CN104357819A - Metal passivator and preparation method thereof - Google Patents

Metal passivator and preparation method thereof Download PDF

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Publication number
CN104357819A
CN104357819A CN201410637293.4A CN201410637293A CN104357819A CN 104357819 A CN104357819 A CN 104357819A CN 201410637293 A CN201410637293 A CN 201410637293A CN 104357819 A CN104357819 A CN 104357819A
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Prior art keywords
parts
mixed solution
metal passivator
hydrogen peroxide
acetic acid
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尤为
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Wuxi Epic Technology Co Ltd
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Wuxi Epic Technology Co Ltd
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Priority to CN201410637293.4A priority Critical patent/CN104357819A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Sludge (AREA)
  • Heat Sensitive Colour Forming Recording (AREA)

Abstract

The invention discloses a metal passivator and a preparation method thereof. The passivator comprises the following steps: cyclohexane, sulfate, acetic acid, sodium nitrate, fluoride salt, nickel sulfate, hydrogen peroxide, zinc fluozirconate and water. The preparation method of the metal passivator comprises the following steps: step 1, weighing cyclohexane, sulfate, acetic acid, sodium nitrate, fluoride salt, nickel sulfate, hydrogen peroxide, zinc fluozirconate and water for later use; step 2, mixing cyclohexane, sulfate, sodium nitrate, fluoride salt, nickel sulfate and zinc fluozirconate with water, stirring and then heating for 13-18 minutes to obtain a mixed solution I; step 3, adding acetic acid and hydrogen peroxide into the mixed solution I, stirring at 40-60 DEG C for 2-5 minutes to obtain a mixed solution II; and step 4, defoaming the mixed solution II to obtain the passivator. The passivator is good in use effect at the low temperature, low in cost and small in pollution.

Description

A kind of metal passivator and preparation method thereof
 
Technical field
The present invention relates to chemical industrial field, be specifically related to a kind of metal passivator and preparation method thereof.
 
Background technology
Passivator generally has the ability forming coating or film in metallic surface.Metallic surface, after overpickling, needs to carry out neutralizing and water flushing, to remove residual acid wherein, and then Passivation Treatment, prevent metal surface corrosion after cleaning from getting rusty, passivation is generally carried out after cleaning.
Conventional passivator has phosphoric acid salt, nitrite, its nitrite can carry out under the temperature that the short period of time is interior and lower again, but in dry environment, there is satisfactory stability, but no matter be phosphoric acid salt or nitrite, in use all can to environment, first need to research and develop a kind of passivator more having passivation ability, and environmental pollution is few.
Application number be 200410066830.0 China application discloses that a kind of passivator of metallic surface, this passivator is mixed by hexahydroaniline, zinc sulfate, tertiary sodium phosphate and water, although relatively good at passivation ability, but contaminate environment, and can only use at normal temperatures, thus be badly in need of researching and developing a kind of pollute little, low temperature under also can form the passivator of passivation layer.
 
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of metal passivator and preparation method thereof, good passivation effect, with low cost.
For solving prior art problem, the technical solution used in the present invention is:
A kind of metal passivator, comprises the following raw material counted by weight: ring is amine 22-34 part, vitriol 10-16 part, acetic acid 2-6 part, SODIUMNITRATE 4-8 part, fluoride salt 5-9 part, single nickel salt 2-6 part, hydrogen peroxide 3-8 part, fluorine zirconic acid zinc 2-6 part, water 18-24 part.
Preferred as above-mentioned metal passivator, comprises the following raw material counted by weight: ring is amine 28-32 part, vitriol 14-16 part, acetic acid 4-6 part, SODIUMNITRATE 5-7 part, fluoride salt 6-8 part, single nickel salt 4-6 part, hydrogen peroxide 5-7 part, fluorine zirconic acid zinc 4-6 part, water 20-24 part.
Preferred as above-mentioned metal passivator, also comprises citric acid 1-4 part.
Preferred as above-mentioned metal passivator, described fluoride salt is the one of Sodium Fluoride or Potassium monofluoride.
The preparation method of above-mentioned metal passivator, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stirs post-heating 13-18 minute, obtains mixed solution I;
Step 3, then add in mixed solution I and add acetic acid and hydrogen peroxide, stir 2-5 minute at 40-60 DEG C, obtain mixed solution II;
Step 4, obtains passivator by after mixed solution II defoaming treatment.
As preparation method preferred of above-mentioned metal passivator, in step 2, Heating temperature is 80-100 DEG C.
As preparation method preferred of above-mentioned metal passivator, in step 3, stirring velocity is 200-400rpm.
As preparation method preferred of above-mentioned metal passivator, in step 3, froth breaking adopts ultrasonic wave froth breaking.
 
beneficial effect
Passivator of the present invention not only can use at normal temperatures, and the passivation layer that still can be formed at low temperatures, meanwhile, the synergy of fluoride salt and fluorine zirconic acid zinc, enhances passivation effect.Preparation cost is cheap, pollutes little, is applicable to promoting.
 
Embodiment
embodiment 1
A kind of metal passivator, comprises the following raw material counted by weight: ring is amine 22 parts, 10 parts, vitriol, acetic acid 2 parts, SODIUMNITRATE 4 parts, Sodium Fluoride 5 parts, single nickel salt 2 parts, 3 parts, hydrogen peroxide, 2 parts, fluorine zirconic acid zinc, 18 parts, water.
The preparation method of above-mentioned metal passivator, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stir post-heating 13 minutes, obtain mixed solution I, wherein Heating temperature is 80 DEG C;
Step 3, then add in mixed solution I and add acetic acid and hydrogen peroxide, stir 2 minutes at 40 DEG C, stirring velocity is that 200rpm obtains mixed solution II;
Step 4, obtains passivator by after mixed solution II ultrasonic wave froth breaking.
 
embodiment 2
A kind of metal passivator, comprises the following raw material counted by weight: ring is amine 28 parts, 14 parts, vitriol, acetic acid 4 parts, SODIUMNITRATE 5 parts, Potassium monofluoride 6 parts, single nickel salt 4 parts, 5 parts, hydrogen peroxide, 4 parts, fluorine zirconic acid zinc, 20 parts, water.
The preparation method of above-mentioned metal passivator, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stir post-heating 15 minutes, obtain mixed solution I, wherein Heating temperature is 90 DEG C;
Step 3, then add in mixed solution I and add acetic acid and hydrogen peroxide, stir 3 minutes at 48 DEG C, stirring velocity is that 300rpm obtains mixed solution II;
Step 4, obtains passivator by after mixed solution II ultrasonic wave froth breaking.
 
embodiment 3
A kind of metal passivator, comprises the following raw material counted by weight: ring is amine 32 parts, 16 parts, vitriol, acetic acid 6 parts, SODIUMNITRATE 7 parts, Sodium Fluoride 8 parts, single nickel salt 6 parts, 7 parts, hydrogen peroxide, 6 parts, fluorine zirconic acid zinc, 24 parts, water.
The preparation method of above-mentioned metal passivator, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stir post-heating 13-18 minute, obtain mixed solution I, wherein Heating temperature is 95 DEG C;
Step 3, then add in mixed solution I and add acetic acid and hydrogen peroxide, stir 4 minutes at 50 DEG C, stirring velocity is that 350rpm obtains mixed solution II;
Step 4, obtains passivator by after mixed solution II ultrasonic wave froth breaking.
 
embodiment 4
A kind of metal passivator, comprises the following raw material counted by weight: ring is amine 34 parts, 16 parts, vitriol, acetic acid 6 parts, SODIUMNITRATE 8 parts, Potassium monofluoride 9 parts, single nickel salt 6 parts, 8 parts, hydrogen peroxide, 6 parts, fluorine zirconic acid zinc, 24 parts, water.
The preparation method of above-mentioned metal passivator, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stir post-heating 18 minutes, obtain mixed solution I, wherein Heating temperature is 100 DEG C;
Step 3, then add in mixed solution I and add acetic acid and hydrogen peroxide, stir 5 minutes at 60 DEG C, stirring velocity is that 400rpm obtains mixed solution II;
Step 4, obtains passivator by after mixed solution II ultrasonic wave froth breaking.
 
embodiment 5
A kind of metal passivator, comprises the following raw material counted by weight: ring is amine 22 parts, 10 parts, vitriol, acetic acid 2 parts, SODIUMNITRATE 4 parts, Sodium Fluoride 5 parts, single nickel salt 2 parts, 3 parts, hydrogen peroxide, 2 parts, fluorine zirconic acid zinc, 18 parts, water, citric acid 1 part.
The preparation method of above-mentioned metal passivator, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stir post-heating 13 minutes, obtain mixed solution I, wherein Heating temperature is 80 DEG C;
Step 3, then add in mixed solution I and add acetic acid, citric acid and hydrogen peroxide, stir 2 minutes at 40 DEG C, stirring velocity is that 200rpm obtains mixed solution II;
Step 4, obtains passivator by after mixed solution II ultrasonic wave froth breaking.
embodiment 6
A kind of metal passivator, comprises the following raw material counted by weight: ring is amine 28 parts, 14 parts, vitriol, acetic acid 4 parts, SODIUMNITRATE 5 parts, Potassium monofluoride 6 parts, single nickel salt 4 parts, 5 parts, hydrogen peroxide, 4 parts, fluorine zirconic acid zinc, 20 parts, water, citric acid 3 parts.
The preparation method of above-mentioned metal passivator, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stir post-heating 13-18 minute, obtain mixed solution I, wherein Heating temperature is 95 DEG C;
Step 3, then add in mixed solution I and add acetic acid, citric acid and hydrogen peroxide, stir 4 minutes at 50 DEG C, stirring velocity is that 350rpm obtains mixed solution II;
Step 4, obtains passivator by after mixed solution II ultrasonic wave froth breaking.
 
embodiment 7
A kind of metal passivator, comprises the following raw material counted by weight: ring is amine 34 parts, 16 parts, vitriol, acetic acid 6 parts, SODIUMNITRATE 8 parts, Potassium monofluoride 9 parts, single nickel salt 6 parts, 8 parts, hydrogen peroxide, 6 parts, fluorine zirconic acid zinc, 24 parts, water, citric acid 4 parts.
The preparation method of above-mentioned metal passivator, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stir post-heating 18 minutes, obtain mixed solution I, wherein Heating temperature is 100 DEG C;
Step 3, then add in mixed solution I and add acetic acid and hydrogen peroxide, stir 5 minutes at 60 DEG C, stirring velocity is that 400rpm obtains mixed solution II;
Step 4, obtains passivator by after mixed solution II ultrasonic wave froth breaking.
 
comparative example 1
A kind of metal passivator, comprises the following raw material counted by weight: ring is amine 22 parts, 10 parts, vitriol, acetic acid 2 parts, SODIUMNITRATE 4 parts, Sodium Fluoride 5 parts, single nickel salt 2 parts, 3 parts, hydrogen peroxide, 18 parts, water.
The preparation method of above-mentioned metal passivator, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stir post-heating 13 minutes, obtain mixed solution I, wherein Heating temperature is 80 DEG C;
Step 3, then add in mixed solution I and add acetic acid and hydrogen peroxide, stir 2 minutes at 40 DEG C, stirring velocity is that 200rpm obtains mixed solution II;
Step 4, obtains passivator by after mixed solution II ultrasonic wave froth breaking.
 
comparative example 2
A kind of metal passivator, comprises the following raw material counted by weight: ring is amine 22 parts, 10 parts, vitriol, acetic acid 2 parts, SODIUMNITRATE 4 parts, single nickel salt 2 parts, 3 parts, hydrogen peroxide, 2 parts, fluorine zirconic acid zinc, 18 parts, water.
The preparation method of above-mentioned metal passivator, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stir post-heating 13 minutes, obtain mixed solution I, wherein Heating temperature is 80 DEG C;
Step 3, then add in mixed solution I and add acetic acid and hydrogen peroxide, stir 2 minutes at 40 DEG C, stirring velocity is that 200rpm obtains mixed solution II;
Step 4, obtains passivator by after mixed solution II ultrasonic wave froth breaking.
 
performance test
The passivator of passivator the present invention prepared, comparative example 1 and comparative example 2 gained carries out Performance comparision, and the data obtained is as shown in the table.
As can be seen from above-mentioned data, the use temperature scope of the passivator prepared by the present invention is wider, as usual use under low temperature, passivation layer is stablized, acid and alkali-resistance is resistance to get rusty, and wherein citric acid contributes to the formation of passivation layer more, known by comparing embodiment 1, comparative example 1 and comparative example 2, fluoride salt and fluorine zirconic acid zinc synergy, enhance passivation effect.

Claims (8)

1. a metal passivator, is characterized in that, comprises the following raw material counted by weight: ring is amine 22-34 part, vitriol 10-16 part, acetic acid 2-6 part, SODIUMNITRATE 4-8 part, fluoride salt 5-9 part, single nickel salt 2-6 part, hydrogen peroxide 3-8 part, fluorine zirconic acid zinc 2-6 part, water 18-24 part.
2. metal passivator according to claim 1, it is characterized in that, comprise the following raw material counted by weight: ring is amine 28-32 part, vitriol 14-16 part, acetic acid 4-6 part, SODIUMNITRATE 5-7 part, fluoride salt 6-8 part, single nickel salt 4-6 part, hydrogen peroxide 5-7 part, fluorine zirconic acid zinc 4-6 part, water 20-24 part.
3. metal passivator according to claim 1, is characterized in that: also comprise citric acid 1-4 part.
4. metal passivator according to claim 1, is characterized in that: described fluoride salt is the one of Sodium Fluoride or Potassium monofluoride.
5. the preparation method of metal passivator according to claim 1, is characterized in that, comprises the following steps:
Step 1, takes ring amine, vitriol, acetic acid, SODIUMNITRATE, fluoride salt, single nickel salt, hydrogen peroxide, fluorine zirconic acid zinc, and water is for subsequent use;
Step 2, by ring amine, vitriol, SODIUMNITRATE, fluoride salt, single nickel salt, after fluorine zirconic acid zinc and water mix, stirs post-heating 13-18 minute, obtains mixed solution I;
Step 3, then add in mixed solution I and add acetic acid and hydrogen peroxide, stir 2-5 minute at 40-60 DEG C, obtain mixed solution II;
Step 4, obtains passivator by after mixed solution II defoaming treatment.
6. the preparation method of metal passivator according to claim 5, is characterized in that: in step 2, Heating temperature is 80-100 DEG C.
7. the preparation method of metal passivator according to claim 5, is characterized in that: in step 3, stirring velocity is 200-400rpm.
8. the preparation method of metal passivator according to claim 5, is characterized in that: in step 3, froth breaking adopts ultrasonic wave froth breaking.
CN201410637293.4A 2014-11-13 2014-11-13 Metal passivator and preparation method thereof Pending CN104357819A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105256299A (en) * 2015-11-02 2016-01-20 常熟风范电力设备股份有限公司 Novel efficient and environment-friendly metal passivation solution and preparing method thereof
CN105331966A (en) * 2015-11-30 2016-02-17 宝山钢铁股份有限公司 Chromium-free surface treatment tinplate, production method thereof and surface treating agent
CN106800845A (en) * 2017-01-22 2017-06-06 安徽臣诺机器人科技有限公司 A kind of mechanical arm spray metal passivator and preparation method thereof

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CN1754985A (en) * 2004-09-29 2006-04-05 上海万森水处理有限公司 Metal surface passivant and its using method
CN1754986A (en) * 2004-09-29 2006-04-05 上海万森水处理有限公司 Metal surface passivant
CN102965654A (en) * 2012-12-16 2013-03-13 况金权 High-salt-fog-resistance aluminum product passivator and preparation method thereof

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CN1715448A (en) * 2004-06-30 2006-01-04 上海万森水处理有限公司 Inactivating agent for metal surface
CN1754985A (en) * 2004-09-29 2006-04-05 上海万森水处理有限公司 Metal surface passivant and its using method
CN1754986A (en) * 2004-09-29 2006-04-05 上海万森水处理有限公司 Metal surface passivant
CN102965654A (en) * 2012-12-16 2013-03-13 况金权 High-salt-fog-resistance aluminum product passivator and preparation method thereof

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杨灵: ""绿色双氧水钝化工艺"", 《清洗世界》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105256299A (en) * 2015-11-02 2016-01-20 常熟风范电力设备股份有限公司 Novel efficient and environment-friendly metal passivation solution and preparing method thereof
CN105331966A (en) * 2015-11-30 2016-02-17 宝山钢铁股份有限公司 Chromium-free surface treatment tinplate, production method thereof and surface treating agent
CN105331966B (en) * 2015-11-30 2018-04-27 宝山钢铁股份有限公司 A kind of Chrome-free surface treatment tin plate, its production method and surface conditioning agent
US11248298B2 (en) 2015-11-30 2022-02-15 Baoshan Iron & Steel Co., Ltd. Chromium-free surface-treated tinplate, production method and surface treating agent therefor
CN106800845A (en) * 2017-01-22 2017-06-06 安徽臣诺机器人科技有限公司 A kind of mechanical arm spray metal passivator and preparation method thereof

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Application publication date: 20150218