CN107365987B - A kind of high adhesion is without selenium room temperature blackening liquid - Google Patents
A kind of high adhesion 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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- C23C22/00—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
- 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 adhesions without selenium room temperature blackening liquid, belongs to steel processing technology field.The present invention extracts first from Chinese medicine has specific sequestering effective component to iron ion, the ferrous ion displaced to chelate shielding from steel surface, it is avoided to hinder steel surface copper facing, steel surface is cleaned with soyasaponin extracting solution again, improve its surface wettability, liquid is set to be easy to soak and sprawl in steel surface, advantageously form uniform black film, finally nitrogen is provided using arabidopsis and yolk fermentation material, sulphur, P elements, it reoxidizes to form a stratification protective film on the copper oxide of steel surface, fill up the hole between black film, increase its glossiness, it can also make to combine between black film and steel substrate simultaneously stronger, improve the adhesion of black film, hair blackening liquid, which is made, in the present invention has film layer uniform, black film glossiness, adhesive force, the good feature of corrosion resistance, ingredient asepsis environment-protecting, application prospect is wide It is wealthy.
Description
Technical field
The present invention relates to a kind of high adhesions without selenium room temperature blackening liquid, belongs to steel processing technology field.
Background technique
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 processing, has both antirust and decorative effect.Traditional nigrescence tank liquor operating temperature is up to 130 DEG C or more, and energy consumption is high, labour item
Part is poor.Compared with alkaline high-temperature oxydation, room temperature blackening operates at normal temperature, and electricity saving and energy saving improves working environment.Currently, real
Room temperature blackening liquid majority contains selenides, and being 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, technological temperature requirement is low, easy to operate, and acquired film layer is handled through closing process
Corrosion resistance is preferable afterwards, and room temperature copper selenium nigrescence system melanism film generated is loose, adhesive force is low, generates precipitating during blacking
It is more, noxious material selenium element is contained in working solution, generated waste liquid, waste residue are all harmful to human body and environment.Make for a long time
With environmental pollution is bound to cause, therefore, it is very necessary for urgently developing a kind of high no selenium room temperature blackening liquid of adhesive force.
Summary of the invention
Present invention mainly solves the technical issues of, be copper selenium nigrescence system for traditional room temperature blackening liquid at present, generate
Melanism film is loose, adhesive force is low, it is more to generate precipitating during blacking, and noxious material selenium element, institute are contained in working solution
Waste liquid, the waste residue of generation can be harmful to human body and environment defect, provide a kind of high adhesion without selenium room temperature blackening liquid.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of high adhesion without selenium room temperature blackening liquid, including sterilization fermentation liquid, Fermented Condensed liquid and soyasaponin extract,
It is characterized by: the sterilization fermentation liquid is the gained that sterilized by Chinese medicine fermented liquid.
The fermentation process of the Chinese medicine fermented liquid is: weighing teasel root, cynomorium songaricum and psoralea corylifolia and is put into powder in medicinal herb grinder
It is broken, mixing traditional Chinese medicine powder is obtained, is fitted into fermentor after mixing traditional Chinese medicine powder and water are mixed, then Grape Skin is added into fermentor,
With stirring rod, sealed fermenter, heat-preservation fermentation obtain Chinese medicine fermented liquid after mixing evenly.
The mixing traditional Chinese medicine powder is according to parts by weight, to weigh 40~50 parts of teasel roots, 60~80 parts of cynomorium songaricums and 30~50
Gained after part psoralea corylifolia crushes, the additional amount of Grape Skin are mix traditional Chinese medicine powder quality 10%, and the temperature of heat-preservation fermentation is 30~45
DEG C, the heat-preservation fermentation time is 10~15 days.
The Fermented Condensed liquid is by being concentrated to get after the mixed mouldy object fermentation of arabidopsis and egg yolk.
The fermentation detailed process is: weighing 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 object, is put into fermentor after mouldy object and water are mixed,
Tank mouth heat-preservation fermentation is sealed, tunning is obtained.
The mass ratio of the arabidopsis and egg yolk is 2:1, and 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
It is 7~10 days.
The extracting method of the soyasaponin extract is:
(1) weighing dregs of beans in mass ratio and be 1:10 and being added to mass fraction is to soak at 60~70 DEG C in 90% methanol solution
3~5h is mentioned, filtering removal filter residue obtains extraction filtrate, then extraction filtrate is put into distillation under pressure device, is distilled to recover methanol
Solution obtains white powder；
It (6) is in mass ratio that 1:5 is mixed to get mixed liquor, then will mix by equal mass ratioes by above-mentioned white powder and petroleum ether
Liquid and mass fraction are closed as the mixing of 50% butanol solution, stratification after oscillation treatment, separation removal petroleum ether layer will be remaining
Butanol solution moves into distilling apparatus, and vacuum distillation recycling butanol obtains soyasaponin extract.
A kind of high adhesion is without selenium room temperature blackening liquid, it is characterised in that specific preparation step are as follows: 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 is to get high adhesion without selenium room temperature blackening liquid after 1~2h of mixing.
The beneficial effects of the present invention are:
(1) present invention displaces the ferrous ion of steel surface using copper ion using copper sulphate as main film forming substance, then
Promote the generation of cupric oxide by ammonium molybdate strong oxidizing property, while ammonium molybdate is reduced into atrament and participates in film forming, from
Extracting in Chinese medicine has specific sequestering effective component to iron ion, the ferrous iron displaced to chelate shielding from steel surface
Ion avoids it from being oxidized and generates loose di-iron trioxide obstruction steel surface copper facing, to form fine and close hard melanism
Film；
(2) contained soyasaponin extracting solution can clean steel surface in the present invention, improve its surface wettability, make liquid
It is easy to soak and sprawl in steel surface, advantageously forms uniform black film, precipitating is avoided to generate, finally utilize arabidopsis and egg
The glucosinolate and ovum congealed fat contained in yellow fermentation material provides nitrogen, sulphur, P elements, on the copper oxide that steel surface generates
It reoxidizes to form a stratification protective film, fills up the hole between black film, increase its glossiness, while black film can also be made
What is combined between steel substrate is stronger, improves the adhesion of black film；
(3) the obtained hair blackening liquid of the present invention has black film flawless, and film layer is uniform, black film glossiness, adhesive force, anti-corrosion
The good feature of property, ingredient asepsis environment-protecting have a extensive future.
Specific embodiment
400~500g teasel root, 600~800g cynomorium songaricum and 300~500g psoralea corylifolia is weighed to be put into medicinal herb grinder and crush
20~30min, obtain mixing traditional Chinese medicine powder, will mixing traditional Chinese medicine powder and water be in mass ratio 1:2 mix after be fitted into fermentor, then to
130~180g Grape Skin is added in fermentor, with stirring rod sealed fermenter after mixing evenly, the heat-preservation fermentation at 30~45 DEG C
10~15 days；It goes out to after fermentation, take out tunning and filter, isolated fermentation liquid, then by fermentation liquid immigration high temperature
In bacterium tank, sterilize 10~15min at 120 DEG C, obtains sterilization fermentation liquid；Weigh 200~400g arabidopsis and 100~200g chicken
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, being placed on temperature is 30~40 DEG C, and relative air humidity is 5~7 days naturally mouldy in the environment of being 50~60%, is obtained mouldy
Object；In mass ratio it is to be put into fermentor after 1:2 is mixed by mouldy object and water, seals tank mouth heat-preservation fermentation 7 at 30~40 DEG C
It~10 days, to take out tunning filtering, isolated filtrate after fermentation, then puts the filtrate into vacuum concentration pot and is concentrated
To the 1/3 of filtrate original volume, Fermented Condensed liquid is obtained；Weighing 800~900g dregs of beans in mass ratio is that 1:10 is added to quality point
Number is that 3~5h is extracted at 60~70 DEG C in 90% methanol solution, and filtering removal filter residue obtains extraction filtrate, then extraction is filtered
Liquid is put into distillation under pressure device, is distilled to recover methanol solution, is obtained white powder；In mass ratio by white powder and petroleum ether
It is mixed to get mixed liquor for 1:5, then be in mass ratio 1:1 by mixed liquor and mass fraction is that 50% butanol solution mixes, is placed on
Remaining butanol solution is moved into distillation dress by stratification after 15~20min of oscillation treatment on shaking table, separation removal petroleum ether layer
In setting, vacuum distillation recycling butanol obtains soyasaponin extract；According to 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 after being stirred 1~2h tinning to get high adhesion without
Selenium room temperature blackening liquid.
Example 1
It weighs 500g teasel root, 800g cynomorium songaricum and 500g psoralea corylifolia to be put into medicinal herb grinder and crush 30min, obtain in mixing
Mixing traditional Chinese medicine powder and water are to be fitted into fermentor after 1:2 is mixed, then 180g grape is added into fermentor by medicinal powder in mass ratio
Skin, with stirring rod sealed fermenter after mixing evenly, heat-preservation fermentation 15 days at 45 DEG C；It is produced to after fermentation, take out fermentation
Object simultaneously filters, isolated fermentation liquid, then fermentation liquid is moved into high-temperature sterilization tank, and sterilize 15min at 120 DEG C, is gone out
Fermented liquid weighs 10 parts of ammonium molybdates, 35 parts of copper sulphate, 3 parts of sodium sulfites, 13.0 parts of sterilization fermentation liquid according to parts by weight
With 60 parts of deionized waters, tinning is poured into mixing and blending machine after being stirred 2h to get high adhesion without selenium room temperature blackening liquid.
Example 2
It weighs 400g arabidopsis and 200g egg yolk is put into tissue pulverizer and crushes 30min, obtain mixed powder and mince, it will
Mixed powder, which minces, to be laid in stainless steel pallet, and being placed on temperature is 40 DEG C, and relative air humidity is sent out naturally in the environment of being 60%
Mould 7 days, obtain mouldy object；In mass ratio it is to be put into fermentor after 1:2 is mixed by mouldy object and water, seals tank mouth at 40 DEG C
Heat-preservation fermentation 10 days, to take out tunning filtering, isolated filtrate after fermentation, then put the filtrate into vacuum concentration pot
In be concentrated into the 1/3 of filtrate original volume, obtain Fermented Condensed liquid；Weighing 900g dregs of beans in mass ratio is that 1:10 is added to quality point
In 90% methanol solution, to extract 5h at 70 DEG C, filtering removal filter residue obtains extraction filtrate, then extraction filtrate is put into and is added number
It presses in distilling apparatus, is distilled to recover methanol solution, obtains white powder；White powder and petroleum ether are mixed in mass ratio for 1:5
Conjunction obtains mixed liquor, then be in mass ratio 1:1 by mixed liquor and mass fraction is that 50% butanol solution mixes, and is placed on shaking table
Stratification after oscillation treatment 20min, separation removal petroleum ether layer, remaining butanol solution is moved into distilling apparatus, decompression
It is distilled to recover butanol, obtains soyasaponin extract；According to parts by weight, 10 parts of ammonium molybdates, 35 parts of copper sulphate, 3 parts of Asias are weighed
Sodium sulphate, 11.0 parts of Fermented Condensed liquid, 2 parts of soyasaponin extracts and 60 parts of deionized waters, pour into mixing and blending machine and stir
Tinning is to get high adhesion without selenium room temperature blackening liquid after mixing 2h.
Example 3
It weighs 500g teasel root, 800g cynomorium songaricum and 500g psoralea corylifolia to be put into medicinal herb grinder and crush 30min, obtain in mixing
Mixing traditional Chinese medicine powder and water are to be fitted into fermentor after 1:2 is mixed, then 180g grape is added into fermentor by medicinal powder in mass ratio
Skin, with stirring rod sealed fermenter after mixing evenly, heat-preservation fermentation 15 days at 45 DEG C；It is produced to after fermentation, take out fermentation
Object simultaneously filters, isolated fermentation liquid, then fermentation liquid is moved into high-temperature sterilization tank, and sterilize 15min at 120 DEG C, is gone out
Fermented liquid；It weighs 400g arabidopsis and 200g egg yolk is put into tissue pulverizer and crushes 30min, obtain mixed powder and mince,
Mixed powder is minced and is laid in stainless steel pallet, being placed on temperature is 40 DEG C, and relative air humidity is natural in the environment of being 60%
Mouldy 7 days, obtain mouldy object；In mass ratio it is to be put into fermentor after 1:2 is mixed by mouldy object and water, seals tank mouth at 40 DEG C
Lower heat-preservation fermentation 10 days to take out tunning filtering, isolated filtrate after fermentation, then puts the filtrate into vacuum concentration
It is concentrated into the 1/3 of filtrate original volume in tank, obtains Fermented Condensed liquid；Weighing 900g dregs of beans in mass ratio is that 1:10 is added to quality
Score is that 5h is extracted at 70 DEG C in 90% methanol solution, and filtering removal filter residue obtains extraction filtrate, then extraction filtrate is put into
In distillation under pressure device, it is distilled to recover methanol solution, obtains white powder；It is in mass ratio 1:5 by white powder and petroleum ether
It is mixed to get mixed liquor, then be in mass ratio 1:1 by mixed liquor and mass fraction is that 50% butanol solution mixes, is placed on shaking table
Stratification after upper oscillation treatment 20min, separation removal petroleum ether layer, remaining butanol solution is moved into distilling apparatus, is subtracted
Pressure is distilled to recover butanol, obtains soyasaponin extract；According to parts by weight, 10 parts of ammonium molybdates, 35 parts of copper sulphate, 3 parts are weighed
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 is stirred after 2h in mixing and blending machine to get high adhesion 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 steps are as follows for specific nigrescence:
(1) it is polished with the matrix steel surface that sand paper treats blackening process, the matrix steel after polishing is used respectively
Petroleum ether, concentration are that 0.5mol/L hydrochloric acid and water are rinsed；
(2) the matrix steel after flushing are soaked in high adhesion prepared by example 1 to example 3 without selenium room temperature blackening liquid
In, impregnate 8min；
(3) the steel sky after blacking is taken out after impregnating and stops 4min, then naturally dry is after being rinsed 2 times with deionized water
Can, form nigrescence film layer.
The nigrescence film layer that example 1 to example 3 is formed is detected.
The test of film adhesive force: being rubbed in nigrescence film surface with medium dynamics back and forth with clean absorbent cotton, until
Certain point occurs writing down Rubbing number when steel matrix.
Corrosion-resistant test: according to the test method GB5936 of ferrous metal chemical coating, it is by concentration with rubber head dropper
3% copper-bath drips 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 (secondary) | 150 | 175 | 190 | 130 |
| Corrosion resistance (s) | 65 | 78 | 90 | 62 |
As known from Table 1, the film layer that hair blackening liquid prepared by the present invention is formed after blacking is fine and close, adhesive force with higher, and
Corrosion resistance is superior.
Claims (3)
1. a kind of high adhesion is without selenium room temperature blackening liquid, including sterilization fermentation liquid, Fermented Condensed liquid and soyasaponin extract,
Be characterized in that: according to 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 parts of sterilization fermentation liquid, 5~10 parts of Fermented Condensed liquid, 1~2 part of above-mentioned soyasaponin extract and 40~60 parts of deionized waters,
Tinning is poured into mixing and blending machine after being stirred 1~2h to get high adhesion without selenium room temperature blackening liquid；The sterilization fermentation
Liquid is the gained that sterilized by Chinese medicine fermented liquid；The fermentation process of the Chinese medicine fermented liquid is: weighing teasel root, cynomorium songaricum and psoralea corylifolia and puts
Enter in medicinal herb grinder and crush, obtains mixing traditional Chinese medicine powder, the mixing traditional Chinese medicine powder is according to parts by weight, to weigh 40~50 parts
Gained after teasel root, 60~80 parts of cynomorium songaricums and 30~50 parts of psoralea corylifolias crush, the additional amount of Grape Skin are mixing traditional Chinese medicine powder quality
10%, the temperature of heat-preservation fermentation is 30~45 DEG C, and the heat-preservation fermentation time is 10~15 days, is filled after mixing traditional Chinese medicine powder and water are mixed
Enter in fermentor, then Grape Skin is added into fermentor, sealed fermenter, heat-preservation fermentation obtain after mixing evenly with stirring rod
Chinese medicine fermented liquid；The Fermented Condensed liquid is by being concentrated to get after the mixed mouldy object fermentation of arabidopsis and egg yolk；
The extracting method of the soyasaponin extract is:
(1) weighing dregs of beans in mass ratio and be 1:10 and being added to mass fraction is to extract 3 at 60~70 DEG C in 90% methanol solution
~5h, filtering removal filter residue obtain extraction filtrate, then extraction filtrate are put into distillation under pressure device, and it is molten to be distilled to recover methanol
Liquid obtains white powder；
It (2) is in mass ratio that 1:5 is mixed to get mixed liquor, then presses equal mass ratioes for mixed liquor by above-mentioned white powder and petroleum ether
It is the mixing of 50% butanol solution, stratification after oscillation treatment, separation removal petroleum ether layer, by remaining butanol with mass fraction
Solution moves into distilling apparatus, and vacuum distillation recycling butanol obtains soyasaponin extract.
2. a kind of high adhesion according to claim 1 is without selenium room temperature blackening liquid, it is characterised in that arabidopsis and egg yolk
Mixed mouldy object fermentation detailed process is: weighing 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 object, is put into fermentor after mouldy object and water are mixed,
Tank mouth heat-preservation fermentation is sealed, tunning is obtained.
3. the detailed process of fermentation according to claim 2, it is characterised in that: the quality of the arabidopsis and egg yolk
Than for 2:1, naturally mouldy temperature is 30~40 DEG C, and naturally mouldy relative air humidity is 50~60%, 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.
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| RU2106328C1 (en) * | 1996-02-28 | 1998-03-10 | Индивидуальное частное предприятие Старикова С.Н. "Зодчий" | Aerosol fertilizer for non-root |
| CN102011117A (en) * | 2010-12-02 | 2011-04-13 | 合肥华清金属表面处理有限责任公司 | Environmental-friendly room-temperature steel blackening agent and preparation method thereof |
| CN103849868A (en) * | 2014-02-14 | 2014-06-11 | 浙江工业大学 | Blackening liquid for chromium-free titanium-zinc panel surface and using method of blackening liquid |
| CN104195538B (en) * | 2014-09-03 | 2016-06-29 | 淮南天力生物工程开发有限公司 | Non-selenium series normal temperature environmental protection steel blackening liquid and preparation method thereof and blackening method |
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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 |