CN103695884B - Passivating metal magnesium particles and passivating method thereof - Google Patents
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Abstract
The invention discloses passivating metal magnesium particles and a passivating method thereof. The passivating metal magnesium particles comprise the following components in percentage by weight: less than or equal to 99% and greater than or equal to 92% of Mg, less than or equal to 0.002% of S, less than or equal to 0.01% of Cu, less than or equal to 0.001% of P and less than or equal to 1.2% and greater than or equal to 0.1% of H2O. The passivating method comprises the following steps: (I), preparing a metal magnesium particle passivator, placing metal magnesium particles in the passivator, and then naturally cooling to room temperature; (II), coating a coating on the surface of the magnesium particles: firstly, coating an organic silicon compound on the surface of the metal magnesium particles, coating magnesium oxide on the surface of the metal magnesium particles, then, coating compound rare earth on the on the surface of the metal magnesium particles, and finally coating graphite powder on the surface of the metal magnesium particles; and (III), sieving the metal magnesium particles cooled to room temperature. The metal magnesium particle passivating layer is uniform in coating, and the storage and use safety is ensured.
Description
Technical field
The present invention relates to a kind of passivating technique, specifically a kind of passive metal magnesium grain and its passivating method.
Background technology
Carried out with metal magnesium desulfurizer desulfurizing iron treatment have many advantages, at present the country some producers for example Baosteel, this steel,
The iron and steel enterprises such as Wuhan Iron and Steel Plant are also begun to using the technique.The activity of magnesium metal is very high, it is therefore necessary to could pacify after being passivated treatment
Transport entirely, store, use；The passivation of metallic magnesium surface has many methods, can such as use organic film Protection Code, galvanoplastic, chromium
Hydrochlorate is passivated embrane method, but this applies in general to the surface treatment of magnesium ingot, the table without being suitable as the magnesium grain that desulfurizing agent is used
Face Passivation Treatment.At present, the surface treatment of magnesium grain has two methods：One is chemical reaction method, the magnesium and passivator on magnesium grain surface
Reaction one finer and close product film layer of generation；Two is using surface cladding process, i.e., to cover another material on magnesium grain surface,
The material not with metal reactive magnesium.The magnesium grain passivation layer processed using method one is uniform, but duration of fire resistance is short, and burning-point is low；Using
Method two is processed, and magnesium metal will not lose, but when the surface covering of magnesium grain is uneven, causes to be passivated uneven, passivation effect difference etc.
Causing the passivation index of a series of problems, current magnesium metal not yet has unified national standard.
Such as published patent of invention, Application No.：A kind of 200610013324.4 " Passivation Treatment skill of magnesium metal grain
Art ", the patent of invention is using physical method passive metal magnesium grain, but during passive metal magnesium grain, and it is uniform that it is coated
Property be difficult control, it is easy to produce security incident, the uniformity of processing procedure coating is unreliable.
The content of the invention
The technical problems to be solved by the invention are the shortcomings for overcoming prior art, there is provided a kind of passive metal magnesium grain and its
Passivating method, it is therefore an objective to increase the duration of fire resistance of magnesium metal grain after passivation, improve burning-point, increase its stability, it is to avoid metal
The uneven grade of magnesium grain coating triggers a series of problem.
In order to solve the above-mentioned technical problem, the technical scheme is that realizing by the following method：
A kind of passive metal magnesium grain, passive metal magnesium grain is by the magnesium metal grain positioned at innermost layer, to be rolled in magnesium metal grain outer
Surface passivator, and it is rolled in the coating composition of passivator outer surface；
Magnesium metal grain weight percent composition be：92%≤Mg≤99%, S≤0.002%, Cu≤0.01%, P≤
0.001%, 0.1%≤H2O≤1.2%, each composition sum of the above is 100%；
Passivator is made up of two hydration sodium tartrates, sodium fluoride, phosphoric acid and potassium chromate, and two hydration sodium tartrates, fluorination
The weight ratio of sodium, phosphoric acid and potassium chromate is 4-6:2-5:1-3:1-4；
Coating is made up of graphite powder, magnesia, compound rare-earth and organo-silicon compound, graphite powder, magnesia, compound rare-earth
It is 1-4 with organo-silicon compound weight ratio:4-6:2-4:2-3；Organic silicon compound is made up of silicone oil and silicones, silicone oil and silicon tree
The weight ratio of fat is 1:2；Compound rare-earth includes following component by weight percentage：La：25-35%, Y：12-15%, Sc：8-
12%, Gd：8-20%, Sm：5-7%, Pr：13-20%, each rare earth composition sum of the above is 100%.
The passivating method of magnesium metal grain, the method is carried out according to the following steps：
(i) preparing metal magnesium grain passivator, magnesium metal grain is put into passivator, and passivation time is：25-35min, passivation
Temperature is：85-95 DEG C, the magnesium metal that will be passivated grain is dried, and drying time is：145-160 DEG C, drying time is：20-
40min, then naturally cools to room temperature；
(ii) the magnesium metal grain surface that will be cooled to room temperature coats one layer of coating, and coating layer thickness is：0.05-0.1mm；
Specific processing method：Organo-silicon compound are first coated in magnesium metal grain surface, are then dried, drying time is：
25-30min, drying temperature is：130-155 DEG C, naturally cool to room temperature；Magnesia is coated in magnesium metal grain surface again, so
After dry, drying time is：25-30min, drying temperature is：130-160 DEG C, naturally cool to room temperature；Compound rare-earth is applied again
Magnesium metal grain surface is overlayed on, drying time is：25-30min, drying temperature is：130-155 DEG C, naturally cool to room temperature；Finally
Graphite powder is coated in magnesium metal grain surface, is then dried, drying time is：25-30min, drying temperature is：135-150 DEG C,
Naturally cool to room temperature；
(iii) the magnesium metal grain screening of room temperature is will be cooled to, finished product is made.
The present invention, wraps up its passivation layer uniform, closely knit, and the control of active content of magnesium, duration of fire resistance and product granularity is accurate,
General machinery mill is rubbed with the hands, extruding is difficult to be allowed to come off, it is ensured that transport, storage and using safety, and hydration resistance is superior, is difficult
The moisture absorption, long shelf-life is adapted to various weather conditions producers and uses.Good mobility, makes it in desulfurization dusting operation, blanking
Smooth, without blocking, expulsion events, desulfurized effect is good, unit consumption is low, it is adaptable to which molten iron pre-processes composite blowing and single spraying magnesium powder work
Skill.
In addition, the present invention is by adding the rare earth of appropriate level, after the grain use of passive metal magnesium, make the molten iron after desulfurization
After being made metal billet, the crystalline structure of metal billet is can obviously improve, be allowed to tough and tensile, cold-forming property improves, it is possible to most
Limits ground obtains rare earth element recovery rate, and it is uniformly distributed in steel, hence it is evident that improves continuous casting billet quality, increases its strong
Degree, wearability, corrosion resistance obtains unexpected technique effect.
It is of the invention it is further restriction technical scheme be：
Foregoing passive metal magnesium grain, the weight percent composition of magnesium metal grain is：Mg：98.7%, S：0.002%, Cu：
0.01%, P：0.001%, H2O：1.2%；The weight ratio of two hydration sodium tartrates, sodium fluoride, phosphoric acid and potassium chromate is 5:2:2:1；
Graphite powder, magnesia, compound rare-earth and organo-silicon compound weight ratio are 4:2:3:2；In compound rare-earth, wrap by weight percentage
Containing following component：La：35%, Y：15%, Sc：12%, Gd：11%, Sm：7%, Pr：20%.
Foregoing passive metal magnesium grain, the weight percent composition of magnesium metal grain is：Mg：98.8%, S:0%, Cu:0%, P:
0%, H2O：1.2%；The weight ratio of two hydration sodium tartrates, sodium fluoride, phosphoric acid and potassium chromate is 4:2:1:3；Graphite powder, oxidation
Magnesium, compound rare-earth and organo-silicon compound weight ratio are 2:5:2:3；In compound rare-earth, by weight percentage comprising following component：
La：35%, Y：15%, Sc：10%, Gd：18%, Sm：7%, Pr：15%.
Foregoing passive metal magnesium grain, the weight percent composition of magnesium metal grain is：Mg：98.9%, S：0%, Cu：0.01%,
P：0%, H2O：1%；The weight ratio of two hydration sodium tartrates, sodium fluoride, phosphoric acid and potassium chromate is 6:2:1:1；Graphite powder, oxidation
Magnesium, compound rare-earth and organo-silicon compound weight ratio are 3:4:3:3；In compound rare-earth, by weight percentage comprising following component：
La：30%, Y：15%, Sc：10%, Gd：20%, Sm：6%, Pr：19%.
The present invention has the following advantages that compared with prior art：
The present invention, first passes through chemical method passive metal magnesium grain, makes the oxidation of the surface formation even compact of magnesium metal grain
Thing, it is to avoid using the inhomogeneities of physical method cladding magnesium metal grain, and a series of safety problems for triggering, by physics
Method make magnesium metal grain surface coat one layer of coating again, it is ensured that its transportation and using process security, increased
The duration of fire resistance of magnesium metal grain, improves burning-point, and increased the hydrophobicity of magnesium metal grain.
The present invention, wraps up its passivation layer uniform, closely knit, and the control of active content of magnesium, duration of fire resistance and product granularity is accurate,
General machinery mill is rubbed with the hands, extruding is difficult to be allowed to come off, it is ensured that transport, storage and using safety, and hydration resistance is superior, is difficult
The moisture absorption, long shelf-life is adapted to various weather conditions producers and uses.Good mobility, makes it in desulfurization dusting operation, blanking
Smooth, without blocking, expulsion events, desulfurized effect is good, unit consumption is low, it is adaptable to which molten iron pre-processes composite blowing and single spraying magnesium powder work
Skill.
The present invention, graphite powder is added in the coating on magnesium metal grain surface, makes the grain of the magnesium metal after passivation chemically steady
It is fixed, do not influenceed by strong acid-base, objectionable impurities is few, and iron sulfur content is low, is metal after passivation with high temperature resistant, lubrication and plasticity
The use reliability of magnesium grain is stronger, and operation strategies are wider.
In addition, the present invention is by adding the rare earth of appropriate level, after the grain use of passive metal magnesium, make the molten iron after desulfurization
After being made metal billet, the crystalline structure of metal billet is can obviously improve, be allowed to tough and tensile, cold-forming property improves, it is possible to most
Limits ground obtains rare earth element recovery rate, and it is uniformly distributed in steel, hence it is evident that improves continuous casting billet quality, increases its strong
Degree, wearability, corrosion resistance obtains unexpected technique effect.
Specific embodiment
Embodiment 1
The present embodiment provide passive metal magnesium grain and its passivating method, the magnesium metal grain weight percent composition be：
Mg：98.7%, S：0.002%, Cu：0.01%, P：0.001%, H2O：1.2%；In compound rare-earth, by weight percentage comprising following
Composition：La：35%, Y：15%, Sc：12%, Gd：11%, Sm：7%, Pr：20%.
The passivating method of magnesium metal grain is carried out according to the following steps：
(i) preparing metal magnesium grain passivator, passivator be two hydration sodium tartrates, sodium fluoride, phosphoric acid, potassium chromate, and passivation
Agent is by weight respectively：5:2:2:1；Magnesium metal grain is put into passivator, passivation time is：22min, passivation temperature is：
85 DEG C, the magnesium metal that will be passivated grain is dried, and drying time is：145 DEG C, drying time is：20min is then naturally cold
But to room temperature；
(ii) the magnesium metal grain surface that will be cooled to room temperature coats one layer of coating, and coating layer thickness is：0.05mm, coating by：Stone
Ink powder, magnesia, organo-silicon compound composition；Graphite powder, magnesia, compound rare-earth and organo-silicon compound weight ratio are：4:
2:3:2；Organic silicon compound is made up of silicone oil and silicones, and the weight ratio of silicone oil and silicones is：1:2；
Specific processing method：Organo-silicon compound are first coated in magnesium metal grain surface, are then dried, drying time is：
30min, drying temperature is：155 DEG C, naturally cool to room temperature；Magnesia is coated in magnesium metal grain surface again, is then dried,
Drying time is：30min, drying temperature is：160 DEG C, naturally cool to room temperature；Rare earth is coated in magnesium metal grain surface again,
Drying time is：30min, drying temperature is：155 DEG C, naturally cool to room temperature；Graphite powder is finally coated in magnesium metal grain table
Face, then dries, and drying time is：30min, drying temperature is：150 DEG C, naturally cool to room temperature；
(iii) the magnesium metal grain screening of room temperature is will be cooled to, finished product is made.
Embodiment 2
The present embodiment provide passive metal magnesium grain and its passivating method, magnesium metal grain weight percent composition be：
Mg：98.8%, S:0%, Cu:0%, P:0%, H2O：1.2%；In compound rare-earth, by weight percentage comprising following component：La：35%,
Y：15%, Sc：10%, Gd：18%, Sm：7%, Pr：15%.
The passivating method of magnesium metal grain is carried out according to the following steps：
(i) preparing metal magnesium grain passivator, passivator be two hydration sodium tartrates, sodium fluoride, phosphoric acid, potassium chromate, and passivation
Agent is by weight respectively：4:2:1:3；Magnesium metal grain is put into passivator, passivation time is：35min, passivation temperature is：
95 DEG C, the magnesium metal that will be passivated grain is dried, and drying time is：160 DEG C, drying time is：40min is then naturally cold
But to room temperature；
(ii) the magnesium metal grain surface that will be cooled to room temperature coats one layer of coating, and coating layer thickness is：0.1mm, coating by：Graphite
Powder, magnesia, organo-silicon compound composition；Graphite powder, magnesia, compound rare-earth and organo-silicon compound weight ratio are：2:5:
2:3；Organic silicon compound is made up of silicone oil and silicones, and the weight ratio of silicone oil and silicones is：1:2；
Specific processing method：Organo-silicon compound are first coated in magnesium metal grain surface, are then dried, drying time is：
25min, drying temperature is：130 DEG C, naturally cool to room temperature；Magnesia is coated in magnesium metal grain surface again, is then dried,
Drying time is：25min, drying temperature is：130 DEG C, naturally cool to room temperature；Compound rare-earth is coated in magnesium metal grain table again
Face, drying time is：25min, drying temperature is：130 DEG C, naturally cool to room temperature；Graphite powder is finally coated in magnesium metal
Grain surface, then dries, and drying time is：25min, drying temperature is：135 DEG C, naturally cool to room temperature；
(iii) the magnesium metal grain screening of room temperature is will be cooled to, finished product is made.
Embodiment 3
The present embodiment provide passive metal magnesium grain and its passivating method, magnesium metal grain weight percent composition be：
Mg：98.9%, S：0%, Cu：0.01%, P：0%, H2O：1%；In compound rare-earth, by weight percentage comprising following component：La：
30%, Y：15%, Sc：10%, Gd：20%, Sm：6%, Pr：19%.
The passivating method of magnesium metal grain is carried out according to the following steps：
(i) preparing metal magnesium grain passivator, passivator be two hydration sodium tartrates, sodium fluoride, phosphoric acid, potassium chromate, by metal
Magnesium grain is put into passivator, and passivation time is：30min, passivation temperature is：90 DEG C, the magnesium metal grain that will be passivated is dried,
Drying time is：150 DEG C, drying time is：32min, then naturally cools to room temperature；
(ii) the magnesium metal grain surface that will be cooled to room temperature coats one layer of coating, and coating layer thickness is：0.08mm, coating by：Stone
Ink powder, magnesia, organo-silicon compound composition；Organic silicon compound is made up of silicone oil and silicones, the weight of silicone oil and silicones
Than for：1:2；
Specific processing method：Organo-silicon compound are first coated in magnesium metal grain surface, are then dried, drying time is：
28min, drying temperature is：140 DEG C, naturally cool to room temperature；Magnesia is coated in magnesium metal grain surface again, is then dried,
Drying time is：26min, drying temperature is：145 DEG C, naturally cool to room temperature；Compound rare-earth is coated in magnesium metal grain table again
Face, drying time is：28min, drying temperature is：140 DEG C, naturally cool to room temperature；Graphite powder is finally coated in magnesium metal
Grain surface, then dries, and drying time is：28min, drying temperature is：142 DEG C, naturally cool to room temperature；
(iii) the magnesium metal grain screening of room temperature is will be cooled to, finished product is made.
So, make magnesium metal grain passivation layer parcel uniform, closely knit, the control of active content of magnesium, duration of fire resistance and product granularity
Accurately, general machinery mill is rubbed with the hands, extruding is difficult to be allowed to come off, and transports, stores and use safety, and hydration resistance is superior, no
The easy moisture absorption, long shelf-life is adapted to various weather conditions producers and uses.Good mobility, makes it in desulfurization dusting operation, under
Material is smooth, and without blocking, expulsion events, desulfurized effect is good, unit consumption is low, it is adaptable to which molten iron pre-processes composite blowing and single spraying magnesium powder work
Skill.
Above example is only explanation technological thought of the invention, it is impossible to limit protection scope of the present invention with this, every
According to technological thought proposed by the present invention, any change done on the basis of technical scheme each falls within the scope of the present invention
Within.
Claims (4)
1. a kind of passive metal magnesium grain, it is characterised in that：The passive metal magnesium grain by positioned at innermost layer magnesium metal grain, be rolled in gold
Category magnesium grain outer surface passivator, and the coating composition for being rolled in passivator outer surface；
The weight percent composition of magnesium metal grain is：92%≤Mg≤99%, S≤0.002%, Cu≤0.01%, P≤
0.001%, 0.1%≤H2O≤1.2%, each composition sum of the above is 100%；
The passivator is made up of two hydration sodium tartrates, sodium fluoride, phosphoric acid and potassium chromate, and two hydration sodium tartrates, fluorination
The weight ratio of sodium, phosphoric acid and potassium chromate is 4-6:2-5:1-3:1-4；
The coating is made up of graphite powder, magnesia, compound rare-earth and organo-silicon compound, the graphite powder, magnesia, compound
Rare earth and organo-silicon compound weight ratio are 1-4:4-6:2-4:2-3；The organic silicon compound is made up of silicone oil and silicones, institute
The weight ratio for stating silicone oil and silicones is 1:2；The compound rare-earth includes following component by weight percentage：La：25-35%,
Y：12-15%, Sc：8-12%, Gd：8-20%, Sm：5-7%, Pr：13-20%, each rare earth composition sum of the above is 100%.
2. passive metal magnesium according to claim 1 grain, it is characterised in that：The weight percent composition of the magnesium metal grain
For：Mg：98.8%, S:0%, Cu:0%, P:0%, H2O：1.2%；
The weight ratio of the two hydrations sodium tartrate, sodium fluoride, phosphoric acid and potassium chromate is 4:2:1:3；
The graphite powder, magnesia, compound rare-earth and organo-silicon compound weight ratio are 2:5:2:3；
In the compound rare-earth, by weight percentage comprising following component：La：35%, Y：15%, Sc：10%, Gd：18%,
Sm：7%, Pr：15%.
3. passive metal magnesium according to claim 1 grain, it is characterised in that：The weight percent composition of the magnesium metal grain
For：Mg：98.9%, S：0%, Cu：0.01%, P：0%, H2O：1%；
The weight ratio of the two hydrations sodium tartrate, sodium fluoride, phosphoric acid and potassium chromate is 6:2:1:1；
The graphite powder, magnesia, compound rare-earth and organo-silicon compound weight ratio are 3:4:3:3；
In the compound rare-earth, by weight percentage comprising following component：La：30%, Y：15%, Sc：10%, Gd：20%,
Sm：6%, Pr：19%.
4. the passivating method of passive metal magnesium as described in any claim in claim 1-3, it is characterised in that：The party
Method is carried out according to the following steps：
(i) preparing metal magnesium grain passivator, magnesium metal grain is put into passivator, and passivation time is：25-35min, passivation temperature
For：85-95 DEG C, the magnesium metal that will be passivated grain is dried, and drying time is：145-160 DEG C, drying time is：20-
40min, then naturally cools to room temperature；
(ii) the magnesium metal grain surface that will be cooled to room temperature coats one layer of coating, and the coating layer thickness is：0.05-0.1mm；
Specific processing method：Organo-silicon compound are first coated in magnesium metal grain surface, are then dried, drying time is：25-
30min, drying temperature is：130-155 DEG C, naturally cool to room temperature；Magnesia is coated in magnesium metal grain surface, Ran Hougan again
Dry, drying time is：25-30min, drying temperature is：130-160 DEG C, naturally cool to room temperature；Compound rare-earth is coated in again
Magnesium metal grain surface, drying time is：25-30min, drying temperature is：130-155 DEG C, naturally cool to room temperature；Finally by stone
Ink powder is coated in magnesium metal grain surface, then dries, and drying time is：25-30min, drying temperature is：It is 135-150 DEG C, natural
It is cooled to room temperature；
(iii) the magnesium metal grain screening of room temperature is will be cooled to, finished product is made.
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| CN104531935B (en) * | 2014-12-29 | 2017-12-05 | 芜湖金龙模具锻造有限责任公司 | A kind of preparation method of high efficiency composition iron melt desulfurizing agent |
| CN104480252B (en) * | 2014-12-29 | 2017-11-03 | 芜湖金龙模具锻造有限责任公司 | A kind of high efficiency composition iron melt desulfurizing agent |
| CN107088655B (en) * | 2016-07-01 | 2019-04-02 | 浏阳市科力烟花材料有限公司 | A kind of deactivating magnesium powder, passivation Al-Mg alloy powder and its wet process technique |
| CN113355486A (en) * | 2021-05-27 | 2021-09-07 | 湛江申翰科技实业有限公司 | Composite desulfurizer and preparation method thereof |
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| CN1598055A (en) * | 2004-08-02 | 2005-03-23 | 吉林大学 | Magnesium alloy phosphorization solution and its phosphorized technology |
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| CN103254762A (en) * | 2013-01-30 | 2013-08-21 | 中国科学院宁波材料技术与工程研究所 | Preparation method of organosilicon sol-gel coating for magnesium alloy substrate surface corrosion resistance |
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| CN101098983A (en) * | 2004-11-10 | 2008-01-02 | 凯密特尔有限责任公司 | Method for coating metallic surfaces with an aqueous composition |
| CN101287784A (en) * | 2005-08-26 | 2008-10-15 | Ppg工业俄亥俄公司 | Coating compositions exhibiting corrosion resistance properties, related coated substrates, and methods |
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