CN103397356B - Non-toxic gold salt for gold plating and synthetic method thereof - Google Patents
Non-toxic gold salt for gold plating and synthetic method thereof Download PDFInfo
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Abstract
The invention discloses a non-toxic gold salt for gold plating and a synthetic method thereof. The method comprises the following steps of: (S1) adding gold chloride into 10 to 100 DEG C water while stirring; (S2) adding strong base solution into the gold chloride water solution; (S3) respectively adding a reducing agent solution and a coordination agent solution into the mixed solution, so as to obtain a clear and transparent solution, wherein the concentration of the reducing agent solution is 0.1-10mol/L, and the concentration of the coordination agent solution is 1.0-10 mol/L; and (S4) cooling the clear and transparent solution obtained in the step (S3) to 20 DEG C below zero-10 DEG C in a cooling container, adding the strong base solution into the cooled solution to separate crystal sediments out of the solution, continuously maintaining the temperature of the solution for 6-48 hours at the cooling temperature to adequately separate the crystal sediments out, and drying, thus obtaining the non-toxic gold salt for the gold plating. The non-toxic gold salt for the gold plating is nontoxic and environment-friendly and is stable in performance; and the coating of the non-toxic gold salt is has strong adhesion to different matrixes and can effectively protect the matrixes from being corroded by the external environment.
Description
Technical field
The present invention relates to technology for gold field is electroplated, more particularly, to a kind of Non-toxic gold salt for gold plating and its synthetic method.
Background technology
China's economy is continued for rapid growth, and world's manufacturing industry is shifted with the center of processing industry to China, plating
Technology is not only played an important role in traditional industry, in new high-tech industry, such as modern electronic technology, microelectric technique,
More and more big effect is played in mechanics of communication and product manufacturing.Due to the high temperature resistant of gold, corrosion-resistant, chemical stability is good, institute
Had a wide range of applications in the electronics industry with electroplating gold.
At present the most popular electroplating technology of China is that alkaline cyanide is gold-plated, and the method is mainly with KAu (CN)2As
Main salt, with KCN as complexing agent, free KCN can be such that bath stability, anode normally dissolves, and improve cathodic polarization, and coating is careful,
The electric conductivity for adding some carbonate to increase plating solution in the plating solution is also needed to simultaneously.Because KCN has good complexing power
And it is relatively inexpensive, therefore extensively favored by most enterprises, but cyanide is extremely toxic substance, to environment and human health
Cause and greatly threaten and endanger.
Therefore, more and more generally carried out using cyanogen-less gold liquid gold-plated, and existing gold-plated cyanogen-less gold liquid is main
For sulfurous acid cyanogen-less gold liquid, thiosulfuric acid gold plating liquid and citrate cyanogen-less gold liquid.
Chinese patent application (Application No. 02805673.6) disclose the plating solution of a kind of deposited Au and billon and
Its application in dentistry moulded parts is prepared.In the plating solution gold is with the presence of sulfurous acid gold complex form.The invention is except optional
Outside other metals for existing and the common additive for this kind of sulfurous acid gold plating solution, also containing at least one bismuth compound.
The bismuth compound is preferably complex, particularly forming agent NTA, HEDTA containing coordination, TEPA, DTPA, EDNTA or EDTA
Complex.The bismuth additive can be added in plating solution in the preparation process of plating solution, and providing the user one kind can grow
The plating solution of phase operation, it need not add other additives before electro-deposition.The weak point of the method is wearing no resistance for coating,
And the high cost of plating solution.
Chinese patent application (Application No. 200910066096.0) discloses a kind of citric acid gold potassium for gilding and its system
Preparation Method.The molecular formula of the citric acid gold potassium is KAu2N4C12H11O8.It is by the way that gold trichloride is dissolved in the water and repeatedly dense
Contracting, dilution, then react in the reactor with potassium citrate, ethylenediamine tetra-acetic acid, malononitrile and are prepared from.The deficiency of the method
Part be preparing raw material malononitrile have certain toxicity and it is gold-plated after waste liquid in still contain a certain amount of CN-。
The content of the invention
It is an object of the invention to provide a kind of Non-toxic gold salt for gold plating and its synthetic method, its stable performance, coating with
Different matrix adhesive abilities is strong, can effectively protect corrosion of the external environment to matrix, and environmental protection.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of Non-toxic gold salt for gold plating synthetic method, it is comprised the following steps：
Step S1：During gold trichloride to be added to 10～100 DEG C of water under conditions of stirring, until the gold trichloride is complete
CL；
Step S2：Strong base solution is added in the aqueous solution of above-mentioned gold trichloride, the pH value for adjusting the mixed solution is
7.5～14；
Step S3：Be separately added into in the mixed solution concentration be 0.1mol/L～10mol/L reductant solution and
Concentration is the coordination agent solution of 1.0mol/L～10mol/L, is sufficiently stirred for, and the pH value for adjusting solution is 1～7, obtains clarification saturating
Bright solution；
Step S4：The solution of clear described in step S3 is positioned in cooling container and is cooled to -20～10 DEG C, then
Strong base solution is added to the solution after cooling, it is 7.5～14 to adjust pH value so that occurs crystal settling in solution, continues institute
State solution to be kept for 6～48 hours under the chilling temperature so that crystal settling is fully separated out, then by the crystal settling 20～
200 DEG C of drying, that is, obtain the Non-toxic gold salt for gold plating.
Further, in above-mentioned Non-toxic gold salt for gold plating synthetic method, the strong base solution is KOH or NaOH solution.
Further, in above-mentioned Non-toxic gold salt for gold plating synthetic method, the reducing agent is potassium citrate or Vitamin C
Acid, the complexant is NC (CH2)mCOO(CH2)nCH3, (m=1～20；N=0～20).
Further, in above-mentioned Non-toxic gold salt for gold plating synthetic method, step S1 is specially：
1.0～2.5L deionized waters are added in reaction vessel, stirring and heater is opened so that the reaction vessel
Interior temperature adds 20～60g gold trichlorides after being increased to 10～100 DEG C, continues to be kept stirring for, until the gold trichloride is complete
Dissolving.
Further, in above-mentioned Non-toxic gold salt for gold plating synthetic method, step S2 is specially：
12～336g highly basic is taken, in being dissolved in 3L, 40～100 DEG C of water, strong base solution is configured to；
The strong base solution is slowly added dropwise into above-mentioned gold trichloride solution, and during the strong base solution is added dropwise
The pH value of the mixed solution is constantly detected, until the pH value of the mixed solution is adjusted to into 7.5～14.
Further, in above-mentioned Non-toxic gold salt for gold plating synthetic method, step S3 is specially：
Appropriate reducing agent and complexant are added in 100 DEG C of water under stirring condition, are sufficiently stirred for, concentration is obtained
For 0.1mol/L～10mol/L reductant solution and concentration for 1.0mol/L～10mol/L coordination agent solution；
The reductant solution and coordination agent solution are slowly dropped in the mixed solution, the pH value for adjusting solution is
1～7, obtain the solution of clear.
Further, in above-mentioned Non-toxic gold salt for gold plating synthetic method, the drying of crystal settling described in step S4
Also include before：
The crystal settling of above-mentioned precipitation is transferred in suction funnel, moisture unnecessary in the crystal settling is filtered off, and
The solid for obtaining is transferred in container.
The present invention also provides a kind of Non-toxic gold salt for gold plating, and its chemical formula is：
Wherein, m=1～20；N=0～
20。
The present invention also provides a kind of Non-toxic gold salt for gold plating, and its chemical formula is：
Wherein, m=1～20；N=0～
20。
The present invention also provides a kind of Non-toxic gold salt for gold plating, and its chemical formula is：
Wherein, m=1～20；N=0
～20.
Non-toxic gold salt for gold plating of the present invention and its synthetic method asepsis environment-protecting, stable performance, its coating and different matrixes
Adhesive ability is strong, can effectively protect corrosion of the external environment to matrix.
Description of the drawings
Fig. 1 is the schematic flow sheet of Non-toxic gold salt for gold plating synthetic method of the present invention.
Specific embodiment
For the ease of understanding the present invention, the present invention is described more fully below with reference to relevant drawings.In accompanying drawing
Give presently preferred embodiments of the present invention.But, the present invention can be realized in many different forms, however it is not limited to this paper institutes
The embodiment of description.On the contrary, the purpose for providing these embodiments is to make the understanding to the disclosure more thorough
Comprehensively.
Fig. 1 is referred to, Fig. 1 is the schematic flow sheet of Non-toxic gold salt for gold plating synthetic method of the present invention.The nontoxic plating of the present invention
Gold gold salt synthetic method is comprised the following steps：
Step S1：During gold trichloride to be added to 10～100 DEG C of water under conditions of stirring, until the gold trichloride is complete
CL；
Step S2：Strong base solution is added in the aqueous solution of above-mentioned gold trichloride, the pH value for adjusting the mixed solution is
7.5～14；In step S2, reaction equation is：Obtain containing AuO- 2
Mixed solution.
Step S3：Be separately added into in the mixed solution concentration be 0.1mol/L～10mol/L reductant solution and
Concentration is the coordination agent solution of 1.0mol/L～10mol/L, is sufficiently stirred for, and the pH value for adjusting solution is 1～7, obtains clarification saturating
Bright solution.
In the step, trivalent gold is reduced to monovalence gold by the reducing agent, and forms complex with complexant.
Step S4：The solution of clear described in step S3 is positioned in cooling container and is cooled to -20～10 DEG C, then
Strong base solution is added to the solution after cooling, it is 7.5～14 to adjust pH value so that occurs crystal settling in solution, continues institute
State solution to be kept for 6～48 hours under the chilling temperature so that crystal settling is fully separated out, then by the crystal settling 20～
200 DEG C of drying, that is, obtain the Non-toxic gold salt for gold plating.
The chemical formula of the gold salt is
Wherein, m=1～20；N=0～
20；Or
Wherein, m=1～20；N=0～
20；Or
Wherein, m=1～20；N=0～
20。
Wherein, the strong base solution is KOH or NaOH solution.
The reducing agent is potassium citrate or ascorbic acid, and the complexant is NC (CH2)mCOO(CH2)nCH3, wherein, m
=1～20；N=0～20.
Step S1 is specially：
1.0～2.5L deionized waters are added in reaction vessel, stirring and heater is opened so that the reaction vessel
Interior temperature adds 20～60g gold trichlorides after being increased to 10～100 DEG C, continues to be kept stirring for, until the gold trichloride is complete
Dissolving.
Step S2 is specially：
12～336g highly basic is taken, in being dissolved in 3L, 40～100 DEG C of water, strong base solution is configured to；
The strong base solution is slowly added dropwise into above-mentioned gold trichloride solution, and during the strong base solution is added dropwise
The pH value of the mixed solution is constantly detected, until the pH value of the mixed solution is adjusted to into 7.5～14.
Step S3 is specially：
Appropriate reducing agent and complexant are added in 100 DEG C of water under stirring condition, are sufficiently stirred for, concentration is obtained
For 0.1mol/L～10mol/L reductant solution and concentration for 1.0mol/L～10mol/L coordination agent solution；
The reductant solution and coordination agent solution are slowly dropped in the mixed solution, the pH value for adjusting solution is
1～7, obtain the solution of clear.
Also include before the drying of crystal settling described in step S4：
The crystal settling of above-mentioned precipitation is transferred in suction funnel, moisture unnecessary in the crystal settling is filtered off, and
The solid for obtaining is transferred in container.
Separately, the present invention also provides a kind of Non-toxic gold salt for gold plating, and its chemical formula is：
Wherein, m=1～20；N=0～
20；Or
Wherein, m=1～20；N=0～
20；Or
Wherein, m=1～20；N=0～
20。
Monovalence gold in Non-toxic gold salt for gold plating of the present invention is in the form of complex compound, to set up in aqueous
Such as(wherein M be part, N-For citrate ion or Vitamin C acid group from
Son) balance, so in electroplating technology, with Au in solution+Consumption, the presence of balance causes free Au+Obtain constantly
Supplement, maintain Au in plating solution+Stablizing for concentration, advantageously forms the coating of densification, excellent performance.
Therefore, compared to prior art, the present invention has following advantages：
The raw material that Non-toxic gold salt for gold plating of the present invention is used is hypotoxic, and the product for obtaining is nontoxic, is one
Environmentally friendly product is planted, and property is very stable, can easily be used and be stored, it is nontoxic gold-plated using the present invention
There can be firm adhesive ability from different matrixes with the coating obtained by gold salt and certain bond strength, energy can be reached
Enough bear certain outer force intensity and do not destroy, and the dense structure of coating, porosity are low, effectively protect external environment pair
The corrosion of matrix.
To sum up, Non-toxic gold salt for gold plating of the present invention and its synthetic method environmental protection, stable performance, its coating from it is different
Matrix adhesive ability is strong, can effectively protect corrosion of the external environment to matrix.
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1
1.0L deionized waters are added in reaction vessel, stirring and heater is opened, temperature is increased to into 10 DEG C, treat temperature
20g gold trichlorides are added after degree is stable, continues to be kept stirring for, until gold trichloride is completely dissolved；16.8g KOH are separately taken, by it
In being dissolved in 3L, 10 DEG C of water, KOH solution is configured to, is slowly added dropwise into above-mentioned gold trichloride solution, side edged surveys pH
Value, it is 7.5 to adjust pH value；Separately be heated in 10 DEG C of water in 3L, under stirring condition add 97.32g potassium citrates and
339gNCCH2COOCH2CH3, it is 1.0mol/ that the potassium citrate solution and concentration that concentration is 0.1mol/L is obtained until completely dissolved
The NCCH of L2COOCH2CH3Solution；By above-mentioned potassium citrate solution and NCCH2COOCH2CH3Solution is slowly dropped to above-mentioned solution
In, it is 1 to adjust pH value, has obtained the solution of clear；Container equipped with clear transparent solutions obtained above is positioned over
In cooling container so that solution is cooled to -20 DEG C, the KOH solution of above-mentioned preparation is added under conditions of stirring, adjusting pH value is
7.5, occur the crystal settling of white in solution, it is -20 DEG C to continue keeping temperature, keeps 6h, crystal is separated out completely；Will be above-mentioned
The precipitation for obtaining is transferred in suction funnel, filters off unnecessary moisture, and the solid for obtaining is transferred in container, is positioned over 20 DEG C
Baking oven in dry, that is, obtain final product.
Embodiment 2
1.5L deionized waters are added in reaction vessel, stirring and heater is opened, temperature is increased to into 40 DEG C, treat temperature
35g gold trichlorides are added after degree is stable, continues to be kept stirring for, until gold trichloride is completely dissolved；336g KOH are separately taken, its is molten
Solution is configured to KOH solution in 3L, 40 DEG C of water, is slowly added dropwise into above-mentioned gold trichloride solution, and side edged surveys pH
Value, it is 9 to adjust pH value；Separately it is heated in 40 DEG C of water in 3L, 52.84g ascorbic acid and 1395gNC is added under stirring condition
(CH2)2COO(CH2)3CH3, it is 3.0mol/L that the ascorbic acid solution and concentration that concentration is 0.1mol/L is obtained until completely dissolved
NC (CH2)2COO(CH2)3CH3Solution, by above-mentioned ascorbic acid solution and NC (CH2)2COO(CH2)3CH3Solution is slowly added dropwise
To in above-mentioned solution, it is 3 to adjust pH value, has obtained the solution of clear；By obtained above equipped with clear transparent solutions
Container is positioned in cooling container so that solution is cooled to -10 DEG C, and the KOH solution of above-mentioned preparation is added under conditions of stirring,
It is 10 to adjust pH value, the crystal settling for occurring white in solution, and it is -10 DEG C to continue keeping temperature, keeps 18h, makes crystal complete
Separate out；Precipitation obtained above is transferred in suction funnel, unnecessary moisture is filtered off, the solid for obtaining is transferred to container
In, be positioned in 80 DEG C of baking oven and dry, that is, obtain final product.
Embodiment 3
2.0L deionized waters are added in reaction vessel, stirring and heater is opened, temperature is increased to into 70 DEG C, treat temperature
45g gold trichlorides are added after degree is stable, continues to be kept stirring for, until gold trichloride is completely dissolved；12g NaOH are separately taken, its is molten
Solution is configured to NaOH solution in 3L, 70 DEG C of water, is slowly added dropwise into above-mentioned gold trichloride solution, and side edged surveys pH
Value, it is 12 to adjust pH value；Separately it is heated in 70 DEG C of water in 3L, 9732g potassium citrates and 2790gNC is added under stirring condition
(CH2)3COO(CH2)2CH3, it is 6.0mol/L that the potassium citrate solution and concentration that concentration is 10mol/L is obtained until completely dissolved
NC (CH2)3COO(CH2)2CH3Solution, by above-mentioned potassium citrate solution and NC (CH2)3COO(CH2)2CH3Solution is slowly added dropwise
To in above-mentioned solution, it is 5 to adjust pH value, has obtained the solution of clear；By obtained above equipped with clear transparent solutions
Container is positioned in cooling container so that solution is cooled to 0 DEG C, and the NaOH solution of above-mentioned preparation is added under conditions of stirring,
It is 12 to adjust pH value, the crystal settling for occurring white in solution, and it is 0 DEG C to continue keeping temperature, keeps 36h, crystal is analysed completely
Go out；Precipitation obtained above is transferred in suction funnel, unnecessary moisture is filtered off, the solid for obtaining is transferred in container,
It is positioned in 160 DEG C of baking oven and dries, that is, obtains final product.
Embodiment 4
2.5L deionized waters are added in reaction vessel, stirring and heater is opened, temperature is increased to into 100 DEG C, treated
60g gold trichlorides are added after temperature stabilization, continues to be kept stirring for, until gold trichloride is completely dissolved；240g NaOH are separately taken, will
It is dissolved in 3L, 100 DEG C of water, is configured to NaOH solution, is slowly added dropwise into above-mentioned gold trichloride solution, side edged
PH value is surveyed, it is 14 to adjust pH value；Separately be heated in 100 DEG C of water in 3L, under stirring condition add 5284g ascorbic acid and
5910gNC(CH2)4COO(CH2)4CH3, ascorbic acid solution and concentration that concentration is 10mol/L are obtained until completely dissolved is
NC (the CH of 10mol/L2)4COO(CH2)4CH3Solution, by above-mentioned potassium citrate solution and NC (CH2)4COO(CH2)4CH3Solution delays
Slowly in being added drop-wise to above-mentioned solution, it is 7 to adjust pH value, has obtained the solution of clear；By obtained above equipped with clear
The container of solution is positioned in cooling container so that solution is cooled to 10 DEG C, and above-mentioned preparation is added under conditions of stirring
NaOH solution, it is 14 to adjust pH value, the crystal settling for occurring white in solution, and it is 10 DEG C to continue keeping temperature, keeps 48h, is made
Crystal is separated out completely；Precipitation obtained above is transferred in suction funnel, unnecessary moisture is filtered off, the solid transfer for obtaining
Into container, it is positioned in 200 DEG C of baking oven and dries, that is, obtains final product.
Here description of the invention and application are illustrative, are not wishing to limit the scope of the invention to above-described embodiment
In.The deformation and change of embodiments disclosed herein is possible, real for those skilled in the art
The replacement and equivalent various parts for applying example is known.It should be appreciated by the person skilled in the art that without departing from the present invention
Spirit or essential characteristics in the case of, the present invention can in other forms, structure, arrangement, ratio, and with other components,
Material and part are realizing.In the case of without departing from scope and spirit of the present invention, embodiments disclosed herein can be entered
Other deformations of row and change.
Claims (9)
1. a kind of Non-toxic gold salt for gold plating synthetic method, it is characterised in that it is comprised the following steps：
Step Sl：During gold trichloride to be added to 10～100 DEG C of water under conditions of stirring, until the gold trichloride is completely molten
Solution；
Step S2：Adding strong base solution in the aqueous solution of above-mentioned gold trichloride, the pH value for adjusting the mixed solution is 7.5～
14；
Step S3：Reductant solution and concentration that concentration is 0.1mol/L～10mol/L are separately added into in the mixed solution
For the coordination agent solution of 1.0mol/L～10mol/L, it is sufficiently stirred for, the pH value for adjusting solution is 1～7, obtains clear
Solution；The reducing agent is potassium citrate or ascorbic acid, and the complexant is NC (CH2)mCOO(CH2)nCH3, wherein, m=l～
20；N=0～20；
Step S4：The solution of clear described in step S3 is positioned in cooling container and is cooled to -20～10 DEG C, then to cold
But the solution after adds strong base solution, and it is 7.5～14 to adjust pH value so that occur crystal settling in solution, continuation will be described molten
Liquid is kept for 6～48 hours under the chilling temperature so that crystal settling is fully separated out, then by the crystal settling 20～200
DEG C drying, that is, obtain the Non-toxic gold salt for gold plating.
2. Non-toxic gold salt for gold plating synthetic method according to claim 1, it is characterised in that the strong base solution is KOH
Or NaOH solution.
3. Non-toxic gold salt for gold plating synthetic method according to claim 1, it is characterised in that step Sl is specially：
1.0～2.5L deionized waters are added in reaction vessel, stirring and heater is opened so that the reaction vessel interior temperature
Degree adds 20～60g gold trichlorides after being increased to 10～100 DEG C, continues to be kept stirring for, until the gold trichloride is completely dissolved.
4. Non-toxic gold salt for gold plating synthetic method according to claim 1, it is characterised in that step S2 is specially：
12～336g highly basic is taken, in being dissolved in 3L, 40～100 DEG C of water, strong base solution is configured to；By the strong base solution
It is slowly added dropwise into above-mentioned gold trichloride solution, and the mixed solution is constantly detected during the strong base solution is added dropwise
PH value, until the pH value of the mixed solution is adjusted to into 7.5～14.
5. Non-toxic gold salt for gold plating synthetic method according to claim 1, it is characterised in that step S3 is specially：
Appropriate reducing agent and complexant are added in 100 DEG C of water under stirring condition, are sufficiently stirred for, prepared concentration is
The reductant solution and concentration of 0.1mol/L～10mol/L is the coordination agent solution of 1.0mol/L～10mol/L；
By the reductant solution and coordination agent solution be slowly dropped in the mixed solution, adjust solution pH value be 1～
7, obtain the solution of clear.
6. Non-toxic gold salt for gold plating synthetic method according to claim 1, it is characterised in that brilliant described in step S4
Also include before body precipitation drying：
The crystal settling of above-mentioned precipitation is transferred in suction funnel, unnecessary moisture in the elimination crystal settling, and will
To solid be transferred in container.
7. a kind of Non-toxic gold salt for gold plating, it is characterised in that its chemical formula is：
,
Wherein, m=l～20；N=0～20.
8. a kind of Non-toxic gold salt for gold plating, it is characterised in that its chemical formula is：
,
Wherein, m=l～20；N=0～20.
9. a kind of Non-toxic gold salt for gold plating, it is characterised in that its chemical formula is：
,
Wherein, m=l～20；N=0～20.
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2013
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|---|---|---|---|---|
| US3929595A (en) * | 1973-11-07 | 1975-12-30 | Degussa | Electrolytic burnished gold bath with higher rate of deposition |
| US4212708A (en) * | 1979-06-05 | 1980-07-15 | Belikin Alexandr V | Gold-plating electrolyte |
| CN101172946A (en) * | 2007-11-20 | 2008-05-07 | 三门峡市恒生生化技术有限公司 | Gold potassium lemon acid for gold plating and method for producing the same |
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|---|---|
| CN103397356A (en) | 2013-11-20 |
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