CN102011117A - Environmental-friendly room-temperature steel blackening agent and preparation method thereof - Google Patents

Environmental-friendly room-temperature steel blackening agent and preparation method thereof Download PDF

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Publication number
CN102011117A
CN102011117A CN 201010570982 CN201010570982A CN102011117A CN 102011117 A CN102011117 A CN 102011117A CN 201010570982 CN201010570982 CN 201010570982 CN 201010570982 A CN201010570982 A CN 201010570982A CN 102011117 A CN102011117 A CN 102011117A
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agent
environment
room temperature
work
friendly type
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饶丹
刘万青
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HEFEI HUAQING METAL SURFACE TREATMENT CO Ltd
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HEFEI HUAQING METAL SURFACE TREATMENT CO Ltd
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Abstract

The invention provides an environmental-friendly room-temperature steel blackening agent and a preparation method thereof. The steel blackening agent comprises the following raw materials by weight: 4-8g/L of CuSO4.5H2O, 6-9g/L of Na2S2O3.5H2O, 5-8g/L of (NH4)6Mo7O24, 2-4g/L of NiSO4.6H2O, 2-4g/L of earth salts, 3-5g/L of catalyst, 2-4g/L of complexing agent, 0.02-0.04g/L of wetting agent, micro pH regulator and the balance water. The blackening film layer generated by the blackening agent has good adhesion and strong corrosion resistance. The blackening agent is simple in processing process, does not contain selenium, phosphorus and other elements which cause pollution to the environment, and is non-toxic and environmental-friendly.

Description

A kind of environment-friendly type iron and steel room temperature blackening agent and preparation method thereof
Technical field
The present invention relates to a kind of blackening agent for iron and steel surface, particularly a kind of environment-friendly type iron and steel room temperature blackening agent and preparation method thereof.
Background technology
The blackening of Steel at Room Temperature process of surface treatment is 20th century conversion film New Process for Treatment that grow up of the mid-80.Compare with the alkaline high temperature blackening of tradition, room temperature blackening technology is not limited by steel type, has a series of advantages such as energy-conservation, efficient, easy to operate simultaneously, makes this technological development rapid.
Present most room temperature blacking liquid is the selenium copper system, and selenium compound costs an arm and a leg and severe toxicity is arranged, life-time service certainly will cause environmental pollution, and remain shortcomings such as, blackout layer many in technology instability, solution precipitation and matrix metal bonding force be relatively poor, so that these technologies are promoted at present at home as yet fully.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of asepsis environment-protecting and can form the environment-friendly type iron and steel room temperature blackening agent of well behaved blackout rete at steel surface.
Another technical problem that the present invention will solve provides a kind of preparation method of above-mentioned environment-friendly type iron and steel room temperature blackening agent.
The technical scheme that the present invention is adopted for the above-mentioned technical purpose of realization is: a kind of environment-friendly type iron and steel room temperature blackening agent, in 1 liter of volume, form by following materials of weight proportions:
CuSO 4·5H 2O 4-8g/L
Na 2S 2O 3·5H 2O 6-9g/L
(NH 4) 6Mo 7O 24 5-8g/L
NiSO 4·6H 2O 2-4g/L
Rare-earth salts 2-4g/L
Catalyzer 3-5g/L
Complexing agent 2-4g/L
Wetting agent 0.02-0.04g/L
PH regulator agent trace
Surplus is a water.
Described rare-earth salts is a cerous nitrate, and described catalyzer is a Glacial acetic acid, and described complexing agent is the oxalic acid tetraacethyl disodium, and described wetting agent is a polyoxyethylene glycol 800, and described pH regulator agent is a sulfuric acid.
A kind of environment-friendly type iron and steel room temperature blackening agent, its preparation method may further comprise the steps:
(1) proportioning by claim 1 takes by weighing raw material;
(2) with CuSO 45H 2O, Na 2S 2O 36H 2O is soluble in water, and to make the work in-process treatment solution standby;
(3) with (NH 4) 6Mo 7O 24, NiSO 46H 2O, rare-earth salts is soluble in water, waits to dissolve that back and step (2) make
The work in-process treatment solution mixes, and fully stirs it is dissolved fully, and it is stand-by to make the work in-process treatment solution;
(4) add catalyzer, complexing agent and wetting agent successively in the work in-process treatment solution that in step (3), makes, evenly stir in the adition process, after the components dissolved for the treatment of to add earlier, continue to add next component again;
(5) adding an amount of water to the volume of treatment agent in the work in-process treatment solution that step (4) makes is 1L, and is 1-3 with pH regulator agent adjusting pH value.
Blackening agent for surface blackening processing technology of the present invention
A, steel surface pre-treatment:
Rust cleaning → degreasing → rinsing → pickling → rinsing
B, blackout are handled: place the described blackening agent for surface film forming of turning black to handle steel part, the treatment time is 5-10min, and pH value is 1-3, and treatment temp is a room temperature.
C, aftertreatment: blackout is after washing → neutralization (Na 2CO 33%, normal temperature, 1-2S) the present invention will be further described below washing → air-dry → immersion oil:
Rare earth element is because its internal layer-4f electronic shell that has one deck not to be filled, because the existence of this undersaturated electronic shell, make the nuclear bad sealing of electron pair of subgrade close, atom has bigger nuclear charge number, show stronger adsorptive power, can be adsorbed on the active site of crystal growth, at the metal base surface forming core, can suppress to close on the growth of matrix, make rete crystallization refinement, rare earth element has katalysis in addition, can make the black film reaction become complicated more, form multiple rich salt, make black film become evenly fine and close, thereby the solidity to corrosion of black film and sticking power are strengthened.Therefore can join rare-earth salts in the blackening agent for surface as additive, be used to remedy the defective of room temperature blackening sticking power and solidity to corrosion difference.Do not have as yet at present and in the normal tamperature environmental protection blackening agent for surface, add the patent that rare-earth salts is used for the steel blackening processing.
Contain the iron sulphide that Sulfothiorine and ammonium molybdate will help generating at steel surface black in the blackening agent for surface, under the situation that contains the catalyzer Glacial acetic acid, copper can generate the Cu of particular tissues form black simultaneously 2The settled layer of O, and react with Cu that steel substrate generation replacement(metathesis)reaction the generates active oxygen that generates that also can interact with the Oxidizing and Reducing Agents in the solution, generate the CuO of black, add the absorption and the katalysis of rare-earth salts in addition, will make steel surface generate composite film with dense structure.
The film adhesion of blackening agent for surface of the present invention blackout is good, and solidity to corrosion is strong, and not containing selenium, phosphorus, chromium etc. in the blackening agent for surface has the element of pollution, nontoxic can directly discharging the, compliance with environmental protection requirements to environment.
Embodiment
Embodiment 1
(1) takes by weighing 4g CuSO 45H 2O, 6g Na 2S 2O 36H 2O adds respectively in the 100ml water, and it is standby that abundant stirring treats to make the work in-process treatment solution after it dissolves fully.
(2) take by weighing 6g (NH respectively 4) 6Mo 7O 24, 2g NiSO 46H 2O, 2g Ce (NO 3) 36H 2O adds respectively in the 100ml water, treats that it dissolves the back and mixes with the work in-process treatment solution that step (1) makes, and it is stand-by that abundant stirring treats to make the work in-process treatment solution after it dissolves fully.
(3) add the 3g Glacial acetic acid successively in the work in-process treatment solution that in step (2), makes, 2g oxalic acid tetraacethyl disodium, 0.03g polyoxyethylene glycol 800 evenly stirs in the adition process, after the components dissolved for the treatment of to add earlier, adds next component again.
(4) adding an amount of water to the volume of treatment agent in the work in-process treatment solution that makes in step (3) is 1L, and is 1～3 with 98% sulfuric acid adjusting PH, so both can obtain required treatment agent of the present invention.
Embodiment 2
(1) takes by weighing 6g CuSO 45H 2O, 8g Na 2S 2O 36H 2O adds respectively in the 100ml water, and it is standby that abundant stirring treats to make the work in-process treatment solution after it dissolves fully.
(2) take by weighing 5g (NH respectively 4) 6Mo 7O 24, 3g NiSO 46H 2O, 3g Ce (NO 3) 36H 2O adds respectively in the 100ml water, treats that it dissolves the back and mixes with the work in-process treatment solution that step (1) makes, and it is stand-by that abundant stirring treats to make the work in-process treatment solution after it dissolves fully.
(3) add the 4g Glacial acetic acid successively in the work in-process treatment solution that in step (2), makes, 3g oxalic acid tetraacethyl disodium, 0.02g polyoxyethylene glycol 800 evenly stirs in the adition process, after the components dissolved for the treatment of to add earlier, adds next component again.
(4) adding an amount of water to the volume of treatment agent in the work in-process treatment solution that makes in step (3) is 1L, and is 1～3 with 98% sulfuric acid adjusting PH, so both can obtain required treatment agent of the present invention.
Embodiment 3
(1) takes by weighing 7g CuSO 45H 2O, 9g Na 2S 2O 36H 2O adds respectively in the 100ml water, and it is standby that abundant stirring treats to make the work in-process treatment solution after it dissolves fully.
(2) take by weighing 7g (NH respectively 4) 6Mo 7O 24, 3g NiSO 46H 2O, 4g Ce (NO 3) 36H 2O adds respectively in the 100ml water, treats that it dissolves the back and mixes with the work in-process treatment solution that step (1) makes, and it is stand-by that abundant stirring treats to make the work in-process treatment solution after it dissolves fully.
(3) add the 4g Glacial acetic acid successively in the work in-process treatment solution that in step (2), makes, 3g oxalic acid tetraacethyl disodium, 0.03g polyoxyethylene glycol 800 evenly stirs in the adition process, after the components dissolved for the treatment of to add earlier, adds next component again.
(4) adding an amount of water to the volume of treatment agent in the work in-process treatment solution that makes in step (3) is 1L, and is 1～3 with 98% sulfuric acid adjusting PH, so both can obtain required treatment agent of the present invention.
Embodiment 4
(1) takes by weighing 8g CuSO 45H 2O, 9g Na 2S 2O 36H 2O adds respectively in the 100ml water, and it is standby that abundant stirring treats to make the work in-process treatment solution after it dissolves fully.
(2) take by weighing 8g (NH respectively 4) 6Mo 7O 24, 4g NiSO 46H 2O, 4g Ce (NO 3) 36H 2O adds respectively in the 100ml water, treats that it dissolves the back and mixes with the work in-process treatment solution that step (1) makes, and it is stand-by that abundant stirring treats to make the work in-process treatment solution after it dissolves fully.
(3) add the 5g Glacial acetic acid successively in the work in-process treatment solution that in step (2), makes, 4g oxalic acid tetraacethyl disodium, 0.04g polyoxyethylene glycol 800 evenly stirs in the adition process, after the components dissolved for the treatment of to add earlier, adds next component again.
(4) adding an amount of water to the volume of treatment agent in the work in-process treatment solution that makes in step (3) is 1L, and is 1～3 with 98% sulfuric acid adjusting PH, so both can obtain required treatment agent of the present invention.
Utilize the treatment agent of embodiment of the invention 1-4 to test and test contrast with following two kinds of treatment process by blackening agent for surface blackening of the present invention:
Contrast technology 1: contain the selenium blackening: place the described selenium blackout treatment agent normal temperature that contains to handle 5-8 minute steel part, its treatment agent raw material consists of: in 1 liter of volume: selenous acid 3g/L, copper sulfate 3g/L, nickelous chloride 1g/L, phosphatase 11 g/L, surplus are water.
Contrast technology 2: conventional high-temperature alkalescence blackening: place described conventional high-temperature alkalescence blackout treatment agent to handle 40 minutes down for 140 ℃ at high temperature steel part, its treatment agent is: 40%NaNO 2The aqueous solution with 30%NaOH.
Because China does not still have the industry standard and the national standard of steel blackening film wear resistance and corrosion resistance testing method at present, therefore adopt conventional testing method that film forming properties is tested to blackening agent for surface of the present invention.
(1) test event and method
The film forming properties of environment-friendly type iron and steel room temperature blackening agent is carried out the detection of following project:
1, outward appearance detects: the shade and the bright degree of observation film
2, wear test: with the filter paper rete that rubs back and forth, the friction cumulative frequency when record exposes matrix.
3, corrosion resistant test: adopt the copper sulfate topical application method, the method for inspection drops on the steel blackening film for getting 1 copper-bath, observes its color and fades to the ruddy time.
(2) result and analysis
The film forming properties detected result of different blackening agent for iron and steel surface sees Table:
Figure BSA00000370846300051
See that by above-mentioned data blackening agent for surface treatment effect of the present invention has exceeded the treatment effect that contains selenium blackening and conventional high-temperature alkalescence blackening, be better than prior art on the performance, and blackening agent for surface blackening processing technology of the present invention is simple, is convenient to actual production.
Starting material manufacturer and standard
CuSO 45H 2O Shanghai Xinhua chemical plant quality standard HG/T 3592-1999
Na 2S 2O 35H 2O changzhou city China reaches chemical plant quality standard HG/T 2328-1999
(NH 4) 6Mo 7O 24The quality standard GB3460-82 of Dongtai city peak-to-peak tungsten Products Co., Ltd
NiSO 46H 2The O Huangyan, Zhejiang is built industry chemical plant quality standard GB/T 6392-86
Cerous nitrate Shandong Zibo Rong Rui reaches powder body material factory quality standard company standard
Glacial acetic acid Jiangsu Suo Pu (group) the standard GB1628.1-2000 of company quality
The oxalic acid tetraacethyl disodium Shanghai reagent one quality standard GB/T 1401-1998 of factory
Source, polyoxyethylene glycol 800 Shanghai leaf bio tech ltd quality standard company standard

Claims (7)

1. environment-friendly type iron and steel room temperature blackening agent is characterized in that: in 1 liter of volume, be made up of following materials of weight proportions:
CuSO 4·5H 2O 4-8g/L
Na 2S 2O 3·5H 2O 6-9g/L
(NH 4) 6Mo 7O 24 5-8g/L
NiSO 4·6H 2O 2-4g/L
Rare-earth salts 2-4g/L
Catalyzer 3-5g/L
Complexing agent 2-4g/L
Wetting agent 0.02-0.04g/L
PH regulator agent trace
Surplus is a water.
2. a kind of environment-friendly type iron and steel room temperature blackening agent according to claim 1 is characterized in that: described rare-earth salts is a cerous nitrate.
3. a kind of environment-friendly type iron and steel room temperature blackening agent according to claim 1 is characterized in that: described catalyzer is a Glacial acetic acid.
4. a kind of environment-friendly type iron and steel room temperature blackening agent according to claim 1 is characterized in that: described complexing agent is the oxalic acid tetraacethyl disodium.
5. a kind of environment-friendly type iron and steel room temperature blackening agent according to claim 1 is characterized in that: described wetting agent is a polyoxyethylene glycol 800.
6. a kind of environment-friendly type iron and steel room temperature blackening agent according to claim 1 is characterized in that: described pH regulator agent is a sulfuric acid.
7. the preparation method of the described environment-friendly type iron and steel room temperature blackening agent of claim 1 is characterized in that: may further comprise the steps:
(1) proportioning by claim 1 takes by weighing raw material;
(2) with CuSO 45H 2O, Na 2S 2O 36H 2O is soluble in water, and to make the work in-process treatment solution standby;
(3) with (NH 4) 6Mo 7O 24, NiSO 46H 2O, rare-earth salts is soluble in water, waits to dissolve the back and mixes with the work in-process treatment solution that step (2) makes, and fully stirs it is dissolved fully, and it is stand-by to make the work in-process treatment solution;
(4) add catalyzer, complexing agent and wetting agent successively in the work in-process treatment solution that in step (3), makes, evenly stir in the adition process, after the components dissolved for the treatment of to add earlier, continue to add next component again;
(5) adding an amount of water to the volume of treatment agent in the work in-process treatment solution that step (4) makes is 1L, and is 1-3 with pH regulator agent adjusting pH value.
CN 201010570982 2010-12-02 2010-12-02 Environmental-friendly room-temperature steel blackening agent and preparation method thereof Pending CN102011117A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102994996A (en) * 2012-12-06 2013-03-27 三达奥克化学股份有限公司 Non-toxic environment-friendly normal temperature steel nigrescence treating agent and preparation method thereof
CN103046038A (en) * 2012-12-06 2013-04-17 安徽未来表面技术有限公司 Room temperature blackening agent suitable for iron casting and method for preparing room temperature blackening agent suitable for iron casting
CN103205790A (en) * 2013-04-09 2013-07-17 安平县千鼎丝网有限公司 Black coloring process of stainless steel precision screen mesh
CN103290400A (en) * 2013-05-24 2013-09-11 湖南大学 Self-healing environment-friendly type steel normal-temperature blackening agent
CN104195538A (en) * 2014-09-03 2014-12-10 淮南天力生物工程开发有限公司 Non-selenium normal-temperature environment-friendly steel blackening liquid as well as preparation method thereof and blackening method
CN104451648A (en) * 2014-12-26 2015-03-25 湖南金裕化工有限公司 Iron and steel normal temperature rapid blackening solution and preparation method thereof
CN106544659A (en) * 2016-11-21 2017-03-29 衡阳市金泰安全生产检测检验有限公司 A kind of iron and steel room temperature blackening agent and preparation method thereof
CN106756922A (en) * 2017-01-23 2017-05-31 江苏理工学院 It is a kind of for the black chemical oxidation liquid of steel and its application
CN107354451A (en) * 2017-06-28 2017-11-17 常州市顺旭商贸有限公司 A kind of iron and steel casting room temperature blacking liquid and preparation method thereof
CN107365987A (en) * 2017-06-07 2017-11-21 常州建轩纺织品有限公司 A kind of high tack is without selenium room temperature blackening liquid
CN112011790A (en) * 2019-05-29 2020-12-01 北京铂阳顶荣光伏科技有限公司 Stainless steel foil blackening liquid for photovoltaic and blackening treatment method of stainless steel foil
CN113981428A (en) * 2021-10-27 2022-01-28 无锡高安科技有限公司 Metal blackening protection treating agent and preparation method thereof

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102994996A (en) * 2012-12-06 2013-03-27 三达奥克化学股份有限公司 Non-toxic environment-friendly normal temperature steel nigrescence treating agent and preparation method thereof
CN103046038A (en) * 2012-12-06 2013-04-17 安徽未来表面技术有限公司 Room temperature blackening agent suitable for iron casting and method for preparing room temperature blackening agent suitable for iron casting
CN103205790A (en) * 2013-04-09 2013-07-17 安平县千鼎丝网有限公司 Black coloring process of stainless steel precision screen mesh
CN103205790B (en) * 2013-04-09 2015-07-22 安平县千鼎丝网有限公司 Black coloring process of stainless steel precision screen mesh
CN103290400B (en) * 2013-05-24 2015-04-08 湖南大学 Self-healing environment-friendly type steel normal-temperature blackening agent
CN103290400A (en) * 2013-05-24 2013-09-11 湖南大学 Self-healing environment-friendly type steel normal-temperature blackening agent
CN104195538A (en) * 2014-09-03 2014-12-10 淮南天力生物工程开发有限公司 Non-selenium normal-temperature environment-friendly steel blackening liquid as well as preparation method thereof and blackening method
CN104451648A (en) * 2014-12-26 2015-03-25 湖南金裕化工有限公司 Iron and steel normal temperature rapid blackening solution and preparation method thereof
CN104451648B (en) * 2014-12-26 2017-07-11 湖南金裕化工有限公司 Steel normal temperature quick black liquid and preparation method thereof
CN106544659A (en) * 2016-11-21 2017-03-29 衡阳市金泰安全生产检测检验有限公司 A kind of iron and steel room temperature blackening agent and preparation method thereof
CN106756922A (en) * 2017-01-23 2017-05-31 江苏理工学院 It is a kind of for the black chemical oxidation liquid of steel and its application
CN107365987A (en) * 2017-06-07 2017-11-21 常州建轩纺织品有限公司 A kind of high tack is without selenium room temperature blackening liquid
CN107354451A (en) * 2017-06-28 2017-11-17 常州市顺旭商贸有限公司 A kind of iron and steel casting room temperature blacking liquid and preparation method thereof
CN112011790A (en) * 2019-05-29 2020-12-01 北京铂阳顶荣光伏科技有限公司 Stainless steel foil blackening liquid for photovoltaic and blackening treatment method of stainless steel foil
CN113981428A (en) * 2021-10-27 2022-01-28 无锡高安科技有限公司 Metal blackening protection treating agent and preparation method thereof

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Application publication date: 20110413