CN107365987A - A kind of high tack is without selenium room temperature blackening liquid - Google Patents
A kind of high tack is without selenium room temperature blackening liquid Download PDFInfo
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- C23—COATING 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
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- C23C22/05—Chemical 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
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Abstract
The present invention relates to a kind of high tack without selenium room temperature blackening liquid, belong to steel processing technology field.Present invention extraction first from Chinese medicine has specific sequestering active ingredient to iron ion,To chelate the ferrous ion that shielding displaces from steel surface,It is avoided to hinder steel surface copper facing,Again steel surface is cleaned with soyasaponin extract solution,Improve its surface wettability,Liquid is set easily to soak and sprawl in steel surface,Advantageously form uniform black film,Finally nitrogen is provided using arabidopsis and yolk fermentate,Sulphur,P elements,Reoxidize to form a stratification diaphragm on the copper oxide of steel surface,The hole filled up between black film,Make the increase of its glossiness,It can also make to combine between black film and steel substrate simultaneously more firm,Improve the tack of black film,The obtained hair blackening liquid of the present invention has film layer homogeneous,Black film glossiness,Adhesive force,The characteristics of corrosion resistance is good,Composition asepsis environment-protecting,Have a extensive future.
Description
Technical field
The present invention relates to a kind of high tack without selenium room temperature blackening liquid, belong to steel processing technology field.
Background technology
Nigrescence is one kind of surface finishing technology, is widely used in the steel and iron parts article such as optical instrument, weapons, standard component
Surface Machining, have antirust and decorative effect concurrently.Traditional nigrescence tank liquor operating temperature is up to more than 130 DEG C, high energy consumption, work bar
Part is poor.Compared with alkaline high-temperature oxydation, room temperature blackening operates at normal temperatures, electricity saving and energy saving, improves working environment.At present, it is real
Room temperature blackening liquid majority contains selenides, is that copper selenium room temperature blackening system ultimately generates black selenium by series of chemical
Change copper and be bonded in steel surface formation melanism film, the technological temperature requires low, easy to operate, and resulting film layer is handled through closing process
Corrosion resistance is preferable afterwards, and the melanism film that normal temperature copper selenium nigrescence system is generated is loose, adhesive force is low, and precipitation is generated during nigrescence
It is more, noxious material selenium element is contained in its working solution, caused waste liquid, waste residue are all harmful to human body and environment.Make for a long time
With that certainly will cause environmental pollution, therefore, it is very necessary urgently to develop a kind of high no selenium room temperature blackening liquid of adhesive force.
The content of the invention
Present invention mainly solves technical problem, be copper selenium nigrescence system for traditional room temperature blackening liquid at present, generation
Melanism film is loose, adhesive force is low, generation precipitation is more during nigrescence, and noxious material selenium element, institute are contained in its working solution
Caused waste liquid, waste residue have the defects of endangering to human body and environment, there is provided a kind of high tack is without selenium room temperature blackening liquid.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
For a kind of high tack without selenium room temperature blackening liquid, including sterilization fermentation liquid, Fermented Condensed liquid and soyasaponin extract, it is special
Sign is：Described sterilization fermentation liquid is by Chinese medicine fermented liquid sterilizing gained.
The fermentation process of described Chinese medicine fermented liquid is：Weigh teasel root, cynomorium songaricum and psoralea corylifolia and be put into powder in medicinal herb grinder
It is broken, obtain mixing traditional Chinese medicine powder, be fitted into after mixing traditional Chinese medicine powder and water are mixed in fermentation tank, then Grape Skin is added into fermentation tank,
Sealed fermenter after being stirred with stirring rod, heat-preservation fermentation, obtains Chinese medicine fermented liquid.
Described mixing traditional Chinese medicine powder is to count in parts by weight, weighs 40~50 parts of teasel roots, 60~80 parts of cynomorium songaricums and 30~50
Gained after part psoralea corylifolia crushes, the addition of Grape Skin is the 10% of mixing traditional Chinese medicine powder quality, and the temperature of heat-preservation fermentation is 30~45
DEG C, the heat-preservation fermentation time is 10~15 days.
Described Fermented Condensed liquid after the mixed mouldy thing fermentation of arabidopsis and egg yolk by being concentrated to give.
Described fermentation detailed process is：Weigh arabidopsis and egg yolk crushes jointly, obtain mixed powder and mince, will mix
Crushed material is laid in stainless steel pallet, naturally mouldy, obtains mouldy thing, is put into after mouldy thing and water are mixed in fermentation tank,
Tank mouth heat-preservation fermentation is sealed, obtains tunning.
Described arabidopsis and the mass ratio of egg yolk are 2:1, naturally mouldy temperature is 30~40 DEG C, naturally mouldy sky
Gas relative humidity is 50~60%, and the naturally mouldy time is 5~7 days, and heat-preservation fermentation temperature is 30~40 DEG C, the heat-preservation fermentation time
For 7~10 days.
The extracting method of described soyasaponin extract is：
（1）It is 1 in mass ratio to weigh dregs of beans:10 are added to mass fraction as in 90% methanol solution, 3 are extracted at 60~70 DEG C
~5h, filter off except filter residue, obtain extracting filtrate, then extraction filtrate is put into distillation under pressure device, it is molten to be distilled to recover methanol
Liquid, obtain white powder；
（6）It is 1 in mass ratio by above-mentioned white powder and petroleum ether:5 are mixed to get mixed liquor, then by etc. mass ratio by mixed liquor
Mix, stratification after oscillation treatment, separated except petroleum ether layer, by remaining butanol for 50% butanol solution with mass fraction
Solution is moved into distilling apparatus, is evaporated under reduced pressure recovery butanol, is obtained soyasaponin extract.
A kind of described high tack is without selenium room temperature blackening liquid, it is characterised in that specifically preparation process is：In parts by weight
Meter, weighs 5~10 parts of ammonium molybdates, 30~35 parts of copper sulphate, 1~3 part of sodium sulfite, 0.5~1.0 part of sterilization fermentation liquid, 5~10
Part Fermented Condensed liquid, 1~2 part of above-mentioned soyasaponin extract and 40~60 parts of deionized waters, pour into mixing and blending machine and stir
Tinning after 1~2h of mixing, produces high tack without selenium room temperature blackening liquid.
The beneficial effects of the invention are as follows：
（1）The present invention displaces the ferrous ion of steel surface using copper ion, then pass through using copper sulphate as main film forming substance
Ammonium molybdate strong oxidizing property promotes the generation of cupric oxide, while ammonium molybdate is reduced into atrament and participates in film forming, from Chinese medicine
Middle extraction has specific sequestering active ingredient to iron ion, to chelate shielding from steel surface displace it is ferrous from
Son, avoid it from being oxidized the loose di-iron trioxide of generation and hinder steel surface copper facing, so as to form fine and close hard melanism film；
（2）Contained soyasaponin extract solution can clean steel surface in the present invention, improve its surface wettability, make liquid easy
Soak and sprawl in steel surface, advantageously form uniform black film, avoid precipitation from producing, finally sent out using arabidopsis and yolk
The glucosinolate and ovum congealed fat that contain in ferment thing provide nitrogen, sulphur, P elements, in oxygen again on copper oxide caused by steel surface
Change and form a stratification diaphragm, the hole filled up between black film, make the increase of its glossiness, while black film and steel can also be made
What is combined between iron-based body is more firm, improves the tack of black film；
（3）The obtained hair blackening liquid of the present invention has black film flawless, and film layer is homogeneous, and black film glossiness, adhesive force, corrosion resistance are good
The characteristics of, composition asepsis environment-protecting, have a extensive future.
Embodiment
400~500g teasel roots, 600~800g cynomorium songaricums and 300~500g psoralea corylifolias is weighed to be put into medicinal herb grinder and crush
20~30min, obtain mixing traditional Chinese medicine powder, be 1 in mass ratio by mixing traditional Chinese medicine powder and water:It is fitted into after 2 mixing in fermentation tank, then to
130~180g Grape Skins, sealed fermenter after being stirred with stirring rod, the heat-preservation fermentation at 30~45 DEG C are added in fermentation tank
10~15 days；After fermentation ends, take out tunning and filter, isolated zymotic fluid, then zymotic fluid immigration high temperature is gone out
In bacterium tank, sterilize 10~15min at 120 DEG C, obtains sterilization fermentation liquid；Weigh 200~400g arabidopsis and 100~200g chickens
Yolk is put into 20~30min of crushing in tissue pulverizer, obtains mixed powder and minces, mixed powder is minced and is laid in stainless steel pallet
In, temperature is placed on as 30~40 DEG C, and relative air humidity is naturally mouldy 5~7 days in the environment of being 50~60%, obtains mouldy
Thing；It is 1 in mass ratio by mouldy thing and water:It is put into after 2 mixing in fermentation tank, seals tank mouth heat-preservation fermentation 7 at 30~40 DEG C
~10 days, tunning filtering, isolated filtrate are taken out after fermentation ends, then filtrate is put into vacuum concentration pot and concentrated
To the 1/3 of filtrate original volume, Fermented Condensed liquid is obtained；It is 1 in mass ratio to weigh 800~900g dregs of beans:10 are added to quality point
Number is in 90% methanol solution, and 3~5h is extracted at 60~70 DEG C, is filtered off except filter residue, obtains extracting filtrate, then extraction is filtered
Liquid is put into distillation under pressure device, is distilled to recover methanol solution, is obtained white powder；By white powder and petroleum ether in mass ratio
For 1:5 are mixed to get mixed liquor, then are 1 in mass ratio:1 mixes mixed liquor and mass fraction for 50% butanol solution, is placed on
Stratification after 15~20min of oscillation treatment, is separated except petroleum ether layer on shaking table, and remaining butanol solution is moved into distillation dress
In putting, recovery butanol is evaporated under reduced pressure, obtains soyasaponin extract；Count in parts by weight, weigh 5~10 parts of ammonium molybdates, 30~
35 parts of copper sulphate, 1~3 part of sodium sulfite, 0.5~1.0 part of sterilization fermentation liquid, 5~10 parts of Fermented Condensed liquid, 1~2 part of soybean soapstock
Glucoside extract and 40~60 parts of deionized waters, pour into mixing and blending machine and be stirred tinning after 1~2h, produce high tack without
Selenium room temperature blackening liquid.
Example 1
Weigh 500g teasel roots, 800g cynomorium songaricums and 500g psoralea corylifolias to be put into medicinal herb grinder and crush 30min, obtain mixing Chinese medicine
Powder, it is 1 in mass ratio by mixing traditional Chinese medicine powder and water:It is fitted into after 2 mixing in fermentation tank, then 180g grapes is added into fermentation tank
Skin, sealed fermenter after being stirred with stirring rod, heat-preservation fermentation 15 days at 45 DEG C；After fermentation ends, fermentation production is taken out
Thing is simultaneously filtered, isolated zymotic fluid, then zymotic fluid is moved into high-temperature sterilization tank, and sterilize 15min at 120 DEG C, is gone out
Fermented liquid, count in parts by weight, weigh 10 parts of ammonium molybdates, 35 parts of copper sulphate, 3 parts of sodium sulfites, 13.0 parts of sterilization fermentation liquid
With 60 parts of deionized waters, pour into mixing and blending machine and be stirred tinning after 2h, produce high tack without selenium room temperature blackening liquid.
Example 2
Weigh 400g arabidopsis and 200g egg yolks are put into tissue pulverizer and crush 30min, obtain mixed powder and mince, will mix
Crushed material is laid in stainless steel pallet, is placed on temperature as 40 DEG C, relative air humidity is naturally mouldy 7 in the environment of 60%
My god, obtain mouldy thing；It is 1 in mass ratio by mouldy thing and water:It is put into after 2 mixing in fermentation tank, sealing tank mouth is protected at 40 DEG C
Temperature fermentation 10 days, tunning filtering, isolated filtrate are taken out after fermentation ends, then filtrate is put into vacuum concentration pot
The 1/3 of filtrate original volume is concentrated into, obtains Fermented Condensed liquid；It is 1 in mass ratio to weigh 900g dregs of beans:10 are added to mass fraction
For in 90% methanol solution, 5h is extracted at 70 DEG C, filter off except filter residue, obtain extracting filtrate, then extraction filtrate is put into pressurization
In distilling apparatus, methanol solution is distilled to recover, obtains white powder；It is 1 in mass ratio by white powder and petroleum ether:5 mixing
Mixed liquor is obtained, then is 1 in mass ratio:1 mixes mixed liquor and mass fraction for 50% butanol solution, is placed on shaking table and shakes
Swing processing 20min after stratification, separate except petroleum ether layer, by remaining butanol solution move into distilling apparatus in, decompression steam
Recovery butanol is evaporated, obtains soyasaponin extract；Count in parts by weight, weigh 10 parts of ammonium molybdates, 35 parts of copper sulphate, 3 parts of sulfurous
Sour sodium, 11.0 parts of Fermented Condensed liquid, 2 parts of soyasaponin extracts and 60 parts of deionized waters, pour into stir in mixing and blending machine and mix
Tinning after conjunction 2h, produces high tack without selenium room temperature blackening liquid.
Example 3
Weigh 500g teasel roots, 800g cynomorium songaricums and 500g psoralea corylifolias to be put into medicinal herb grinder and crush 30min, obtain mixing Chinese medicine
Powder, it is 1 in mass ratio by mixing traditional Chinese medicine powder and water:It is fitted into after 2 mixing in fermentation tank, then 180g grapes is added into fermentation tank
Skin, sealed fermenter after being stirred with stirring rod, heat-preservation fermentation 15 days at 45 DEG C；After fermentation ends, fermentation production is taken out
Thing is simultaneously filtered, isolated zymotic fluid, then zymotic fluid is moved into high-temperature sterilization tank, and sterilize 15min at 120 DEG C, is gone out
Fermented liquid；Weigh 400g arabidopsis and 200g egg yolks be put into tissue pulverizer and crush 30min, obtain mixed powder and mince,
Mixed powder is minced and is laid in stainless steel pallet, is placed on temperature as 40 DEG C, relative air humidity is natural in the environment of being 60%
Mouldy 7 days, obtain mouldy thing；It is 1 in mass ratio by mouldy thing and water:It is put into after 2 mixing in fermentation tank, sealing tank mouth is at 40 DEG C
Lower heat-preservation fermentation 10 days, tunning filtering, isolated filtrate are taken out after fermentation ends, then filtrate is put into vacuum concentration
The 1/3 of filtrate original volume is concentrated into tank, obtains Fermented Condensed liquid；It is 1 in mass ratio to weigh 900g dregs of beans:10 are added to quality
Fraction is in 90% methanol solution, extracts 5h at 70 DEG C, filters off except filter residue, obtains extracting filtrate, then extraction filtrate is put into
In distillation under pressure device, methanol solution is distilled to recover, obtains white powder；It is 1 in mass ratio by white powder and petroleum ether:5
Mixed liquor is mixed to get, then is 1 in mass ratio:1 mixes mixed liquor and mass fraction for 50% butanol solution, is placed on shaking table
Stratification after upper oscillation treatment 20min, is separated except petroleum ether layer, and remaining butanol solution is moved into distilling apparatus, subtracted
Pressure is distilled to recover butanol, obtains soyasaponin extract；Count in parts by weight, weigh 10 parts of ammonium molybdates, 35 parts of copper sulphate, 3 parts
Sodium sulfite, 1.0 parts of sterilization fermentation liquid, 10 parts of Fermented Condensed liquid, 2 parts of soyasaponin extracts and 60 parts of deionized waters, are poured into
Tinning after 2h is stirred in mixing and blending machine, produces high tack without selenium room temperature blackening liquid.
Reference examples：Copper selenium hair blackening liquid
Hair blackening liquid using example 1 to example 3 and reference examples blacks to steel, and specific nigrescence step is as follows：
（1）The matrix steel surface that blackening process is treated with sand paper is polished, and the matrix steel after polishing is used into oil respectively
Ether, concentration are that 0.5mol/L hydrochloric acid and water are rinsed；
（2）Matrix steel after flushing are soaked in high tack prepared by example 1 to example 3 without in selenium room temperature blackening liquid, leaching
Steep 8min；
（3）The steel sky that immersion is taken out after blacking after terminating stops 4min, then with naturally dry after deionized water rinsing 2 times,
Form nigrescence film layer.
The nigrescence film layer that example 1 to example 3 is formed is detected.
Film adhesive force is tested：Rubbed back and forth with medium dynamics in nigrescence film surface with clean absorbent cotton, until
Certain point occurs writing down Rubbing number during steel matrix.
Corrosion-resistant test：According to the method for testing GB5936 of ferrous metal chemical coating, it is by concentration with rubber head dropper
3% copper-bath is dropped in nigrescence film layer, and under the conditions of 26 DEG C, it is resistance to evaluate its that the brick-red time occurs earliest in record
Corrosive nature.
Testing result such as table 1.
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Film adhesive force（It is secondary） | 150 | 175 | 190 | 130 |
| Decay resistance（s） | 65 | 78 | 90 | 62 |
As known from Table 1, the film layer that the hair blackening liquid that prepared by the present invention is formed after blacking is fine and close, has higher adhesive force, and corrosion resistant
Lose superior performance.
Claims (8)
1. a kind of high tack is without selenium room temperature blackening liquid, including sterilization fermentation liquid, Fermented Condensed liquid and soyasaponin extract, its
It is characterised by：Described sterilization fermentation liquid is by Chinese medicine fermented liquid sterilizing gained.
2. a kind of high tack according to claim 1 is without selenium room temperature blackening liquid, it is characterised in that：Described herb fermenting
The fermentation process of liquid is：Weigh teasel root, cynomorium songaricum and psoralea corylifolia and be put into medicinal herb grinder and crush, obtain mixing traditional Chinese medicine powder, will be mixed
It is fitted into after closing traditional Chinese medicine powder and water mixing in fermentation tank, then Grape Skin is added into fermentation tank, is sealed after being stirred with stirring rod
Fermentation tank, heat-preservation fermentation, obtain Chinese medicine fermented liquid.
3. the fermentation process of Chinese medicine fermented liquid according to claim 2, it is characterised in that：Described mixing traditional Chinese medicine powder be by
Parts by weight meter, weighs gained after 40~50 parts of teasel roots, 60~80 parts of cynomorium songaricums and 30~50 parts of psoralea corylifolias crush, and Grape Skin adds
Enter amount to mix the 10% of traditional Chinese medicine powder quality, the temperature of heat-preservation fermentation is 30~45 DEG C, and the heat-preservation fermentation time is 10~15 days.
4. a kind of high tack according to claim 1 is without selenium room temperature blackening liquid, it is characterised in that：Described Fermented Condensed
Liquid after the mixed mouldy thing fermentation of arabidopsis and egg yolk by being concentrated to give.
5. arabidopsis according to claim 4 and the mixed mouldy thing fermentation of egg yolk, it is characterised in that：Described hair
Ferment detailed process is：Weigh arabidopsis and egg yolk crushes jointly, obtain mixed powder and mince, mixed powder is minced, and it is stainless to be laid in
It is naturally mouldy in steel tray, mouldy thing is obtained, is put into after mouldy thing and water are mixed in fermentation tank, seals tank mouth heat-preservation fermentation,
Obtain tunning.
6. the detailed process of fermentation according to claim 5, it is characterised in that：Described arabidopsis and the quality of egg yolk
Than for 2:1, naturally mouldy temperature is 30~40 DEG C, and naturally mouldy relative air humidity is 50~60%, and the naturally mouldy time is
5~7 days, heat-preservation fermentation temperature was 30~40 DEG C, and the heat-preservation fermentation time is 7~10 days.
7. a kind of high tack according to claim 1 is without selenium room temperature blackening liquid, it is characterised in that：Described soyasaponin
The extracting method of extract is：
（1）It is 1 in mass ratio to weigh dregs of beans:10 are added to mass fraction as in 90% methanol solution, 3 are extracted at 60~70 DEG C
~5h, filter off except filter residue, obtain extracting filtrate, then extraction filtrate is put into distillation under pressure device, it is molten to be distilled to recover methanol
Liquid, obtain white powder；
（6）It is 1 in mass ratio by above-mentioned white powder and petroleum ether:5 are mixed to get mixed liquor, then by etc. mass ratio by mixed liquor
Mix, stratification after oscillation treatment, separated except petroleum ether layer, by remaining butanol for 50% butanol solution with mass fraction
Solution is moved into distilling apparatus, is evaporated under reduced pressure recovery butanol, is obtained soyasaponin extract.
8. a kind of high tack according to claim 1 is without selenium room temperature blackening liquid, it is characterised in that specifically preparation process is：
Count in parts by weight, weigh 5~10 parts of ammonium molybdates, 30~35 parts of copper sulphate, 1~3 part of sodium sulfite, 0.5~1.0 part of sterilizing hair
Zymotic fluid, 5~10 parts of Fermented Condensed liquid, 1~2 part of above-mentioned soyasaponin extract and 40~60 parts of deionized waters, pour into mixing and stir
Mix and tinning after 1~2h is stirred in machine, produce high tack without selenium room temperature blackening liquid.
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Effective date of registration: 20181112 Address after: 314200 No. 500 Xingping road two, Pinghu Economic Development Zone, Jiaxing, Zhejiang. Applicant after: Pinghu Rising Metal Craft Co.,Ltd. Address before: 213000 room 103, unit 59, 59 Li Hua Village, Tianning District, Changzhou, Jiangsu Applicant before: Zhu Wenjie |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A high adhesion selenium-free normal temperature blackening liquid Effective date of registration: 20230104 Granted publication date: 20181228 Pledgee: Pinghu Rural Commercial Bank of Zhejiang, Limited by Share Ltd. Pledgor: Pinghu Rising Metal Craft Co.,Ltd. Registration number: Y2023990000004 |