CN114807951A - Method for quickly removing glass residues on surface of platinum alloy - Google Patents
Method for quickly removing glass residues on surface of platinum alloy Download PDFInfo
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- CN114807951A CN114807951A CN202210481287.9A CN202210481287A CN114807951A CN 114807951 A CN114807951 A CN 114807951A CN 202210481287 A CN202210481287 A CN 202210481287A CN 114807951 A CN114807951 A CN 114807951A
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- 229910001260 Pt alloy Inorganic materials 0.000 title claims abstract description 123
- 239000011521 glass Substances 0.000 title claims abstract description 116
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000012459 cleaning agent Substances 0.000 claims abstract description 55
- 238000010438 heat treatment Methods 0.000 claims abstract description 41
- 230000002378 acidificating effect Effects 0.000 claims abstract description 39
- 239000002253 acid Substances 0.000 claims abstract description 28
- 238000004140 cleaning Methods 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 18
- 230000008018 melting Effects 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 230000000149 penetrating effect Effects 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004321 preservation Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- -1 polyoxyethylene Polymers 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 6
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 46
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 46
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 27
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 27
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 8
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 150000004996 alkyl benzenes Chemical group 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 50
- 239000012535 impurity Substances 0.000 description 17
- 239000000956 alloy Substances 0.000 description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 10
- 238000001802 infusion Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 150000005691 triesters Chemical class 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 150000005690 diesters Chemical class 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 5
- 239000010452 phosphate Substances 0.000 description 5
- 239000004094 surface-active agent Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 2
- 229940077388 benzenesulfonate Drugs 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000002357 osmotic agent Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002419 bulk glass Substances 0.000 description 1
- 150000001728 carbonyl compounds Chemical class 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/28—Cleaning or pickling metallic material with solutions or molten salts with molten salts
- C23G1/32—Heavy metals
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
Abstract
The application relates to the technical field of waste metal recycling, and particularly discloses a method for quickly removing glass residues on the surface of a platinum alloy. The method for rapidly removing the glass residue on the surface of the platinum alloy comprises the following steps: s1: adding the platinum alloy deposited with the glass residues into the alkaline melting material to obtain a mixture, heating the mixture until the alkaline melting material is melted, and preserving heat for 40-60 min; s2: taking out the platinum alloy subjected to heat preservation treatment in S1, placing the platinum alloy into an acidic cleaning agent to obtain a cleaning mixture, and carrying out ultrasonic treatment on the cleaning mixture for reaction for 5-15 min; s3: taking out the platinum alloy after the reaction in the S2, and washing and drying the platinum alloy; the acid cleaning agent comprises the following raw materials in parts by weight: 50-70 parts of sulfamic acid; 0.8-1.6 parts of alkylphenol polyoxyethylene; 4-6 parts of hydrochloric acid; 2-4 parts of a penetrating agent. This application has clean efficient advantage.
Description
Technical Field
The application relates to the technical field of waste metal recycling, in particular to a method for quickly removing glass residues on the surface of a platinum alloy.
Background
In the glass production industry, platinum alloy is generally used as a container for glass, such as a platinum alloy bushing used in the fiberglass industry, a platinum channel used in the high-end glass industry, and the like. When the service life of the platinum alloy products is over, the waste platinum alloy materials are generally recycled and reprocessed for use, but glass residues are often mixed in the platinum alloy materials, and the glass residues are unfavorable for the subsequent recycling treatment of the platinum alloy, so that the glass residues on the surfaces of the waste platinum alloy materials need to be removed in advance.
In the related art, when removing the glass residue on the surface of the platinum alloy material, a hydrofluoric acid solution is generally used to soak the platinum alloy material, and the hydrofluoric acid is contacted with the glass residue in the soaking process, so as to achieve the purpose of removing the glass residue by corrosion.
In view of the above related technologies, although hydrofluoric acid can effectively remove glass residues on the surface of the platinum alloy material, hydrofluoric acid is volatile, has extremely strong corrosivity, is extremely harmful to human bodies, needs to be used in a closed environment, and has high safety production investment; moreover, the hydrofluoric acid treatment period is long, the time is as long as 7-15 days, and the cleaning efficiency is low.
Disclosure of Invention
In order to improve the cleaning efficiency, the application provides a method for quickly removing glass residues on the surface of the platinum alloy.
The application provides a method for rapidly removing glass residues on the surface of a platinum alloy, which adopts the following technical scheme: a method for rapidly removing glass residues on the surface of a platinum alloy comprises the following steps:
s1: adding the platinum alloy deposited with the glass residues into the alkaline melting material to obtain a mixture, heating the mixture until the alkaline melting material is melted, and preserving heat for 40-60 min;
s2: taking out the platinum alloy subjected to heat preservation treatment in S1, placing the platinum alloy into an acidic cleaning agent to obtain a cleaning mixture, and carrying out ultrasonic treatment on the cleaning mixture for reaction for 5-15 min;
s3: taking out the platinum alloy after the reaction in the S2, and washing and drying the platinum alloy;
the acid cleaning agent comprises the following raw materials in parts by weight: 50-70 parts of sulfamic acid; 0.8-1.6 parts of alkylphenol polyoxyethylene; 4-6 parts of hydrochloric acid; 2-4 parts of a penetrating agent.
Optionally, the bulk glass impurities on the surface of the platinum alloy are physically broken and removed prior to the operation of S1.
By adopting the technical scheme, the large glass which is easy to remove is knocked to be broken in advance by physical crushing modes such as hammer knocking and the like, and then subsequent fusion corrosion operation is carried out, so that the fusion corrosion time is favorably shortened, the whole time period of the process flow for removing glass impurities is shortened, and the production efficiency is favorably improved.
In the heat preservation process, the molten alkaline melting material can react with silicon dioxide in the glass residues, so that the glass residues are corroded and dissolved into the molten alkaline melting material to form a eutectic, and the platinum alloy material is fished out of the eutectic after a period of time, so that the purpose of removing the glass residues on the surface of the platinum alloy is achieved.
After the heat preservation is finished, acid cleaning is carried out on the platinum alloy through an acid cleaning agent, and firstly, alkaline melting materials remained on the surface of the platinum alloy can be removed; secondly, acid washing can remove part of glass residues which are not dissolved in the alkaline melting materials; finally, the acid wash removes other materials from the glass residue that do not react with the alkaline melt (e.g., MgO, Al added during glass production) 2 O 3 Basic oxides such as CaO); thereby completely removing the glass residue on the surface of the platinum alloy. The penetrating agent in the acid cleaning agent can promote the speed of the reaction of sulfamic acid, hydrochloric acid and insoluble substances in glass residues in the acid cleaning agent, and the alkylphenol polyoxyethylene ether can promote the promotion of the penetrating agent on the performance of the acid cleaning agent, so that the speed of the reaction of the insoluble substances in the platinum alloy surface glass residues and the glass residues is further promoted by the penetrating agent, and the cleaning efficiency and the cleaning effect of the platinum alloy surface glass residues are improved.
And then washing with water to remove the acid water washing agent, and drying to obtain the platinum alloy material with a clean surface. The method has higher reaction rate for corroding and dissolving the glass residues through the molten alkaline melting material, so that the glass residues on the surface of the platinum alloy can be quickly and thoroughly removed, the molten alkaline melting material cannot corrode the platinum alloy, and the possibility of generating quality defects such as cracks, bubbles, shrinkage cavities and the like on the surface of the platinum alloy is effectively reduced.
Optionally, on the basis of the penetrant, the penetrant comprises the following raw materials in parts by weight: 20-50 parts of isooctyl alcohol polyoxyethylene ether; 5-9 parts of phosphorus pentoxide; 3-5 parts of phosphorus oxychloride.
By adopting the technical scheme, phosphorus pentoxide and phosphorus oxychloride react with isooctyl alcohol polyoxyethylene ether to generate the phosphate surfactant with coexistent mono-, di-and tri-esters and high tri-ester content, and when the content of the di-esters and the tri-esters is high, the phosphate surfactant has good wettability and can reduce dynamic surface tension and static surface tension to ensure that the phosphate surfactant can rapidly migrate on the surfaces of glass residues and glass residue alkaline infusions, so that the permeation rate of the acid cleaning agent to the glass residues and the glass residue alkaline infusions is increased, and the rate of eliminating the glass residues and the glass residue alkaline infusions by acid components in the acid cleaning agent is increased.
Optionally, the penetrant is prepared by a method comprising the following steps: placing isooctanol polyoxyethylene ether in a container, heating and stirring, adding phosphorus pentoxide and phosphorus oxychloride into the container containing the isooctanol polyoxyethylene ether, mixing the phosphorus pentoxide, the phosphorus oxychloride and the isooctanol polyoxyethylene ether, continuing to heat, reacting for a period of time, and then cooling to obtain the penetrant.
By adopting the technical scheme, the phosphate surfactant with high contents of diester and triester is obtained, and the removal efficiency of acid cleaning on glass residues is improved.
Optionally, in the heating and stirring processes, the heating temperature is 30-50 ℃, the heating time is 30-60min, the temperature for continuously heating up after adding phosphorus pentoxide and phosphorus oxychloride is 65-75 ℃, the reaction time for continuously heating up is 4-5h, and the temperature is reduced to less than 50 ℃.
By adopting the technical scheme, the raw materials are fully reacted, and the prepared penetrant enables the acidic cleaning agent to have better removal performance and higher removal rate on the glass residues and the alkaline infusible matters in the glass residues, so that the removal efficiency of the glass residues on the surface of the platinum alloy is improved.
Optionally, on the basis of the acidic cleaning agent, the acidic cleaning agent further comprises 1.5-3.5 parts of secondary sodium alkyl benzene sulfonate; 1.5-2.5 parts of nonylphenol polyoxyethylene ether.
By adopting the technical scheme, on one hand, the combined action of the secondary alkyl sodium sulfonate, the nonylphenol polyoxyethylene ether and the penetrant improves the osmosis of the acidic cleaning agent and the efficiency of removing the glass residues by the acidic cleaning agent, and on the other hand, the combined action of the secondary alkyl sodium sulfonate and the nonylphenol polyoxyethylene ether improves the acid resistance of the penetrant, so that the penetrant can better promote the process of removing the glass residues and the alkaline infusions in the glass residues by the acidic cleaning agent, and the removal efficiency of the alkaline infusions in the glass residues on the surface of the platinum alloy and the glass residues is improved.
Optionally, the mass concentration of the sulfamic acid is not less than 1% all the time in the reaction process.
By adopting the technical scheme, the acid cleaning agent can fully react with the glass residues on the surface of the platinum alloy in the reaction process, and the removal efficiency of the glass residues on the surface of the platinum alloy and the alkaline infusible matters in the glass residues is improved.
Optionally, the alkaline melt is selected from any one or two of sodium hydroxide, potassium hydroxide and calcium hydroxide.
By adopting the technical scheme, the alkaline melting material can fully react with silicon dioxide in the glass residues, and is favorable for quickly and thoroughly corroding and dissolving the glass residues on the surface of the platinum alloy and alkaline infusible substances in the glass residues.
Optionally, the heating temperature in S1 is 500-650 ℃.
By adopting the technical scheme, the heating temperature can fully melt the alkaline melting material, and the molten alkaline melting material can completely coat the glass residue on the surface of the platinum alloy, so that the contact area of the alkaline melting material and the glass residue is increased, and the reaction rate is accelerated; on the other hand, the high-temperature environment is also favorable for accelerating the reaction rate of the molten alkaline melting material and the glass residues, thereby being convenient for quickly dissolving and corroding the glass residues on the surface of the platinum alloy. And the glass residue can be softened in a high-temperature environment, so that other substances in the glass residue can be dissolved and dispersed in the molten alkaline melting material conveniently, and the platinum alloy surface glass residue and the alkaline infusible substance in the glass residue can be corroded and dissolved rapidly and thoroughly.
Optionally, the ultrasonic power of the ultrasonic treatment in S2 is 500W-700W.
By adopting the technical scheme, firstly, the ultrasonic power can enable the medium around the ultrasonic vibration to do violent forced motion, any substance has fixed vibration frequency, and the glass residues belong to inorganic substancesThe vibration frequency is different from that of the platinum alloy material, so that the ultrasonic wave generates resonance on the glass residues attached to the platinum alloy and gradually separates from the surface of the platinum alloy; secondly, ultrasonic cavitation increases the water-dissolving capacity, causing the glass residue to dissolve in the acidic cleaning agent. Simultaneously, the H produced by the acoustic decomposition of water + The free radicals have a relatively long life, and the reduction effect generated by the free radicals can peel off the glass residues from the surface of the platinum alloy; finally, the ultrasonic wave propagates in the medium, causing the mass point to vibrate, so that the mass point obtains kinetic energy. Meanwhile, the glass residues are deformed by the ultrasonic power, so that the glass residues have heat energy, and the higher the ultrasonic vibration frequency is, the more remarkable the heat absorption phenomenon is, thereby destroying the stable existence condition of the glass residues; therefore, the method is favorable for promoting the removal efficiency of the glass residue on the surface of the platinum alloy and the alkaline infusible matters in the glass residue.
In summary, the present application has the following beneficial effects:
1. because this application adopts penetrant, alkylphenol ethoxylates and acid solution preparation to obtain the acid cleaning solution, on the one hand, has promoted the rate of sulfamic acid, hydrochloric acid in the acid cleaning agent and the insoluble substance reaction in the glass residue, and on the other hand, alkylphenol ethoxylates can promote the penetrant to the promotion of acid cleaning agent performance to improve the cleaning efficiency and the clean effect of platinum alloy surface glass residue.
2. The penetrant prepared by the method is a phosphate surfactant with high diester and triester contents, so that the penetrant has excellent wettability, and can reduce dynamic surface tension and static surface tension, so that the penetrant can rapidly migrate on the surfaces of glass residues and glass residue alkaline infusions, and the penetration rate of the acidic cleaning agent to the glass residues and the glass residue alkaline infusions is increased.
3. Because the sodium secondary alkylbenzene sulfonate and the nonylphenol polyoxyethylene ether are adopted, on one hand, the penetrating action of the acidic cleaning agent is improved under the combined action of the sodium secondary alkylbenzene sulfonate and the nonylphenol polyoxyethylene ether, and on the other hand, the acid resistance of the penetrating agent is improved, so that the removal efficiency of the acidic cleaning agent on the surface of the platinum alloy and the alkaline infusible matters in the glass residues is improved.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example of penetrant
Preparation example 1
A preparation method of the penetrant comprises the following steps:
placing 35kg of isooctanol polyoxyethylene ether in a container, heating and stirring, adding 7kg of phosphorus pentoxide and 4kg of phosphorus oxychloride into the container containing the isooctanol polyoxyethylene ether, mixing the phosphorus pentoxide, the phosphorus oxychloride and the isooctanol polyoxyethylene ether, continuing to heat, reacting for a period of time, and then cooling to obtain a penetrating agent; in the heating and stirring process, the heating temperature is 40 ℃, the heating time is 45min, the temperature for continuously heating up after adding phosphorus pentoxide and phosphorus oxychloride is 70 ℃, the reaction time for continuously heating up is 4.5h, and the temperature is reduced to 30 ℃.
Preparation example 2
A preparation method of the penetrant comprises the following steps:
placing 20kg of isooctanol polyoxyethylene ether in a container, heating and stirring, adding 5kg of phosphorus pentoxide and 3kg of phosphorus oxychloride into the container containing the isooctanol polyoxyethylene ether, mixing the phosphorus pentoxide, the phosphorus oxychloride and the isooctanol polyoxyethylene ether, continuing to heat, reacting for a period of time, and then cooling to obtain a penetrating agent; in the heating and stirring process, the heating temperature is 30 ℃, the heating time is 30min, the temperature for continuously heating up after adding phosphorus pentoxide and phosphorus oxychloride is 65 ℃, the reaction time after continuously heating up is 4h, and the temperature is reduced to 20 ℃.
Preparation example 3
A preparation method of the penetrant comprises the following steps:
placing 50kg of isooctanol polyoxyethylene ether in a container, heating and stirring, adding 9kg of phosphorus pentoxide and 5kg of phosphorus oxychloride into the container containing the isooctanol polyoxyethylene ether, mixing the phosphorus pentoxide, the phosphorus oxychloride and the isooctanol polyoxyethylene ether, continuing to heat, reacting for a period of time, and then cooling to obtain a penetrating agent; in the heating and stirring process, the heating temperature is 50 ℃, the heating time is 60min, the temperature for continuously heating after adding phosphorus pentoxide and phosphorus oxychloride is 75 ℃, the reaction time after continuously heating is 5h, and the temperature is reduced to 40 ℃.
Preparation example 4
An osmotic agent which is different from that of preparation example 1 in that phosphorus pentoxide is not used in the preparation process of the osmotic agent.
Preparation example 5
A penetrant which is different from that of preparation example 1 in that phosphorus oxychloride is not used in the preparation process of the penetrant.
Preparation example 6
A penetrant differing from that of preparation example 1 in that the temperature to be continuously raised after phosphorus pentoxide and phosphorus oxychloride were added was 50 ℃.
Preparation example 7
A penetrant differing from that of preparation example 1 in that the temperature to be continuously raised after phosphorus pentoxide and phosphorus oxychloride were added was 90 ℃.
Preparation example of acidic cleaning agent
The mass concentration of sulfamic acid used in the application is 10-20%, and the mass concentration of hydrochloric acid is 5-15%.
Preparation example 8
An acidic cleaning agent comprises the following raw materials by weight:
60kg of sulfamic acid; 1.2kg of alkylphenol polyoxyethylene; 5kg of hydrochloric acid; 3kg of penetrant, the penetrant being prepared according to preparation example 1.
Preparation example 9
An acidic cleaning agent comprises the following raw materials by weight:
50kg of sulfamic acid; 0.8kg of alkylphenol polyoxyethylene; 4kg of hydrochloric acid; 2kg of penetrant, the penetrant being prepared according to preparation example 2.
Preparation example 10
An acidic cleaning agent comprises the following raw materials by weight:
70kg of sulfamic acid; 1.6kg of alkylphenol polyoxyethylene; 6kg of hydrochloric acid; 4kg of penetrant, the penetrant being prepared according to preparation example 3.
Preparation example 11
An acidic cleaning agent, which is different from preparation example 8 in that a penetrant used was prepared in preparation example 4.
Preparation example 12
An acidic cleaning agent, which is different from preparation example 8 in that a penetrant used was prepared in preparation example 5.
Preparation example 13
An acidic cleaning agent, which is different from preparation example 8 in that a penetrant used was prepared in preparation example 6.
Preparation example 14
An acidic cleaning agent, which is different from preparation example 8 in that a penetrant used was prepared in preparation example 7.
Preparation example 15
An acidic cleaning agent, which is different from the preparation example 8 in that the acidic cleaning agent also comprises 2.5kg of sodium secondary alkylbenzene sulfonate; nonylphenol polyoxyethylene ether 2 kg.
Examples
Example 1
A method for rapidly removing glass residues on the surface of a platinum alloy comprises the following steps:
s1: the method comprises the steps of physically crushing and removing large glass impurities on the surface of the platinum alloy, adding the platinum alloy deposited with glass residues into sodium hydroxide to obtain a mixture, heating the mixture until the sodium hydroxide is molten and the platinum alloy is completely covered, wherein the temperature is 600 ℃, and the heat preservation time is 50 min.
S2: taking out the platinum alloy subjected to heat preservation treatment in S1, placing the platinum alloy into an acidic cleaning agent to obtain a cleaning mixture, and carrying out ultrasonic treatment on the cleaning mixture, wherein the ultrasonic power is 600W, and the reaction time is 10 min; the acidic cleaning agent used was prepared from preparation 8.
S3: and (4) taking out the platinum alloy after the vibration cleaning in the S2, washing with clear water, removing residual impurities visible on the surface of the platinum alloy by using a stainless steel brush in the washing process until no residual impurities exist on the surface of the platinum alloy, finishing washing until the platinum alloy is observed by naked eyes, and drying the platinum alloy.
Example 2
A method for rapidly removing glass residues on the surface of a platinum alloy comprises the following steps:
s1: physically crushing and removing large glass impurities on the surface of the platinum alloy, adding the platinum alloy deposited with glass residues into potassium hydroxide to obtain a mixture, heating the mixture until the potassium hydroxide is molten and the platinum alloy is completely covered, wherein the temperature is 500 ℃, and the heat preservation time is 60 min.
S2: taking out the platinum alloy subjected to heat preservation treatment in S1, placing the platinum alloy into an acidic cleaning agent to obtain a cleaning mixture, and carrying out ultrasonic treatment on the cleaning mixture, wherein the ultrasonic power is 500W, and the reaction time is 15 min; the acidic cleaning agent used was prepared according to preparation example 9.
S3: and (4) taking out the platinum alloy after the vibration cleaning in the S2, washing with clear water, removing residual impurities visible on the surface of the platinum alloy by using a stainless steel brush in the washing process until no residual impurities exist on the surface of the platinum alloy, finishing washing until the platinum alloy is observed by naked eyes, and drying the platinum alloy.
Example 3
A method for rapidly removing glass residues on the surface of a platinum alloy comprises the following steps:
s1: the method comprises the steps of physically crushing and removing large glass impurities on the surface of the platinum alloy, adding the platinum alloy deposited with glass residues into calcium hydroxide to obtain a mixture, heating the mixture until the calcium hydroxide is molten and the platinum alloy is completely covered, wherein the temperature is 650 ℃, and the heat preservation time is 40 min.
S2: taking out the platinum alloy subjected to heat preservation treatment in S1, placing the platinum alloy into an acidic cleaning agent to obtain a cleaning mixture, and carrying out ultrasonic treatment on the cleaning mixture, wherein the ultrasonic power is 700W, and the reaction time is 5 min; the acidic cleaning agent used was prepared according to preparation example 10.
S3: and (4) taking out the platinum alloy after the vibration cleaning in the S2, washing with clear water, removing residual impurities visible on the surface of the platinum alloy by using a stainless steel brush in the washing process until no residual impurities exist on the surface of the platinum alloy, finishing washing until the platinum alloy is observed by naked eyes, and drying the platinum alloy.
Examples 4 to 8
A method for rapidly removing glass residues on the surface of a platinum alloy is different from that of example 1 in that the acid cleaning agents used in examples 4 to 8 are prepared in preparation examples 11 to 15, and are specifically shown in Table 1.
TABLE 1
| Examples | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 |
| Preparation example | Preparation example 11 | Preparation example 12 | Preparation example 13 | Preparation example 14 | Preparation example 15 |
Comparative example
Comparative example 1
The method for quickly removing the glass residue on the surface of the platinum alloy is different from the method in the embodiment 8 in that the acid cleaning agent does not comprise a penetrating agent.
Comparative example 2
The method for quickly removing the glass residues on the surface of the platinum alloy is different from the method in the embodiment 8 in that alkylphenol ethoxylates is not included in the acid cleaning agent.
Comparative example 3
The difference between the method for quickly removing the glass residue on the surface of the platinum alloy and the method in the embodiment 8 is that the weight of the penetrating agent in the acid cleaning agent is 0.5 kg.
Comparative example 4
The difference between the method for quickly removing the glass residue on the surface of the platinum alloy and the method in the embodiment 8 is that the weight of the penetrating agent in the acid cleaning agent is 6 kg.
Detection method
Firstly, platinum alloy surface observation.
Test samples: the platinum alloy materials obtained in examples 1 to 8 were used as test samples 1 to 8, and the platinum alloy materials obtained in comparative examples 1 to 4 were used as control samples 1 to 4.
The test method comprises the following steps: the morphology and color of the platinum alloy material surface, the presence of glass inclusions and other impurity particles remaining, and the presence of pits, cracks, and craters on the material surface were observed and recorded in table 2.
And secondly, testing the efficiency of removing glass impurities.
The test method comprises the following steps: two portions of 30kg of the same batch of recovered platinum alloy were collected and the operation of removing glass residues from the surface of the platinum alloy was carried out in accordance with the methods of comparative examples 1 to 4, respectively, and the time was counted from the start of the operation and stopped after the completion of the operation, and the time required for each of the two operation methods was calculated and recorded in Table 2.
TABLE 2
By combining examples 1-8, comparative example 1 and table 2, it can be seen that the use of phosphorus pentoxide and phosphorus oxychloride in the preparation of the penetrant enables a large amount of diester and triester to be generated in the penetrant, and the permeability of the penetrant is improved, so that the penetration of acidic components in the acidic cleaning agent to the glass impurities and the glass alkaline infusions on the surface of the platinum alloy is improved, the dissolving capacity of the acidic cleaning agent to the glass impurities and the glass alkaline infusions is improved, and the efficiency and the cleaning effect of removing the glass residues on the surface of the platinum alloy are improved.
In the process of preparing the penetrant, the excessive or insufficient temperature of the continuous heating after the phosphorus pentoxide and the phosphorus oxychloride are added influences the color of the recovered platinum alloy, because the excessive or insufficient temperature of the continuous heating can generate carbonyl compound impurities in the penetrant, the color of the finished penetrant is deepened, and the color of the surface of the platinum alloy is influenced.
After the secondary sodium alkyl benzene sulfonate and the nonylphenol polyoxyethylene ether are added into the acidic cleaning agent, the two are compounded with the penetrant, so that the penetration effect and the acid resistance of the acidic cleaning agent are improved, the removal efficiency of the acidic cleaning agent on the platinum alloy surface glass residues and alkaline infusible matters in the glass residues is improved, and the cleaning effect is improved.
When the amount of the penetrant is too high, the acidic cleaning agent can be promoted to generate destructive effect on the surface of the platinum alloy despite short time for removing the glass impurities on the surface of the platinum alloy, and further the color forming of the surface of the platinum alloy is influenced, and the quality of the recovered platinum alloy is influenced.
By compounding alkylphenol ethoxylates and the penetrant, the performance of the penetrant on the acidic cleaning agent can be promoted, so that the cleaning efficiency and the cleaning effect of the glass residues on the surface of the platinum alloy are improved.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. A method for rapidly removing glass residues on the surface of a platinum alloy is characterized by comprising the following steps:
s1: adding the platinum alloy deposited with the glass residues into the alkaline melting material to obtain a mixture, heating the mixture until the alkaline melting material is melted, and preserving heat for 40-60 min;
s2: taking out the platinum alloy subjected to heat preservation treatment in S1, placing the platinum alloy into an acidic cleaning agent to obtain a cleaning mixture, and carrying out ultrasonic treatment on the cleaning mixture for reaction for 5-15 min;
s3: taking out the platinum alloy after the reaction in the S2, and washing and drying the platinum alloy;
the acid cleaning agent comprises the following raw materials in parts by weight: 50-70 parts of sulfamic acid; 0.8-1.6 parts of alkylphenol polyoxyethylene; 4-6 parts of hydrochloric acid; 2-4 parts of a penetrating agent.
2. The method for rapidly removing the glass residue on the surface of the platinum alloy as claimed in claim 1, wherein the penetrating agent comprises the following raw materials in parts by weight: 20-50 parts of isooctyl alcohol polyoxyethylene ether; 5-9 parts of phosphorus pentoxide; 3-5 parts of phosphorus oxychloride.
3. The method for rapidly removing the glass residue on the surface of the platinum alloy as claimed in claim 2, wherein the penetrating agent is prepared by a method comprising the following steps: placing isooctanol polyoxyethylene ether in a container, heating and stirring, adding phosphorus pentoxide and phosphorus oxychloride into the container containing the isooctanol polyoxyethylene ether, mixing the phosphorus pentoxide, the phosphorus oxychloride and the isooctanol polyoxyethylene ether, continuing to heat, reacting for a period of time, and then cooling to obtain the penetrant.
4. The method for rapidly removing the glass residue on the surface of the platinum alloy as claimed in claim 3, wherein: in the heating and stirring process, the heating temperature is 30-50 ℃, the heating time is 30-60min, the temperature for continuously heating up after adding phosphorus pentoxide and phosphorus oxychloride is 65-75 ℃, the reaction time after continuously heating up is 4-5h, and the temperature is reduced to be less than 50 ℃.
5. The method for rapidly removing the glass residue on the surface of the platinum alloy as claimed in claim 1, wherein: based on the acidic cleaning agent, the acidic cleaning agent also comprises 1.5-3.5 parts of sodium secondary alkylbenzene sulfonate; 1.5-2.5 parts of nonylphenol polyoxyethylene ether.
6. The method for rapidly removing the glass residue on the surface of the platinum alloy as claimed in claim 1, wherein: the mass concentration of the sulfamic acid is not lower than 1% all the time in the reaction process.
7. The method for rapidly removing the glass residue on the surface of the platinum alloy as claimed in claim 1, wherein: the alkaline melt is selected from any one or two of sodium hydroxide, potassium hydroxide and calcium hydroxide.
8. The method for rapidly removing the glass residue on the surface of the platinum alloy as claimed in claim 7, wherein: the heating temperature in S1 is 500-650 ℃.
9. The method for rapidly removing the glass residue on the surface of the platinum alloy as claimed in claim 1, wherein: the ultrasonic power of the ultrasonic treatment in the S2 is 500W-700W.
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