CN105908236B - Coloring agent and preparation method thereof - Google Patents
Coloring agent and preparation method thereof Download PDFInfo
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- CN105908236B CN105908236B CN201610309064.9A CN201610309064A CN105908236B CN 105908236 B CN105908236 B CN 105908236B CN 201610309064 A CN201610309064 A CN 201610309064A CN 105908236 B CN105908236 B CN 105908236B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
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Abstract
The present invention relates to a kind of coloring agents and preparation method thereof.The coloring agent includes following component: the acid red 94 of 0.285~0.485 grams per liter, the acid black 172 of 0.0015~0.0215 grams per liter, 0.00668~0.00868 grams per liter the grams per liter of acid black 1 68 and 0.032~0.052 acid orange 74.Above-mentioned coloring agent can make the color on the surface of metalwork close with rose golden.
Description
Technical field
The present invention relates to a kind of coloring agents and preparation method thereof.
Background technique
Metal product generally will do it anodized such as aluminium alloy, magnesium alloy or titanium alloy, in its surface shape
At the preferable anode oxide film of wearability.To keep product surface color diversified, product can be carried out at dyeing after anodic oxidation
Reason or spray treatment.Since rose golden is more beautiful, it is favored by people, and the colouring method of current rose golden obtains
The color of metal surface differ larger with rose golden.
Summary of the invention
In consideration of it, being more nearly the color on the surface of metalwork using the coloring agent it is necessary to provide a kind of coloring agent
Rose golden.
In addition, also providing a kind of preparation method of coloring agent.
A kind of coloring agent, including following component: 94,0.0015~0.0215 grams of the acid red of 0.285~0.485 grams per liter/
The acid orange 74 of the grams per liter of acid black 1 68 and 0.032~0.052 of the acid black 172,0.00668~0.00868 grams per liter that rise.
The coloring agent further includes 0.0005~0.0025 ml l of buffer in one of the embodiments, described
In buffer comprising mass percentage be 3~6% acetic acid and 28~35% sodium acetate.
The coloring agent further includes the sodium sulphate of 1~4 grams per liter in one of the embodiments,.
It in one of the embodiments, include following component: the acid of the acid red 94 of 0.385 grams per liter, 0.0115 grams per liter
The acid orange 74 of the grams per liter of acid black 1 68 and 0.042 of black 172,0.00768 grams per liter of property.
A kind of preparation method of coloring agent, includes the following steps:
Weigh each component according to the following ratio: 94,0.0015~0.0215 grams of the acid red of 0.285~0.485 grams per liter/
The acid orange 74 of the grams per liter of acid black 1 68 and 0.032~0.052 of the acid black 172,0.00668~0.00868 grams per liter that rise;
The acid red 94, the acid black 172, the acid black 1 68 and the acid orange 74 are mixed in water, obtained
To the coloring agent.
It in one of the embodiments, further include the buffer for weighing 0.0005~0.0025 ml l, the buffer
In comprising mass percentage be 3~6% acetic acid and 28~35% sodium acetate, wherein by the acid red 94, the acid
The step of property is black 172, the acid black 1 68 and the acid orange 74 mix in water specifically: by the acid red 94, described
Acid black 172, the acid black 1 68, the acid orange 74 and the buffer mix in water.
It in one of the embodiments, further include the sodium sulphate for weighing 1~4 grams per liter, wherein by the acid red 94, institute
State the step of acid black 172, the acid black 1 68 and the acid orange 74 mix in water specifically: by the acid red 94,
The acid black 172, the acid black 1 68, the acid orange 74 and the sodium sulphate mix in water.
Coloring agent of the coloring agent of above-mentioned formula as metalwork can make the color and rose golden on the surface of metalwork
It is close.
Detailed description of the invention
Fig. 1 is the preparation flow figure of the coloring agent of an embodiment.
Specific embodiment
To facilitate the understanding of the present invention, a more comprehensive description of the invention is given in the following sections with reference to the relevant attached drawings.In attached drawing
Give preferred embodiment of the invention.But the invention can be realized in many different forms, however it is not limited to herein
Described embodiment.On the contrary, purpose of providing these embodiments is keeps the understanding to the disclosure more saturating
It is thorough comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
As shown in Figure 1, the coloring agent of an embodiment, which is a kind of rose golden coloring agent, can be used for metal
The dyeing of part, such as mobile phone shell etc..The coloring agent includes following component: the acid red 94,0.0015 of 0.285~0.485 grams per liter
The acid black 172 of~0.0215 grams per liter, the acid black 1 68 of 0.00668~0.00868 grams per liter, 0.032~0.052 grams per liter
The sodium sulphate of acid orange 74,0.0005~0.0025 ml l of buffer and 1~4 grams per liter.Wherein, solvent is water.
That is in 1 liter of coloring agent, acid red 94 is 0.285~0.485 gram, and acid black 172 is 0.0015~0.0215 gram, acid
Property black 168 for 0.00668~0.00868 gram, acid orange 74 be 0.032~0.052 gram, buffer be 0.0005~0.0025 milli
It rises, sodium sulphate is 1~4 gram.
Preferably, coloring agent includes following component: the acid black of the acid red 94 of 0.385 grams per liter, 0.0115 grams per liter
172, the acid black 1 68 of 0.00768 grams per liter, the acid orange 74 of 0.042 grams per liter, 0.0015 ml l of buffer and 1~4
The sodium sulphate of grams per liter.
Wherein, the molecular formula of acid red 94 is C20H2Cl4I4Na2O5.Wherein, acid red 94 can be wild red property dyestuff difficult to understand
139。
Wherein, the molecular formula of acid black 172 is C40H20CrN6O14S2.3Na。
Wherein, acid black 1 68 is also referred to as neutral black BL.Wherein, acid black 172 and acid black 1 68 can be difficult to understand wild by being added
The mode of black dyes 402 is added.
Wherein, the molecular formula of acid orange 74 is C16H11N5O7S。
It wherein, is 3~6% acetic acid and 28~35% sodium acetate comprising mass percentage in buffer.Buffer
It can be wild aluminium oxidation dye pH-5 buffer difficult to understand.Buffer also can make the color on the surface after metallochromy be more nearly rose
Rare gold.Wherein, the coloring agent of the buffer containing said ratio and sodium sulphate can make the face of the metallic surface after dyeing
Color is more uniform, is not in spot.
It is appreciated that in other embodiments, buffer also can be omitted.Sodium sulphate also can be omitted.
The coloring agent of above-mentioned formula enables to the surface of metalwork in rose golden, and has preferable glossiness.
As shown in Figure 1, the preparation method of the coloring agent of an embodiment, includes the following steps;
Step S110: each component is weighed according to the following ratio: the acid red 94,0.0015 of 0.285~0.485 grams per liter~
Acid black 1 68 and 0.032~0.052 grams per liter of the acid black 172 of 0.0215 grams per liter, 0.00668~0.00868 grams per liter
Acid orange 74.
Wherein, acid red 94 can be wild red property dyestuff 139 difficult to understand;Wherein, acid black 172 and acid black 1 68 can be Austria
Wild black dyes 402.Wherein, buffer can be wild aluminium oxidation dye pH-5 buffer difficult to understand.
Step S120: acid red 94, acid black 172, acid black 1 68 and acid orange 74 are mixed in water, dyed
Agent.
Further, further include the buffer for weighing 0.0005~0.0025 ml l, include quality percentage in buffer
Content is 3~6% acetic acid and 28~35% sodium acetate, wherein by acid red 94, acid black 172, acid black 1 68 and acid
The step of property orange 74 mixes in water specifically: by acid red 94, acid black 172, acid black 1 68, acid orange 74 and buffer
Yu Shuizhong mixing.
It further, further include the sodium sulphate for weighing 1~4 grams per liter, wherein by acid red 94, acid black 172, acid black
168 and acid orange 74 the step of being mixed in water specifically: by acid red 94, acid black 172, acid black 1 68, acid orange 74 and
Sodium sulphate mixes in water.
Wherein, the coloring agent containing said ratio buffer and sodium sulphate can make the color of the metallic surface after dyeing
It is more uniform, it is not in spot.
Preferably, in S110, each component is weighed according to the following ratio: the acid red 94 of 0.285~0.485 grams per liter,
The acid black 1 68 and 0.032~0.052 of the acid black 172 of 0.0015~0.0215 grams per liter, 0.00668~0.00868 grams per liter
The sodium sulphate of the acid orange 74 of grams per liter, 0.0005~0.0025 ml l of buffer and 1~4 grams per liter.It wherein, will be acid
Red 94, the step of acid black 172, acid black 1 68 and acid orange 74 mix in water specifically: by acid red 94, acid black
172, acid black 1 68, acid orange 74, buffer and copper sulphate mix in water.
Preferably, coloring agent includes following component: the acid black of the acid red 94 of 0.385 grams per liter, 0.0115 grams per liter
172, the acid black 1 68 of 0.00768 grams per liter, the acid orange 74 of 0.042 grams per liter, 0.0015 ml l of buffer and 1~4
The sodium sulphate of grams per liter.
The preparation method of above-mentioned coloring agent is simply easy to industrialized production.
The following are specific embodiment parts:
Embodiment 1
The preparation step of the present embodiment coloring agent is as follows:
(1) each component is weighed according to the following ratio: the acid black of the acid red 94 of 0.385 grams per liter, 0.0115 grams per liter
172, the acid orange 74 of the grams per liter of acid black 1 68 and 0.042 of 0.00768 grams per liter.
(2) acid red 94, acid black 172, acid black 1 68 and acid orange 74 are mixed in water, obtains coloring agent.
The step of colouring method of above-mentioned coloring agent, is as follows:
(1) metalwork is clamped on the hanger of transfer matic, metalwork is soaked at normal temperature first and is filled with degreaser
Degreasing tank in, impregnated 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser containing 35% organic acid sodium
Salt, 9% corrosion inhibiter and 12% complexing agent, wherein organic acid sodium salt is sodium citrate, and corrosion inhibiter is ethylene glycol, complexing agent
For sodium pyrophosphate.
(2) at normal temperature, the metalwork after oil removing is impregnated 20 seconds in the rinsing bowl for be filled with water, then at normal temperature will
Metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds.Wherein, nitric acid and mixing except film
The concentration for closing the nitric acid in liquid is 240g/L, except the concentration of film is 120g/L.
(3) at normal temperature, the metalwork of step (2) is impregnated 20 seconds in the rinsing bowl for be filled with water, then by metalwork
Under the conditions of 85 DEG C, impregnated 110 seconds in the chemical polishing bath for be filled with chemical polishing solution, to carry out chemical polishing.Wherein, change
Optical polishing liquid includes phosphoric acid, additive and sulfuric acid, and the mass ratio of phosphoric acid in chemical polishing solution, additive and sulfuric acid is 7:2:
1, wherein according to mass percentage, in additive containing 5% copper sulphate, 15% polyethylene glycol, 20% sulfuric acid and
40% phosphoric acid.
(4) metalwork after polishing impregnates to 20 seconds in the rinsing bowl for be filled with water at normal temperature, then at normal temperature
By metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds, then again at normal temperature by metal
Part impregnates 20 seconds in the rinsing bowl for be filled with water.Wherein, nitric acid and except in the mixed liquor of film, the concentration of nitric acid is
240g/L, except the concentration of film is 120g/L.
(5) under conditions of 19 DEG C, 15V, metalwork is aoxidized in anodizing solution at progress anodic oxidation in 2400 seconds
Reason, so that the surface of metalwork forms porous oxidation film.Wherein, anodizing solution includes sulfuric acid and aluminium ion, anodic oxidation
Aluminum ions concentration in liquid is 6 grams per liters.Wherein, the concentration of sulfuric acid is 180 grams per liters in anodizing solution.
(6) metalwork for being formed with oxidation film is impregnated 20 seconds in the rinsing bowl for be filled with water at normal temperature, then by shape
At there is the metalwork of oxidation film to be ultrasonically treated 180 seconds in activator under conditions of 50 DEG C, so that oxidation film activates.Wherein,
Activator includes water and solute, and according to mass percentage, solute includes 75% sodium citrate and 25% sodium acetate.
(7) metalwork of oxidation film impregnates in the rinsing bowl for be filled with water 20 seconds the formation after activation under room temperature,
The metalwork for being formed with oxidation film is impregnated 180 seconds in above-mentioned coloring agent again, so that oxidation film adsorbs coloring agent.
(8) there is the metalwork of oxidation film at normal temperature in the water for being filled with water the formation after dyeing that step (7) obtains
Impregnated 20 seconds in washing trough, then under conditions of 90 DEG C by the metalwork for being formed with oxidation film in the aqueous solution for being filled with hole sealing agent
2100 seconds progress sealing pores are impregnated in sealing of hole slot.Wherein, the concentration of hole sealing agent is 10 grams per liters in the aqueous solution of hole sealing agent.Its
In, according to mass percentage, hole sealing agent include 75% nickel acetate, 20% complexing agent and 5% surfactant.Complexing
Agent is citric acid.Surfactant is triethanolamine soap.
(9) metalwork of oxidation film cleans in the rinsing bowl for be filled with water 20 seconds the formation after sealing pores, then
The metalwork for being formed with oxidation film is impregnated 90 seconds in nitric acid under conditions of room temperature, wherein the concentration of nitric acid be 100 grams/
It rises.
(10) formation at normal temperature obtaining step (9) has the metalwork of oxidation film clear in the rinsing bowl for be filled with water
It washes 20 seconds, then is ultrasonically treated in water 30 seconds under conditions of 70 DEG C, then clean 30 seconds in water under conditions of 70 DEG C, finally
It is 1200 seconds dry in 70 DEG C, the metalwork after being dyed.Then the metalwork after dyeing is removed.
The color on the surface of the metalwork after testing the dyeing of the present embodiment using color difference meter.Wherein, L represents color depth
Shallowly;A is that positive number indicates partially red, negative number representation is partially green;B is that positive number indicates that Huang, negative number representation are partially blue partially.And observe the gold after dyeing
The surface for belonging to part whether there is spot, to illustrate whether the color on surface of the metalwork after dyeing is uniform.The dye of the present embodiment
The spot phenomenon on the surface of the color and metalwork after dyeing on the surface of the metalwork after color is shown in Table 1.
Embodiment 2
The preparation step of the present embodiment coloring agent is as follows:
(1) each component is weighed according to the following ratio: the acid black of the acid red 94 of 0.385 grams per liter, 0.0115 grams per liter
172, the acid black 1 68 of 0.00768 grams per liter, the acid orange 74 of 0.042 grams per liter and 0.0015 ml l of buffer.Wherein,
In buffer comprising mass percentage be 4% acetic acid and 32% sodium acetate.
(2) acid red 94, acid black 172, acid black 1 68, acid orange 74 and buffer are mixed in water, is dyed
Agent.
The step of colouring method of above-mentioned coloring agent, is as follows:
(1) metalwork is clamped on the hanger of transfer matic, metalwork is soaked at normal temperature first and is filled with degreaser
Degreasing tank in, impregnated 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser containing 35% organic acid sodium
Salt, 9% corrosion inhibiter and 12% complexing agent, wherein organic acid sodium salt is sodium citrate, and corrosion inhibiter is ethylene glycol, complexing agent
For sodium pyrophosphate.
(2) at normal temperature, the metalwork after oil removing is impregnated 20 seconds in the rinsing bowl for be filled with water, then at normal temperature will
Metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds.Wherein, nitric acid and mixing except film
The concentration for closing the nitric acid in liquid is 240g/L, except the concentration of film is 120g/L.
(3) at normal temperature, the metalwork of step (2) is impregnated 20 seconds in the rinsing bowl for be filled with water, then by metalwork
Under the conditions of 85 DEG C, impregnated 110 seconds in the chemical polishing bath for be filled with chemical polishing solution, to carry out chemical polishing.Wherein, change
Optical polishing liquid includes phosphoric acid, additive and sulfuric acid, and the mass ratio of phosphoric acid in chemical polishing solution, additive and sulfuric acid is 7:2:
1, wherein according to mass percentage, in additive containing 5% copper sulphate, 15% polyethylene glycol, 20% sulfuric acid and
40% phosphoric acid.
(4) metalwork after polishing impregnates to 20 seconds in the rinsing bowl for be filled with water at normal temperature, then at normal temperature
By metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds, then again at normal temperature by metal
Part impregnates 20 seconds in the rinsing bowl for be filled with water.Wherein, nitric acid and except in the mixed liquor of film, the concentration of nitric acid is
240g/L, except the concentration of film is 120g/L.
(5) under conditions of 19 DEG C, 15V, metalwork is aoxidized in anodizing solution at progress anodic oxidation in 2400 seconds
Reason, so that the surface of metalwork forms porous oxidation film.Wherein, anodizing solution includes sulfuric acid and aluminium ion, anodic oxidation
Aluminum ions concentration in liquid is 6 grams per liters.Wherein, the concentration of sulfuric acid is 180 grams per liters in anodizing solution.
(6) metalwork for being formed with oxidation film is impregnated 20 seconds in the rinsing bowl for be filled with water at normal temperature, then by shape
At there is the metalwork of oxidation film to be ultrasonically treated 180 seconds in activator under conditions of 50 DEG C, so that oxidation film activates.Wherein,
Activator includes water and solute, and according to mass percentage, solute includes 75% sodium citrate and 25% sodium acetate.
(7) metalwork of oxidation film impregnates in the rinsing bowl for be filled with water 20 seconds the formation after activation under room temperature,
The metalwork for being formed with oxidation film is impregnated 180 seconds in above-mentioned coloring agent again, so that oxidation film adsorbs coloring agent.
(8) there is the metalwork of oxidation film at normal temperature in the water for being filled with water the formation after dyeing that step (7) obtains
Impregnated 20 seconds in washing trough, then under conditions of 90 DEG C by the metalwork for being formed with oxidation film in the aqueous solution for being filled with hole sealing agent
2100 seconds progress sealing pores are impregnated in sealing of hole slot.Wherein, the concentration of hole sealing agent is 10 grams per liters in the aqueous solution of hole sealing agent.Its
In, according to mass percentage, hole sealing agent include 75% nickel acetate, 20% complexing agent and 5% surfactant.Complexing
Agent is citric acid.Surfactant is triethanolamine soap.
(9) metalwork of oxidation film cleans in the rinsing bowl for be filled with water 20 seconds the formation after sealing pores, then
The metalwork for being formed with oxidation film is impregnated 90 seconds in nitric acid under conditions of room temperature, wherein the concentration of nitric acid be 100 grams/
It rises.
(10) formation at normal temperature obtaining step (9) has the metalwork of oxidation film clear in the rinsing bowl for be filled with water
It washes 20 seconds, then is ultrasonically treated in water 30 seconds under conditions of 70 DEG C, then clean 30 seconds in water under conditions of 70 DEG C, finally
It is 1200 seconds dry in 70 DEG C, the metalwork after being dyed.Then the metalwork after dyeing is removed.
After the color and dyeing on the surface for obtaining the metalwork after the dyeing of the present embodiment using the identical method of embodiment 1
The spot phenomenon on surface of metalwork be shown in Table 1.
Embodiment 3
The preparation step of the present embodiment coloring agent is as follows:
(1) each component is weighed according to the following ratio: the acid black of the acid red 94 of 0.385 grams per liter, 0.0115 grams per liter
172, the sodium sulphate of the acid black 1 68 of 0.00768 grams per liter, the acid orange 74 of 0.042 grams per liter and 3 grams per liters.
(2) acid red 94, acid black 172, acid black 1 68, acid orange 74, buffer and sodium sulphate are mixed in water,
Obtain coloring agent.
The step of colouring method of above-mentioned coloring agent, is as follows:
(1) metalwork is clamped on the hanger of transfer matic, metalwork is soaked at normal temperature first and is filled with degreaser
Degreasing tank in, impregnated 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser containing 35% organic acid sodium
Salt, 9% corrosion inhibiter and 12% complexing agent, wherein organic acid sodium salt is sodium citrate, and corrosion inhibiter is ethylene glycol, complexing agent
For sodium pyrophosphate.
(2) at normal temperature, the metalwork after oil removing is impregnated 20 seconds in the rinsing bowl for be filled with water, then at normal temperature will
Metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds.Wherein, nitric acid and mixing except film
The concentration for closing the nitric acid in liquid is 240g/L, except the concentration of film is 120g/L.
(3) at normal temperature, the metalwork of step (2) is impregnated 20 seconds in the rinsing bowl for be filled with water, then by metalwork
Under the conditions of 85 DEG C, impregnated 110 seconds in the chemical polishing bath for be filled with chemical polishing solution, to carry out chemical polishing.Wherein, change
Optical polishing liquid includes phosphoric acid, additive and sulfuric acid, and the mass ratio of phosphoric acid in chemical polishing solution, additive and sulfuric acid is 7:2:
1, wherein according to mass percentage, in additive containing 5% copper sulphate, 15% polyethylene glycol, 20% sulfuric acid and
40% phosphoric acid.
(4) metalwork after polishing impregnates to 20 seconds in the rinsing bowl for be filled with water at normal temperature, then at normal temperature
By metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds, then again at normal temperature by metal
Part impregnates 20 seconds in the rinsing bowl for be filled with water.Wherein, nitric acid and except in the mixed liquor of film, the concentration of nitric acid is
240g/L, except the concentration of film is 120g/L.
(5) under conditions of 19 DEG C, 15V, metalwork is aoxidized in anodizing solution at progress anodic oxidation in 2400 seconds
Reason, so that the surface of metalwork forms porous oxidation film.Wherein, anodizing solution includes sulfuric acid and aluminium ion, anodic oxidation
Aluminum ions concentration in liquid is 6 grams per liters.Wherein, the concentration of sulfuric acid is 180 grams per liters in anodizing solution.
(6) metalwork for being formed with oxidation film is impregnated 20 seconds in the rinsing bowl for be filled with water at normal temperature, then by shape
At there is the metalwork of oxidation film to be ultrasonically treated 180 seconds in activator under conditions of 50 DEG C, so that oxidation film activates.Wherein,
Activator includes water and solute, and according to mass percentage, solute includes 75% sodium citrate and 25% sodium acetate.
(7) metalwork of oxidation film impregnates in the rinsing bowl for be filled with water 20 seconds the formation after activation under room temperature,
The metalwork for being formed with oxidation film is impregnated 180 seconds in above-mentioned coloring agent again, so that oxidation film adsorbs coloring agent.
(8) there is the metalwork of oxidation film at normal temperature in the water for being filled with water the formation after dyeing that step (7) obtains
Impregnated 20 seconds in washing trough, then under conditions of 90 DEG C by the metalwork for being formed with oxidation film in the aqueous solution for being filled with hole sealing agent
2100 seconds progress sealing pores are impregnated in sealing of hole slot.Wherein, the concentration of hole sealing agent is 10 grams per liters in the aqueous solution of hole sealing agent.Its
In, according to mass percentage, hole sealing agent include 75% nickel acetate, 20% complexing agent and 5% surfactant.Complexing
Agent is citric acid.Surfactant is triethanolamine soap.
(9) metalwork of oxidation film cleans in the rinsing bowl for be filled with water 20 seconds the formation after sealing pores, then
The metalwork for being formed with oxidation film is impregnated 90 seconds in nitric acid under conditions of room temperature, wherein the concentration of nitric acid be 100 grams/
It rises.
(10) formation at normal temperature obtaining step (9) has the metalwork of oxidation film clear in the rinsing bowl for be filled with water
It washes 20 seconds, then is ultrasonically treated in water 30 seconds under conditions of 70 DEG C, then clean 30 seconds in water under conditions of 70 DEG C, finally
It is 1200 seconds dry in 70 DEG C, the metalwork after being dyed.Then the metalwork after dyeing is removed.
After the color and dyeing on the surface for obtaining the metalwork after the dyeing of the present embodiment using the identical method of embodiment 1
The spot phenomenon on surface of metalwork be shown in Table 1.
Embodiment 4
The preparation step of the present embodiment coloring agent is as follows:
(1) each component is weighed according to the following ratio: the acid black of the acid red 94 of 0.385 grams per liter, 0.0115 grams per liter
172, the acid black 1 68 of 0.00768 grams per liter, the acid orange 74 of 0.042 grams per liter, 0.0015 ml l of buffer and 3 grams/
The sodium sulphate risen.It wherein, is 4% acetic acid and 32% sodium acetate comprising mass percentage in buffer.
(2) acid red 94, acid black 172, acid black 1 68, acid orange 74, buffer and sodium sulphate are mixed in water,
Obtain coloring agent.
The step of colouring method of above-mentioned coloring agent, is as follows:
(1) metalwork is clamped on the hanger of transfer matic, metalwork is soaked at normal temperature first and is filled with degreaser
Degreasing tank in, impregnated 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser containing 35% organic acid sodium
Salt, 9% corrosion inhibiter and 12% complexing agent, wherein organic acid sodium salt is sodium citrate, and corrosion inhibiter is ethylene glycol, complexing agent
For sodium pyrophosphate.
(2) at normal temperature, the metalwork after oil removing is impregnated 20 seconds in the rinsing bowl for be filled with water, then at normal temperature will
Metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds.Wherein, nitric acid and mixing except film
The concentration for closing the nitric acid in liquid is 240g/L, except the concentration of film is 120g/L.
(3) at normal temperature, the metalwork of step (2) is impregnated 20 seconds in the rinsing bowl for be filled with water, then by metalwork
Under the conditions of 85 DEG C, impregnated 110 seconds in the chemical polishing bath for be filled with chemical polishing solution, to carry out chemical polishing.Wherein, change
Optical polishing liquid includes phosphoric acid, additive and sulfuric acid, and the mass ratio of phosphoric acid in chemical polishing solution, additive and sulfuric acid is 7:2:
1, wherein according to mass percentage, in additive containing 5% copper sulphate, 15% polyethylene glycol, 20% sulfuric acid and
40% phosphoric acid.
(4) metalwork after polishing impregnates to 20 seconds in the rinsing bowl for be filled with water at normal temperature, then at normal temperature
By metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds, then again at normal temperature by metal
Part impregnates 20 seconds in the rinsing bowl for be filled with water.Wherein, nitric acid and except in the mixed liquor of film, the concentration of nitric acid is
240g/L, except the concentration of film is 120g/L.
(5) under conditions of 19 DEG C, 15V, metalwork is aoxidized in anodizing solution at progress anodic oxidation in 2400 seconds
Reason, so that the surface of metalwork forms porous oxidation film.Wherein, anodizing solution includes sulfuric acid and aluminium ion, anodic oxidation
Aluminum ions concentration in liquid is 6 grams per liters.Wherein, the concentration of sulfuric acid is 180 grams per liters in anodizing solution.
(6) metalwork for being formed with oxidation film is impregnated 20 seconds in the rinsing bowl for be filled with water at normal temperature, then by shape
At there is the metalwork of oxidation film to be ultrasonically treated 180 seconds in activator under conditions of 50 DEG C, so that oxidation film activates.Wherein,
Activator includes water and solute, and according to mass percentage, solute includes 75% sodium citrate and 25% sodium acetate.
(7) metalwork of oxidation film impregnates in the rinsing bowl for be filled with water 20 seconds the formation after activation under room temperature,
The metalwork for being formed with oxidation film is impregnated 180 seconds in above-mentioned coloring agent again, so that oxidation film adsorbs coloring agent.
(8) there is the metalwork of oxidation film at normal temperature in the water for being filled with water the formation after dyeing that step (7) obtains
Impregnated 20 seconds in washing trough, then under conditions of 90 DEG C by the metalwork for being formed with oxidation film in the aqueous solution for being filled with hole sealing agent
2100 seconds progress sealing pores are impregnated in sealing of hole slot.Wherein, the concentration of hole sealing agent is 10 grams per liters in the aqueous solution of hole sealing agent.Its
In, according to mass percentage, hole sealing agent include 75% nickel acetate, 20% complexing agent and 5% surfactant.Complexing
Agent is citric acid.Surfactant is triethanolamine soap.
(9) metalwork of oxidation film cleans in the rinsing bowl for be filled with water 20 seconds the formation after sealing pores, then
The metalwork for being formed with oxidation film is impregnated 90 seconds in nitric acid under conditions of room temperature, wherein the concentration of nitric acid be 100 grams/
It rises.
(10) formation at normal temperature obtaining step (9) has the metalwork of oxidation film clear in the rinsing bowl for be filled with water
It washes 20 seconds, then is ultrasonically treated in water 30 seconds under conditions of 70 DEG C, then clean 30 seconds in water under conditions of 70 DEG C, finally
It is 1200 seconds dry in 70 DEG C, the metalwork after being dyed.Then the metalwork after dyeing is removed.
After the color and dyeing on the surface for obtaining the metalwork after the dyeing of the present embodiment using the identical method of embodiment 1
The spot phenomenon on surface of metalwork be shown in Table 1.
Embodiment 5
The preparation step of the present embodiment coloring agent is as follows:
(1) each component is weighed according to the following ratio: the acid black of the acid red 94 of 0.285 grams per liter, 0.0015 grams per liter
172, the acid black 1 68 of 0.00868 grams per liter, the acid orange 74 of 0.032 grams per liter, 0.0005 ml l of buffer and 1 gram/
The sodium sulphate risen.It wherein, is 3% acetic acid and 35% sodium acetate comprising mass percentage in buffer.
(2) acid red 94, acid black 172, acid black 1 68, acid orange 74, buffer and sodium sulphate are mixed in water,
Obtain coloring agent.
The step of colouring method of above-mentioned coloring agent, is as follows:
(1) metalwork is clamped on the hanger of transfer matic, metalwork is soaked at normal temperature first and is filled with degreaser
Degreasing tank in, impregnated 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser containing 35% organic acid sodium
Salt, 9% corrosion inhibiter and 12% complexing agent, wherein organic acid sodium salt is sodium citrate, and corrosion inhibiter is ethylene glycol, complexing agent
For sodium pyrophosphate.
(2) at normal temperature, the metalwork after oil removing is impregnated 20 seconds in the rinsing bowl for be filled with water, then at normal temperature will
Metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds.Wherein, nitric acid and mixing except film
The concentration for closing the nitric acid in liquid is 240g/L, except the concentration of film is 120g/L.
(3) at normal temperature, the metalwork of step (2) is impregnated 20 seconds in the rinsing bowl for be filled with water, then by metalwork
Under the conditions of 85 DEG C, impregnated 110 seconds in the chemical polishing bath for be filled with chemical polishing solution, to carry out chemical polishing.Wherein, change
Optical polishing liquid includes phosphoric acid, additive and sulfuric acid, and the mass ratio of phosphoric acid in chemical polishing solution, additive and sulfuric acid is 7:2:
1, wherein according to mass percentage, in additive containing 5% copper sulphate, 15% polyethylene glycol, 20% sulfuric acid and
40% phosphoric acid.
(4) metalwork after polishing impregnates to 20 seconds in the rinsing bowl for be filled with water at normal temperature, then at normal temperature
By metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds, then again at normal temperature by metal
Part impregnates 20 seconds in the rinsing bowl for be filled with water.Wherein, nitric acid and except in the mixed liquor of film, the concentration of nitric acid is
240g/L, except the concentration of film is 120g/L.
(5) under conditions of 19 DEG C, 15V, metalwork is aoxidized in anodizing solution at progress anodic oxidation in 2400 seconds
Reason, so that the surface of metalwork forms porous oxidation film.Wherein, anodizing solution includes sulfuric acid and aluminium ion, anodic oxidation
Aluminum ions concentration in liquid is 6 grams per liters.Wherein, the concentration of sulfuric acid is 180 grams per liters in anodizing solution.
(6) metalwork for being formed with oxidation film is impregnated 20 seconds in the rinsing bowl for be filled with water at normal temperature, then by shape
At there is the metalwork of oxidation film to be ultrasonically treated 180 seconds in activator under conditions of 50 DEG C, so that oxidation film activates.Wherein,
Activator includes water and solute, and according to mass percentage, solute includes 75% sodium citrate and 25% sodium acetate.
(7) metalwork of oxidation film impregnates in the rinsing bowl for be filled with water 20 seconds the formation after activation under room temperature,
The metalwork for being formed with oxidation film is impregnated 180 seconds in above-mentioned coloring agent again, so that oxidation film adsorbs coloring agent.
(8) there is the metalwork of oxidation film at normal temperature in the water for being filled with water the formation after dyeing that step (7) obtains
Impregnated 20 seconds in washing trough, then under conditions of 90 DEG C by the metalwork for being formed with oxidation film in the aqueous solution for being filled with hole sealing agent
2100 seconds progress sealing pores are impregnated in sealing of hole slot.Wherein, the concentration of hole sealing agent is 10 grams per liters in the aqueous solution of hole sealing agent.Its
In, according to mass percentage, hole sealing agent include 75% nickel acetate, 20% complexing agent and 5% surfactant.Complexing
Agent is citric acid.Surfactant is triethanolamine soap.
(9) metalwork of oxidation film cleans in the rinsing bowl for be filled with water 20 seconds the formation after sealing pores, then
The metalwork for being formed with oxidation film is impregnated 90 seconds in nitric acid under conditions of room temperature, wherein the concentration of nitric acid be 100 grams/
It rises.
(10) formation at normal temperature obtaining step (9) has the metalwork of oxidation film clear in the rinsing bowl for be filled with water
It washes 20 seconds, then is ultrasonically treated in water 30 seconds under conditions of 70 DEG C, then clean 30 seconds in water under conditions of 70 DEG C, finally
It is 1200 seconds dry in 70 DEG C, the metalwork after being dyed.Then the metalwork after dyeing is removed.
After the color and dyeing on the surface for obtaining the metalwork after the dyeing of the present embodiment using the identical method of embodiment 1
The spot phenomenon on surface of metalwork be shown in Table 1.
Embodiment 6
The preparation step of the present embodiment coloring agent is as follows:
(1) each component is weighed according to the following ratio: the acid black of the acid red 94 of 0.485 grams per liter, 0.0215 grams per liter
172, the acid black 1 68 of 0.00668 grams per liter, the acid orange 74 of 0.052 grams per liter, 0.0025 ml l of buffer and 4 grams/
The sodium sulphate risen.It wherein, is 6% acetic acid and 28% sodium acetate comprising mass percentage in buffer.
(2) acid red 94, acid black 172, acid black 1 68, acid orange 74, buffer and sodium sulphate are mixed in water,
Obtain coloring agent.
The step of colouring method of above-mentioned coloring agent, is as follows:
(1) metalwork is clamped on the hanger of transfer matic, metalwork is soaked at normal temperature first and is filled with degreaser
Degreasing tank in, impregnated 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser containing 35% organic acid sodium
Salt, 9% corrosion inhibiter and 12% complexing agent, wherein organic acid sodium salt is sodium citrate, and corrosion inhibiter is ethylene glycol, complexing agent
For sodium pyrophosphate.
(2) at normal temperature, the metalwork after oil removing is impregnated 20 seconds in the rinsing bowl for be filled with water, then at normal temperature will
Metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds.Wherein, nitric acid and mixing except film
The concentration for closing the nitric acid in liquid is 240g/L, except the concentration of film is 120g/L.
(3) at normal temperature, the metalwork of step (2) is impregnated 20 seconds in the rinsing bowl for be filled with water, then by metalwork
Under the conditions of 85 DEG C, impregnated 110 seconds in the chemical polishing bath for be filled with chemical polishing solution, to carry out chemical polishing.Wherein, change
Optical polishing liquid includes phosphoric acid, additive and sulfuric acid, and the mass ratio of phosphoric acid in chemical polishing solution, additive and sulfuric acid is 7:2:
1, wherein according to mass percentage, in additive containing 5% copper sulphate, 15% polyethylene glycol, 20% sulfuric acid and
40% phosphoric acid.
(4) metalwork after polishing impregnates to 20 seconds in the rinsing bowl for be filled with water at normal temperature, then at normal temperature
By metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds, then again at normal temperature by metal
Part impregnates 20 seconds in the rinsing bowl for be filled with water.Wherein, nitric acid and except in the mixed liquor of film, the concentration of nitric acid is
240g/L, except the concentration of film is 120g/L.
(5) under conditions of 19 DEG C, 15V, metalwork is aoxidized in anodizing solution at progress anodic oxidation in 2400 seconds
Reason, so that the surface of metalwork forms porous oxidation film.Wherein, anodizing solution includes sulfuric acid and aluminium ion, anodic oxidation
Aluminum ions concentration in liquid is 6 grams per liters.Wherein, the concentration of sulfuric acid is 180 grams per liters in anodizing solution.
(6) metalwork for being formed with oxidation film is impregnated 20 seconds in the rinsing bowl for be filled with water at normal temperature, then by shape
At there is the metalwork of oxidation film to be ultrasonically treated 180 seconds in activator under conditions of 50 DEG C, so that oxidation film activates.Wherein,
Activator includes water and solute, and according to mass percentage, solute includes 75% sodium citrate and 25% sodium acetate.
(7) metalwork of oxidation film impregnates in the rinsing bowl for be filled with water 20 seconds the formation after activation under room temperature,
The metalwork for being formed with oxidation film is impregnated 180 seconds in above-mentioned coloring agent again, so that oxidation film adsorbs coloring agent.
(8) there is the metalwork of oxidation film at normal temperature in the water for being filled with water the formation after dyeing that step (7) obtains
Impregnated 20 seconds in washing trough, then under conditions of 90 DEG C by the metalwork for being formed with oxidation film in the aqueous solution for being filled with hole sealing agent
2100 seconds progress sealing pores are impregnated in sealing of hole slot.Wherein, the concentration of hole sealing agent is 10 grams per liters in the aqueous solution of hole sealing agent.Its
In, according to mass percentage, hole sealing agent include 75% nickel acetate, 20% complexing agent and 5% surfactant.Complexing
Agent is citric acid.Surfactant is triethanolamine soap.
(9) metalwork of oxidation film cleans in the rinsing bowl for be filled with water 20 seconds the formation after sealing pores, then
The metalwork for being formed with oxidation film is impregnated 90 seconds in nitric acid under conditions of room temperature, wherein the concentration of nitric acid be 100 grams/
It rises.
(10) formation at normal temperature obtaining step (9) has the metalwork of oxidation film clear in the rinsing bowl for be filled with water
It washes 20 seconds, then is ultrasonically treated in water 30 seconds under conditions of 70 DEG C, then clean 30 seconds in water under conditions of 70 DEG C, finally
It is 1200 seconds dry in 70 DEG C, the metalwork after being dyed.Then the metalwork after dyeing is removed.
After the color and dyeing on the surface for obtaining the metalwork after the dyeing of the present embodiment using the identical method of embodiment 1
The spot phenomenon on surface of metalwork be shown in Table 1.
Comparative example 1
The coloring agent of comparative example 1 are as follows: the acid red 94 of 0.255 grams per liter, the acid black 172 of 0.0235 grams per liter, 0.00788
The acid black 1 68 of grams per liter, the acid orange 74 of 0.052 grams per liter, the buffer of 0.0015 milliliter/L and the sodium sulphate of 2.5 grams per liters.
It wherein, is 4% acetic acid and 32% sodium acetate comprising mass percentage in buffer.
The step of colouring method of above-mentioned coloring agent, is as follows:
(1) metalwork is clamped on the hanger of transfer matic, metalwork is soaked at normal temperature first and is filled with degreaser
Degreasing tank in, impregnated 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser containing 35% organic acid sodium
Salt, 9% corrosion inhibiter and 12% complexing agent, wherein organic acid sodium salt is sodium citrate, and corrosion inhibiter is ethylene glycol, complexing agent
For sodium pyrophosphate.
(2) at normal temperature, the metalwork after oil removing is impregnated 20 seconds in the rinsing bowl for be filled with water, then at normal temperature will
Metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds.Wherein, nitric acid and mixing except film
The concentration for closing the nitric acid in liquid is 240g/L, except the concentration of film is 120g/L.
(3) at normal temperature, the metalwork of step (2) is impregnated 20 seconds in the rinsing bowl for be filled with water, then by metalwork
Under the conditions of 85 DEG C, impregnated 110 seconds in the chemical polishing bath for be filled with chemical polishing solution, to carry out chemical polishing.Wherein, change
Optical polishing liquid includes phosphoric acid, additive and sulfuric acid, and the mass ratio of phosphoric acid in chemical polishing solution, additive and sulfuric acid is 7:2:
1, wherein according to mass percentage, in additive containing 5% copper sulphate, 15% polyethylene glycol, 20% sulfuric acid and
40% phosphoric acid.
(4) metalwork after polishing impregnates to 20 seconds in the rinsing bowl for be filled with water at normal temperature, then at normal temperature
By metalwork in be filled with nitric acid and neutralization chamber except the mixed liquor of film in mouth impregnate 60 seconds, then again at normal temperature by metal
Part impregnates 20 seconds in the rinsing bowl for be filled with water.Wherein, nitric acid and except in the mixed liquor of film, the concentration of nitric acid is
240g/L, except the concentration of film is 120g/L.
(5) under conditions of 19 DEG C, 15V, metalwork is aoxidized in anodizing solution at progress anodic oxidation in 2400 seconds
Reason, so that the surface of metalwork forms porous oxidation film.Wherein, anodizing solution includes sulfuric acid and aluminium ion, anodic oxidation
Aluminum ions concentration in liquid is 6 grams per liters.Wherein, the concentration of sulfuric acid is 180 grams per liters in anodizing solution.
(6) metalwork for being formed with oxidation film is impregnated 20 seconds in the rinsing bowl for be filled with water at normal temperature, then by shape
At there is the metalwork of oxidation film to be ultrasonically treated 180 seconds in activator under conditions of 50 DEG C, so that oxidation film activates.Wherein,
Activator includes water and solute, and according to mass percentage, solute includes 75% sodium citrate and 25% sodium acetate.
(7) metalwork of oxidation film impregnates in the rinsing bowl for be filled with water 20 seconds the formation after activation under room temperature,
The metalwork for being formed with oxidation film is impregnated 180 seconds in above-mentioned coloring agent again, so that oxidation film adsorbs coloring agent.
(8) there is the metalwork of oxidation film at normal temperature in the water for being filled with water the formation after dyeing that step (7) obtains
Impregnated 20 seconds in washing trough, then under conditions of 90 DEG C by the metalwork for being formed with oxidation film in the aqueous solution for being filled with hole sealing agent
2100 seconds progress sealing pores are impregnated in sealing of hole slot.Wherein, the concentration of hole sealing agent is 10 grams per liters in the aqueous solution of hole sealing agent.Its
In, according to mass percentage, hole sealing agent include 75% nickel acetate, 20% complexing agent and 5% surfactant.Complexing
Agent is citric acid.Surfactant is triethanolamine soap.
(9) metalwork of oxidation film cleans in the rinsing bowl for be filled with water 20 seconds the formation after sealing pores, then
The metalwork for being formed with oxidation film is impregnated 90 seconds in nitric acid under conditions of room temperature, wherein the concentration of nitric acid be 100 grams/
It rises.
(10) formation at normal temperature obtaining step (9) has the metalwork of oxidation film clear in the rinsing bowl for be filled with water
It washes 20 seconds, then is ultrasonically treated in water 30 seconds under conditions of 70 DEG C, then clean 30 seconds in water under conditions of 70 DEG C, finally
It is 1200 seconds dry in 70 DEG C, the metalwork after being dyed.Then the metalwork after dyeing is removed.
After the color and dyeing on the surface for obtaining the metalwork after the dyeing of comparative example 1 using the identical method of embodiment 1
The spot phenomenon on surface of metalwork be shown in Table 1.
Table 1 is the color on surface for using the metalwork after the staining reagent of Examples 1 to 6 and comparative example 1, rose gold
The spot phenomenon on the surface of the color and metalwork after dyeing of color.
Table 1
From table 1 it follows that it is seen from the above data that a value and b value on the surface of the metalwork of Examples 1 to 6
For comparative example 1, differ smaller with a value of rose golden and b value.And as can be seen that working as from Examples 1 to 6
When also containing buffer and sodium sulphate in coloring agent, the surface immaculate of metalwork, more uniformly.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (6)
1. a kind of coloring agent, which is characterized in that the coloring agent is used for the dyeing of metalwork, and the coloring agent includes such as the following group
Point: the acid red 94 of 0.285~0.485 grams per liter, the acid black 172 of 0.0015~0.0215 grams per liter, 0.00668~
The acid black 1 68 of 0.00868 grams per liter, the acid orange 74 of 0.032~0.052 grams per liter, 0.0005~0.0025 ml l slow
The sodium sulphate and water of fliud flushing, 1~4 grams per liter, in the buffer comprising mass percentage be 3~6% acetic acid and 28~
35% sodium acetate.
2. coloring agent according to claim 1, which is characterized in that including following component: the acid red 94 of 0.385 grams per liter,
The acid black 172 of 0.0115 grams per liter, the acid black 1 68 of 0.00768 grams per liter, the acid orange 74 of 0.042 grams per liter, 0.0015 milli
Rise/liter buffer, 1~4 grams per liter sodium sulphate and water.
3. coloring agent according to claim 1, which is characterized in that the coloring agent includes following component: 0.385 grams per liter
Acid red 94, the acid black 172 of 0.0115 grams per liter, the acid black 1 68 of 0.00768 grams per liter, 0.042 grams per liter acid orange
74, the sodium sulphate and water of 0.0015 ml l of buffer, 3 grams per liters, wherein in buffer is comprising mass percentage
4% acetic acid and 32% sodium acetate.
4. coloring agent according to claim 1, which is characterized in that the coloring agent includes following component: 0.285 grams per liter
Acid red 94, the acid black 172 of 0.0115 grams per liter, the acid black 1 68 of 0.00868 grams per liter, 0.032 grams per liter acid orange
74, the sodium sulphate and water of 0.0005 ml l of buffer, 1 grams per liter, wherein in buffer is comprising mass percentage
3% acetic acid and 35% sodium acetate.
5. coloring agent according to claim 1, which is characterized in that the coloring agent includes following component: 0.485 grams per liter
Acid red 94, the acid black 172 of 0.0215 grams per liter, the acid black 1 68 of 0.00668 grams per liter, 0.052 grams per liter acid orange
74, the sodium sulphate and water of 0.0025 ml l of buffer, 4 grams per liters, wherein in buffer is comprising mass percentage
6% acetic acid and 28% sodium acetate.
6. a kind of preparation method of coloring agent as described in claim 1, which comprises the steps of:
Weigh each component according to the following ratio: the acid red 94 of 0.285~0.485 grams per liter, 0.0015~0.0215 grams per liter
Acid black 172, the acid black 1 68 of 0.00668~0.00868 grams per liter, the acid orange 74 of 0.032~0.052 grams per liter, 0.0005
The sodium sulphate of~0.0025 ml l of buffer and 1~4 grams per liter, in the buffer comprising mass percentage be 3~
6% acetic acid and 28~35% sodium acetate;
By the acid red 94, the acid black 172, the acid black 1 68, the acid orange 74, the buffer and described
Sodium sulphate mixes in water, obtains the coloring agent.
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