CN107574429A - A kind of organic nigrescence oil and preparation method thereof - Google Patents
A kind of organic nigrescence oil and preparation method thereof Download PDFInfo
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Abstract
Black the invention discloses a kind of organic waste heat oily, mixed together by the component of following mass fraction：5~10 parts of base oils, 2~5 parts of oil-soluble antirust corrosion inhibiter, 0.5~1 part of emulsifying agent, pH buffer, 0.3~1 part of coalescents, water:75~85 parts, water-base resin：0.5~1.25 part, aqueous color paste：0.05~0.125 part and 1~3 part of complexing agent.The invention also discloses above-mentioned organic nigrescence oil and preparation method thereof.The nigrescence oil of the present invention can workpiece surface be formed densification oxidation black film, because the black film has very high corrosion resistance and bright property in itself, so as to substantially increase the decay resistance of workpiece, and make the workpiece that draws not only black but also bright；The organic principle to black in addition in the present invention used in oil will not pollute to environment；The preparation method technical process of the nigrescence oil of the present invention is simple, and energy consumption is low, cost is low.
Description
Technical field
Black the present invention relates to one kind oily, more particularly to a kind of organic waste heat nigrescence oil, the invention further relates to above-mentioned organic
The preparation method of waste heat nigrescence oil.
Background technology
Blackening refers to the method by physics or chemistry, and the black protective film of densification is formed in surface of workpiece
Layer, so as to strengthen the antirust ability of workpiece, while beautifies the outward appearance of workpiece.Different according to film forming mechanism, blackening can divide
For oxidizing blackening, room temperature blackening, phosphatization blacks, phosphatization blacks and blacked with waste heat.
Oxidizing blackening is to form one layer of fine and close ferroso-ferric oxide film layer in steel surface, so as to reach the purpose of nigrescence.
Most common oxidizing blackening mode is that soda boiling blacks, and main technique is by sodium hydroxide, sodium nitrate, natrium nitrosum and some additions
Agent wiring solution-forming in proportion, then invades solution 30-40 minutes by steel under conditions of 140-180 degree, obtains four oxidations
Three-iron film layer.Nigrescence film layer that the technique obtains is fine and close, corrosion resistance is good, and thickness does not have to workpiece size precision in 1 microns
It is obvious to influence, but the process energy consumption is high, pollution is big, efficiency is low, very big to operator's actual bodily harm, is forced to wash in a pan
Eliminate.
The technology that room temperature blackening grows up the eighties from twentieth century, general principle is base material table in acid condition
Face occurs displacement reaction with the soluble copper salt in solution and produces copper, reacts, generates with the other compositions in solution immediately
The insoluble mantoquita of black simultaneously deposits to substrate surface, so as to reach the purpose of nigrescence.Room temperature blackening is broadly divided into system containing selenium
With without selenium system.The oxide of selenium is needed to use in system containing selenium, its is expensive, has severe toxicity, environment can be polluted, together
When very big injury is caused to human body, significantly limit its development, no selenium system is the master of present room temperature blackening technology development
Stream.The maximum feature of room temperature blackening is to black at normal temperatures, and energy consumption is low；Its speed development simultaneously is fast, and stoste, which blacks, to be needed only to
Ten seconds or so, improve production efficiency；The technology is applicable different metal materials simultaneously.But existing room temperature blackening technique
Generally existing be difficult to control film forming matter deposition uniformity, stability is poor, solution is difficult to safeguard, film layer corrosion-resistant, attached
Put forth effort the shortcomings of poor, to workpiece degreasing and rust removal pre-processing requirements height, complex process.
Waste heat black be using workpiece surface heat treatment or other process in waste heat, make iron and steel parts with
The moment contacted in hair blackening liquid with hair blackening liquid, surface formed one layer be firmly combined with, black high molecula resin film difficult for drop-off
Layer.The technique is simple to operation, does not require thorough degreasing and rust removal before workpiece nigrescence, and production efficiency is high, is adapted to production line balance, groove
Liquid length digestion period, film adhesion is strong, color is uniform.Chinese patent CN105063598A discloses one kind and utilizes workpiece quenching
Or the residual temperature after tempering uses the method that thermoplastic resin and colourless mill base black in workpiece surface.But the nigrescence mode obtains
Film layer plays pigmentation, but salt-fog resistant time does not reach more than 8 hours, and obtains black film and lack gloss, Wu Faman
The long-term anti-corrosion in outdoor of sufficient workpiece and shinny requirement.Therefore, a kind of oxidizing blackening film layer that densification can be formed in workpiece surface, from
And the exploitation for improving the salt fog time of workpiece and the waste heat nigrescence oil of bright property is necessary.
The content of the invention
Technical problem：To be solved by this invention to be to provide a kind of organic waste heat nigrescence oil, nigrescence oil is utilized more than workpiece
Heat, the double-deck nigrescence film layer of densification can be formed in workpiece surface, because the duplicature has very high corrosion resistance in itself, and
And film layer has oil component in itself, so as to substantially increase the decay resistance of workpiece and glossiness so that workpiece seem and
It is black and bright.The present invention also technical problems to be solved are to provide the preparation method of above-mentioned organic waste heat blackening agent for surface, the preparation in addition
Technique is simple, and cost is low.
Technical scheme：In order to solve the above technical problems, the technical solution adopted in the present invention is：
A kind of organic waste heat nigrescence oil of the present invention, is mixed together by the component of following mass fraction：5~10 parts of bases
Plinth oil, 2~5 parts of oil-soluble antirust corrosion inhibiter, 0.5~1 part of emulsifying agent, pH buffer, 0.3~1 part of coalescents, water:75~
85 parts, water-base resin：0.5~1.25 part, aqueous color paste：0.05~0.125 part and 1~3 part of complexing agent.
Further preferably, described base oil be white oil, paraffin oil, naphthenic oil either in lubricating oil any one or
Any two kinds of mixing in any proportion.
Further preferably, described oil-soluble inhibitor is alkali salt, lead naphthenate, the ring of aliphatic acid or aphthenic acids
Alkanoic acid zinc, petroleum sodium sulfonate, barium mahogany sulfonate, calcium mahogany sulfonate, three oleic acid tallow diamines, rosin amine, anhydrous sorbitol list oil
Acid esters, glycol dioleate, polyglycol distearate, oleoylsarcosine and its amine salt, amide imidazoline, benzo
Any one in triazole or alkyl phosphate or any two kinds of mixing in any proportion.
Further preferably, described coalescents include wetting agent, bactericide, defoamer and levelling agent；
Wherein, described wetting agent is Nonyl pheno base ether, octyl phenol polyoxyethylene ether, fatty alcohol polyoxy second
Either any one in alkylphenol-polyethenoxy base ether or any two kinds of mixing proportionally of alkene ether, polyethylene glycol；
Described bactericide is sodium benzoate, ethoxy perhydro-s-triazine, the chloro- 3- methylphenols of 4-, the iodo- 2-propynyls of 3-
Any one in butyl carbamate or 2- methyl sulphur -4- ethylamino -6- spy's fourth amino -1,3,5- triazines is any two kinds
Mixing in any proportion；
The defoamer be higher alcohol, organosiloxane or polyoxyethylene polyoxypropylene copolymer in any one or
Any two kinds mix in any proportion；
The levelling agent be silicone oil, dipropylene glycol methyl ether, ethylene glycol phenyl ether, glycerine phenylate or the third three it is purebred any one
Or any two kinds proportionally mix；
Further preferably, the water-base resin is water soluble acrylic resin, pure-acrylic emulsion, styrene-acrylic emulsion, polyurethane breast
Any one in liquid or polycarbonate emulsion or any two kinds of mixing in any proportion.
Further preferably, described emulsifying agent be S-80, T-80, T-60, OP-10, it is milky white spirit or paraffinic base emulsifying agent
In any one or any two kinds of mixing in any proportion.
Further preferably, described complexing agent is ethylenediamine tetra-acetic acid, tartaric acid, citric acid, malic acid, lactic acid or Portugal
The sylvite of any one in grape saccharic acid；The complexing agent be ethylenediamine tetra-acetic acid, tartaric acid, citric acid, malic acid, lactic acid or
The sodium salt of any one in gluconic acid；Described complexing agent is ethylenediamine tetra-acetic acid, tartaric acid, citric acid, malic acid, breast
The ammonium salt of any one in acid or gluconic acid.
The preparation method of above-mentioned organic waste heat nigrescence oil of the present invention, comprises the following steps：
Step 1, base oil, oil-soluble inhibitor, water, pH adjusting agent, bactericide are added sequentially in stirred tank, stirred
It is under 50-100 revs/min that material stirring is uniform to mix speed；
Step 2, while stirring toward adding required water in the mixed material in step 1, in 50-100/ points of stir speed (S.S.)
It is lower that material stirring is uniform；
Step 3, while stirring toward required coalescents are added in the mixed material in step 1, in stir speed (S.S.) 50-
It is under 100/ point that material stirring is uniform；
Step 4, while stirring toward adding required water-base resin and aqueous color paste in the mixed material in step 1,
Uniformly can set aside for use by material stirring under 30-70/ points of stir speed (S.S.).
The above-mentioned waste heat nigrescence oil being made into is diluted with water into 2%-8% hair blackening liquid, is 400-600 degree steels by temperature
In workpiece intrusion hair blackening liquid, workpiece is taken out after the 10-90 seconds with hot blast drying, drying or is dried in atmosphere, it is possible in work
Part surface forms corrosion resistance, the good black film of glossiness.
The pH adjusting agent is ammoniacal liquor, monoethanolamine, diethanol amine, triethanolamine, 2-amino-2-methyl-1-propanol, 2-
In amino -2- ethyl -1,3- propane diols or 2- dimethylaminos -2- methyl isophthalic acids-propyl alcohol any one or it is any two kinds by any
The mixing of ratio.
Beneficial effect：Compared to existing waste heat blackening agent for surface, nigrescence oil of the invention can form densification in workpiece surface
Oxidation film layer, because the film layer has high decay resistance in itself, so as to substantially increase the decay resistance of workpiece；In addition
Contain base oil in the present invention, it is all no longer to need to carry out anti-corrosion toward workpiece surface dip-coating machinery oil, greatly save cost；Also
Organic principle used in present invention nigrescence oil will not pollute to environment；The nigrescence oil of the last present invention can be widely applied to
Fastener, chain piece, spring, saw blade and the blackening process of all kinds of machineries and auto parts and components of all size, especially for heat
Continuous production technology is handled, workpiece is brought directly to enter in nigrescence groove after melting down by guipure to black, and by guipure from nigrescence
Taken out of in groove, so as to improve the efficiency of whole production process, the present invention blacks, and oily preparation method is simple, and energy consumption is low, cost
It is low.
Embodiment
Example is applied according to following, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that implement
Content described by example is merely to illustrate the present invention, without should be also without limitation on the present invention described in detail in power book.
Example is applied according to following, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that implement
Content described by example is merely to illustrate the present invention, without should be also without limitation on the present invention described in detail in power book.
Embodiment 1：
By 5.3 parts of naphthene base crude oils, 2.5 parts of oil-soluble inhibitors, 1 part of S-80 and T-80 mixture, 0.7 part of water, 0.3 part three
Monoethanolamine, 0.2 part of bactericide, under 60 revs/min of stirring, add the emulsion that water is diluted to 15% mass concentration；By second two
1 part of amine tetrem acid sodium-salt, 0.05 part of octyl phenol polyoxyethylene ether, 0.05 part of organosiloxane, 0.05 part of dipropylene glycol methyl ether,
0.5 part of 3824 acrylic resin, 0.05 part of carbon black color paste, the hair blackening liquid of 1.25 parts of compositions of water stir under 60 turns of stirrings；
Then the hair blackening liquid is added in above emulsification dilution, the waste heat nigrescence oil of the present invention is made after stirring.
Bolt is heated to 450 degree in net belt type tempering furnace, after being incubated one hour, is immersed with guipure and implements to send out in 1
In dirty oil, workpiece with guipure is lifted out liquid after being soaked 20 seconds in the oil that blacks, by workpiece in 80 degree of hot blast dryings, in workpiece surface
Fine and close oxidation film layer is formed, and glossiness is good.Change workpiece and carry out 5% neutral salt spray test, 8 hours nothings according to GB/T 10125
Corrosion.
The waste heat that present invention nigrescence oil is carried using workpiece in preceding working procedure, in the presence of workpiece waste heat, black oil
Middle composition forms dense oxide film layer in workpiece surface.Simultaneously because base oil composition in the oil that blacks so that the black film is again black
It is again bright.
Present invention nigrescence oil can be widely applied to fastener, chain piece, spring, the saw blade and all kinds of mechanical zero of all size
The blackening process of part.Especially for heat treatment continuous production technology, it is brought directly to black by guipure after the tempered stove of workpiece
Blackening process is carried out in groove, and is taken out of by guipure from nigrescence groove, nigrescence workpiece is not bonded on guipure.The present invention blacks oil in work
Part surface forms even film layer, and 3% cupric sulphate dropping test meets GB/T15519 criterion of acceptability, 8 hours nothings of nigrescence workpiece
Rust staining point；According to 5% neutral salt spray test standard method in GB/T10125, non-corroding in nigrescence workpiece 8 hours.
Embodiment 2：
By 5 parts of 150SN base oils, 2.4 parts of oil-soluble inhibitors, 0.8 part of S-80 and T-80 mixture, 1.3 parts of water, 0.25
Part triethanolamine, 0.25 part of bactericide, under 80 revs/min of stirring, add the emulsion that water is diluted to 14% mass concentration；By
1.5 parts of ethylene diamine tetraacetic acid sylvites, 0.05 part of alkylphenol-polyethenoxy base ether, 0.08 part of higher alcohol, 0.08 part, 1 part of silicone oil
3100 acrylic resins, 0.1 part of carbon black color paste, the hair blackening liquid of 2.8 parts of compositions of water stir under 80 turns of stirrings；Then this
Hair blackening liquid is added in above emulsification dilution, and the waste heat nigrescence oil of the present invention is made after stirring.
Metal nut is heated to 500 degree in net belt type tempering furnace, after being incubated one hour, is immersed with guipure and implements 2
In the middle oil that blacks, workpiece with guipure is lifted out liquid after being soaked 15 seconds in the oil that blacks, by workpiece in 100 degree of hot blast dryings, in work
Part surface forms the oxidation film layer of densification, and glossiness is good.Change workpiece according to GB/T10125 carry out 5% neutral salt spray test, 8
Hour non-corroding.
The waste heat that present invention nigrescence oil is carried using workpiece in preceding working procedure, in the presence of workpiece waste heat, black oil
Middle composition forms dense oxide film layer in workpiece surface.Simultaneously because base oil composition in the oil that blacks so that the black film is again black
It is again bright.
Present invention nigrescence oil can be widely applied to fastener, chain piece, spring, the saw blade and all kinds of mechanical zero of all size
The blackening process of part.Especially for heat treatment continuous production technology, it is brought directly to black by guipure after the tempered stove of workpiece
Blackening process is carried out in groove, and is taken out of by guipure from nigrescence groove, nigrescence workpiece is not bonded on guipure.The present invention blacks oil in work
Part surface forms even film layer, and 3% cupric sulphate dropping test meets GB/T15519 criterion of acceptability, 8 hours nothings of nigrescence workpiece
Rust staining point；According to 5% neutral salt spray test standard method in GB/T10125, non-corroding in nigrescence workpiece 8 hours.
Embodiment 3:
By 5.4 parts of white oil (kinematic viscosity 22MM2/ S), 2.6 parts of oil-soluble inhibitors, 0.9 part of S-80 and T-80 mixture,
0.6 part of water, 0.26 part of triethanolamine, 0.24 part of bactericide, under 90 revs/min of stirring, it is dense that addition water is diluted to 12% mass
The emulsion of degree；By 2 parts of glucose sodium salts, 0.15 part of Nonyl pheno base ether, 0.15 part of polyoxyethylene polyoxypropylene, second
0.15 part, 1.5 part 3100 acrylic resin of glycol phenylate, 0.15 part of carbon black color paste, the hair blackening liquid of 4.35 parts of compositions of water is at 90 turns
Stirred under stirring；Then the hair blackening liquid is added in above emulsification dilution, the remaining of the present invention is made after stirring
Heat blacks oily.
Metal nut is heated to 400 degree in net belt type tempering furnace, after being incubated one hour, is immersed with guipure and implements 2
In the middle oil that blacks, workpiece with guipure is lifted out liquid after being soaked 30 seconds in the oil that blacks, by workpiece in 90 degree of hot blast dryings, in workpiece
Surface forms the oxidation film layer of densification, and glossiness is good.Change workpiece and carry out 5% neutral salt spray test according to GB/T10125,8 is small
When non-corroding.
The waste heat that present invention nigrescence oil is carried using workpiece in preceding working procedure, in the presence of workpiece waste heat, black oil
Middle composition forms dense oxide film layer in workpiece surface.Simultaneously because base oil composition in the oil that blacks so that the black film is again black
It is again bright.
Present invention nigrescence oil can be widely applied to fastener, chain piece, spring, the saw blade and all kinds of mechanical zero of all size
The blackening process of part.Especially for heat treatment continuous production technology, it is brought directly to black by guipure after the tempered stove of workpiece
Blackening process is carried out in groove, and is taken out of by guipure from nigrescence groove, nigrescence workpiece is not bonded on guipure.The present invention blacks oil in work
Part surface forms even film layer, and 3% cupric sulphate dropping test meets GB/T15519 criterion of acceptability, 8 hours nothings of nigrescence workpiece
Rust staining point；According to 5% neutral salt spray test standard method in GB/T10125, non-corroding in nigrescence workpiece 8 hours.
Claims (10)
1. a kind of organic nigrescence oil, it is characterised in that organic nigrescence oil is mixed together by the component of following mass fraction：
2. organic nigrescence oil according to claim 1, it is characterised in that：Described base oil is white oil, paraffin oil, cycloalkanes
Any one in oily either lubricating oil or any two kinds of mixing in any proportion.
3. organic nigrescence oil according to claim 1, it is characterised in that：Described oil-soluble inhibitor is aliphatic acid or ring
The alkali salt of alkanoic acid, lead naphthenate, zinc naphthenate, petroleum sodium sulfonate, barium mahogany sulfonate, calcium mahogany sulfonate, three oleic acid oxen
Tallow diamine, rosin amine, sorbitan monooleate, glycol dioleate, polyglycol distearate, oleoyl flesh
In propylhomoserin and its amine salt, amide imidazoline, BTA or alkyl phosphate any one or it is any two kinds by any
The mixing of ratio.
4. organic nigrescence oil according to claim 1, it is characterised in that：Described coalescents include wetting agent, sterilization
Agent, defoamer and levelling agent；
Wherein, described wetting agent is Nonyl pheno base ether, octyl phenol polyoxyethylene ether, aliphatic alcohol polyethenoxy base
Either any one in alkylphenol-polyethenoxy base ether or any two kinds of mixing proportionally of ether, polyethylene glycol；
Described bactericide is sodium benzoate, ethoxy perhydro-s-triazine, the chloro- 3- methylphenols of 4-, the iodo- 2-propynyl butyl of 3-
Any one in carbamate or 2- methyl sulphur -4- ethylamino -6- spy's fourth amino -1,3,5- triazines or it is any two kinds by appoint
The mixing of meaning ratio；
The defoamer is any one in higher alcohol, organosiloxane or polyoxyethylene polyoxypropylene copolymer or any
Two kinds mix in any proportion；
The levelling agent be silicone oil, dipropylene glycol methyl ether, ethylene glycol phenyl ether, glycerine phenylate or the third three it is purebred any one or
Any two kinds proportionally mix.
5. organic nigrescence oil according to claim 1, it is characterised in that：The water-base resin is water-soluble acrylic tree
In fat, pure-acrylic emulsion, styrene-acrylic emulsion, polyaminoester emulsion or polycarbonate emulsion any one or it is any two kinds in any proportion
Mixing.
6. organic nigrescence oil according to claim 1, it is characterised in that：Pigment used is charcoal in described aqueous color paste
Any one or any two kinds in black, iron oxide black, chrome black or nigrosine mix in any proportion.
7. organic nigrescence oil according to claim 1, it is characterised in that：Described emulsifying agent be S-80, T-80, T-60,
Any one in OP-10, milky white spirit or paraffinic base emulsifying agent or any two kinds of mixing in any proportion.
8. organic nigrescence oil according to claim 1, it is characterised in that：Described complexing agent is ethylenediamine tetra-acetic acid, wine
The sylvite of any one in stone acid, citric acid, malic acid, lactic acid or gluconic acid；Or, the complexing agent is ethylenediamine tetrem
The sodium salt of any one in acid, tartaric acid, citric acid, malic acid, lactic acid or gluconic acid；Or, described complexing agent is second two
The ammonium salt of any one in amine tetraacethyl, tartaric acid, citric acid, malic acid, lactic acid or gluconic acid.
9. a kind of preparation method of nigrescence oil organic as claimed in claim 1, it is characterised in that the preparation method includes following step
Suddenly：
Step 1, base oil, oil-soluble inhibitor, water, pH adjusting agent, bactericide are added sequentially in stirred tank, in stirring speed
Rate is under 50-100 revs/min that material stirring is uniform；
Step 2, while stirring toward adding required water in the mixed material in step 1,50-100/ points of stir speed (S.S.) is lower will
Material stirring is uniform；
Step 3, while stirring toward required coalescents are added in the mixed material in step 1, in stir speed (S.S.) 50-100/
It is under point that material stirring is uniform；
Step 4, stirred while stirring toward required water-base resin and aqueous color paste is added in the mixed material in step 1
Uniformly can set aside for use by material stirring under 30-70/ points of speed.
10. the preparation method of organic nigrescence oil according to claim 9, it is characterised in that the pH adjusting agent is ammoniacal liquor, one
Monoethanolamine, diethanol amine, triethanolamine, 2-amino-2-methyl-1-propanol, 2- amino -2- ethyl -1,3- propane diols or 2- bis-
Any one in methylamino -2- methyl isophthalic acids-propyl alcohol or any two kinds of mixing in any proportion.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108300173A (en) * | 2018-02-07 | 2018-07-20 | 东南大学 | A kind of steel surface low temperature exhaust heat blackening agent for surface and its methods for making and using same |
| CN109097780A (en) * | 2018-09-18 | 2018-12-28 | 苏州市金翔钛设备有限公司 | A kind of process of surface treatment of copper-titanium alloy tubing |
| CN109735181A (en) * | 2018-12-26 | 2019-05-10 | 南京科润工业介质股份有限公司 | A kind of emulsification hair blackening liquid used under the conditions of hardness |
| CN110185689A (en) * | 2019-05-21 | 2019-08-30 | 邵东县中南锻压工具制造有限公司 | A kind of Hardware fitting that hardness high corrosion resistance is strong and its processing method |
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| CN110643986A (en) * | 2019-10-30 | 2020-01-03 | 湖南金裕环保科技有限公司 | Residual heat blackening agent, preparation method and use method |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108300173A (en) * | 2018-02-07 | 2018-07-20 | 东南大学 | A kind of steel surface low temperature exhaust heat blackening agent for surface and its methods for making and using same |
| CN109097780A (en) * | 2018-09-18 | 2018-12-28 | 苏州市金翔钛设备有限公司 | A kind of process of surface treatment of copper-titanium alloy tubing |
| CN109735181A (en) * | 2018-12-26 | 2019-05-10 | 南京科润工业介质股份有限公司 | A kind of emulsification hair blackening liquid used under the conditions of hardness |
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| CN110607523A (en) * | 2019-10-10 | 2019-12-24 | 石家庄高新区海怡防腐科技有限公司 | High-temperature online water-based steel antirust agent |
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