CN103666005A - Nickel-coated bentonite or diatomite composite powder and preparation method thereof - Google Patents
Nickel-coated bentonite or diatomite composite powder and preparation method thereof Download PDFInfo
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- CN103666005A CN103666005A CN201310714023.4A CN201310714023A CN103666005A CN 103666005 A CN103666005 A CN 103666005A CN 201310714023 A CN201310714023 A CN 201310714023A CN 103666005 A CN103666005 A CN 103666005A
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Abstract
The invention discloses nickel-coated bentonite or diatomite composite powder and a preparation method thereof, and belongs to the field of preparation of thermal spraying materials. The preparation process comprises the following steps: firstly, carrying out dewatering and activating treatment on bentonite or diatomite; secondly, carrying out nickel coating by adopting a high-pressure hydrogen reduction method; the nickel-coated bentonite or diatomite composite powder prepared by the method has the advantages of uniform particles, adjustable nickel content and coating thickness, complete and continuous coating and high reaction speed. The nickel-coated bentonite or diatomite is mainly used as core powder of a thermal spraying powder material in the fields of aviation and aerospace, and can also be directly used as the thermal spraying powder material. The preparation method is simple, has good repeatability, is easy to realize industrialization, and the production scale can be adjusted randomly according to needs.
Description
Technical field
The present invention relates to thermal spraying material field, particularly relate to and be a kind ofly suitable as the intermediate raw material of thermal spraying material or directly as a kind of nickel bag wilkinite of hot spraying powder powder material or the compound powder of diatomite and preparation method thereof.
Background technology
In recent years, the development of sealing coating material has obtained certain progress, by its use temperature, divides, and can be divided into low temperature coating, and temperature is below 400 ℃, as aluminium silicon polybenzoate, yellow gold etc.; Middle temperature coating, use temperature is at 400～700 ℃, as nickel graphite, copper aluminium nickel graphite, nickel chromium triangle aluminium nickel graphite etc.; High temperature coating, use temperature is greater than 700 ℃, as nickel chromium triangle aluminium wilkinite, nickel chromium triangle aluminium diatomite etc.Yet China is not also haveing breakthrough aspect the development of high temperature sealing coating material.Because wilkinite (or diatomite) surfactivity is not high, reduced nickel is difficult to coated complete even, and the preparation of nickel bag wilkinite (or diatomite) is the important step of restriction high temperature sealing coating material development always.
The method of metallizing can be divided into physical method and chemical process at present.When adopting the physical methods such as vapour deposition, because being difficult to realize, powder suspends, be difficult for realizing evenly coated and industrial-scale production.Chemical process mainly comprises electroless plating, carbonyl decomposition method and electrochemical plating etc.Wherein, chemical nickel plating is to utilize suitable reductive agent that nickel ion is reduced and a kind of chemical treatment method of nickel layer selectively on the surface through catalysis, chemical nickel plating chemical nickel-plating liquid used consists of components such as nickel salt, complexing agent, stablizer and reductive agents, be equipped with again the processing condition such as suitable temperature, pH value, stirring, make powder in plating solution, be wrapped by layer of metal nickel.Carbonyl decomposition method is under certain condition, and when active nickel contacts with carbon monoxide, 1 nickle atom combines with 4 gas molecules, generates nickel tetracarbonyl compound.This reaction is reversible, and in the temperature range of 150～316 ℃, nickle carbonoxide can be decomposed into metallic nickel and carbon monoxide again, and wherein CO can recycle.Electrochemical plating are prepared nickel cladded type composite powder and are different from general plating, and its electrode is by granulometric composition.
In each method of above-mentioned chemical process, though electroless plating use is extensively, but wayward, be difficult to reach required thickness of coating, process is slower, easily produces the nickel that dissociates.Although carbonyl decomposition method raw material availability is high, covered effect is good, CO and Ni (CO)
4be highly toxic substance, and Ni (CO)
4high volatility, thereby require very strict airtight gas precautions, affected the application of the method.And electrochemical plating are only applicable to metal-powder, to non-metal powder, need to first with additive method, apply one deck nickel film on its surface can adopt.
Summary of the invention
The present invention can solve the existing problem of existing chemical process metallizing, effectively improve clad ratio, provide that a kind of technique is simple, production process is controlled, cost is low, the nickel bag wilkinite of easy popularization or the compound powder of diatomite and preparation method thereof, make powder nickel content adjustable, coated evenly complete, can meet nickel bag wilkinite or the diatomite powder of follow-up flouring technology and final powder property needs.
For solving the problems of the technologies described above, the invention provides a kind of nickel bag wilkinite or the compound powder of diatomite, this composite powder is coated on wilkinite by nickel or diatomite surface forms, and powder size is 45～150 microns, and in composite powder, the quality percentage composition of nickel is 50%～80%.
The present invention also provides the preparation method of a kind of nickel bag wilkinite or the compound powder of diatomite, is a kind of method of preparing nickel bag wilkinite of the present invention or the compound powder of diatomite, comprising:
Take wilkinite or diatomite as raw material, wilkinite or diatomite are dewatered and organic and inorganic compound surface activation treatment;
To described dewater and surface activation process after wilkinite or diatomite carry out High Pressure Hydrogen reduction reaction, described High Pressure Hydrogen reduction reaction adopts organically-modified nickeliferous reaction soln;
The reaction product of described High Pressure Hydrogen reduction reaction is carried out to pure water washing, oven dry, obtain the compound powder of nickel bag wilkinite or diatomite.
Beneficial effect of the present invention is: by first to the wilkinite as raw material or diatomite remove water treatment and surface activation process can make coated more easily, more complete, more even; And adopt High Pressure Hydrogen reduction method to carry out the coated of nickel, can effectively control the nickel content in composite powder, improve clad ratio, nickel bag wilkinite (or diatomite) composite powder prepared by the method can be adjusted industrial scale as required, its technique is simple, is applicable to suitability for industrialized production.
Embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Based on embodiments of the invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to protection scope of the present invention.
The embodiment of the present invention provides a kind of nickel bag wilkinite or the compound powder of diatomite, and this composite powder is coated on wilkinite by nickel or diatomite surface forms, and powder size is 45～150 microns, and in composite powder, the quality percentage composition of nickel is 50%～80%.
The embodiment of the present invention also provides a kind of method of preparing above-mentioned nickel bag wilkinite or the compound powder of diatomite, comprises the following steps:
Step 1, take wilkinite or diatomite as raw material, and wilkinite or diatomite are removed to water treatment and organic and inorganic compound surface activation treatment;
Step 2, to dewater and surface activation process after wilkinite or diatomite carry out High Pressure Hydrogen reduction reaction, High Pressure Hydrogen reduction reaction adopts organically-modified nickeliferous reaction soln;
Step 3, washs, dries the reaction product of High Pressure Hydrogen reduction reaction, obtains the compound powder of nickel bag wilkinite or diatomite.
In above-mentioned preparation method, dewatering that wilkinite or diatomite are carried out is treated to: adopt thermal treatment, heat treatment time is 1～8 hour, bentonitic thermal treatment temp is 100～600 ℃, diatomaceous thermal treatment temp is 800～1200 ℃, thermal treatment can be removed wilkinite or diatomaceous planar water and be made it lose water-retaining capacity, is convenient to follow-up activated bentonite or diatomaceous processing.
In above-mentioned preparation method, except after water treatment, wilkinite or diatomite are sieved, selecting granularity is that the wilkinite of 30～150 microns or diatomite are as the raw material of subsequent disposal.
In above-mentioned preparation method, the surface activation process that wilkinite or diatomite are carried out is: adopt organic and inorganic compound activator solution that described wilkinite or diatomite are soaked completely, the general time of soaking is completely 10～480 minutes, the temperature of soaking 70～200 ℃ of rear employings is dried, and completes surface activation process after oven dry.
In above-mentioned surface activation process, organic and inorganic compound activator solution concentration is 1.3～3.8%, and wherein organic activator is as solvent, comprises a kind of or wherein several in ethanol, polyoxyethylene glycol, polyacrylamide, acetone etc., inorganic activator, as solute, is mainly Palladous chloride.
In above-mentioned preparation method, High Pressure Hydrogen reduction reaction is: described wilkinite or diatomite are joined in described organically-modified nickeliferous reaction soln, in every liter of organically-modified nickeliferous reaction soln, add wilkinite or diatomite 20g～100g, in described nickeliferous reaction soln, add additive again, the described described organically-modified nickeliferous reaction soln that is added with described wilkinite or diatomite and additive is reacted in autoclave, temperature of reaction in autoclave is that 205～280 ℃, hydrogen pressure are 3.0MPa～10.0MPa, and the reaction times is 2～10 hours.
In above-mentioned High Pressure Hydrogen reduction reaction, organically-modified nickeliferous reaction soln is the mixing solutions of polyoxyethylene glycol, single nickel salt, ammonium sulfate, ammoniacal liquor and pure water, contains polyoxyethylene glycol 10～30g, single nickel salt 220～380g, ammonium sulfate 80～220g, ammoniacal liquor 100～200g, all the other are pure water in the mixing solutions that the proportioning of described mixing solutions is every liter.
In above-mentioned High Pressure Hydrogen reduction reaction, additive adopts any one or several mixture in polyoxyethylene glycol, polyacrylamide, anthraquinone, hydrazine hydrate, and the add-on of described additive is: every 100g wilkinite or diatomite add additive 35～100g.Mixture when additive employing polyoxyethylene glycol, polyacrylamide, anthraquinone and hydrazine hydrate, has the polyoxyethylene glycol of 10～50g, the polyacrylamide of 5～20g, 5～20g anthraquinone and 5～10g hydrazine hydrate in the described additive that every 100g wilkinite or diatomite add.
In above-mentioned preparation method, reaction product is carried out pure water washing, is dried be: adopt pure water to wash described reaction product, after washing, adopt the temperature of 70～200 ℃ to dry.
Above-mentioned preparation method, by removing water treatment and surface-active-treatment as pre-treatment, coordinate with High Pressure Hydrogen reduction reaction, realization with compared with short processes flow process, that nickel content has been prepared in better simply operation is adjustable, coated evenly complete, can meet nickel bag wilkinite (or diatomite) composite powder material of follow-up flouring technology and final powder property needs, the method industrial scale is controlled, be suitable for suitability for industrialized production, the powdered material of preparation can be used as the intermediate raw material of used for hot spraying nickel chromium triangle aluminium wilkinite (or diatomite).
Below in conjunction with specific embodiment, the invention will be further described
The present embodiment provides the preparation method of a kind of nickel bag wilkinite (or diatomite) composite powder, and concrete steps are as follows:
(1) wilkinite (or diatomite) except water pretreatment: adopt heat-treating methods to remove water pretreatment wilkinite (or diatomite) raw material, heat treatment time is 1～8 hour, bentonitic thermal treatment temp is 100～600 ℃, and diatomaceous thermal treatment temp is 800～1200 ℃; After naturally cooling, carry out material screening, selection granularity is wilkinite (or diatomite) raw material for standby of 30～150 microns;
(2) activation treatment of wilkinite (or diatomite): to carrying out surface activation process through above wilkinite (or diatomite) raw material except water treatment, adopt the organic and inorganic activator solution that concentration is 1.3～3.8% that wilkinite (or diatomite) surface is soaked completely, the general time of soaking is completely 10～480 minutes, carry out afterwards drying and processing, bake out temperature is 70～200 ℃;
(3) the High Pressure Hydrogen reduced nickel coating reaction of wilkinite (or diatomite): specifically wilkinite (or diatomite) is added in organically-modified nickeliferous reaction soln, add additive (playing surface-active effect), in carrying out enclosed high pressure axe, constant temperature, hydrogenation, pressurization are reacted again; Wherein, organically-modified nickeliferous reaction soln proportioning is polyoxyethylene glycol 10～30g/L, single nickel salt 220～380g/L, ammonium sulfate 80～220g/L, ammoniacal liquor 100～200g/L, all the other are pure water, according to adding the ratio of 20g～100g by through pouring in above-mentioned organically-modified nickeliferous reaction soln except the wilkinite (or diatomite) of water treatment and organic and inorganic compound surface activation treatment in every liter of organically-modified nickeliferous reaction soln, additive is added in above-mentioned organically-modified nickeliferous reaction soln simultaneously; Additive is selected from a kind of or wherein several of polyoxyethylene glycol, polyacrylamide, anthraquinone, hydrazine hydrate, no matter additive is to comprise one or more components, its consumption is to add 35～100g in every 100g wilkinite (or diatomite), when additive is mixed by polyoxyethylene glycol, polyacrylamide, anthraquinone and hydrazine hydrate, add-on is that every 100g wilkinite (or diatomite) adds the polyoxyethylene glycol of 10～50g, the anthraquinone of the polyacrylamide of 5～20g, 5～20g and the hydrazine hydrate of 5～10g; Above solution and admixture are fully stirred, and being placed in liner is the enclosed high pressure axe of corrosion resistant material, 205～280 ℃ of reactions of constant temperature 2～10 hours, and air pressure is 3～10MPa;
(4) throw out (being reaction product) that reaction generates, after pure water washs, filters, adopts the temperature of 70～200 ℃ to dry, obtains nickel bag wilkinite (or diatomite) composite powder.
Key problem in technology and the craft feature of product of the present invention are:
Adopt wilkinite except water treatment and surface activation process can make coated more easily, more complete, more even.Adopt High Pressure Hydrogen reduction method to be coated, can effectively control the nickel content in composite powder.Adopt above method to prepare nickel bag wilkinite (or diatomite) composite powder and can adjust as required industrial scale.
Wilkinite take below as raw material describes above-mentioned nickel bag preparation method for bentonite, be specially:
Get wilkinite and heat-treat at 200 ℃, soaking time 1 hour, sieves after naturally cooling, obtains the wilkinite 400g of granularity between 45～150 microns; Get concentration and be after 1.5% organic and inorganic activator solution 200ml soaks above wilkinite completely and dry, bake out temperature is 120 ℃; Polyoxyethylene glycol 10g, single nickel salt 300g, ammonium sulfate 100g, ammoniacal liquor 150ml are mixed, add 6L pure water, stir, wilkinite after drying is added wherein, add while stirring polyacrylamide 160g, above mixing solutions is stirred and is placed in 10L autoclave, and temperature passes into hydrogen while rising to 210 ℃, and makes hydrogen pressure remain at 6MPa; After reaction finishes, throw out washed, be dried, obtain nickel bag wilkinite 682g altogether, nickel content is 61.7%.
Nickel bag wilkinite of the present invention (or diatomite) cladded type composite powder material, it is a kind of intermediate raw material (also can be used as thermal spraying material) of preparing thermal spraying material, can be used for preparing Aeronautics and Astronautics engine clearance control high-temperature abradable seal coating, this material has good in oxidation resistance, hardness is low and bonding strength is high feature.
The above; be only the present invention's embodiment preferably, but protection scope of the present invention is not limited to this, is anyly familiar with in technical scope that those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (10)
1. the compound powder of nickel bag wilkinite or diatomite, is characterized in that, this composite powder is coated on wilkinite by nickel or diatomite surface forms, and powder size is 45～150 microns, and in composite powder, the quality percentage composition of nickel is 50%～80%.
2. a preparation method for nickel bag wilkinite or the compound powder of diatomite, is characterized in that, for the preparation of nickel bag wilkinite claimed in claim 1 or the compound powder of diatomite, comprising:
Take wilkinite or diatomite as raw material, described wilkinite or diatomite are removed to water treatment and organic and inorganic compound surface activation treatment;
Described wilkinite or the diatomite removing after water treatment and surface activation process is carried out to High Pressure Hydrogen reduction reaction, and described High Pressure Hydrogen reduction reaction adopts organically-modified nickeliferous reaction soln;
The reaction product of described High Pressure Hydrogen reduction reaction is carried out to pure water washing, oven dry, obtain the compound powder of nickel bag wilkinite or diatomite.
3. the preparation method of nickel bag wilkinite according to claim 2 or the compound powder of diatomite, is characterized in that,
Described dewatering that wilkinite or diatomite are carried out is treated to: adopt thermal treatment, heat treatment time is 1～8 hour, and bentonitic thermal treatment temp is 100～600 ℃, and diatomaceous thermal treatment temp is 800～1200 ℃;
Described reaction product is carried out pure water washing, is dried be: adopt pure water to wash described reaction product, after washing, adopt the temperature of 70～200 ℃ to dry.
4. according to the preparation method of the nickel bag wilkinite described in claim 2 or 3 or the compound powder of diatomite, it is characterized in that, except after water treatment, described wilkinite or diatomite are sieved, selecting granularity is that the wilkinite of 30～150 microns or diatomite are as the raw material of subsequent disposal.
5. the preparation method of nickel bag wilkinite according to claim 2 or the compound powder of diatomite, it is characterized in that, the described organic and inorganic compound surface activation treatment that wilkinite or diatomite are carried out is: adopt organic and inorganic compound activator solution that described wilkinite or diatomite are soaked completely, the time of soaking is 10～480 minutes, the temperature of soaking 70～200 ℃ of rear employings is dried, and completes organic and inorganic compound surface activation treatment after oven dry.
6. according to the preparation method of the nickel bag wilkinite described in claim 2 or 5 or the compound powder of diatomite, it is characterized in that, the mass concentration of described organic and inorganic compound activator solution is 1.3～3.8%, wherein organic activator is as solvent, be selected from one or more in ethanol, polyoxyethylene glycol, polyacrylamide, acetone, inorganic activator, as solute, adopts Palladous chloride.
7. the preparation method of nickel bag wilkinite according to claim 2 or the compound powder of diatomite, it is characterized in that, described High Pressure Hydrogen reduction reaction is: described wilkinite or diatomite are joined in described organically-modified nickeliferous reaction soln, in every liter of organically-modified nickeliferous reaction soln, add wilkinite or diatomite 20g～100g, in described nickeliferous reaction soln, add additive again, the described described organically-modified nickeliferous reaction soln that is added with described wilkinite or diatomite and additive is reacted in autoclave, temperature of reaction in described autoclave is 205～280 ℃, hydrogen pressure is 3.0MPa～10.0MPa, reaction times is 2～10 hours.
8. according to the preparation method of the nickel bag wilkinite described in claim 2 or 7 or the compound powder of diatomite, it is characterized in that, the mixing solutions that described organically-modified nickeliferous reaction soln is polyoxyethylene glycol, single nickel salt, ammonium sulfate, ammoniacal liquor and pure water, contains polyoxyethylene glycol 10～30g, single nickel salt 220～380g, ammonium sulfate 80～220g, ammoniacal liquor 100～200g, all the other are pure water in the mixing solutions that the proportioning of described mixing solutions is every liter.
9. the preparation method of nickel bag wilkinite according to claim 8 or the compound powder of diatomite, it is characterized in that, described additive adopts any one or several mixture in polyoxyethylene glycol, polyacrylamide, anthraquinone, hydrazine hydrate, and the add-on of described additive is: every 100g wilkinite or diatomite add additive 35～100g.
10. the preparation method of nickel bag wilkinite according to claim 9 or the compound powder of diatomite, it is characterized in that, described additive adopts the mixture of polyoxyethylene glycol, polyacrylamide, anthraquinone and hydrazine hydrate, has the polyoxyethylene glycol of 10～50g, the polyacrylamide of 5～20g, 5～20g anthraquinone and 5～10g hydrazine hydrate in the described additive that every 100g wilkinite or diatomite add.
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Cited By (1)
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| CN104289721A (en) * | 2014-10-26 | 2015-01-21 | 李万青 | Preparation method of superfine Ni-Co alloy powder of polyurethane coatings and adhesive |
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