CN104004397B - Masking liquid used for surface protection of neodymium iron boron magnet, and preparation method thereof - Google Patents
Masking liquid used for surface protection of neodymium iron boron magnet, and preparation method thereof Download PDFInfo
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- CN104004397B CN104004397B CN201310430430.2A CN201310430430A CN104004397B CN 104004397 B CN104004397 B CN 104004397B CN 201310430430 A CN201310430430 A CN 201310430430A CN 104004397 B CN104004397 B CN 104004397B
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Abstract
The invention provides a masking liquid used for surface protection of a neodymium iron boron permanent magnet material, and a preparation method thereof. The masking liquid is composed of an A material, a B material and a C material. The A material is mainly composed of squamaceous zinc and aluminium powder; the B material is mainly composed of chromic acid; and the C material is cellulose for increasing viscosity of the masking liquid. The masking liquid is simple and easily operable in preparation and application processes. The masking liquid is advantageous in that (1) the masking liquid can be reused without resource waste while various indicators are qualified; (2) enclosed spraying room employed in application of the masking liquid does not cause pollution to the environment; and (3) a coating sprayed by the masking liquid has better binding force and corrosion resistance than a conventional zinc coating.
Description
Technical field
The present invention relates to the manufacture field of Nd-Fe-B permanent magnet material, particularly to a kind of Nd-Fe-B permanent magnet material that is applied to
Masking liquid and preparation method thereof used in novel surface process for protecting processing procedure.
Background technology
At present, the known surface protection technique for Nd-Fe-B permanent magnet material mainly has electrogalvanizing (zn), nickel-copper-nickel
(ni-cu-ni), the film layer such as ni-cu-ni+ electrophoresis epoxy.And above-mentioned technology all can use passivating solution, using complete can produce useless
Liquid needs to process, and on the one hand environment can be caused with certain pollution, on the other hand also substantially increase production cost.
Content of the invention
In order to overcome the deficiency of the environmental pollution that the existing anticorrosion technique for Nd-Fe-B permanent magnet material brings, this
A kind of bright offer anti-corrosion masking liquid of new Nd-Fe-B permanent magnet material, the coating being sprayed into using this masking liquid not only makes matrix have by force
Corrosion resistance and high adhesion, and there is environment friendly.
The surfacecti proteon masking liquid of the Nd-Fe-B permanent magnet material that the present invention provides, is mainly expected by a, b material and c material form, with matter
Amount ratio meter a:b:c=1:1～1.5:0.00025～0.0025, wherein:
A material includes following component by percentage to the quality:
Zinc powder: 35-55%, preferably 40-52.6%；
Aluminium powder: 5-15%, preferably 8-14%；
Cosolvent: 35-55%, preferably 40-52%；
Surfactant: 0.5-2%, preferably 0.8-1.6%；
B material includes following component by percentage to the quality:
Chromic acid: 5-15%, preferably 6-10%；
Ph regulator: 1.0-3%, preferably 1.5-2.8%；
Zinc oxide: 1.0-3%, preferably 1.4-2.8%
Brium carbonate: 1.0-3%, preferably 1.6-2.4%
Water: 85-90%；
C expects for thickening agent.
Described in wherein said a material, cosolvent is selected from: triethylene glycol, diethylene glycol, ethylene glycol, n-butyl alcohol or propylene glycol first
Ether acetate etc., preferably triethylene glycol.
In wherein said a material, surfactant is selected from: alkylphenol polyoxyethylene, zinc stearate, lauryl alcohol polyoxyethylene
Ether and/or dodecyl sodium sulfate etc., preferably alkylphenol polyoxyethylene op-4 or alkylphenol polyoxyethylene op-7.
In wherein said b material, ph regulator is selected from: boric acid, calcium oxide or Lithium hydrate, Calcium Carbonate etc., preferably boric acid.
In wherein said b material, water is deionized water or distilled water, preferably deionized water.
In wherein said c material, thickening agent is selected from: hydroxyethyl cellulose, methylcellulose, hydroxymethyl cellulose or hydroxypropyl
Methylcellulose etc., preferably hydroxyethyl cellulose.
Zinc powder described in wherein said a material is flakey, and its average piece footpath is 15-25 μm, and thickness is 0.1-0.3 μm.
Aluminium powder described in wherein said a material is flakey, and its average piece footpath is 15-25 μm, and thickness is 0.1-0.3 μm.
The present invention also provides the compound method of described masking liquid
1) weigh corresponding material according to aforementioned,
2) by the raw material mix and blend of composition a material, gained slurry is polished that a expects；
3) by the raw material mix and blend of composition b material, standing obtains b material for 10～20 hours；
4) by gained b material according to aforementioned ratio, add in a material by several times, mix and blend, 30 DEG C -40 of monitoring mixed material temperature
DEG C, highest may not exceed 38 DEG C；
5) add c material, the finished product masking liquid of continuously stirred 10～20 hours, wherein question response temperature are down to when 35 DEG C and mixing
No granule in material, the mode slowly through vibrations adds c to expect.
Specific embodiment
With reference to non-limiting embodiment, the present invention is further detailed.
Preparation embodiment 1:
A material raw material:
Weigh zinc powder, flakey, average piece footpath is 15 μm, thickness is 0.1 μm, 3.4kg
Aluminium powder, flakey, average piece footpath is 15 μm, and thickness is 0.1 μm, 0.83kg
Triethylene glycol cosolvent 3.98kg；
Alkylphenol polyoxyethylene surfactant (op4,7): 0.09kg.
B material raw material:
Chromic acid: 0.88kg；
Boric acid: 0.16kg；
Zinc oxide: 0.18kg
Brium carbonate: 0.12kg
Deionized water: 10.35kg.
C expects hydroxyethyl cellulose: 0.015kg.
1. the preparation of a material
I () pours enough triethylene glycols in a material blender into；
(ii) alkylphenol polyoxyethylene mixed liquor is poured in a material blender；
(iii) start after pouring enough aluminium powders into stir, pour enough zinc powders after stirring with aluminium powder into, continue to stir
Mix；
(iv) mixing direction of blender will convert a direction every 15 minutes, gets out, now after positive and negative stirring 4 hours
Aluminum zinc powder more open；
V the slurry that blender stirs can be used after three-roll grinder grinding by ().When crossing three-roll grinder
Wanted twice so that the cohesiveness of aluminum zinc powder is compacter, and made finished product will not produce bubble.
2. the preparation of b material
I () pours enough deionized waters in b material blender into；
(ii) pour enough chromic acid, zinc oxide, boric acid and brium carbonate successively into, open blender and stir 4 hours；
(iii) place after having stirred and can use for 12 hours.
The preparation of finished product masking liquid
1. they can be stored after having prepared by a material and b material respectively with metal bucket and Plastic Drum；
2. first will be equipped with a material metal bucket put into water bath (need in the winter time by a material and b material put in water bath in advance
Row preheating, just can be prepared when temperature rises to 25 DEG C) in blender under, fix blender, rotating speed be adjusted to 7hz
It is stirred；
3. lentamente dividing 3 times after a material stirs adds b material to proceed to stir, and will measure after adding b material every time
Reaction temperature, prevents that reaction temperature is too high to cause masking liquid aging；
4. the maximum temperature of masking liquid to be measured in stirring, normal reaction temperature is 30 DEG C -35 DEG C, and highest can not
More than 38 DEG C；
5., after question response temperature is down to when 35 DEG C and is not had granule in masking liquid, the mode slowly through vibrations adds c
Material is so that c material can fully dissolve.Add c material number can be adjusted according to the viscosity of masking liquid；
6. the viscosity with the addition masking liquid of c material is gradually increased, and therefore needs for rotating speed to be adjusted to 8.5hz when adding c material,
Can use after continuously stirred 12 hours.
Preparation embodiment 2:
A material raw material:
Weigh zinc powder, flakey, average piece footpath is 20 μm, thickness is 0.2 μm, 3.7kg
Aluminium powder, flakey, average piece footpath is 20 μm, and thickness is 0.2 μm, 1.1kg
Diethylene glycol cosolvent 3.4kg；
Alkylphenol polyoxyethylene surfactant (op4,7): 0.1kg.
B material raw material:
Chromic acid: 1.0kg；
Boric acid: 0.2kg；
Zinc oxide: 0.3kg
Brium carbonate: 0.2kg
Distilled water: 10kg.
C expects hydroxyethyl cellulose: 0.01kg.
Other operations are as prepared embodiment 1
Preparation embodiment 3
A material raw material:
Weigh zinc powder, flakey, average piece footpath is 25 μm, thickness is 0.3 μm, 3.6kg
Aluminium powder, flakey, average piece footpath is 25 μm, and thickness is 0.3 μm, 1kg
Triethylene glycol cosolvent 3.6kg；
Sodium lauryl sulphate: 0.07kg.
B material raw material:
Chromic acid: 0.9kg；
Boric acid: 0.21kg；
Zinc oxide: 0.17kg
Brium carbonate: 0.21kg
Deionized water: 10.2kg.
C expects hydroxyethyl cellulose: 0.013kg.
Other operations are as prepared embodiment 1
Preparation embodiment 4
A material raw material:
Weigh zinc powder, flakey, average piece footpath is 15 μm, thickness is 0.1 μm, 4.04kg aluminium powder, flakey, average piece footpath
For 15 μm, thickness is 0.1 μm, 0.91kg
Triethylene glycol cosolvent 3.24kg；
Alkylphenol polyoxyethylene surfactant (op4,7): 0.11kg.
B material raw material:
Chromic acid: 0.7kg；
Boric acid: 0.26kg；
Zinc oxide: 0.15kg
Brium carbonate: 0.17kg
Deionized water: 10.42kg.
C expects methylcellulose: 0.012kg.
Other operations are as prepared embodiment 1
Preparation embodiment 5
A material raw material:
Weigh zinc powder, flakey, average piece footpath is 15 μm, thickness is 0.1 μm, 4.11kg aluminium powder, flakey, average piece footpath
For 15 μm, thickness is 0.1 μm, 0.67kg
Triethylene glycol cosolvent 3.45kg；
Alkylphenol polyoxyethylene surfactant (op4,7): 0.07kg.
B material raw material:
Chromic acid: 1.1kg；
Boric acid: 0.17kg；
Zinc oxide: 0.19kg
Brium carbonate: 0.23kg
Deionized water: 10.03kg.
C expects hydroxyethyl cellulose: 0.015kg.
Other operations are as prepared embodiment 1
The following parameter of masking liquid is measured, using aperture, No. 2 cups of Chai Shi for 2.74mm are carried out measurement viscosity, masking liquid
In cr6+Content, is measured using Ferrous ammonium sulfate titration method.
| Parameter name | Range |
| Apply fluid viscosity | The 20-30 second |
| Masking liquid proportion | 1.30-1.36 |
| The ph value of masking liquid | 3.8-5.2 |
| Cr in masking liquid6+Content | >=25g/l |
| The temperature of use environment | <20℃ |
| The humidity of use environment | 45%-65% |
Points for attention in use: 1. masking liquid needs persistently to be stirred, but can not stir too fast, prevent due to quickly stirring
Mix and cause masking liquid aging；
2. masking liquid needs persistently to enter the measurement of line parameter in use, as cr in masking liquid6+Content is less than 20g/l, meeting
So that the adhesion of spraying workpiece and salt spray test effect reduce, now need more to renew the masking liquid of preparation；
3., when applying the masking liquid in flow container and be very few, need first remaining masking liquid is carried out with the detection of parameters, if
Parameters index is all normal, then can add the new masking liquid prepared in flow container to applying, be continuing with.Which reduces masking liquid
Waste.
4. the new masking liquid prepared needs to be filtered with the screen cloth of 100 mesh before initial use, reuses No. 2 cups of Chai Shi and surveys
Amount viscosity.
Carry out spraying the neodymium iron boron magnetic body obtaining using galvanized method (matched group) with using the chromium masking liquid that has of the present invention, enter
The adhesion of row finished product and the contrast of neutral salt spray test.Adhesion is according to the People's Republic of China (PRC) the 4th Machinery Ministry ministerial standard
Sj1282-77 is carried out.Take 100 magnetic steel of motor samples, be divided into 10 groups to measure, every group of measurement result is averaged,
Finally again the meansigma methodss of 10 groups of samples are averaged again.Testing result contrast table is as follows:
The comparing result of table 1 adhesion
Neutral salt spray test is carried out according to People's Republic of China's rare-earth trade standard xb/t903-2002.Test side
Method be magnetic steel of motor is magnetized after mutually rubbed, friction respectively places in salt spray test chamber for 1-5 time and is tested.Test
Comparing result is as follows:
Table 2 neutral salt spray test comparing result
Masking liquid in the present invention uses closed spraying method in use, and can constantly add new
The masking liquid prepared, does not result in masking liquid and wastes, will not produce waste water and waste liquid yet, environment will not be impacted.
The workpiece processing using this novel surface process for protecting and through this masking liquid, not only can improve permanent magnet material coating
Adhesion, corrosion resistance and there is good environment friendly.
Claims (1)
1. a kind of surfacecti proteon masking liquid of Nd-Fe-B permanent magnet material is it is characterised in that be prepared by the following method acquisition:
Weigh a material raw material: weigh zinc powder 3.4kg, it is flakey, average piece footpath is 15 μm, and thickness is 0.1 μm；Weigh aluminium powder
0.83kg, it is flakey, and average piece footpath is 15 μm, and thickness is 0.1 μm；Weigh triethylene glycol cosolvent 3.98kg；Weigh alkane
Base phenol polyethenoxy ether surface active agent 0.09kg；
Weigh b material raw material: weigh chromic acid 0.88kg；Boric acid 0.16kg；Zinc oxide 0.18kg；Brium carbonate 0.12kg；Deionized water:
10.35kg；
Weigh c material hydroxyethyl cellulose 0.015kg；
The compound method of described a material is:
I () is poured into triethylene glycol, alkylphenol polyoxyethylene and aluminium powder in a material blender by proportioning and is started to stir, to be mixed
Pour zinc powder after uniformly into, continue stirring；
(ii) blender stirring gained slurry is ground through twice；
The compound method of described b material is:
By proportioning, deionized water, chromic acid, zinc oxide, boric acid and brium carbonate are poured in b material blender successively, open blender and stir
Mix 4 hours；Place after having stirred and can use for 12 hours；
A is expected, b material and c material carry out the preparation of finished product masking liquid:
I a material is stirred by (), after a material stirs, point 3 addition b material proceed to stir, and control mixed material temperature
For 30 DEG C -38 DEG C；
(ii), after question response temperature is down to and is not had granule in 35 DEG C and masking liquid, c is added to expect by way of vibrations, continuously stirred
Obtain final product after 12 hours.
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| CN201310430430.2A CN104004397B (en) | 2013-09-18 | 2013-09-18 | Masking liquid used for surface protection of neodymium iron boron magnet, and preparation method thereof |
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| CN104004397B true CN104004397B (en) | 2017-01-25 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104250462A (en) * | 2014-08-21 | 2014-12-31 | 王广波 | Dacromet coating |
| CN104894553B (en) * | 2015-04-09 | 2017-12-26 | 中国科学院宁波材料技术与工程研究所 | Improve the method and its application of material surface modifying layer performance |
| CN104795199A (en) * | 2015-05-14 | 2015-07-22 | 海安县巨力磁材有限责任公司 | Corrosion-proof radial-anisotropy magnetic ring |
| CN106128744B (en) * | 2016-08-16 | 2019-04-19 | 安徽大地熊新材料股份有限公司 | A kind of Sintered NdFeB magnet surface temporary protection organic coating and preparation method |
| CN107424829B (en) * | 2017-09-08 | 2019-06-11 | 京磁材料科技股份有限公司 | The preparation method of corrosion-resistant Ne-Fe-B magnet |
| CN112517602B (en) * | 2020-11-12 | 2022-02-01 | 北京工业大学 | Pretreatment method for recycling neodymium iron boron waste with adhesive tape oil sludge |
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| CN1128547A (en) * | 1993-08-05 | 1996-08-07 | 日本达克乐沙慕陆股份有限公司 | Surface coating method |
| CN1229821A (en) * | 1999-02-09 | 1999-09-29 | 王璐 | Zinc base water soluble anti-corrosion paint for metal surface and its prepn. method |
| CN1428379A (en) * | 2002-12-19 | 2003-07-09 | 殷跃军 | Production method of coating material |
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