CN105908236A - Coloring agent and preparation method thereof - Google Patents

Coloring agent and preparation method thereof Download PDF

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Publication number
CN105908236A
CN105908236A CN201610309064.9A CN201610309064A CN105908236A CN 105908236 A CN105908236 A CN 105908236A CN 201610309064 A CN201610309064 A CN 201610309064A CN 105908236 A CN105908236 A CN 105908236A
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acid
metalwork
seconds
grams per
water
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CN201610309064.9A
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CN105908236B (en
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王天宇
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Guangdong Evenwin Precision Technology Co Ltd
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Guangdong Evenwin Precision Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation

Abstract

The invention relates to a coloring agent and a preparation method thereof. The coloring agent is prepared from 0.285-0.485 g/L of acid red 94, 0.0015-0.0215 g/L of acid black 172, 0.00668-0.00868 g/L of acid black 168 and 0.032-0.052 g/L of acid orange 74. The coloring agent can make the color of the surface of a metal piece close to the rose gold color.

Description

Stain and preparation method thereof
Technical field
The present invention relates to a kind of stain and preparation method thereof.
Background technology
Metal product, such as aluminium alloy, magnesium alloy or titanium alloy, typically can carry out anodized, with Its surface forms wearability preferably anode oxide film.For making the variation of product surface color, after anodic oxidation Product can be carried out dyeing process or spray treatment.Owing to rose golden is the most attractive in appearance, it is loved by the people, And the color of the metal surface that the colouring method of current rose golden obtains differs bigger with rose golden.
Summary of the invention
In consideration of it, be necessary to provide a kind of stain, use this stain make metalwork surface color more Add close to rose golden.
Additionally, also provide for the preparation method of a kind of stain.
A kind of stain, including following component: the Xylene Red 94,0.0015~0.0215 of 0.285~0.485 grams per liter The acid black 172 of grams per liter, 0.00668~0.00868 acid black 1 68 and 0.032~0.052 grams per liter of grams per liter Acid orange 74.
Wherein in an embodiment, described stain also includes the buffer of 0.0005~0.0025 ml l, Comprising weight/mass percentage composition in described buffer is 3~the acetic acid of 6% and 28~the sodium acetate of 35%.
Wherein in an embodiment, described stain also includes the sodium sulfate of 1~4 grams per liters.
Wherein in an embodiment, including following component: the Xylene Red of 0.385 grams per liter 94,0.0115 gram/ The acid black 172 that rises, the acid orange 74 of acid black 1 68 and 0.042 grams per liter of 0.00768 grams per liter.
The preparation method of a kind of stain, comprises the steps:
Each component is weighed: the Xylene Red 94,0.0015~0.0215 of 0.285~0.485 grams per liter according to following proportioning The acid black 172 of grams per liter, 0.00668~0.00868 acid black 1 68 and 0.032~0.052 grams per liter of grams per liter Acid orange 74;
By described Xylene Red 94, described acid black 172, described acid black 1 68 and described acid orange 74 in water Middle mixing, obtains described stain.
Wherein in an embodiment, also include the buffer weighing 0.0005~0.0025 ml l, described slow Rush that to comprise weight/mass percentage composition in liquid be 3~the acetic acid of 6% and 28~the sodium acetate of 35%, wherein, by described acid The step that property is red 94, described acid black 172, described acid black 1 68 and described acid orange 74 mix in water Particularly as follows: by described Xylene Red 94, described acid black 172, described acid black 1 68, described acid orange 74 Mix in water with described buffer.
Wherein in an embodiment, also include the sodium sulfate weighing 1~4 grams per liters, wherein, by described acidity The step tool that red 94, described acid black 172, described acid black 1 68 and described acid orange 74 mix in water Body is: by described Xylene Red 94, described acid black 172, described acid black 1 68, described acid orange 74 and Described sodium sulfate mixes in water.
The stain of above-mentioned formula is as the stain of metalwork, it is possible to make color and the rose on the surface of metalwork Rare gold is close.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of the stain of an embodiment.
Detailed description of the invention
For the ease of understanding the present invention, below with reference to relevant drawings, the present invention is described more fully. Accompanying drawing gives the preferred embodiment of the present invention.But, the present invention can come in many different forms Realize, however it is not limited to embodiment described herein.On the contrary, provide the purpose of these embodiments be make right The understanding of the disclosure is more thorough comprehensively.
Unless otherwise defined, all of technology used herein and scientific terminology and the technology belonging to the present invention The implication that the technical staff in field is generally understood that is identical.The art used the most in the description of the invention Language is intended merely to describe the purpose of specific embodiment, it is not intended that in limiting the present invention.
As it is shown in figure 1, the stain of an embodiment, this stain is a kind of rose golden stain, can For the dyeing of metalwork, such as mobile phone shell etc..This stain includes following component: 0.285~0.485 gram/ The acid black 172 of Xylene Red 94,0.0015~0.0215 grams per liter that rises, 0.00668~0.00868 acid of grams per liter The property acid orange 74 of black 168,0.032~0.052 grams per liter, 0.0005~0.0025 buffer and 1~4 of ml l The sodium sulfate of grams per liter.Wherein, solvent is water.
In i.e. 1 liter stain, Xylene Red 94 is 0.285~0.485 gram, and acid black 172 is 0.0015~0.0215 Gram, acid black 1 68 is 0.00668~0.00868 gram, acid orange 74 is 0.032~0.052 gram, and buffer is 0.0005~0.0025 milliliter, sodium sulfate is 1~4 gram.
Preferably, stain includes following component: the acid of Xylene Red 94,0.0115 grams per liter of 0.385 grams per liter The property acid orange 74 of acid black 1 68,0.042 grams per liter of black 172,0.00768 grams per liter, 0.0015 milliliter/ The buffer risen and the sodium sulfate of 1~4 grams per liters.
Wherein, the molecular formula of Xylene Red 94 is C20H2Cl4I4Na2O5.Wherein, Xylene Red 94 can be difficult to understand Wild red property dyestuff 139.
Wherein, the molecular formula of acid black 172 is C40H20CrN6O14S2.3Na。
Wherein, acid black 1 68 also referred to as neutral black BL.Wherein, acid black 172 and acid black 1 68 can lead to The mode crossing addition wild black dyes 402 difficult to understand adds.
Wherein, the molecular formula of acid orange 74 is C16H11N5O7S。
Wherein, comprising weight/mass percentage composition in buffer is 3~the acetic acid of 6% and 28~the sodium acetate of 35%.Slow Rushing liquid can be wild aluminum oxidation dyestuff pH-5 buffer difficult to understand.Buffer also is able to the surface after making metallochromy Color is more nearly rose golden.Wherein, the stain of buffer containing said ratio and sodium sulfate can The color making the metallic surface after dyeing is more uniform, does not haves speckle.
Being appreciated that in other embodiments, buffer can also omit.Sodium sulfate can also omit.
It is rose golden that the stain of above-mentioned formula enables to the surface of metalwork, and has preferable gloss Degree.
As it is shown in figure 1, the preparation method of the stain of an embodiment, comprise the steps;
Step S110: weigh each component according to following proportioning: the Xylene 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 acid black 1 68 and of grams per liter The acid orange 74 of 0.032~0.052 grams per liter.
Wherein, Xylene Red 94 can be wild red property dyestuff 139 difficult to understand;Wherein, acid black 172 and acid black 1 68 It can be wild black dyes 402 difficult to understand.Wherein, buffer can be wild aluminum oxidation dyestuff pH-5 buffer difficult to understand.
Step S120: Xylene Red 94, acid black 172, acid black 1 68 and acid orange 74 are mixed in water, Obtain stain.
Further, also include the buffer weighing 0.0005~0.0025 ml l, buffer comprises quality Percentage composition is 3~the acetic acid of 6% and 28~the sodium acetate of 35%, wherein, by Xylene Red 94, acid black 172, Step that acid black 1 68 and acid orange 74 mix in water particularly as follows: by Xylene Red 94, acid black 172, Acid black 1 68, acid orange 74 and buffer mix in water.
Further, also include the sodium sulfate weighing 1~4 grams per liters, wherein, by Xylene Red 94, acid black 172, Step that acid black 1 68 and acid orange 74 mix in water particularly as follows: by Xylene Red 94, acid black 172, Acid black 1 68, acid orange 74 and sodium sulfate mix in water.
Wherein, the metallic surface after the stain containing said ratio buffer and sodium sulfate can make dyeing Color more uniform, do not have speckle.
Preferably, in S110, weigh each component according to following proportioning: the Xylene Red of 0.285~0.485 grams per liter 94, the acid black 172 of 0.0015~0.0215 grams per liter, 0.00668~0.00868 acid black 1 68 and of grams per liter The acid orange 74 of 0.032~0.052 grams per liter, 0.0005~0.0025 ml l buffer and the sulfur of 1~4 grams per liters Acid sodium.Wherein, Xylene Red 94, acid black 172, acid black 1 68 and acid orange 74 are mixed in water Step is particularly as follows: by Xylene Red 94, acid black 172, acid black 1 68, acid orange 74, buffer and sulfur Acid copper mixes in water.
Preferably, stain includes following component: the acid of Xylene Red 94,0.0115 grams per liter of 0.385 grams per liter The property acid orange 74 of acid black 1 68,0.042 grams per liter of black 172,0.00768 grams per liter, 0.0015 milliliter/ The buffer risen and the sodium sulfate of 1~4 grams per liters.
The preparation method of above-mentioned stain is simply prone to industrialized production.
It is below specific embodiment part:
Embodiment 1
The preparation process of the present embodiment stain is as follows:
(1) each component is weighed according to following proportioning: the acid of Xylene Red 94,0.0115 grams per liter of 0.385 grams per liter The acid orange 74 of acid black 1 68 and 0.042 grams per liter of black 172,0.00768 grams per liter of property.
(2) Xylene Red 94, acid black 172, acid black 1 68 and acid orange 74 are mixed in water, To stain.
The step of the colouring method of above-mentioned stain is as follows:
(1) metalwork is clamped on the hanger of transfer matic, first metalwork is soaked at normal temperatures and is filled with In the degreasing tank of degreaser, soak 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser Containing the organic acid sodium salt of 35%, the corrosion inhibiter of 9% and the chelating agent of 12%, wherein, organic acid sodium salt is lemon Lemon acid sodium, corrosion inhibiter is ethylene glycol, and chelating agent is sodium pyrophosphate.
(2) at normal temperatures, the metalwork after oil removing is soaked 20 seconds in the rinsing bowl be filled with water, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent.Its In, the concentration of the nitric acid in the mixed liquor of nitric acid and membrane removal agent is 240g/L, and the concentration of membrane removal agent is 120g/L.
(3) at normal temperatures, the metalwork of step (2) is soaked 20 seconds in the rinsing bowl be filled with water, Again by metalwork under the conditions of 85 DEG C, soak 110 seconds in the chemical polishing bath be filled with chemical polishing solution, To carry out chemical polishing.Wherein, chemical polishing solution includes phosphoric acid, additive and sulphuric acid, and chemical polishing solution In the mass ratio of phosphoric acid, additive and sulphuric acid be 7:2:1, wherein, according to weight/mass percentage composition, additive In containing 5% copper sulfate, the Polyethylene Glycol of 15%, the sulphuric acid of 20% and the phosphoric acid of 40%.
(4) metalwork after polishing is soaked at normal temperatures in the rinsing bowl be filled with water 20 seconds, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent, connect And the most at normal temperatures metalwork is soaked 20 seconds in the rinsing bowl be filled with water.Wherein, nitric acid and membrane removal In the mixed liquor of agent, the concentration of nitric acid is 240g/L, and the concentration of membrane removal agent is 120g/L.
(5) 19 DEG C, under conditions of 15V, metalwork is aoxidized 2400 seconds in anodizing solution and carries out Anodized, so that the surface of metalwork forms the oxide-film of porous.Wherein, anodizing solution includes Sulphuric acid and aluminium ion, the aluminum ions concentration in anodizing solution is 6 grams per liters.Wherein, in anodizing solution The concentration of sulphuric acid is 180 grams per liters.
(6) metalwork that will be formed with oxide-film at normal temperatures soaks 20 seconds in the rinsing bowl be filled with water, Will be formed with again the metalwork of oxide-film under conditions of 50 DEG C in activator supersound process 180 seconds so that Oxide-film activates.Wherein, activator includes water and solute, and according to weight/mass percentage composition, solute includes 75% Sodium citrate and the sodium acetate of 25%.
(7) under room temperature, the metalwork being formed with oxide-film after activation is soaked in the rinsing bowl be filled with water 20 seconds, then the metalwork that will be formed with oxide-film soaks 180 seconds in above-mentioned stain, so that oxide-film is inhaled Attached stain.
(8) metalwork being formed with oxide-film after dyeing step (7) obtained is at normal temperatures in taking up Have in the rinsing bowl of water and soak 20 seconds, then under conditions of 90 DEG C, will be formed with the metalwork of oxide-film in taking up Have hole sealing agent aqueous solution sealing of hole groove in soak within 2100 seconds, carry out sealing pores.Wherein, hole sealing agent is water-soluble In liquid, the concentration of hole sealing agent is 10 grams per liters.Wherein, according to weight/mass percentage composition, hole sealing agent includes the vinegar of 75% Acid nickel, the chelating agent of 20% and the surfactant of 5%.Chelating agent is citric acid.Surfactant is three second Alcohol amine soap.
(9) metalwork being formed with oxide-film after sealing pores is cleaned 20 in the rinsing bowl be filled with water Second, then the metalwork that will be formed with oxide-film under conditions of room temperature soaks 90 seconds, wherein, nitre in nitric acid The concentration of acid is 100 grams per liters.
(10) metalwork being formed with oxide-film step (9) obtained at normal temperatures is in the water being filled with water Washing trough is cleaned 20 seconds, then under conditions of 70 DEG C in water supersound process 30 seconds, then the condition at 70 DEG C Under in water clean 30 seconds, finally in 70 DEG C be dried 1200 seconds, the metalwork after being dyeed.Then will Metalwork after dyeing takes off.
Employing color difference meter tests the color on the surface of the metalwork after the dyeing of the present embodiment.Wherein, L represents face Color depth is shallow;A is that positive number represents the reddest, negative number representation is the greenest;B is that positive number represents partially yellow, negative number representation is the most blue. And whether the surface observing the metalwork after dyeing exists speckle, the surface of the metalwork after dyeing with explanation Color is the most uniform.Metalwork after the color on the surface of the metalwork after the dyeing of the present embodiment and dyeing The speckle phenomenon on surface is shown in Table 1.
Embodiment 2
The preparation process of the present embodiment stain is as follows:
(1) each component is weighed according to following proportioning: the acid of Xylene Red 94,0.0115 grams per liter of 0.385 grams per liter The acid orange 74 of acid black 1 68,0.042 grams per liter of black 172,0.00768 grams per liter of property and 0.0015 milliliter/ The buffer risen.Wherein, buffer comprises acetic acid and the sodium acetate of 32% that weight/mass percentage composition is 4%.
(2) Xylene Red 94, acid black 172, acid black 1 68, acid orange 74 and buffer are mixed in water Close, obtain stain.
The step of the colouring method of above-mentioned stain is as follows:
(1) metalwork is clamped on the hanger of transfer matic, first metalwork is soaked at normal temperatures and is filled with In the degreasing tank of degreaser, soak 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser Containing the organic acid sodium salt of 35%, the corrosion inhibiter of 9% and the chelating agent of 12%, wherein, organic acid sodium salt is lemon Lemon acid sodium, corrosion inhibiter is ethylene glycol, and chelating agent is sodium pyrophosphate.
(2) at normal temperatures, the metalwork after oil removing is soaked 20 seconds in the rinsing bowl be filled with water, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent.Its In, the concentration of the nitric acid in the mixed liquor of nitric acid and membrane removal agent is 240g/L, and the concentration of membrane removal agent is 120g/L.
(3) at normal temperatures, the metalwork of step (2) is soaked 20 seconds in the rinsing bowl be filled with water, Again by metalwork under the conditions of 85 DEG C, soak 110 seconds in the chemical polishing bath be filled with chemical polishing solution, To carry out chemical polishing.Wherein, chemical polishing solution includes phosphoric acid, additive and sulphuric acid, and chemical polishing solution In the mass ratio of phosphoric acid, additive and sulphuric acid be 7:2:1, wherein, according to weight/mass percentage composition, additive In containing 5% copper sulfate, the Polyethylene Glycol of 15%, the sulphuric acid of 20% and the phosphoric acid of 40%.
(4) metalwork after polishing is soaked at normal temperatures in the rinsing bowl be filled with water 20 seconds, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent, connect And the most at normal temperatures metalwork is soaked 20 seconds in the rinsing bowl be filled with water.Wherein, nitric acid and membrane removal In the mixed liquor of agent, the concentration of nitric acid is 240g/L, and the concentration of membrane removal agent is 120g/L.
(5) 19 DEG C, under conditions of 15V, metalwork is aoxidized 2400 seconds in anodizing solution and carries out Anodized, so that the surface of metalwork forms the oxide-film of porous.Wherein, anodizing solution includes Sulphuric acid and aluminium ion, the aluminum ions concentration in anodizing solution is 6 grams per liters.Wherein, in anodizing solution The concentration of sulphuric acid is 180 grams per liters.
(6) metalwork that will be formed with oxide-film at normal temperatures soaks 20 seconds in the rinsing bowl be filled with water, Will be formed with again the metalwork of oxide-film under conditions of 50 DEG C in activator supersound process 180 seconds so that Oxide-film activates.Wherein, activator includes water and solute, and according to weight/mass percentage composition, solute includes 75% Sodium citrate and the sodium acetate of 25%.
(7) under room temperature, the metalwork being formed with oxide-film after activation is soaked in the rinsing bowl be filled with water 20 seconds, then the metalwork that will be formed with oxide-film soaks 180 seconds in above-mentioned stain, so that oxide-film is inhaled Attached stain.
(8) metalwork being formed with oxide-film after dyeing step (7) obtained is at normal temperatures in taking up Have in the rinsing bowl of water and soak 20 seconds, then under conditions of 90 DEG C, will be formed with the metalwork of oxide-film in taking up Have hole sealing agent aqueous solution sealing of hole groove in soak within 2100 seconds, carry out sealing pores.Wherein, hole sealing agent is water-soluble In liquid, the concentration of hole sealing agent is 10 grams per liters.Wherein, according to weight/mass percentage composition, hole sealing agent includes the vinegar of 75% Acid nickel, the chelating agent of 20% and the surfactant of 5%.Chelating agent is citric acid.Surfactant is three second Alcohol amine soap.
(9) metalwork being formed with oxide-film after sealing pores is cleaned 20 in the rinsing bowl be filled with water Second, then the metalwork that will be formed with oxide-film under conditions of room temperature soaks 90 seconds, wherein, nitre in nitric acid The concentration of acid is 100 grams per liters.
(10) metalwork being formed with oxide-film step (9) obtained at normal temperatures is in the water being filled with water Washing trough is cleaned 20 seconds, then under conditions of 70 DEG C in water supersound process 30 seconds, then the condition at 70 DEG C Under in water clean 30 seconds, finally in 70 DEG C be dried 1200 seconds, the metalwork after being dyeed.Then will Metalwork after dyeing takes off.
Use the identical method of embodiment 1 obtain the metalwork after the dyeing of the present embodiment surface color and The speckle phenomenon on the surface of the metalwork after dyeing is shown in Table 1.
Embodiment 3
The preparation process of the present embodiment stain is as follows:
(1) each component is weighed according to following proportioning: the acid of Xylene Red 94,0.0115 grams per liter of 0.385 grams per liter The acid orange 74 of acid black 1 68,0.042 grams per liter of black 172,0.00768 grams per liter of property and the sulphuric acid of 3 grams per liters Sodium.
(2) by Xylene Red 94, acid black 172, acid black 1 68, acid orange 74, buffer and sodium sulfate Yu Shuizhong mixes, and obtains stain.
The step of the colouring method of above-mentioned stain is as follows:
(1) metalwork is clamped on the hanger of transfer matic, first metalwork is soaked at normal temperatures and is filled with In the degreasing tank of degreaser, soak 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser Containing the organic acid sodium salt of 35%, the corrosion inhibiter of 9% and the chelating agent of 12%, wherein, organic acid sodium salt is lemon Lemon acid sodium, corrosion inhibiter is ethylene glycol, and chelating agent is sodium pyrophosphate.
(2) at normal temperatures, the metalwork after oil removing is soaked 20 seconds in the rinsing bowl be filled with water, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent.Its In, the concentration of the nitric acid in the mixed liquor of nitric acid and membrane removal agent is 240g/L, and the concentration of membrane removal agent is 120g/L.
(3) at normal temperatures, the metalwork of step (2) is soaked 20 seconds in the rinsing bowl be filled with water, Again by metalwork under the conditions of 85 DEG C, soak 110 seconds in the chemical polishing bath be filled with chemical polishing solution, To carry out chemical polishing.Wherein, chemical polishing solution includes phosphoric acid, additive and sulphuric acid, and chemical polishing solution In the mass ratio of phosphoric acid, additive and sulphuric acid be 7:2:1, wherein, according to weight/mass percentage composition, additive In containing 5% copper sulfate, the Polyethylene Glycol of 15%, the sulphuric acid of 20% and the phosphoric acid of 40%.
(4) metalwork after polishing is soaked at normal temperatures in the rinsing bowl be filled with water 20 seconds, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent, connect And the most at normal temperatures metalwork is soaked 20 seconds in the rinsing bowl be filled with water.Wherein, nitric acid and membrane removal In the mixed liquor of agent, the concentration of nitric acid is 240g/L, and the concentration of membrane removal agent is 120g/L.
(5) 19 DEG C, under conditions of 15V, metalwork is aoxidized 2400 seconds in anodizing solution and carries out Anodized, so that the surface of metalwork forms the oxide-film of porous.Wherein, anodizing solution includes Sulphuric acid and aluminium ion, the aluminum ions concentration in anodizing solution is 6 grams per liters.Wherein, in anodizing solution The concentration of sulphuric acid is 180 grams per liters.
(6) metalwork that will be formed with oxide-film at normal temperatures soaks 20 seconds in the rinsing bowl be filled with water, Will be formed with again the metalwork of oxide-film under conditions of 50 DEG C in activator supersound process 180 seconds so that Oxide-film activates.Wherein, activator includes water and solute, and according to weight/mass percentage composition, solute includes 75% Sodium citrate and the sodium acetate of 25%.
(7) under room temperature, the metalwork being formed with oxide-film after activation is soaked in the rinsing bowl be filled with water 20 seconds, then the metalwork that will be formed with oxide-film soaks 180 seconds in above-mentioned stain, so that oxide-film is inhaled Attached stain.
(8) metalwork being formed with oxide-film after dyeing step (7) obtained is at normal temperatures in taking up Have in the rinsing bowl of water and soak 20 seconds, then under conditions of 90 DEG C, will be formed with the metalwork of oxide-film in taking up Have hole sealing agent aqueous solution sealing of hole groove in soak within 2100 seconds, carry out sealing pores.Wherein, hole sealing agent is water-soluble In liquid, the concentration of hole sealing agent is 10 grams per liters.Wherein, according to weight/mass percentage composition, hole sealing agent includes the vinegar of 75% Acid nickel, the chelating agent of 20% and the surfactant of 5%.Chelating agent is citric acid.Surfactant is three second Alcohol amine soap.
(9) metalwork being formed with oxide-film after sealing pores is cleaned 20 in the rinsing bowl be filled with water Second, then the metalwork that will be formed with oxide-film under conditions of room temperature soaks 90 seconds, wherein, nitre in nitric acid The concentration of acid is 100 grams per liters.
(10) metalwork being formed with oxide-film step (9) obtained at normal temperatures is in the water being filled with water Washing trough is cleaned 20 seconds, then under conditions of 70 DEG C in water supersound process 30 seconds, then the condition at 70 DEG C Under in water clean 30 seconds, finally in 70 DEG C be dried 1200 seconds, the metalwork after being dyeed.Then will Metalwork after dyeing takes off.
Use the identical method of embodiment 1 obtain the metalwork after the dyeing of the present embodiment surface color and The speckle phenomenon on the surface of the metalwork after dyeing is shown in Table 1.
Embodiment 4
The preparation process of the present embodiment stain is as follows:
(1) each component is weighed according to following proportioning: the acid of Xylene Red 94,0.0115 grams per liter of 0.385 grams per liter The property acid orange 74 of acid black 1 68,0.042 grams per liter of black 172,0.00768 grams per liter, 0.0015 milliliter/ The buffer risen and the sodium sulfate of 3 grams per liters.Wherein, buffer comprises the acetic acid that weight/mass percentage composition is 4% With 32% sodium acetate.
(2) by Xylene Red 94, acid black 172, acid black 1 68, acid orange 74, buffer and sodium sulfate Yu Shuizhong mixes, and obtains stain.
The step of the colouring method of above-mentioned stain is as follows:
(1) metalwork is clamped on the hanger of transfer matic, first metalwork is soaked at normal temperatures and is filled with In the degreasing tank of degreaser, soak 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser Containing the organic acid sodium salt of 35%, the corrosion inhibiter of 9% and the chelating agent of 12%, wherein, organic acid sodium salt is lemon Lemon acid sodium, corrosion inhibiter is ethylene glycol, and chelating agent is sodium pyrophosphate.
(2) at normal temperatures, the metalwork after oil removing is soaked 20 seconds in the rinsing bowl be filled with water, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent.Its In, the concentration of the nitric acid in the mixed liquor of nitric acid and membrane removal agent is 240g/L, and the concentration of membrane removal agent is 120g/L.
(3) at normal temperatures, the metalwork of step (2) is soaked 20 seconds in the rinsing bowl be filled with water, Again by metalwork under the conditions of 85 DEG C, soak 110 seconds in the chemical polishing bath be filled with chemical polishing solution, To carry out chemical polishing.Wherein, chemical polishing solution includes phosphoric acid, additive and sulphuric acid, and chemical polishing solution In the mass ratio of phosphoric acid, additive and sulphuric acid be 7:2:1, wherein, according to weight/mass percentage composition, additive In containing 5% copper sulfate, the Polyethylene Glycol of 15%, the sulphuric acid of 20% and the phosphoric acid of 40%.
(4) metalwork after polishing is soaked at normal temperatures in the rinsing bowl be filled with water 20 seconds, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent, connect And the most at normal temperatures metalwork is soaked 20 seconds in the rinsing bowl be filled with water.Wherein, nitric acid and membrane removal In the mixed liquor of agent, the concentration of nitric acid is 240g/L, and the concentration of membrane removal agent is 120g/L.
(5) 19 DEG C, under conditions of 15V, metalwork is aoxidized 2400 seconds in anodizing solution and carries out Anodized, so that the surface of metalwork forms the oxide-film of porous.Wherein, anodizing solution includes Sulphuric acid and aluminium ion, the aluminum ions concentration in anodizing solution is 6 grams per liters.Wherein, in anodizing solution The concentration of sulphuric acid is 180 grams per liters.
(6) metalwork that will be formed with oxide-film at normal temperatures soaks 20 seconds in the rinsing bowl be filled with water, Will be formed with again the metalwork of oxide-film under conditions of 50 DEG C in activator supersound process 180 seconds so that Oxide-film activates.Wherein, activator includes water and solute, and according to weight/mass percentage composition, solute includes 75% Sodium citrate and the sodium acetate of 25%.
(7) under room temperature, the metalwork being formed with oxide-film after activation is soaked in the rinsing bowl be filled with water 20 seconds, then the metalwork that will be formed with oxide-film soaks 180 seconds in above-mentioned stain, so that oxide-film is inhaled Attached stain.
(8) metalwork being formed with oxide-film after dyeing step (7) obtained is at normal temperatures in taking up Have in the rinsing bowl of water and soak 20 seconds, then under conditions of 90 DEG C, will be formed with the metalwork of oxide-film in taking up Have hole sealing agent aqueous solution sealing of hole groove in soak within 2100 seconds, carry out sealing pores.Wherein, hole sealing agent is water-soluble In liquid, the concentration of hole sealing agent is 10 grams per liters.Wherein, according to weight/mass percentage composition, hole sealing agent includes the vinegar of 75% Acid nickel, the chelating agent of 20% and the surfactant of 5%.Chelating agent is citric acid.Surfactant is three second Alcohol amine soap.
(9) metalwork being formed with oxide-film after sealing pores is cleaned 20 in the rinsing bowl be filled with water Second, then the metalwork that will be formed with oxide-film under conditions of room temperature soaks 90 seconds, wherein, nitre in nitric acid The concentration of acid is 100 grams per liters.
(10) metalwork being formed with oxide-film step (9) obtained at normal temperatures is in the water being filled with water Washing trough is cleaned 20 seconds, then under conditions of 70 DEG C in water supersound process 30 seconds, then the condition at 70 DEG C Under in water clean 30 seconds, finally in 70 DEG C be dried 1200 seconds, the metalwork after being dyeed.Then will Metalwork after dyeing takes off.
Use the identical method of embodiment 1 obtain the metalwork after the dyeing of the present embodiment surface color and The speckle phenomenon on the surface of the metalwork after dyeing is shown in Table 1.
Embodiment 5
The preparation process of the present embodiment stain is as follows:
(1) each component is weighed according to following proportioning: the acid of Xylene Red 94,0.0015 grams per liter of 0.285 grams per liter The property acid orange 74 of acid black 1 68,0.032 grams per liter of black 172,0.00868 grams per liter, 0.0005 milliliter/ The buffer risen and the sodium sulfate of 1 grams per liter.Wherein, buffer comprises the acetic acid that weight/mass percentage composition is 3% With 35% sodium acetate.
(2) by Xylene Red 94, acid black 172, acid black 1 68, acid orange 74, buffer and sodium sulfate Yu Shuizhong mixes, and obtains stain.
The step of the colouring method of above-mentioned stain is as follows:
(1) metalwork is clamped on the hanger of transfer matic, first metalwork is soaked at normal temperatures and is filled with In the degreasing tank of degreaser, soak 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser Containing the organic acid sodium salt of 35%, the corrosion inhibiter of 9% and the chelating agent of 12%, wherein, organic acid sodium salt is lemon Lemon acid sodium, corrosion inhibiter is ethylene glycol, and chelating agent is sodium pyrophosphate.
(2) at normal temperatures, the metalwork after oil removing is soaked 20 seconds in the rinsing bowl be filled with water, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent.Its In, the concentration of the nitric acid in the mixed liquor of nitric acid and membrane removal agent is 240g/L, and the concentration of membrane removal agent is 120g/L.
(3) at normal temperatures, the metalwork of step (2) is soaked 20 seconds in the rinsing bowl be filled with water, Again by metalwork under the conditions of 85 DEG C, soak 110 seconds in the chemical polishing bath be filled with chemical polishing solution, To carry out chemical polishing.Wherein, chemical polishing solution includes phosphoric acid, additive and sulphuric acid, and chemical polishing solution In the mass ratio of phosphoric acid, additive and sulphuric acid be 7:2:1, wherein, according to weight/mass percentage composition, additive In containing 5% copper sulfate, the Polyethylene Glycol of 15%, the sulphuric acid of 20% and the phosphoric acid of 40%.
(4) metalwork after polishing is soaked at normal temperatures in the rinsing bowl be filled with water 20 seconds, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent, connect And the most at normal temperatures metalwork is soaked 20 seconds in the rinsing bowl be filled with water.Wherein, nitric acid and membrane removal In the mixed liquor of agent, the concentration of nitric acid is 240g/L, and the concentration of membrane removal agent is 120g/L.
(5) 19 DEG C, under conditions of 15V, metalwork is aoxidized 2400 seconds in anodizing solution and carries out Anodized, so that the surface of metalwork forms the oxide-film of porous.Wherein, anodizing solution includes Sulphuric acid and aluminium ion, the aluminum ions concentration in anodizing solution is 6 grams per liters.Wherein, in anodizing solution The concentration of sulphuric acid is 180 grams per liters.
(6) metalwork that will be formed with oxide-film at normal temperatures soaks 20 seconds in the rinsing bowl be filled with water, Will be formed with again the metalwork of oxide-film under conditions of 50 DEG C in activator supersound process 180 seconds so that Oxide-film activates.Wherein, activator includes water and solute, and according to weight/mass percentage composition, solute includes 75% Sodium citrate and the sodium acetate of 25%.
(7) under room temperature, the metalwork being formed with oxide-film after activation is soaked in the rinsing bowl be filled with water 20 seconds, then the metalwork that will be formed with oxide-film soaks 180 seconds in above-mentioned stain, so that oxide-film is inhaled Attached stain.
(8) metalwork being formed with oxide-film after dyeing step (7) obtained is at normal temperatures in taking up Have in the rinsing bowl of water and soak 20 seconds, then under conditions of 90 DEG C, will be formed with the metalwork of oxide-film in taking up Have hole sealing agent aqueous solution sealing of hole groove in soak within 2100 seconds, carry out sealing pores.Wherein, hole sealing agent is water-soluble In liquid, the concentration of hole sealing agent is 10 grams per liters.Wherein, according to weight/mass percentage composition, hole sealing agent includes the vinegar of 75% Acid nickel, the chelating agent of 20% and the surfactant of 5%.Chelating agent is citric acid.Surfactant is three second Alcohol amine soap.
(9) metalwork being formed with oxide-film after sealing pores is cleaned 20 in the rinsing bowl be filled with water Second, then the metalwork that will be formed with oxide-film under conditions of room temperature soaks 90 seconds, wherein, nitre in nitric acid The concentration of acid is 100 grams per liters.
(10) metalwork being formed with oxide-film step (9) obtained at normal temperatures is in the water being filled with water Washing trough is cleaned 20 seconds, then under conditions of 70 DEG C in water supersound process 30 seconds, then the condition at 70 DEG C Under in water clean 30 seconds, finally in 70 DEG C be dried 1200 seconds, the metalwork after being dyeed.Then will Metalwork after dyeing takes off.
Use the identical method of embodiment 1 obtain the metalwork after the dyeing of the present embodiment surface color and The speckle phenomenon on the surface of the metalwork after dyeing is shown in Table 1.
Embodiment 6
The preparation process of the present embodiment stain is as follows:
(1) each component is weighed according to following proportioning: the acid of Xylene Red 94,0.0215 grams per liter of 0.485 grams per liter The property acid orange 74 of acid black 1 68,0.052 grams per liter of black 172,0.00668 grams per liter, 0.0025 milliliter/ The buffer risen and the sodium sulfate of 4 grams per liters.Wherein, buffer comprises the acetic acid that weight/mass percentage composition is 6% With 28% sodium acetate.
(2) by Xylene Red 94, acid black 172, acid black 1 68, acid orange 74, buffer and sodium sulfate Yu Shuizhong mixes, and obtains stain.
The step of the colouring method of above-mentioned stain is as follows:
(1) metalwork is clamped on the hanger of transfer matic, first metalwork is soaked at normal temperatures and is filled with In the degreasing tank of degreaser, soak 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser Containing the organic acid sodium salt of 35%, the corrosion inhibiter of 9% and the chelating agent of 12%, wherein, organic acid sodium salt is lemon Lemon acid sodium, corrosion inhibiter is ethylene glycol, and chelating agent is sodium pyrophosphate.
(2) at normal temperatures, the metalwork after oil removing is soaked 20 seconds in the rinsing bowl be filled with water, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent.Its In, the concentration of the nitric acid in the mixed liquor of nitric acid and membrane removal agent is 240g/L, and the concentration of membrane removal agent is 120g/L.
(3) at normal temperatures, the metalwork of step (2) is soaked 20 seconds in the rinsing bowl be filled with water, Again by metalwork under the conditions of 85 DEG C, soak 110 seconds in the chemical polishing bath be filled with chemical polishing solution, To carry out chemical polishing.Wherein, chemical polishing solution includes phosphoric acid, additive and sulphuric acid, and chemical polishing solution In the mass ratio of phosphoric acid, additive and sulphuric acid be 7:2:1, wherein, according to weight/mass percentage composition, additive In containing 5% copper sulfate, the Polyethylene Glycol of 15%, the sulphuric acid of 20% and the phosphoric acid of 40%.
(4) metalwork after polishing is soaked at normal temperatures in the rinsing bowl be filled with water 20 seconds, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent, connect And the most at normal temperatures metalwork is soaked 20 seconds in the rinsing bowl be filled with water.Wherein, nitric acid and membrane removal In the mixed liquor of agent, the concentration of nitric acid is 240g/L, and the concentration of membrane removal agent is 120g/L.
(5) 19 DEG C, under conditions of 15V, metalwork is aoxidized 2400 seconds in anodizing solution and carries out Anodized, so that the surface of metalwork forms the oxide-film of porous.Wherein, anodizing solution includes Sulphuric acid and aluminium ion, the aluminum ions concentration in anodizing solution is 6 grams per liters.Wherein, in anodizing solution The concentration of sulphuric acid is 180 grams per liters.
(6) metalwork that will be formed with oxide-film at normal temperatures soaks 20 seconds in the rinsing bowl be filled with water, Will be formed with again the metalwork of oxide-film under conditions of 50 DEG C in activator supersound process 180 seconds so that Oxide-film activates.Wherein, activator includes water and solute, and according to weight/mass percentage composition, solute includes 75% Sodium citrate and the sodium acetate of 25%.
(7) under room temperature, the metalwork being formed with oxide-film after activation is soaked in the rinsing bowl be filled with water 20 seconds, then the metalwork that will be formed with oxide-film soaks 180 seconds in above-mentioned stain, so that oxide-film is inhaled Attached stain.
(8) metalwork being formed with oxide-film after dyeing step (7) obtained is at normal temperatures in taking up Have in the rinsing bowl of water and soak 20 seconds, then under conditions of 90 DEG C, will be formed with the metalwork of oxide-film in taking up Have hole sealing agent aqueous solution sealing of hole groove in soak within 2100 seconds, carry out sealing pores.Wherein, hole sealing agent is water-soluble In liquid, the concentration of hole sealing agent is 10 grams per liters.Wherein, according to weight/mass percentage composition, hole sealing agent includes the vinegar of 75% Acid nickel, the chelating agent of 20% and the surfactant of 5%.Chelating agent is citric acid.Surfactant is three second Alcohol amine soap.
(9) metalwork being formed with oxide-film after sealing pores is cleaned 20 in the rinsing bowl be filled with water Second, then the metalwork that will be formed with oxide-film under conditions of room temperature soaks 90 seconds, wherein, nitre in nitric acid The concentration of acid is 100 grams per liters.
(10) metalwork being formed with oxide-film step (9) obtained at normal temperatures is in the water being filled with water Washing trough is cleaned 20 seconds, then under conditions of 70 DEG C in water supersound process 30 seconds, then the condition at 70 DEG C Under in water clean 30 seconds, finally in 70 DEG C be dried 1200 seconds, the metalwork after being dyeed.Then will Metalwork after dyeing takes off.
Use the identical method of embodiment 1 obtain the metalwork after the dyeing of the present embodiment surface color and The speckle phenomenon on the surface of the metalwork after dyeing is shown in Table 1.
Comparative example 1
The stain of comparative example 1 is: the acid black 172 of Xylene Red 94,0.0235 grams per liter of 0.255 grams per liter, The acid orange 74 of acid black 1 68,0.052 grams per liter of 0.00788 grams per liter, 0.0015 milliliter/L buffer and The sodium sulfate of 2.5 grams per liters.Wherein, buffer comprises acetic acid and the vinegar of 32% that weight/mass percentage composition is 4% Acid sodium.
The step of the colouring method of above-mentioned stain is as follows:
(1) metalwork is clamped on the hanger of transfer matic, first metalwork is soaked at normal temperatures and is filled with In the degreasing tank of degreaser, soak 180 seconds in degreaser under conditions of 50 DEG C.Wherein, in degreaser Containing the organic acid sodium salt of 35%, the corrosion inhibiter of 9% and the chelating agent of 12%, wherein, organic acid sodium salt is lemon Lemon acid sodium, corrosion inhibiter is ethylene glycol, and chelating agent is sodium pyrophosphate.
(2) at normal temperatures, the metalwork after oil removing is soaked 20 seconds in the rinsing bowl be filled with water, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent.Its In, the concentration of the nitric acid in the mixed liquor of nitric acid and membrane removal agent is 240g/L, and the concentration of membrane removal agent is 120g/L.
(3) at normal temperatures, the metalwork of step (2) is soaked 20 seconds in the rinsing bowl be filled with water, Again by metalwork under the conditions of 85 DEG C, soak 110 seconds in the chemical polishing bath be filled with chemical polishing solution, To carry out chemical polishing.Wherein, chemical polishing solution includes phosphoric acid, additive and sulphuric acid, and chemical polishing solution In the mass ratio of phosphoric acid, additive and sulphuric acid be 7:2:1, wherein, according to weight/mass percentage composition, additive In containing 5% copper sulfate, the Polyethylene Glycol of 15%, the sulphuric acid of 20% and the phosphoric acid of 40%.
(4) metalwork after polishing is soaked at normal temperatures in the rinsing bowl be filled with water 20 seconds, then At normal temperatures by metalwork in being filled with mouth immersion 60 seconds in the neutralization chamber of mixed liquor of nitric acid and membrane removal agent, connect And the most at normal temperatures metalwork is soaked 20 seconds in the rinsing bowl be filled with water.Wherein, nitric acid and membrane removal In the mixed liquor of agent, the concentration of nitric acid is 240g/L, and the concentration of membrane removal agent is 120g/L.
(5) 19 DEG C, under conditions of 15V, metalwork is aoxidized 2400 seconds in anodizing solution and carries out Anodized, so that the surface of metalwork forms the oxide-film of porous.Wherein, anodizing solution includes Sulphuric acid and aluminium ion, the aluminum ions concentration in anodizing solution is 6 grams per liters.Wherein, in anodizing solution The concentration of sulphuric acid is 180 grams per liters.
(6) metalwork that will be formed with oxide-film at normal temperatures soaks 20 seconds in the rinsing bowl be filled with water, Will be formed with again the metalwork of oxide-film under conditions of 50 DEG C in activator supersound process 180 seconds so that Oxide-film activates.Wherein, activator includes water and solute, and according to weight/mass percentage composition, solute includes 75% Sodium citrate and the sodium acetate of 25%.
(7) under room temperature, the metalwork being formed with oxide-film after activation is soaked in the rinsing bowl be filled with water 20 seconds, then the metalwork that will be formed with oxide-film soaks 180 seconds in above-mentioned stain, so that oxide-film is inhaled Attached stain.
(8) metalwork being formed with oxide-film after dyeing step (7) obtained is at normal temperatures in taking up Have in the rinsing bowl of water and soak 20 seconds, then under conditions of 90 DEG C, will be formed with the metalwork of oxide-film in taking up Have hole sealing agent aqueous solution sealing of hole groove in soak within 2100 seconds, carry out sealing pores.Wherein, hole sealing agent is water-soluble In liquid, the concentration of hole sealing agent is 10 grams per liters.Wherein, according to weight/mass percentage composition, hole sealing agent includes the vinegar of 75% Acid nickel, the chelating agent of 20% and the surfactant of 5%.Chelating agent is citric acid.Surfactant is three second Alcohol amine soap.
(9) metalwork being formed with oxide-film after sealing pores is cleaned 20 in the rinsing bowl be filled with water Second, then the metalwork that will be formed with oxide-film under conditions of room temperature soaks 90 seconds, wherein, nitre in nitric acid The concentration of acid is 100 grams per liters.
(10) metalwork being formed with oxide-film step (9) obtained at normal temperatures is in the water being filled with water Washing trough is cleaned 20 seconds, then under conditions of 70 DEG C in water supersound process 30 seconds, then the condition at 70 DEG C Under in water clean 30 seconds, finally in 70 DEG C be dried 1200 seconds, the metalwork after being dyeed.Then will Metalwork after dyeing takes off.
Use the identical method of embodiment 1 obtain the metalwork after the dyeing of comparative example 1 surface color and The speckle phenomenon on the surface of the metalwork after dyeing is shown in Table 1.
Table 1 be use embodiment 1~6 and comparative example 1 staining reagent after metalwork surface color, The speckle phenomenon on the surface of the metalwork after the color of rose golden and dyeing.
Table 1
From table 1 it follows that it is seen from the above data that a on the surface of the metalwork of embodiment 1~6 Value and b value, for comparative example 1, all differ less with a value of rose golden and b value.And from reality Execute in example 1~6 it can be seen that when in stain possibly together with buffer and sodium sulfate, the surface of metalwork without Speckle, the most uniformly.
Each technical characteristic of embodiment described above can combine arbitrarily, for making description succinct, the most right The all possible combination of each technical characteristic in above-described embodiment is all described, but, if these skills There is not contradiction in the combination of art feature, is all considered to be the scope that this specification is recorded.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, But can not therefore be construed as limiting the scope of the patent.It should be pointed out that, for this area For those of ordinary skill, without departing from the inventive concept of the premise, it is also possible to make some deformation and change Entering, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be with appended power Profit requires to be as the criterion.

Claims (7)

1. a stain, it is characterised in that include following component: the Xylene Red of 0.285~0.485 grams per liter 94, the acid black 172 of 0.0015~0.0215 grams per liter, 0.00668~0.00868 acid black 1 68 and of grams per liter The acid orange 74 of 0.032~0.052 grams per liter.
Stain the most according to claim 1, it is characterised in that described stain also includes The buffer of 0.0005~0.0025 ml l, comprises the vinegar that weight/mass percentage composition is 3~6% in described buffer Acid and 28~the sodium acetate of 35%.
Stain the most according to claim 1 and 2, it is characterised in that described stain also includes 1~4 The sodium sulfate of grams per liter.
Stain the most according to claim 1, it is characterised in that include following component: 0.385 gram/ The acid black 172 of Xylene Red 94,0.0115 grams per liter of liter, the acid black 1 68 and 0.042 of 0.00768 grams per liter The acid orange 74 of grams per liter.
5. the preparation method of a stain, it is characterised in that comprise the steps:
Each component is weighed: the Xylene Red 94,0.0015~0.0215 of 0.285~0.485 grams per liter according to following proportioning The acid black 172 of grams per liter, 0.00668~0.00868 acid black 1 68 and 0.032~0.052 grams per liter of grams per liter Acid orange 74;
By described Xylene Red 94, described acid black 172, described acid black 1 68 and described acid orange 74 in water Middle mixing, obtains described stain.
The preparation method of stain the most according to claim 5, it is characterised in that also include weighing The buffer of 0.0005~0.0025 ml l, comprises the vinegar that weight/mass percentage composition is 3~6% in described buffer Acid and 28~the sodium acetate of 35%, wherein, by described Xylene Red 94, described acid black 172, described acid black 168 and the step that mixes in water of described acid orange 74 particularly as follows: by described Xylene Red 94, described acid black 172, described acid black 1 68, described acid orange 74 and described buffer mix in water.
The preparation method of stain the most according to claim 5, it is characterised in that also include weighing 1~4 The sodium sulfate of grams per liter, wherein, by described Xylene Red 94, described acid black 172, described acid black 1 68 and Step that described acid orange 74 mixes in water particularly as follows: by described Xylene Red 94, described acid black 172, Described acid black 1 68, described acid orange 74 and described sodium sulfate mix in water.
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