CN105315829A - Room-temperature rust removal blackening agent and preparation method thereof - Google Patents

Room-temperature rust removal blackening agent and preparation method thereof Download PDF

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Publication number
CN105315829A
CN105315829A CN201510888692.2A CN201510888692A CN105315829A CN 105315829 A CN105315829 A CN 105315829A CN 201510888692 A CN201510888692 A CN 201510888692A CN 105315829 A CN105315829 A CN 105315829A
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blackening
emulsion
normal temperature
stir
parts
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CN105315829B (en
Inventor
古绪鹏
邰淼
陈乐柱
乔红斌
夏友谊
胡红霞
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MAANSHAN AHUT INDUSTRIAL TECHNOLOGY RESEARCH INSTITUTE Co Ltd
MAANSHAN SANJIANG MACHINERY CO Ltd
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MAANSHAN AHUT INDUSTRIAL TECHNOLOGY RESEARCH INSTITUTE Co Ltd
MAANSHAN SANJIANG MACHINERY CO Ltd
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Abstract

The invention discloses a room-temperature rust removal blackening agent and a preparation method thereof, and belongs to the technical field of metal surface anti-corrosion treatment. The rust removal blackening agent is prepared from a rust removal solution, a blackening solution, a composite emulsion, nano-montmorillonite, a polyaniline emulsion, texanol ester alcohol, glycerinum and deionized water. The method comprises the following steps: preparing the rust removal solution, the blackening solution and the composite emulsion, and then respectively adding the nano-montmorillonite, the glycerinum and the polyaniline emulsion to the specified amount of deionized water; adding the rust removal solution under a continuous stirring condition, stirring evenly, and slowly adding the blackening solution; further stirring and dispersing, and then slowly adding the composite emulsion; and slowly adding the texanol ester alcohol and further stirring under a room temperature condition, so as to prepare the room-temperature rust removal blackening agent. The room-temperature rust removal blackening agent disclosed by the invention can directly carry out rust removal and blackening on the steel surface to replace the technologies of acid pickling, rust removing and the like. The room-temperature rust removal blackening agent has the characteristics of high rust removal blackening speed, excellent antiseptic property and the like.

Description

A kind of normal temperature rust cleaning blackening agent for surface and preparation method thereof
Technical field:
The invention belongs to Metal surface anti-corrosion processing technology field, be specifically related to relate to a kind of steel surface process normal temperature rust cleaning blackening agent for surface and preparation method thereof.
Background technology:
At present, needing to carry out its technique of blackening process at component surface for preventing the rust corrosion of steel-iron components generally adopts oil removing → water rinse → rust cleaning → water rinse → activation → water rinse → blackout → water rinse → leaching dewatering rust preventive oil to close, most room temperature blacking liquids that prior art uses are all containing selenide, selenide price is not only expensive but also have severe toxicity, and life-time service certainly will cause environmental pollution.Chinese patent CN201310199938.6 discloses a kind of self-healing Environmental Blackening Agent At Room Temperature For Steel, this blackening agent for surface adopts the preparations such as cupric nitrate, Ammonium Molybdate Tetrahydrate, Sulfothiorine, SODIUM PHOSPHATE, MONOBASIC, oxalic acid, single nickel salt, dimethyl formamide, lanthanum trioxide, potassium aluminium sulfate, sodium-chlor, citric acid and tensio-active agent, this blackening agent for surface blackout ability is comparatively strong, simple without selenium environmental protection, technique, the Chemical Colouring of Steel at Room Temperature rete of blackout gained has good solidity to corrosion and self-healing, but have that solution precipitation is many, blackout layer and the shortcoming such as matrix metal bonding force is poor.Chinese patent CN201110030425.3 discloses a kind of zinc-chromium membrane blackening agent, and raw material is in mass ratio: trifluorochloroethylene: 78-90%; Blackening agent for surface (carbon black): 2-5%; Vinyl chlorosilane: 0.1-0.5%; Primary zinc phosphate and ferric sulfate: 3-5%; Sodium laurylsulfonate: 0.1-1%; Full methyl-etherified aminoresin: 0.1-0.6% mixes, blackening layer of this invention process is the rete that one deck contains fluoride resin, and rete outward appearance is evenly shiny black, avoids traditional enamelling process and to show money or valuables one carries unintentionally phenomenon, but blackening agent for surface poor stability prepared by this technique, resin and carbon black dispersion are stable not.Both invention disclosed patents all need acid pickling and rust removing above, blackening agent for surface blackening agent for surface of the present invention is simple without selenium environmental protection, preparation technology, directly in steel surface rust cleaning blackout, with techniques such as alternative acid pickling and rust removings, and the feature that blackout speed is fast and antiseptic property is excellent that eliminates rust can be had.
Summary of the invention:
The present invention is directed to the above-mentioned technical problem that rust cleaning blackening agent for surface exists, a kind of normal temperature rust cleaning blackening agent for surface and preparation method are provided, this blackening agent for surface can directly in steel surface rust cleaning blackout, in order to avoid remove the techniques such as acid pickling and rust removing and selenium-containing compound, and there is the rust cleaning blackout speed advantage that blackout is even, antiseptic property is excellent soon.
Composition and the mass percent thereof of a kind of normal temperature rust cleaning blackening agent for surface provided by the present invention are:
Described composite emulsion is modified acroleic acid antirust emulsion, ACURE805 emulsion and epoxy emulsion are composited; Described rust removing solution is that oxalic acid, phosphoric acid, zinc phosphate and deionized water are composited; Described hair blackening liquid is that pyrogallol, Whitfield's ointment, Sunmorl N 60S and deionized water are composited; Described Polyaniline emulsion is with Witco 1298 Soft Acid and Weibull Tree-tea interplantation and employing micro emulsion legal system is standby.
Preparation method's concrete steps of a kind of normal temperature rust cleaning blackening agent for surface provided by the present invention are as follows:
(1) rust removing solution is prepared:
Get 5 parts of oxalic acids to be added in 70 parts of deionizations water and to stir and make it dissolve completely, then the phosphoric acid slowly adding 20 parts of 85wt% stirs, finally add 5 parts of zinc phosphates continue to stir 0.5h under normal temperature condition after obtained described rust removing solution.
(2) hair blackening liquid is prepared:
In 78 parts of deionized waters, first add 10 parts of pyrogallols stir and make it dissolve completely, then add 10 parts of Whitfield's ointments and stir, finally add 2 parts of Sunmorl N 60Ss, obtained described hair blackening liquid after continuing to stir 0.5h under normal temperature condition.
(3) composite emulsion is prepared:
Get 10 parts of epoxy emulsions to be added in 60 parts of modification acrylate antirust emulsions and to stir, then add 30 parts of described ACURE805 emulsions, obtained described composite emulsion after stirring at normal temperature 20min makes it be uniformly dispersed completely.
(4) target product normal temperature rust cleaning blackening agent for surface is prepared:
In the deionized water of specified amount, add described nano imvite, glycerine and Polyaniline emulsion respectively stir, rust removing solution prepared by step (1) is first added when constantly stirring, hair blackening liquid prepared by step (2) is slowly added again after stirring, continue dispersed with stirring 20min, slowly add composite emulsion prepared by step (3) again, finally slowly add lauryl alcohol ester, continue to stir 0.5h at normal temperature condition and obtain described normal temperature rust cleaning blackening agent for surface.
Described modified acroleic acid antirust emulsion is the WH3108 type antirust emulsion that Ningjin, Shandong five lakes Chemical Co., Ltd. produces; Described ACURE805 emulsion is a kind of aliphatics Anionic Polyurethane Dispersion containing polycarbonate of source, Shanghai standing grain Chemical Manufacture; Described nano imvite is the SMP-X40 model nano imvite that Zhejiang Fenghong New Material Co., Ltd. produces.
It is composite cleverly that the present invention adopts rust removing solution, hair blackening liquid and composite emulsion to carry out, directly can eliminate rust on the surface of the steel and iron member got rusty, turn black and film forming thus by rust cleaning, turn black in one, there is the feature of Simplified flowsheet, decreasing pollution; Substitute toxic selenium-containing compound owing to adopting the environment-friendly type hair blackening liquid of pyrogallol, Whitfield's ointment, Sunmorl N 60S composition and create beyond thought blackout preservative effect at compound system, because filming emulsion and Polyaniline emulsion can make film forming after blackout fine and close and due to the fabulous corrosion inhibition of polyaniline, add film coalescence aid lauryl alcohol ester and nano imvite, thus significantly improve blackening agent for surface antiseptic property.In addition, owing to adopting the compound of modified acroleic acid, water-base epoxy and the aliphatics Anionic Polyurethane Dispersion containing polycarbonate, play performance outstanding separately, because urethane, epoxy resin have low, the excellent water tolerance of film-forming temperature and sticking power, acrylic resin, urethane have good weathering resistance, gloss retention, make film forming matter emulsion " maximize favourable factors and minimize unfavourable ones " separately therefore can to produce beyond thought positively effect.
The present invention have rust cleaning and blackout speed fast and evenly, room temperature blackening, easy construction, the rust cleaning that directly can be used in steel beam column surface, blackout, rotproofing and containing features such as toxic substances, therefore product energy-conserving and environment-protective of the present invention.
Embodiment:
Embodiment 1: preparation method's concrete steps of a kind of normal temperature of the present invention rust cleaning blackening agent for surface are as follows:
(1) preparation of rust removing solution:
Get 5 grams of oxalic acids to be added in 70 grams of deionizations water and to stir and make it dissolve completely, then the phosphoric acid slowly adding 20 gram 85% stirs, and finally adds after 5 grams of zinc phosphates continue to stir 0.5h under normal temperature condition and just can obtain rust removing solution.
(2) preparation of hair blackening liquid:
In 78 grams of deionized waters, first add 10 grams of pyrogallols stir and make it dissolve completely, then add 10 grams of Whitfield's ointments and stir, finally add 2 grams of Sunmorl N 60Ss, continue to stir 0.5h under normal temperature condition after just can obtain hair blackening liquid.
(3) preparation of composite emulsion:
Get 10 grams of epoxy emulsions to be added in 60 grams of modification acrylate antirust emulsions and to stir, then add 30 grams of ACURE805 emulsions, stirring at normal temperature 20min makes it be uniformly dispersed completely just can obtain composite emulsion.
(4) target product normal temperature rust cleaning blackening agent for surface is prepared:
In 60 grams of deionized waters, add 0.1 gram of nano imvite, 0.4 gram of glycerine and 0.5 gram of Polyaniline emulsion respectively stir, rust removing solution prepared by 10 grams of steps (1) is first added when constantly stirring, hair blackening liquid prepared by 5 grams of steps (2) is slowly added again after stirring, continue dispersed with stirring 20min, slowly add 20 grams of step (3) composite emulsion again, finally slowly add 0.5 gram of lauryl alcohol ester, continue to stir 0.5h at normal temperature condition and obtain described normal temperature rust cleaning blackening agent for surface.
Embodiment 2: preparation method's concrete steps of a kind of normal temperature of the present invention rust cleaning blackening agent for surface are as follows:
Step (1), (2) and (3) are with embodiment 1.
(4) target product normal temperature rust cleaning blackening agent for surface is prepared:
In 50 grams of deionized waters, add 0.05 gram of nano imvite, 0.2 gram of glycerine and 0.6 gram of Polyaniline emulsion respectively stir, rust removing solution prepared by 16 grams of steps (1) is first added when constantly stirring, hair blackening liquid prepared by 4 grams of steps (2) is slowly added again after stirring, continue dispersed with stirring 20min, slowly add 15 grams of step (3) composite emulsion again, finally slowly add 0.5 gram of lauryl alcohol ester, continue to stir 0.5h at normal temperature condition and obtain described normal temperature rust cleaning blackening agent for surface.
Embodiment 3: preparation method's concrete steps of a kind of normal temperature of the present invention rust cleaning blackening agent for surface are as follows:
Step (1), (2) and (3) are with embodiment 1.
(4) target product normal temperature rust cleaning blackening agent for surface is prepared:
In 65 grams of deionized waters, add 0.15 gram of nano imvite, 0.3 gram of glycerine and 0.8 gram of Polyaniline emulsion respectively stir, rust removing solution prepared by 6 grams of steps (1) is first added when constantly stirring, hair blackening liquid prepared by 10 grams of steps (2) is slowly added again after stirring, continue dispersed with stirring 20min, slowly add 25 grams of step (3) composite emulsion again, finally slowly add 1 gram of lauryl alcohol ester, continue to stir 0.5h at normal temperature condition and obtain described normal temperature rust cleaning blackening agent for surface.
Embodiment 4: preparation method's concrete steps of a kind of normal temperature of the present invention rust cleaning blackening agent for surface are as follows:
Step (1), (2) and (3) are with embodiment 1.
(4) target product normal temperature rust cleaning blackening agent for surface is prepared:
In 65 grams of deionized waters, add 0.1 gram of nano imvite, 0.2 gram of glycerine and 0.5 gram of Polyaniline emulsion respectively stir, rust removing solution prepared by 10 grams of steps (1) is first added when constantly stirring, hair blackening liquid prepared by 7 grams of steps (2) is slowly added again after stirring, continue dispersed with stirring 20min, slowly add 20 grams of step (3) composite emulsion again, finally slowly add 0.8 gram of lauryl alcohol ester, continue to stir 0.5h at normal temperature condition and obtain described normal temperature rust cleaning blackening agent for surface.
Embodiment 5: preparation method's concrete steps of a kind of normal temperature of the present invention rust cleaning blackening agent for surface are as follows:
Step (1), (2) and (3) are with embodiment 1.
(4) target product normal temperature rust cleaning blackening agent for surface is prepared:
In 55 grams of deionized waters, add 0.15 gram of nano imvite, 0.5 gram of glycerine and 0.5 gram of Polyaniline emulsion respectively stir, rust removing solution prepared by 10 grams of steps (1) is first added when constantly stirring, hair blackening liquid prepared by 8 grams of steps (2) is slowly added again after stirring, continue dispersed with stirring 20min, slowly add 20 grams of step (3) composite emulsion again, finally slowly add 0.8 gram of lauryl alcohol ester, continue to stir 0.5h at normal temperature condition and obtain described normal temperature rust cleaning blackening agent for surface.
Embodiment 6: preparation method's concrete steps of a kind of normal temperature of the present invention rust cleaning blackening agent for surface are as follows:
Step (1), (2) and (3) are with embodiment 1.
(4) target product normal temperature rust cleaning blackening agent for surface is prepared:
In 60 grams of deionized waters, add 0.15 gram of nano imvite, 0.2 gram of glycerine and 0.6 gram of Polyaniline emulsion respectively stir, rust removing solution prepared by 15 grams of steps (1) is first added when constantly stirring, hair blackening liquid prepared by 10 grams of steps (2) is slowly added again after stirring, continue dispersed with stirring 20min, slowly add 25 grams of step (3) composite emulsion again, finally slowly add 0.6 gram of lauryl alcohol ester, continue to stir 0.5h at normal temperature condition and obtain described normal temperature rust cleaning blackening agent for surface.
Embodiment 7: preparation method's concrete steps of a kind of normal temperature of the present invention rust cleaning blackening agent for surface are as follows:
Step (1), (2) and (3) are with embodiment 1.
(4) target product normal temperature rust cleaning blackening agent for surface is prepared:
In 65 grams of deionized waters, add 0.12 gram of nano imvite, 0.4 gram of glycerine and 0.6 gram of Polyaniline emulsion respectively stir, rust removing solution prepared by 15 grams of steps (1) is first added when constantly stirring, hair blackening liquid prepared by 8 grams of steps (2) is slowly added again after stirring, continue dispersed with stirring 20min, slowly add 20 grams of step (3) composite emulsion again, finally slowly add 1 gram of lauryl alcohol ester, continue to stir 0.5h at normal temperature condition and obtain described normal temperature rust cleaning blackening agent for surface.
Embodiment 8: preparation method's concrete steps of a kind of normal temperature of the present invention rust cleaning blackening agent for surface are as follows:
Step (1), (2) and (3) are with embodiment 1.
(4) target product normal temperature rust cleaning blackening agent for surface is prepared:
In 50 grams of deionized waters, add 0.1 gram of nano imvite, 0.2 gram of glycerine and 0.6 gram of Polyaniline emulsion respectively stir, rust removing solution prepared by 8 grams of steps (1) is first added when constantly stirring, hair blackening liquid prepared by 8 grams of steps (2) is slowly added again after stirring, continue dispersed with stirring 20min, slowly add 20 grams of step (3) composite emulsion again, finally slowly add 0.5 gram of lauryl alcohol ester, continue to stir 0.5h at normal temperature condition and obtain described normal temperature rust cleaning blackening agent for surface.
Be placed in normal temperature rust cleaning blackening agent for surface prepared by embodiment of the present invention 1-8 by needing the steel and iron member of blackout at normal temperature and soak 3-5min, take out nature and dry and detect its performance, main detected result is in table 1.
Table 1 invention target product embodiment salient features
Embodiment Surface drying time/min Sticking power/time Resistance to copper sulfate time/min Blackening effect
1 42 560 770 Well
2 41 576 755 Well
3 46 570 760 Well
4 43 568 780 Well
5 44 575 760 Well
6 46 570 765 Well
7 45 569 755 Well
8 45 570 765 Well
CuSO 4drop is tested: take out the copper-bath drop of sample by standard after specimen surface is done, and then observes and record to occur the bolarious time.
Sticking power (bonding force) is tested: the greasy dirt cleaning specimen surface with the absorbent cotton being stained with alcohol, after its surface is completely dry, evenly rubs back and forth in the medium dynamics in the surface of sample with clean qualitative filter paper.Until write down Rubbing number when matrix appears in a certain point, be for 50-60 time generally qualified.

Claims (3)

1. a normal temperature rust cleaning blackening agent for surface, is characterized in that the composition of this normal temperature rust cleaning blackening agent for surface and mass percent thereof are:
Described composite emulsion is modified acroleic acid antirust emulsion, ACURE805 emulsion and epoxy emulsion are composited; Described rust removing solution is that oxalic acid, phosphoric acid, zinc phosphate and deionized water are composited; Described hair blackening liquid is that pyrogallol, Whitfield's ointment, Sunmorl N 60S and deionized water are composited; Described Polyaniline emulsion is with Witco 1298 Soft Acid and Weibull Tree-tea interplantation and employing micro emulsion legal system is standby.
2. a kind of normal temperature rust cleaning blackening agent for surface according to claim 1, is characterized in that described modified acroleic acid antirust emulsion is the WH3108 type antirust emulsion that Ningjin, Shandong five lakes Chemical Co., Ltd. produces; Described ACURE805 emulsion is a kind of aliphatics Anionic Polyurethane Dispersion containing polycarbonate of source, Shanghai standing grain Chemical Manufacture; Described nano imvite is the SMP-X40 model nano imvite that Zhejiang Fenghong New Material Co., Ltd. produces.
3. the preparation method of a kind of normal temperature rust cleaning blackening agent for surface described in claim 1, is characterized in that the method concrete steps are as follows:
(1) rust removing solution is prepared:
Get 5 parts of oxalic acids to be added in 70 parts of deionizations water and to stir and make it dissolve completely, then the phosphoric acid slowly adding 20 parts of 85wt% stirs, finally add 5 parts of zinc phosphates continue to stir 0.5h under normal temperature condition after obtained described rust removing solution;
(2) hair blackening liquid is prepared:
In 78 parts of deionized waters, first add 10 parts of pyrogallols stir and make it dissolve completely, then add 10 parts of Whitfield's ointments and stir, finally add 2 parts of Sunmorl N 60Ss, obtained described hair blackening liquid after continuing to stir 0.5h under normal temperature condition;
(3) composite emulsion is prepared:
Get 10 parts of epoxy emulsions to be added in 60 parts of modification acrylate antirust emulsions and to stir, then add 30 parts of described ACURE805 emulsions, obtained described composite emulsion after stirring at normal temperature 20min makes it be uniformly dispersed completely;
(4) normal temperature rust cleaning blackening agent for surface is prepared:
In the deionized water of specified amount, add described nano imvite, glycerine and Polyaniline emulsion respectively stir, rust removing solution prepared by step (1) is first added when constantly stirring, hair blackening liquid prepared by step (2) is slowly added again after stirring, continue dispersed with stirring 20min, slowly add composite emulsion prepared by step (3) again, finally slowly add lauryl alcohol ester, continue to stir 0.5h at normal temperature condition and obtain described normal temperature rust cleaning blackening agent for surface.
CN201510888692.2A 2015-12-02 2015-12-02 Room-temperature rust removal blackening agent and preparation method thereof Active CN105315829B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106868490A (en) * 2016-12-22 2017-06-20 当涂县宏宇金属炉料有限责任公司 A kind of environmentally friendly stainless steel blackening process method
CN110527397A (en) * 2018-05-24 2019-12-03 中山市珍视新材料科技有限公司 A kind of aqueous steel surface blackening agent for surface and preparation method thereof
CN110923683A (en) * 2019-12-30 2020-03-27 湖南金化科技集团有限公司 Self-repairing normal-temperature blackening agent for cold-drawn steel pipe and preparation method and application thereof
CN111087877A (en) * 2019-12-30 2020-05-01 湖南金化科技集团有限公司 Oil immersion-free antirust blackening agent and preparation method and application thereof
CN115613019A (en) * 2022-09-29 2023-01-17 南京科润工业介质股份有限公司 Waste heat blackening liquid for workpiece suitable for full-automatic weighing and packaging machine subpackaging

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CN102154638A (en) * 2011-03-21 2011-08-17 厦门大学 Brass part blackening solution and preparation method and application thereof
CN103450762A (en) * 2013-09-24 2013-12-18 安徽工业大学 Water-based polyaniline composite epoxy rusted anti-corrosion paint and preparation method thereof
CN103726060A (en) * 2013-12-18 2014-04-16 江苏富邦纺织有限公司 Metal surface rust remover

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CN102031510A (en) * 2010-12-30 2011-04-27 合肥华清金属表面处理有限责任公司 Metal zinc coating blackening agent and preparation method thereof
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106868490A (en) * 2016-12-22 2017-06-20 当涂县宏宇金属炉料有限责任公司 A kind of environmentally friendly stainless steel blackening process method
CN110527397A (en) * 2018-05-24 2019-12-03 中山市珍视新材料科技有限公司 A kind of aqueous steel surface blackening agent for surface and preparation method thereof
CN110923683A (en) * 2019-12-30 2020-03-27 湖南金化科技集团有限公司 Self-repairing normal-temperature blackening agent for cold-drawn steel pipe and preparation method and application thereof
CN111087877A (en) * 2019-12-30 2020-05-01 湖南金化科技集团有限公司 Oil immersion-free antirust blackening agent and preparation method and application thereof
CN111087877B (en) * 2019-12-30 2021-10-08 湖南金化科技集团有限公司 Oil immersion-free antirust blackening agent and preparation method and application thereof
CN110923683B (en) * 2019-12-30 2021-11-02 湖南金化科技集团有限公司 Self-repairing normal-temperature blackening agent for cold-drawn steel pipe and preparation method and application thereof
CN115613019A (en) * 2022-09-29 2023-01-17 南京科润工业介质股份有限公司 Waste heat blackening liquid for workpiece suitable for full-automatic weighing and packaging machine subpackaging

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