CN113529144A - Finished product of sulfite cyanide-free electroformed gold liquid capable of being burnt - Google Patents

Finished product of sulfite cyanide-free electroformed gold liquid capable of being burnt Download PDF

Info

Publication number
CN113529144A
CN113529144A CN202110845819.8A CN202110845819A CN113529144A CN 113529144 A CN113529144 A CN 113529144A CN 202110845819 A CN202110845819 A CN 202110845819A CN 113529144 A CN113529144 A CN 113529144A
Authority
CN
China
Prior art keywords
gold
sulfite
cyanide
free
volume
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110845819.8A
Other languages
Chinese (zh)
Inventor
沈小四
肖彬
张飞飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenzhen Dingtai Yingsheng Technology Co ltd
Original Assignee
Shenzhen Dingtai Yingsheng Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenzhen Dingtai Yingsheng Technology Co ltd filed Critical Shenzhen Dingtai Yingsheng Technology Co ltd
Publication of CN113529144A publication Critical patent/CN113529144A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/48Electroplating: Baths therefor from solutions of gold

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The invention relates to the technical field of gold products, in particular to a sulfite cyanide-free electroforming gold liquid with a finished product capable of being burnt by fire. The gold product obtained by electroforming the cyanide-free sulfite gold plating solution has no bubble on the surface after being fired, which shows that the gold product obtained by preparation can resist firing. At present, no cyanide-free sulfite hard gold electroforming solution capable of passing fire exists in the field of cyanide-free hard gold industry, and the phenomena of foaming, deformation, crushing and the like can occur in the current hard gold products on the market only by burning with fire.

Description

Finished product of sulfite cyanide-free electroformed gold liquid capable of being burnt
Technical Field
The invention relates to the technical field of gold products, in particular to a sulfite cyanide-free electroforming gold liquid with a finished product capable of being burnt by fire.
Background
Along with the increasing living standard of people, the gold product is more and more favored by consumers. At present, gold products produced by electroplating are more and more. Cyanide gold plating technology is commonly used in the market, but is not environment-friendly due to toxicity and harm.
In order to overcome the above-mentioned defects of the gold plating technique with cyanogen, in recent years, some enterprises have adopted a solution containing gold sulfite (gold potassium sulfite and/or gold sodium sulfite) instead of a solution containing gold potassium cyanide as a plating solution to prepare gold products.
However, gold ornaments obtained by the cyanide-free gold plating technology on the market at present cannot be over-fired, cannot be used for real gold, are not afraid of fire refining, and have the defects of damage, incapability of maintenance and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a sulfite cyanide-free electroformed gold liquid with a finished product capable of being burnt.
The method of the invention can be used for preparing qualified gold sodium sulfite electroforming gold liquid and providing raw materials for supplementing gold consumption in the hard gold electroforming process.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation method of the finished product of the sulfite cyanide-free electroformed gold liquid capable of being burnt by fire is provided, and comprises the following steps:
s1, reacting gold flakes with aqua regia to generate gold chlorate;
s2, cooling after nitrate removal is finished;
s3, reacting with ammonia water to generate gold fulminate;
s4, filtering and washing the reactant, and reacting the reactant with sodium sulfite to generate gold sodium sulfite electroforming solution.
As a preferable embodiment of the preparation method, the gold sheet has a thickness of 0.8-1.2 mm.
As a preferred embodiment of the preparation method of the present invention, the aqua regia contains the following components: pure water, nitric acid and hydrochloric acid.
As a preferred embodiment of the preparation method, the volume ratio of the components of the aqua regia is as follows: pure water: nitric acid: hydrochloric acid 13:13: 63.
As a preferred embodiment of the preparation method of the present invention, step S1 specifically includes the following steps:
(1) adding 13 parts by volume of pure water and 13 parts by volume of concentrated nitric acid into the mixture, and uniformly stirring the mixture to obtain dilute nitric acid;
(2) and (2) placing gold flakes into a triangular flask, pouring 13 parts by volume of dilute nitric acid obtained in the step (1), pouring 38 parts by volume of concentrated hydrochloric acid, heating to 60-70 ℃ for reaction, supplementing the remaining 13 parts by volume of dilute nitric acid and 25 parts by volume of hydrochloric acid in turn after the reaction is mild, and slowly reacting until the gold flakes are completely dissolved.
The invention also provides the sulfite cyanide-free electroformed gold liquid prepared by the preparation method.
The invention also provides application of the sulfite cyanide-free electroformed gold liquid in preparation of gold products.
The invention has the beneficial effects that:
the gold product obtained by electroforming the cyanide-free sulfite gold plating solution has no bubble on the surface after being fired, which shows that the gold product obtained by preparation can resist firing. At present, no cyanide-free sulfite hard gold electroforming solution capable of passing fire exists in the field of cyanide-free hard gold industry, and the phenomena of foaming, deformation, crushing and the like can occur in the current hard gold products on the market only by burning with fire.
Drawings
FIG. 1 is a drawing showing the fire of gold product number 1 obtained by electroforming the sulfite cyanide-free electroformed gold solution of the present invention.
FIG. 2 is a photograph of a gold product No. 2 obtained by the sulfite cyanide-free electroforming of a gold solution according to the present invention after firing.
Detailed Description
To more clearly illustrate the technical solutions of the present invention, the following embodiments are further described, but the present invention is not limited thereto, and these embodiments are only some examples of the present invention.
Example 1 preparation of gold sodium sulfite electroforming solution
The preparation principle of the gold sodium sulfite electroforming solution is as follows:
pressing gold blocks with the color of 99.99% into gold sheets with the thickness of about 1mm, firstly reacting with a proper amount of aqua regia to generate gold chlorate, cooling after nitrate removal, reacting with a proper amount of ammonia water to generate gold fulminate, filtering and washing reactants, and fully reacting with calculated amount of sodium sulfite to generate gold sodium sulfite electroforming solution.
The instrument and the medicine adopted by the invention are as follows:
1) 1, tabletting machine;
2) 3 sets of good air draft cabinets;
3) vacuum pump 1 (6 air extraction interfaces);
4) an electric heating reaction sleeve and a matched triangular flask (the volume is 20000 ml);
5) 6 sets of Buchner funnels and filter flasks (10L);
6) a bronsted reactor;
7) a gold sodium sulfite reactor;
8) the glue basin, the ladle and the colloid rice scoop 2 are sleeved;
9) 4 each of 1L and 5L colloid measuring cups;
10) 5 150L white glue barrels;
11) 6 watering pots are provided; 12) 8 pieces of filter cloth (330mm) in diameter and 4 pieces of quick filter paper (330mm in diameter);
13) analytically pure hydrochloric acid 5L (huachengda);
14) analytically pure nitric acid 1L (huachenda); 15) 7.5L of analytically pure ammonia (science of Szelong); 16) analytically pure sulfuric acid 200ml (huachengda);
17) 6Kg of analytically pure sodium sulfite;
18) stabilizers A1 a2 each 1000m 1;
19) and (4) pH test paper.
This example illustrates a preparation process of a gold solution for electroforming sodium gold sulfite by using 2.5kg of gold lumps as an example, and the specific operation steps are as follows:
(1) tabletting: pressing 2.5kg gold block into gold sheet with width of about 5cm and thickness of 1mm, cutting into small segments, and cleaning with ethanol to remove oil stain on the surface.
Notes in step (1):
firstly, when the tablet pressing staff operates, the staff wears gloves, and the attention needs to be concentrated and the staff is attentive to invest the gloves so as to avoid accidentally injuring fingers;
secondly, in the tabletting process, personnel needing to be in a gold storehouse are on site for inspection;
thirdly, after tabletting is finished, the gold storehouse supervision personnel need to check the weight before and after tabletting, and the weight error before and after tabletting is not more than 0.1 g.
(2) Dissolving gold in aqua regia: placing the gold flakes into a triangular flask, pouring 1300ml of pure water and 1300ml of concentrated nitric acid into a 5L measuring cup, uniformly stirring, pouring 1300ml of dilute nitric acid into the triangular flask, pouring 1 half (about 3800ml) of concentrated hydrochloric acid, heating to 60-70 ℃, heating for reaction, supplementing the rest 1300ml of nitric acid and 2500ml of hydrochloric acid after the reaction is mild, pouring 300-400ml of hydrochloric acid once, slowly reacting until the gold flakes are completely dissolved, and finishing within about 2 hours. The aqua regia comprises the following components: 1300ml of pure water, 1300ml of nitric acid and 6300ml of hydrochloric acid.
Notes in step (2):
firstly, before dissolving gold flakes, processing the gold flakes into a pleated pen shape, and carefully putting the gold flakes into a three-necked flask so as to avoid damaging the flask;
secondly, in the process that the gold water staff receives gold tablets and adds the gold tablets into the reaction flask, the gold storehouse inspector needs to accompany the gold tablets;
thirdly, before the gold flakes are completely decomposed, the inspector can not leave the molten gold room.
(3) Nitrate removal: after the gold flakes are completely dissolved, the heating power is adjusted to a proper temperature.
Notes in step (3):
the process is completed in about 30 minutes, and during the heating process, liquid drops formed by hot steam at the feeding opening need to be cleaned frequently.
(4) And (3) generating gold fulminate: pumping the solution cooled in the step (3) into a gold Raleic acid reaction device, adding 10L of pure water, covering a cover, connecting an exhaust tube, starting a stirring motor, slowly pouring 2 bottles of half 6300ml of ammonia water, and stirring for about half an hour.
(5) And (3) suction filtration: preparing 4 clean buchner funnels and 6 filter flasks, putting a layer of filter cloth in each buchner funnel, then spraying a small amount of water to wet the filter cloth and attach the filter cloth to the filter cloth on the uppermost layer, connecting an exhaust tube, starting a vacuum pump, slowly scooping the aureoleic acid into the funnel, scooping the aureoleic acid into a aureoleic acid reactor after one-time pumping, adding about 25L of 70 ℃ pure water, stirring for 5 minutes, and performing suction filtration again. After repeated suction filtration for about 8 times, the gold fulminate is transferred into a rubber basin.
Notes in step (5):
when placing the funnel, the inclined plane of the outlet of the funnel is a front-back air extraction interface.
② the gold fulminate needs to be shoveled outwards from the middle of the filtering layer when scooping out, and care needs to be taken in the process of transferring out and using a rubber basin to receive leakage, and the gold fulminate cannot be splashed.
Thirdly, in the process of pumping, the gold fulminate is kept moist and can not be pumped to be dry, when the water content in the funnel is reduced gradually, the gold fulminate mud is required to be uniformly coated on the filter cloth and the cracking position of the inner wall of the funnel, and the gold fulminate with fine grains due to the upwarp of the filter layer is prevented from leaking into the filter flask.
Fourthly, after the filtration is finished for 8 times, checking whether the filtered water is neutral by using a pH test paper, dropping 3 drops of silver nitrate with the concentration of 0.1mol/L to check whether a small amount of white precipitate is generated (compared with tap water), and finishing the filtration if the two precipitates are met, otherwise, carrying out the filtration again.
Fifthly, the leaching wastewater contains trace unreacted gold-containing compounds existing in an ionic state, and the gold-containing compounds need to be stored for recycling.
(6) And (3) generating gold sodium sulfite: the water bath of the sodium gold sulfite reactor was first warmed to 75 ℃ half an hour in advance. Adding 11 bottles of half 5750ml of sodium sulfite into a gold sodium sulfite reactor, adding 15L of hot pure water at 70 ℃, stirring until the sodium sulfite is completely dissolved, taking 500ml of anhydrous sodium sulfite for cleaning, firstly cleaning gold utensils containing fuluric acid such as a funnel, a filter cloth and a ladle in the reactor, then transferring into a rubber barrel for cleaning, scooping the fuluric acid in the rubber basin into the reactor after the cleaning, finally cleaning the rubber basin and the spoon in the rubber barrel, pouring the cleaning solution in the rubber barrel back into the reactor after the cleaning, then lifting into a water bath, connecting an exhaust pipe, switching on a power supply and starting a stirring switch. After about 2-3 hours of reaction, 120ml of dilute sulfuric acid was slowly added to 5L twice, with a 5-minute interval between the two times, and the reaction was maintained for 12 hours after measuring pH to not less than 10.
Notes in step (6):
firstly, sulfuric acid is added to neutralize part of sodium hydroxide generated by reaction, so that the pH value is 10, the formation and the stability of a sodium gold sulfite complex are facilitated, and the dilute sulfuric acid is slowly poured in to avoid reduction of gold caused by overhigh local acidity;
preparing dilute sulfuric acid, namely slowly adding 240m of 1 sulfuric acid into 10L of pure water and uniformly stirring;
(7) adding a stabilizer: 10-100g/L of triethylene triamine; the organic polyamine is selected from 10-100g/L of glycerol, 10-100g/L of malonic acid, 10-100g/L of triethylene triamine and 10-10010 g/L of dipotassium hydrogen phosphate in tetraethylenepentamine after the reaction is finished, the gold sodium sulfite and the gold water are light yellow, then the stabilizer A1A 2 is added for 1000m1 respectively, the reaction is kept for half an hour, the gold water is filtered after being cooled, and the upper layer of filter paper on the lower layer of filter cloth is obtained during the filtering.
(8) Sampling and bottling the molten gold: the filtered molten gold is stirred uniformly, then 1L of the molten gold is sampled, and then the molten gold is filled into a clean and numbered white empty bottle (5L) with the weighed weight.
Notes in step (8):
firstly, in the process of bottling and sampling, a gold shop clerk needs to follow up;
secondly, after the gold water is filled, cleaning the glue barrel, recovering the cleaning water, and not adding the gold water bottle;
③ the newly prepared golden water has the quality guarantee period of 1 month and can not be stored for a long time.
(9) Weighing and warehousing: and (5) registering the gold water batch, weighing gross weight and calculating net weight, and warehousing.
EXAMPLE 2 Properties of gold products obtained by electroforming of gold solution by sodium gold sulfite electroforming
Gold products with the style of calabash are obtained by electroforming the cyanide-free sulfite gold plating solution prepared in the example 1, and parameters of the electroplating process are shown in the table 1.
TABLE 1 plating parameters
Figure BDA0003180508230000061
The prepared cucurbit gold product is burnt by a fire gun at the temperature of 800-1000 ℃, whether the surface of the burnt cucurbit is foamed or not is observed, and as can be seen from the table 2 and the figures 1-2, the gold product obtained by electroforming the cyanide-free sulfite gold plating solution has no surface foamed after being burnt, which indicates that the prepared gold product can resist to burning. At present, no cyanide-free sulfite hard gold electroforming solution capable of passing fire exists in the field of cyanide-free hard gold industry, and the phenomena of foaming, deformation, crushing and the like can occur in the current hard gold products on the market only by burning with fire.
TABLE 2 effect of gold product obtained by electroforming after firing
Product numbering Whether or not foaming occurs
1 Not foaming
2 Not foaming
3 Not foaming
4 Not foaming
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (7)

1. A method for preparing a finished product of sulfite cyanide-free electroformed gold liquid capable of being burnt is characterized by comprising the following steps:
s1, reacting gold flakes with aqua regia to generate gold chlorate;
s2, cooling after nitrate removal is finished;
s3, reacting with ammonia water to generate gold fulminate;
s4, filtering and washing the reactant, and reacting the reactant with sodium sulfite to generate gold sodium sulfite electroforming solution.
2. The method according to claim 1, wherein the gold flakes have a thickness of 0.8 to 1.2 mm.
3. The method of claim 1, wherein the aqua regia comprises the following components: pure water, nitric acid and hydrochloric acid.
4. The method according to claim 3, wherein the aqua regia comprises the following components in volume ratio: pure water: nitric acid: hydrochloric acid 13:13: 63.
5. The method according to claim 4, wherein step S1 specifically comprises the steps of:
(1) adding 13 parts by volume of pure water and 13 parts by volume of concentrated nitric acid into the mixture, and uniformly stirring the mixture to obtain dilute nitric acid;
(2) and (2) placing gold flakes into a triangular flask, pouring 13 parts by volume of dilute nitric acid obtained in the step (1), pouring 38 parts by volume of concentrated hydrochloric acid, heating to 60-70 ℃ for reaction, supplementing the remaining 13 parts by volume of dilute nitric acid and 25 parts by volume of hydrochloric acid in turn after the reaction is mild, and slowly reacting until the gold flakes are completely dissolved.
6. The sulfite cyanide-free electroformed gold liquid prepared by the preparation method according to any one of claims 1 to 5.
7. Use of the sulfite cyanide-free electroformed gold solution of claim 6 for preparing a gold product.
CN202110845819.8A 2020-08-07 2021-07-26 Finished product of sulfite cyanide-free electroformed gold liquid capable of being burnt Pending CN113529144A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2020107913637 2020-08-07
CN202010791363 2020-08-07

Publications (1)

Publication Number Publication Date
CN113529144A true CN113529144A (en) 2021-10-22

Family

ID=78121287

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110845819.8A Pending CN113529144A (en) 2020-08-07 2021-07-26 Finished product of sulfite cyanide-free electroformed gold liquid capable of being burnt

Country Status (1)

Country Link
CN (1) CN113529144A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101734708A (en) * 2009-12-22 2010-06-16 三门峡朝阳科技有限公司 Preparation method of cyanide-free gold sodium sulfite complex for gold plating
CN105568269A (en) * 2015-12-16 2016-05-11 励福(江门)环保科技股份有限公司 Preparation method of cyanide-free gold plating reagent sodium gold sulfite
CN108728873A (en) * 2018-06-20 2018-11-02 深圳市金宝盈文化股份有限公司 A kind of production method of casting gold process product
CN110607539A (en) * 2019-09-29 2019-12-24 深圳市金久缘珠宝有限公司 Processing technology of gold jewelry

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101734708A (en) * 2009-12-22 2010-06-16 三门峡朝阳科技有限公司 Preparation method of cyanide-free gold sodium sulfite complex for gold plating
CN105568269A (en) * 2015-12-16 2016-05-11 励福(江门)环保科技股份有限公司 Preparation method of cyanide-free gold plating reagent sodium gold sulfite
CN108728873A (en) * 2018-06-20 2018-11-02 深圳市金宝盈文化股份有限公司 A kind of production method of casting gold process product
CN110607539A (en) * 2019-09-29 2019-12-24 深圳市金久缘珠宝有限公司 Processing technology of gold jewelry

Similar Documents

Publication Publication Date Title
CN101328541B (en) Gold wet purification process
CN111032917A (en) Ammonia distillation recycling process and system for alkaline etching waste liquid of circuit board
CN107099666B (en) A kind of extraction and separation thulium, ytterbium, lutetium method
CN102229691A (en) Method for preparing polycarboxylic acid water reducing agent by using tail solution of producing acrylaldehyde
CN101597769B (en) Normal temperature and pressure quick desorption electrolysis method of gold loaded carbon
CN107478765A (en) A kind of nickel-silicon nitride method in thick gold
CN102167405B (en) New method for preparing ruthenium nitrosylnitrate solid
CN113529144A (en) Finished product of sulfite cyanide-free electroformed gold liquid capable of being burnt
CN103936870A (en) Method for shortening soaking time of corns by combining pressurization and compound enzymatic method
CN102817039A (en) Method for preventing quinolone injection from discoloring in preparation and filling process
CN105648482A (en) Cyanide-free cadmium plating process for part surface
CN105441970A (en) New method for removing impurities in tellurium electrolyte
CN107505313A (en) Selenium quantity measuring method in a kind of impure selenium
CN205953737U (en) It uses gold recovery equipment to contain golden waste water regeneration cycle
CN105253866B (en) A kind of method for removing organic matter in ketazine process hydrazine hydrate
CN211770344U (en) Double-circulation type waste liquid treatment device
CN113584539A (en) Method for preparing gold salt solution and recovering gold and cyanide-free gold electroplating solution
CN112301388A (en) Cyanide-free electroplating process
CN106086449A (en) Palladium recovery technique in a kind of alkalescence palladium liquid
CN105814216B (en) The recovery method of palladium
CN106191971A (en) The method reclaiming the silver-plated hanger of high-voltage diode pin
CN102776496B (en) Tin layer anti-blushing agent for high-temperature backflow as well as preparation method and use method of tin layer anti-blushing agent
CN214131594U (en) Reation kettle is used in production of low modulus sodium silicate
CN101514041B (en) Catalyst plant carclazyte waste water processing agent and using method thereof
CN105001116A (en) Preparation of highly sensitive 2,4-dinitrophenylhydrazine

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20211022