CN104004397A - 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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- CN104004397A CN104004397A CN201310430430.2A CN201310430430A CN104004397A CN 104004397 A CN104004397 A CN 104004397A CN 201310430430 A CN201310430430 A CN 201310430430A CN 104004397 A CN104004397 A CN 104004397A
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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-Bo permanent magnet material, particularly a kind of masking liquid of using in the novel surface process for protecting treating processes of Nd-Fe-Bo permanent magnet material and preparation method thereof that is applicable to.
Background technology
At present, the known surface protection technique for Nd-Fe-Bo permanent magnet material mainly contains the retes such as electro-galvanizing (Zn), nickel-copper-nickel (Ni-Cu-Ni), Ni-Cu-Ni+ electrophoresis epoxy.And above-mentioned technology all can be used passivating solution, use and can need to process by generation waste liquid, can cause certain pollution to environment on the one hand, also greatly improve on the other hand production cost.
Summary of the invention
In order to overcome the deficiency of the existing environmental pollution bringing for the anticorrosion technique of Nd-Fe-Bo permanent magnet material, the invention provides the anticorrosion masking liquid of a kind of novel Nd-Fe-Bo permanent magnet material, use the coating that this masking liquid is sprayed into not only to make matrix there is strong erosion resistance and high bonding force, and there is environment friendly.
The surfacecti proteon masking liquid of Nd-Fe-Bo permanent magnet material provided by the invention, is mainly made up of A material, B material and C material, A:B:C=1:1～1.5:0.00025～0.0025 by quality ratio, wherein:
A material comprises following component by percentage to the quality:
Zinc powder: 35-55%, preferably 40-52.6%;
Aluminium powder: 5-15%, preferably 8-14%;
Solubility promoter: 35-55%, preferably 40-52%;
Tensio-active agent: 0.5-2%, preferably 0.8-1.6%;
B material comprises following component by percentage to the quality:
Chromic acid: 5-15%, preferably 6-10%;
PH adjusting agent: 1.0-3%, preferably 1.5-2.8%;
Zinc oxide: 1.0-3%, preferably 1.4-2.8%
Barium carbonate: 1.0-3%, preferably 1.6-2.4%
Water: 85-90%;
C material is thickening material.
Described in wherein said A material, solubility promoter is selected from: triethylene glycol, Diethylene Glycol, ethylene glycol, propyl carbinol or 1-Methoxy-2-propyl acetate etc., be preferably triethylene glycol.
In wherein said A material, tensio-active agent is selected from: alkylphenol polyoxyethylene, Zinic stearas, Dodecyl Polyoxyethylene Ether and/or sodium laurylsulfonate etc., be preferably alkylphenol polyoxyethylene OP-4 or alkylphenol polyoxyethylene OP-7.
In wherein said B material, pH adjusting agent is selected from: boric acid, calcium oxide or lithium hydroxide, calcium carbonate etc., be preferably boric acid.
In wherein said B material, water is deionized water or distilled water, is preferably deionized water.
In wherein said C material, thickening material is selected from: Natvosol, methylcellulose gum, Walocel MT 20.000PV or Vltra tears etc., be preferably Natvosol.
Zinc powder described in wherein said A material is flakey, and its average sheet footpath is 15-25 μ m, and thickness is 0.1-0.3 μ m.Aluminium powder described in wherein said A material is flakey, and its average sheet footpath is 15-25 μ m, and thickness is 0.1-0.3 μ m.
The present invention also provides the compound method of described masking liquid
1) take corresponding material according to aforementioned,
2), by the raw material mix and blend of composition A material, gained soup compound obtains A material after grinding;
3), by the raw material mix and blend of composition B material, leave standstill 10～20 hours and obtain B material;
4) gained B is expected according to aforementioned ratio, gradation adds in A material, mix and blend, and 30 DEG C-40 DEG C of monitoring mixture temperature, the highlyest can not exceed 38 DEG C;
5) add C material, continue to stir the finished product masking liquid of 10～20 hours, without particle, add C material by the mode of vibrations lentamente when wherein question response temperature is down to 35 DEG C and in mixture.
Embodiment
Below in conjunction with nonrestrictive embodiment, the present invention is further detailed.
Preparation Example 1:
A expects raw material:
Take zinc powder, flakey, average sheet footpath is 15 μ m, thickness is 0.1 μ m, 3.4kg
Aluminium powder, flakey, average sheet footpath is 15 μ m, thickness is 0.1 μ m, 0.83kg
Triethylene glycol solubility promoter 3.98kg;
Alkylphenol polyoxyethylene tensio-active agent (OP4,7): 0.09kg.
B expects raw material:
Chromic acid: 0.88kg;
Boric acid: 0.16kg;
Zinc oxide: 0.18kg
Barium carbonate: 0.12kg
Deionized water: 10.35kg.
C expects Natvosol: 0.015kg.
1. the preparation of A material
(i) enough triethylene glycols are poured in A material stirrer;
(ii) alkylphenol polyoxyethylene mixed solution is poured in A material stirrer;
(iii) pour into after enough aluminium powders and start to stir, after stirring with aluminium powder, pour enough zinc powders into, continue to stir;
(iv) mixing direction of stirrer will every 15 minutes conversion first power to, get out after 4 hours until positive and negative stirring, aluminum zinc powder is now more open;
(v) soup compound stirrer being stirred can use after three-roll grinder grinds.In the time crossing three-roll grinder, wanted twice, and made the cohesive force of aluminum zinc powder compacter, and made finished product can not produce bubble.
2. the preparation of B material
(i) enough deionized waters are poured in B material stirrer;
(ii) pour successively enough chromic acid, zinc oxide, boric acid and barium carbonate into, open stirrer and stir 4 hours;
(iii) having stirred rear placement can use for 12 hours.
The preparation of finished product masking liquid
1. A material and B material can be stored them respectively after having prepared with metal bucket and plastic tank;
2. first the metal bucket that A material is housed being put into water bath (needs A material and B to expect that putting in advance water bath carries out preheating in the winter time, in the time that temperature rises to 25 DEG C, just can prepare) in stirrer under, fix stirrer, rotating speed is adjusted to 7Hz and stirs;
3. after A material stirs, divide lentamente and add for 3 times B material to proceed to stir, all will measure temperature of reaction after adding B material at every turn, prevent that the too high masking liquid that causes of temperature of reaction is aging;
4. in the time stirring, will measure the maximum temperature of masking liquid, normal temperature of reaction is 30 DEG C-35 DEG C, the highlyest can not exceed 38 DEG C;
5. when question response temperature is down to 35 DEG C and in masking liquid, do not have after particle, add C material by the mode of vibrations lentamente, C material can fully be dissolved.Add C material number can adjust according to the viscosity of masking liquid;
6. along with the viscosity that adds masking liquid of C material increases gradually, therefore in the time adding C material, rotating speed need to be adjusted to 8.5Hz, continue to stir after 12 hours and can use.
Preparation Example 2:
A expects raw material:
Take zinc powder, flakey, average sheet footpath is 20 μ m, thickness is 0.2 μ m, 3.7kg
Aluminium powder, flakey, average sheet footpath is 20 μ m, thickness is 0.2 μ m, 1.1kg
Diethylene Glycol solubility promoter 3.4kg;
Alkylphenol polyoxyethylene tensio-active agent (OP4,7): 0.1kg.
B expects raw material:
Chromic acid: 1.0kg;
Boric acid: 0.2kg;
Zinc oxide: 0.3kg
Barium carbonate: 0.2kg
Distilled water: 10kg.
C expects Natvosol: 0.01kg.
Other operates as Preparation Example 1
Preparation Example 3
A expects raw material:
Take zinc powder, flakey, average sheet footpath is 25 μ m, thickness is 0.3 μ m, 3.6kg
Aluminium powder, flakey, average sheet footpath is 25 μ m, thickness is 0.3 μ m, 1kg
Triethylene glycol solubility promoter 3.6kg;
Sodium lauryl sulphate: 0.07kg.
B expects raw material:
Chromic acid: 0.9kg;
Boric acid: 0.21kg;
Zinc oxide: 0.17kg
Barium carbonate: 0.21kg
Deionized water: 10.2kg.
C expects Natvosol: 0.013kg.
Other operates as Preparation Example 1
Preparation Example 4
A expects raw material:
Take zinc powder, flakey, average sheet footpath is 15 μ m, thickness is 0.1 μ m, 4.04kg aluminium powder, flakey, average sheet footpath is 15 μ m, thickness is 0.1 μ m, 0.91kg
Triethylene glycol solubility promoter 3.24kg;
Alkylphenol polyoxyethylene tensio-active agent (OP4,7): 0.11kg.
B expects raw material:
Chromic acid: 0.7kg;
Boric acid: 0.26kg;
Zinc oxide: 0.15kg
Barium carbonate: 0.17kg
Deionized water: 10.42kg.
C expects methylcellulose gum: 0.012kg.
Other operates as Preparation Example 1
Preparation Example 5
A expects raw material:
Take zinc powder, flakey, average sheet footpath is 15 μ m, thickness is 0.1 μ m, 4.11kg aluminium powder, flakey, average sheet footpath is 15 μ m, thickness is 0.1 μ m, 0.67kg
Triethylene glycol solubility promoter 3.45kg;
Alkylphenol polyoxyethylene tensio-active agent (OP4,7): 0.07kg.
B expects raw material:
Chromic acid: 1.1kg;
Boric acid: 0.17kg;
Zinc oxide: 0.19kg
Barium carbonate: 0.23kg
Deionized water: 10.03kg.
C expects Natvosol: 0.015kg.
Other operates as Preparation Example 1
Following parameter to masking liquid is measured, and measures viscosity and adopts No. 2 cups of Chai Shi that aperture is 2.74mm to carry out, the Cr in masking liquid
6+content, adopts ferrous ammonium sulphate titration method to measure.
| Parameter name | Use range |
| Be coated with fluid viscosity | 20-30 second |
| Masking liquid proportion | 1.30-1.36 |
| The pH value of masking liquid | 3.8-5.2 |
| Cr in masking liquid 6+Content | ≥25g／L |
| The temperature of environment for use | <20℃ |
| The humidity of environment for use | 45％-65％ |
Precaution in use: 1. masking liquid need to continue to stir, but can not stir too fastly, prevent because rapid stirring causes masking liquid aging;
2. masking liquid in use needs to continue to carry out the measurement of parameter, as Cr in masking liquid
6+content, lower than 20g/L, can make the bonding force and the salt-fog test effect that spray workpiece reduce, and now needs more to renew the masking liquid of preparation;
3. in the time that the masking liquid in painting flow container is very few, need first carry out remaining masking liquid the detection of parameters, if parameters index is all normal, can add the new masking liquid of preparing to being coated with in flow container, continue to use.So just reduce the waste of masking liquid.
4. the masking liquid of new preparation needs to filter with 100 object screen clothes before bringing into use, and re-uses No. 2 cups of Chai Shi and measures viscosity.
Use galvanized method (control group) and use of the present inventionly to have chromium masking liquid to spray the neodymium iron boron magnetic body obtaining, carry out the bonding force of finished product and the contrast of neutral salt spray test.Bonding force is carried out according to the 4th Machinery Ministry ministerial standard SJ1282-77 of the People's Republic of China (PRC).Get 100 magnetic steel of motor samples, be divided into 10 groups and measure, the measuring result of every group is averaged, and finally the mean value of 10 groups of samples is averaged again again.Detected result contrast table is as follows:
The comparing result of table 1 bonding force
Neutral salt spray test carries out according to the rare-earth trade standard x B/T903-2002 of the People's Republic of China (PRC).Test method is mutually to rub after magnetic steel of motor is magnetized, and rubs respectively to put into salt-spray cabinet for 1-5 time again and test.Experimental Comparison result is as follows:
Table 2 neutral salt spray test comparing result
What the masking liquid in the present invention in use adopted is closed spraying method, and can constantly add the masking liquid of new preparation, can not cause masking liquid waste, also can not produce waste water and waste liquid, can not impact environment.
The workpiece that utilizes this novel surface process for protecting and processed through this masking liquid, not only can improve the bonding force of permanent magnet material coating, corrosion resistance and have good environment friendly.
Claims (9)
1. a surfacecti proteon masking liquid for Nd-Fe-Bo permanent magnet material, is characterized in that being mainly made up of A material, B material and C material, by quality ratio, and A:B:C=1:1～1.5:0.00025～0.0025,
Wherein:
A material comprises following component by percentage to the quality:
Zinc powder: 35-55%;
Aluminium powder: 5-15%;
Solubility promoter: 35-55%;
Tensio-active agent: 0.5-2%;
B material comprises following component by percentage to the quality:
Chromic acid: 5-15%;
PH adjusting agent: 1.0-3%;
Zinc oxide: 1.0-3%
Barium carbonate: 1.0-3%
Water: 85-90%;
C material is thickening material.
2. the surfacecti proteon masking liquid of Nd-Fe-Bo permanent magnet material according to claim 1, wherein:
A material comprises following component by percentage to the quality:
Zinc powder: 40-52.6%;
Aluminium powder: 8-14%;
Solubility promoter: 40-52%;
Tensio-active agent: 0.8-1.6%;
B material comprises following component:
Chromic acid: 6-10%;
PH adjusting agent: 1.5-2.8%;
Zinc oxide: 1.4-2.8%;
Barium carbonate: 1.6-2.4%;
Water: 85-90%.
3. the surfacecti proteon masking liquid of Nd-Fe-Bo permanent magnet material according to claim 1, described in wherein said A material, solubility promoter is selected from: triethylene glycol, Diethylene Glycol, ethylene glycol, propyl carbinol and/or 1-Methoxy-2-propyl acetate, in wherein said A material, tensio-active agent is selected from: alkylphenol polyoxyethylene, Zinic stearas, Dodecyl Polyoxyethylene Ether or sodium laurylsulfonate.
4. the surfacecti proteon masking liquid of Nd-Fe-Bo permanent magnet material according to claim 1, in wherein said B material, pH adjusting agent is selected from: boric acid, calcium oxide, lithium hydroxide and/or calcium carbonate, in wherein said B material, water is deionized water or distilled water.
5. the surfacecti proteon masking liquid of Nd-Fe-Bo permanent magnet material according to claim 1, in wherein said C material, thickening material is selected from: Natvosol, methylcellulose gum, Walocel MT 20.000PV and/or Vltra tears.
6. the surfacecti proteon masking liquid of Nd-Fe-Bo permanent magnet material according to claim 1, described in wherein said A material, solubility promoter is triethylene glycol, in A material, tensio-active agent is alkylphenol polyoxyethylene OP-4 or alkylphenol polyoxyethylene OP-7, in described B material, pH adjusting agent is boric acid, in described B material, water is deionized water, and in wherein said C material, thickening material is Natvosol.
7. according to the surfacecti proteon masking liquid of arbitrary described Nd-Fe-Bo permanent magnet material in claim 1-6, described in wherein said A material, zinc powder is flakey, its average sheet footpath is 15-25 μ m, thickness is 0.1-0.3 μ m, described aluminium powder is flakey, its average sheet footpath is 15-25 μ m, and thickness is 0.1-0.3 μ m.
8. according to the compound method of the surfacecti proteon masking liquid of arbitrary described Nd-Fe-Bo permanent magnet material in claim 1-7
1) take in proportion material;
2), by the raw material mix and blend of composition A material, gained soup compound obtains A material after grinding;
3), by the raw material mix and blend of composition B material, leave standstill 10～20 hours and obtain B material;
4) gained B material is added in A material to mix and blend, 30 DEG C-40 DEG C of monitoring mixture temperature;
5) add C material, continue to stir the finished product masking liquid of 10～20 hours.
9. the compound method of the surfacecti proteon masking liquid of Nd-Fe-Bo permanent magnet material according to claim 8, wherein step 4) in monitoring mixture temperature be no more than 38 DEG C; Wherein step 5) in question response temperature while being down to 35 DEG C and in mixture without particle, add C material by the mode of vibrations lentamente.
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Cited By (6)
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| CN104250462A (en) * | 2014-08-21 | 2014-12-31 | 王广波 | Dacromet coating |
| 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 |
| WO2016161742A1 (en) * | 2015-04-09 | 2016-10-13 | 中国科学院宁波材料技术与工程研究所 | Method for improving performance of modification layer of material surface and application thereof |
| CN106128744A (en) * | 2016-08-16 | 2016-11-16 | 安徽大地熊新材料股份有限公司 | A kind of organic coating of Sintered NdFeB magnet surface temporary protection and preparation method thereof |
| CN107424829A (en) * | 2017-09-08 | 2017-12-01 | 京磁材料科技股份有限公司 | The preparation method of corrosion-resistant Ne-Fe-B magnet |
| CN112517602A (en) * | 2020-11-12 | 2021-03-19 | 北京工业大学 | Pretreatment method for recycling neodymium iron boron waste with adhesive tape oil sludge |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN112517602A (en) * | 2020-11-12 | 2021-03-19 | 北京工业大学 | Pretreatment method for recycling neodymium iron boron waste with adhesive tape oil sludge |
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