying to obtain candle ash, be cut into 3cm*1.5cm*1.5cm fritters, be designated as P14.
Embodiment 15：Au plasma enrichment method, comprises the following steps in a kind of soil：
S1：5g soil patterns are weighed, are placed in porcelain cupel, are placed in Muffle furnace with 5 DEG C/min programming rate from normal temperature
650 DEG C are warming up to, 1.5h is incubated, after being naturally cooling to normal temperature, is transferred in container；
S2：The 1 of 50mL is added in step S1 container:1 chloroazotic acid and 1mL 100g/L Fe3+Solution, cap upper surface ware, adds
Heat boiling 2h；Heating evaporation is concentrated into acidity 8%, is diluted with water to 100mL, an extract solution is made, standby；
S3：Candle ash modified foamed plastics of the 0.3g marked as P1 is added in a step S2 extract solution, is put in container
Enter the first limiter, foamed plastics is blocked in below the liquid level of an extract solution, boils and shake 60min；As shown in figure 1,
The first limiter 2 being related in step S3 includes fixed part 21, stop part 22 and for connecting portion 21 and stop part 22
Connecting portion 23, fixed part 21 are disc-shaped, are overlapped in the opening of container 1；Stop part 22 is disc-shaped, the outer rim of stop part 22
Coordinate with the inwall gap of container 1, stop part 22 is provided with small opening 3, and the size of small opening 3 is less than foamed plastics；First limiter 2 is logical
Body is made of the corrosion resistant polytetrafluoroethylmaterial material of acid and alkali-resistance, and it, which is conducted oneself with dignity, meet to be more than the buoyancy that foamed plastics is subject to,
Its height should meet that the bottom of stop part can be immersed below the liquid level of an extract solution；
S4：Foamed plastics is taken out, is rinsed well with deionized water, is dried；
S5：The thiourea solution that concentration is 10g/L is added in a reservoir, by the second limiter in the foamed plastics in step S4
Gold ion extracted；
As shown in Fig. 2 the second limiter 4 includes the press section 42 of fixed cup 41 and the cup-shaped in fixed cup 41, press section
42 are sheathed in fixed cup 41, and outer wall and the internal wall transitions of fixed cup 41 of press section 42 coordinate；The outer circumference of the upper end of fixed cup 41
Flange 411 is provided with upwards, flange 411 is overlapped in the opening of container 1；Set between press section 42 and the flange of fixed cup 41 411
There is spring 43, spring 43 and the flange 411 of fixed cup 41 are fixed；The bottom of fixed cup 41 is provided with small opening 3, press section 42 and fixation
Gap 44 is provided between the bottom of cup 41, the size in gap 44 is at least the size of foamed plastics；The bottom of press section 42 is provided with
Small opening 3, the size of small opening 3 are less than foamed plastics；The entire body of second limiter 4 uses the corrosion resistant polytetrafluoroethylmaterial material of acid and alkali-resistance
It is made, the deadweight of press section 42 should meet to be more than the buoyancy that foamed plastics is subject to, and the height of press section 42 should meet to extrude
The bottom in portion 42 can be immersed below the liquid level of thiourea solution, and the bottom of press section 42 is touched under 43 complete pressured state of spring
Touch the bottom of fixed cup 41；
In extraction process, fixed cup 41 is put into the container 1 equipped with thiourea solution first, places into foamed plastics, then will
Press section 42 is placed in fixed cup 41, and the bottom of press section 42 contacts with thiourea solution, so as to by the position restriction of foamed plastics
Below the liquid level of thiourea solution；Covered in the opening of the second limiter 4 with culture dish, by container 1 in boiling water bath
Heat 50min；By pressing the crushed foam plastics repeatedly of press section 42 in extraction process；Foamed plastics and the second limit are taken out while hot
Position device 4, foamed plastics and the second limiter 4 are rinsed with 10g/L thiourea solution, then be settled to 10g/L thiourea solution
50mL obtains concentrated extracting solution.
Embodiment 16-28：Au plasma enrichment method in a kind of soil, compared with embodiment 15, it differs only in step
In rapid S3, the foamed plastics used is different, and embodiment 16-28 corresponds to the P2-P14 for using and being prepared in embodiment 2-14 respectively
The modified foamed plastics of candle ash.
Embodiment 29：Au plasma enrichment method in a kind of soil, compared with embodiment 15, used first limiter
With the second limiter all same, herein not reinflated explanation；The present embodiment comprises the following steps：
S1：5g soil patterns are weighed, are placed in porcelain cupel, are placed in Muffle furnace with 5 DEG C/min programming rate from normal temperature
650 DEG C are warming up to, 1.5h is incubated, after being naturally cooling to normal temperature, is transferred in container；
S2：The 1 of 45mL is added in step S1 container:1 chloroazotic acid and 1mL 100g/L Fe3+Solution, cap upper surface ware, adds
Heat boiling 3h；Heating evaporation is concentrated into acidity 10%, is diluted with water to 100mL, an extract solution is made, standby；
S3：Candle ash modified foamed plastics of the 0.2g marked as P1 is added in a step S2 extract solution, is put in container
Enter the first limiter, foamed plastics is blocked in below the liquid level of an extract solution, boils and shake 60min；
S4：Foamed plastics is taken out, is rinsed well with deionized water, is dried；
S5：The thiourea solution that concentration is 12g/L is added in a reservoir, and fixed cup is put into the container equipped with thiourea solution, then
Foamed plastics is put into, then press section is placed in fixed cup, the bottom of press section contacts with thiourea solution, so as to by foam plastic
The position restriction of material is below the liquid level of thiourea solution；Covered in the opening of the second limiter, by container in boiling water bath
Middle heating 50min；By pressing press section crushed foam plastics repeatedly in extraction process；Foamed plastics and the second limit are taken out while hot
Position device, foamed plastics and the second limiter are rinsed with 12g/L thiourea solution, then 50mL is settled to 12g/L thiourea solution
Obtain concentrated extracting solution.
Embodiment 30：Au plasma enrichment method in a kind of soil, compared with embodiment 15, used first limiter
With the second limiter all same, herein not reinflated explanation；The present embodiment comprises the following steps：
S1：5g soil patterns are weighed, are placed in porcelain cupel, are placed in Muffle furnace with 5 DEG C/min programming rate from normal temperature
650 DEG C are warming up to, 1.5h is incubated, after being naturally cooling to normal temperature, is transferred in container；
S2：The 1 of 60mL is added in step S1 container:1 chloroazotic acid and 1mL 100g/L Fe3+Solution, cap upper surface ware, adds
Heat boiling 1.5h；Heating evaporation is concentrated into acidity 5%, is diluted with water to 100mL, an extract solution is made, standby；
S3：Candle ash modified foamed plastics of the 0.5g marked as P1 is added in a step S2 extract solution, is put in container
Enter the first limiter, foamed plastics is blocked in below the liquid level of an extract solution, boils and shake 60min；
S4：Foamed plastics is taken out, is rinsed well with deionized water, is dried；
S5：The thiourea solution that concentration is 12g/L is added in a reservoir, and fixed cup is put into the container equipped with thiourea solution, then
Foamed plastics is put into, then press section is placed in fixed cup, the bottom of press section contacts with thiourea solution, so as to by foam plastic
The position restriction of material is below the liquid level of thiourea solution；Covered in the opening of the second limiter, by container in boiling water bath
Middle heating 50min；By pressing press section crushed foam plastics repeatedly in extraction process；Foamed plastics and the second limit are taken out while hot
Position device, foamed plastics and the second limiter are rinsed with 12g/L thiourea solution, then 50mL is settled to 12g/L thiourea solution
Obtain concentrated extracting solution.
Embodiment 31：Au plasma enrichment method in a kind of soil, compared with embodiment 15, differ only in step S3
The concussion time be 45min；The heat time is 50min in boiling water bath in step S5.
Embodiment 32：Au plasma enrichment method in a kind of soil, compared with embodiment 15, differ only in step S3
The concussion time be 75min；The heat time is 50min in boiling water bath in step S5.
Embodiment 33：Au plasma enrichment method in a kind of soil, compared with embodiment 15, differ only in step S3
The concussion time be 90min；The heat time is 50min in boiling water bath in step S5.
Embodiment 34：Au plasma enrichment method in a kind of soil, compared with embodiment 15, differ only in step S3
The concussion time be 60min；The heat time is 30min in boiling water bath in step S5.
Embodiment 35：Au plasma enrichment method in a kind of soil, compared with embodiment 15, differ only in step S3
The concussion time be 60min；The heat time is 40min in boiling water bath in step S5.
Embodiment 36：Au plasma enrichment method in a kind of soil, compared with embodiment 15, differ only in step S3
The concussion time be 60min；The heat time is 60min in boiling water bath in step S5.
Following comparative example is prepared as control.
Comparative example 1：Au plasma enrichment method, comprises the following steps in a kind of soil：
S1：5g soil patterns are weighed, are placed in porcelain cupel, are placed in Muffle furnace with 5 DEG C/min programming rate from normal temperature
650 DEG C are warming up to, 1.5h is incubated, after being naturally cooling to normal temperature, is transferred in container；
S2：The 1 of 50mL is added in step S1 container:1 chloroazotic acid and 1mL 100g/L Fe3+Solution, cap upper surface ware, adds
Heat boiling 2h；Heating evaporation is concentrated into acidity 8%, is diluted with water to 100mL, an extract solution is made, standby；
S3：Candle ash modified foamed plastics of the addition 0.3g marked as P1 in a step S2 extract solution, cap upper surface ware,
Boil and shake 60min；
S4：Foamed plastics is taken out, is rinsed well with deionized water, is dried；
S5：The thiourea solution that concentration is 10g/L, the foamed plastics being put into step S4, in the opening of container are added in a reservoir
Place is covered with surface plate, and container is heated into 50min in boiling water bath；Foamed plastics is taken out while hot, it is molten with 10g/L thiocarbamide
Liquid rinses foamed plastics, then is settled to 50mL with 10g/L thiourea solution and obtains concentrated extracting solution.
Test portion
Test the gold ion content in concentrated extracting solution using atomic absorption spectrophotometer and calculate the gold in soil pattern
Ion concentration；Comprise the following steps：
(1) preparation of test sample：The soil pattern of areal sampling is selected, is crushed after coarse filtration in disintegrating machine, then pass through
Ground uniformly in mortar after meticulous filtering, extracted according to embodiment 15-36, comparative example 1 method, concentration extraction is made
Liquid, it is test sample；
(2) configuration of standard working curve：Gold ion is diluted to 5ug/L, 10ug/L, 20ug/ respectively with 10g/L thiourea solutions
L, 30ug/L, 40ug/L, blank is used as using 10g/L thiourea solutions；
(3) prepared by matrix modifier (20g/L ascorbic acid)：20g ascorbic acid is weighed to be dissolved in 1L distilled water；
(4) sample detection：20 μ l test samples are taken to be well mixed rear sample detection, each test sample with 5 μ l matrix modifiers respectively
Test three groups of data to average, test the content of gold ion in concentrated extracting solution, and calculate the content of gold ion in soil.
(5) test result collects to table 2.
The content measuring result table of gold ion in the soil pattern of table 2
Analysis of experimental results：Other laboratory facilities are all identical, accuracy of detection is identical and do the bar of three groups of parallel tests
Under part, it is believed that the concentration that detects is higher show it is higher to the extraction efficiency of the gold ion in soil.
The result of comparative example 15 and comparative example 1 understands that the use of the first limiter and the second limiter is to improving gold
The extraction efficiency of ion has critical effect, on the one hand, foamed plastics is limited in extract solution by the first limiter
Below liquid level, increase the contact area of foamed plastics and an extract solution, improve adsorption efficiency；Second limiter is by foamed plastics
It is limited in below the liquid level of thiourea solution and constantly crushed foam plastics is completed in bubble and in solution during experiment
Fluid exchange, so as to which the gold ion in bubble fully be extracted, improve extraction efficiency.
The result of comparative example 15 and embodiment 28 is understood, foamed plastics is modified with candle ash, it is possible to increase bubble
Foam plastics, because candle ash is a kind of material with loose structure, have stronger to the absorption property of gold ion in soil
Absorption property, improved by the modified foamed plastics porosity of candle ash, so as to improve the absorption property to gold ion.
The result of comparative example 15 and embodiment 27 is understood, candle ash is used further into changing for foamed plastics after oversintering
Property, compared with directly the candle being collected into ash is used for foamed plastics be modified, the former adsorption effect to gold ion is more preferable, because
It can aid in removing the component that is not carbonized in candle ash through oversintering, more complete pore structure be formed, so as to improve to gold
The adsorption efficiency of ion.
Comparative example 15-17 result understands that the sintering temperature of candle ash is constant, with the increasing of sintered heat insulating time
Greatly, the gold ion concentration measured is higher, shows that sintering time can influence the extraction efficiency of gold ion, is because sintering can be auxiliary
The component that is not carbonized removed in candle ash is helped, more complete pore structure is formed, so as to improve the adsorption efficiency to gold ion；
After soaking time increases to a certain extent, gold ion concentration is kept approximately constant.The knot of comparative example 5, embodiment 18-19
Fruit understands that the candle ash sintered heat insulating time is constant, and with the raising of the sintering temperature of candle ash, the gold ion concentration measured is got over
Height, show that sintering temperature can influence the extraction efficiency of gold ion, be because sintering temperature is higher, can aid in removing candle ash
In the component that is not carbonized, more complete pore structure is formed, so as to improve the adsorption efficiency to gold ion.
Comparative example 15, embodiment 20-21 results showed that blowing temperature and foamed time are to foamed plastics
Absorption property tool has a certain impact, and when blowing temperature and foamed time are respectively 65 DEG C and 22min, foams obtained foam
Plastics have optimal absorption property to gold ion.
Comparative example 15, embodiment 22-24 result are understood, under conditions of other components content is constant, with bubble
The increase of the content of candle ash, foamed plastics also improve constantly to the absorption property of gold ion in foam plastics, when the use of candle ash
When amount increases to 4.8 parts, saturation value is reached, i.e. foamed plastics no longer improves to the absorption property of gold ion.Contrast is real
Apply example 15, embodiment 25-26 result understands that, from the formula of embodiment 1, the foamed plastics being prepared has to gold ion
Optimal absorption property.
The results showed that adsorption time (i.e. concussion time in step S3) of comparative example 15, embodiment 31-36
Foamed plastics is had a certain impact to the absorption property tool of gold ion with desorption time (i.e. heat time in step S5), when
It is 60min from adsorption time, when desorption time is 50min, can reaches preferable degree of absorption, continues to increase the time pair
The raising effect of absorption property is little.
Claims (10)
1. Au plasma enrichment method in a kind of soil, it is characterized in that, comprise the following steps：S1：Weigh sample, calcination, cooling
After be transferred in container；S2：1 is added in step S1 container:The Fe of 1 chloroazotic acid and 95-120g/L3+Solution, chloroazotic acid and Fe3+
The volume ratio of solution is 45-60:1, ebuillition of heated 1.5-3h；Heating evaporation is concentrated into acidity in 5%-10%, is diluted with water into
Extract solution, it is standby；S3：Foamed plastics is added in a step S2 extract solution, places the first limiter in a reservoir
So as to below the liquid level of an extract solution, boil and shake 45-90min the position restriction of foamed plastics；S4：Take out foam
Plastics, cleaned up, dried with water；S5：Foamed plastics in step S4 is put into container, adding concentration in a reservoir is
10-12g/L thiourea solution, the second limiter is placed in a reservoir so that by the position restriction of foamed plastics in thiourea solution
Below liquid level；Covered in the opening of container, container is heated into 30-60min in boiling water bath；Foamed plastics is taken out while hot
Constant volume obtains concentrated extracting solution afterwards.
2. Au plasma enrichment method in a kind of soil according to claim 1, it is characterized in that：The first limiter bag
Include fixed part, stop part and be overlapped in the opening of container for connecting portion and the connecting portion of stop part, the fixed part,
The stop part is provided with small opening, and the size of the small opening is less than foamed plastics.
3. Au plasma enrichment method in a kind of soil according to claim 2, it is characterized in that：The second limiter bag
Include fixed cup and the press section in fixed cup, the fixed cup upper end is overlapped in the opening of container, the press section and
Spring is provided between fixed cup, the spring is fixed with any one in fixed cup or press section；The bottom of the fixed cup
Provided with small opening, gap is provided between the press section and the bottom of fixed cup, the size in gap is at least the size of foamed plastics.
4. Au plasma enrichment method in a kind of soil according to claim 3, it is characterized in that：The press section is cup-shaped
Set, outer wall and the fixed cup internal wall transitions of the press section coordinate；The bottom of the press section is provided with small opening, the small opening
Size is less than foamed plastics.
5. Au plasma enrichment method in a kind of soil according to claim 4, it is characterized in that：Comprise the following steps：S1：
Sample is weighed, calcination, is transferred to after cooling in container；S2：1 is added in step S1 container:The Fe of 1 chloroazotic acid and 100g/L3+
Solution, chloroazotic acid and Fe3+The volume ratio of solution is 50:1, ebuillition of heated 1.5-3h；Heating evaporation is concentrated into acidity in 5%-10%,
An extract solution is diluted with water into, it is standby；S3：Foamed plastics is added in a step S2 extract solution, is put into container
First limiter, foamed plastics is blocked in below the liquid level of an extract solution, boils and shake 45-90min；S4：Take out bubble
Foam plastics, are cleaned up with water, are dried；S5：The thiourea solution that concentration is 10-12g/L is added in a reservoir, first by fixed cup
It is put into container, the foamed plastics placed into step S4, then press section is placed in fixed cup, the bottom of press section and sulphur
Urea solution contacts, so that by the position restriction of foamed plastics below the liquid level of thiourea solution；By by extrusion in extraction process
Splenium crushed foam plastics repeatedly；Covered in the opening of container, container is heated into 30-60min in boiling water bath；While hot
Constant volume obtains concentrated extracting solution after taking out foamed plastics.
6. Au plasma enrichment method in a kind of soil according to claim 1 or 4, it is characterized in that：In the step S1,
The technique of calcination is to be warming up to 650 DEG C from normal temperature in Muffle furnace with 5 DEG C/min programming rate, is incubated 1.5h, Temperature fall.
7. Au plasma enrichment method in a kind of soil according to claim 1 or 4, it is characterized in that：In the step S3,
The addition mass ratio of the foamed plastics and an extract solution is 2-5：1000.
8. Au plasma enrichment method in a kind of soil according to claim 1 or 4, it is characterized in that：The foamed plastics
For the modified foamed plastics of candle ash, it is prepared as follows to obtain：A1：The preparation of candle ash：The glass cleaned up is put
Candle ash is gathered above the candle flame being burning；It is after candle ash accumulates to certain thickness that candle ash collection is standby；
A2：Candle ash is cooled down after calcination 1-2h under the conditions of 500-600 DEG C standby；A3：Candle ash in step A2 and polyethers is more
First alcohol, diisocyanate, water, catalyst, organic foam stabilizer are added in the container for scribbling releasing agent, are mixed under agitation
Foamed afterwards in 60-70 DEG C of baking oven, foamed time 20-25min；In parts by weight, the content of each component is as follows：
Candle ash：1.6-6.4 part；PPG：20-25 parts；Diisocyanate：45-60 parts；Water：3.0-3.4 part；Catalyst：
1.5-2.5 part；Organic foam stabilizer：0.5-0.65 parts；A4：The demoulding, after foam is cut with ethanol, isopropanol, wash it is clean
Essence and water clean up the rear modified foamed plastics of drying to obtain candle ash.
9. Au plasma enrichment method in a kind of soil according to claim 8, it is characterized in that：The calcination of the step A2
Technique is：200 DEG C are warming up to 5 DEG C/min programming rate, 30min is incubated, continues to be warming up to 5 DEG C/min programming rate
500-600 DEG C, 1-2h is incubated, naturally cools to room temperature.
10. Au plasma enrichment method in a kind of soil according to claim 8, it is characterized in that：In the step A3, wax
Candle ash mixes with PPG first, and ultrasonic wave added disperses, then is mixed with other components.
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