CN105834450A - Preparing method for silver powder - Google Patents
Preparing method for silver powder Download PDFInfo
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- CN105834450A CN105834450A CN201610315653.8A CN201610315653A CN105834450A CN 105834450 A CN105834450 A CN 105834450A CN 201610315653 A CN201610315653 A CN 201610315653A CN 105834450 A CN105834450 A CN 105834450A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a preparing method for silver powder. The preparing method for the silver powder comprises the steps that a water reaction system A containing silver ions, a reducing agent solution B containing silver ions and a dispersing agent solution C containing silver ions are prepared; the water reaction system A, the reducing agent solution B and the dispersing agent solution C are injected into a continuous pipeline type reactor to be mixed for the reaction, and accordingly silver particles are deposited; and the silver particles are dried, ground and screened, and the silver powder is obtained.
Description
Technical field
The present invention relates to the preparation method of a kind of argentum powder, more particularly it relates to an the preparation method of the argentum powder for electronic unit.
Background technology
Argent has conduction, heat conduction and the non-oxidizability of excellence, suffers from being widely applied electrician and electron trade.The silver adaptable electronic unit of material, including the interior electrode of multi-layer capacitor, the printed circuit of circuit board, electrode of solar battery, the conventional electrocondution slurry of electrode of Plasmia indicating panel (PDP) base material, generally by mixing argentum powder, glass dust and inorganic assistant etc. in organic carrier, agitated grinding rolling forms, wherein mass fraction shared by argentum powder is the highest, and the quality of argentum powder greatly affects the performance of final slurry.Along with the reduction of these component size, need, for the argentum powder of electrocondution slurry, there is the least particle diameter and the narrowest particle size range, to form the printed circuit with high density and fine line.Especially current research and the solar cell size extensive, consumption is huge, because sintering time is short, needing enough sintering activities, suitable dissolving diffusion, research shows, can obtain more preferable electricity, mechanical property by collocation distribution of particles argentum powder narrow, size uniform.
The existing method preparing ultra tiny argentum powder has multiple, and liquid phase method, solid phase method and vapor phase method have for studying, but the most frequently used, most economical large scale production method remains liquid-phase precipitation method.But great majority prepare silver powder particles for batch process in liquid-phase precipitation method.The patent of such as patent No. CN200480020987.8 provides the manufacture method of a kind of microgranule argentum powder, silver nitrate aqueous solution and ammonia hybrid reaction is made to obtain silver ammonia complex aqueous solution, by adding reducing agent in this silver ammonia complex aqueous solution, reduction separates out silver particles, carry out filtering, wash, be dried to obtain microgranule argentum powder, it is characterized in that, above-mentioned silver ammonia complex aqueous solution is made to contact mixing with organic reducing agent, and, in solution upon mixing, silver concentration maintains 1g/l～6g/l, organic reducing agent concentration maintains 1g/l～3g/l to reduce precipitation silver particles.
The patent of such as patent No. CN200480020988.2 provides the manufacture method of a kind of microgranule argentum powder, silver nitrate aqueous solution and ammonia hybrid reaction is made to obtain silver ammonia complex aqueous solution, silver particles is separated out by adding reducing agent reduction in this silver ammonia complex aqueous solution, filter, washing, it is dried to obtain microgranule argentum powder, it is characterized in that, above-mentioned silver ammonia complex aqueous solution is made to contact mixing with organic reducing agent, and silver concentration maintains 1g/l～6g/l in solution upon mixing, organic reducing agent concentration maintains 1g/l～3g/l to reduce precipitation silver particles, this silver particles is filtered, washing, wash with excessive amount of ethanol solution.
In a word, in prior art, general employing batch process prepares argentum powder, and products obtained therefrom can meet the needs of general conductive silver paste, but there is also a lot of problem, and such as single batch of limits throughput, when high-volume expanding production, quality is unstable, and production process is various waits deficiency.This is because batch process produces in the whole production process of argentum powder, the diffusion of the concentration of material, stirring, ion, the formation of nucleus and growth are all continually changing.Therefore, when prepared by laboratory, owing to mixing effect is the best, stirring is easily uniform, and measures few, and the response time is short, is typically easy to prepare the argentum powder sample of excellent performance, but comparatively speaking, the uniformity of industrialization product, dispersibility are with regard to deviation.
Hence it is highly desirable to by formula and the improvement of production technology, by continuity method, more efficiently prepare the argentum powder that dispersibility is high, uniformity is good.
Summary of the invention
In order to solve the problems referred to above, one aspect of the present invention provides the preparation method of a kind of argentum powder, including:
It is respectively configured water reaction system A of silver ion, reductant solution B, dispersant solution C；
A, B and C being injected in continuous conduit formula reactor, hybrid reaction, to deposit Argent grain；With dry described Argent grain, crush and screen and obtain.
In a kind of embodiment of the inventive method, water reaction system A of described silver ion comprises silver-containing material and pure water.
In a kind of embodiment of the inventive method, at least one in lower group of described silver-containing material: silver chloride, silver nitrate, silver acetate, Disilver carbonate and silver sulfate.
In a kind of embodiment of the inventive method, described reductant solution B comprises reducing agent and pure water.
In a kind of embodiment of the inventive method, at least one in lower group of described reducing agent: formaldehyde, formic acid, vitamin C, hydrazine hydrate, oxammonium sulfate., glucose, sodium borohydride, alkanolamine and hydroquinone.
In a kind of embodiment of the inventive method, described dispersant solution C comprises:
Dispersant；
With at least one in pure water or ethanol.
In a kind of embodiment of the inventive method, at least one in lower group of described dispersant: fatty acid, soap, surfactant, organic metal, chelating agen, hydroxy polymer, ethyoxyl polymer and protecting colloid.
In a kind of embodiment of the inventive method, the described injection mode by A, B and C injection continuous conduit formula reactor one in lower group:
C with A is mixed, then A/C mixed liquor and B are injected separately into continuous conduit formula reactor；
C with B is mixed, then B/C mixed liquor and A are injected separately into continuous conduit formula reactor；
A, B, C are injected separately into continuous conduit formula reactor；
A Yu B is injected separately into continuous conduit formula reactor, and after the contact point of A Yu B, injects C.
In a kind of embodiment of the inventive method, the internal diameter of described continuous conduit formula reactor is 10mm-200mm, a length of 10cm-10m.
In a kind of embodiment of the inventive method, the inside of described continuous conduit formula reactor equipped with in mechanical stirring device and ultrasound wave vibrating bar one or both.
The present invention can obtain the argentum powder of the good variable grain size of uniformity by adjusting the PH of reactant liquor, by adjusting addition and the injection mode of dispersant, the built-in stirring of binding reactor and ultrasound wave dispersal device, can well adjust the dispersibility of powder body, the uniformity of particle diameter distribution.Granule described herein uniformly can from sem observation to, particle size can be adjusted to several microns from tens nanometers.Argentum powder is particularly suited for solar energy face electrode slurry, PDP slurry slug type etc..
It is more readily understood the above-mentioned of the application and other features, aspect and advantage with reference to described further below.
Detailed description of the invention
Participate in the election of the detailed description being preferable to carry out method of the invention below and the embodiment that includes can be more easily understood present disclosure.Unless otherwise defined, all technology used herein and scientific terminology have the identical implication being generally understood that with one skilled in the art of the present invention.When there is contradiction, it is as the criterion with the definition in this specification.
Term as used herein " by ... preparation " and " comprising " synonym.Term used herein " comprises ", " including ", " having ", " containing " or its other deformation any, it is intended that cover the including of non-exclusionism.Such as, comprise the compositions of listed elements, step, method, goods or device and be not necessarily solely those key elements, but other not expressly listed key element or the intrinsic key element of this kind of compositions, step, method, goods or device can be included.
Conjunction " Consists of " gets rid of any key element, step or component do not pointed out.If in claim, this phrase will make claim be closed so that it is does not comprise the material in addition to the material that those describe, but except relative customary impurities.When being rather than immediately following during phrase " Consists of " occurs in the clause of claim main body after theme, it is only limited to the key element described in this clause；Other key element is not excluded outside as overall described claim.
During the Range Representation that equivalent, concentration or other value or parameter limit with scope, preferred scope or a series of upper limit preferred value and lower preferable values, this is appreciated that and specifically discloses all scopes formed by arbitrary pairing of any range limit or preferred value and any range lower limit or preferred value, regardless of whether whether this scope separately discloses.Such as, when disclosing scope " 1 to 5 ", described scope should be interpreted as including scope " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to 5 ", " 1 to 3 and 5 " etc..When numerical range is described in this article, unless otherwise indicated, otherwise this scope is intended to include its end value and all integers within the range and mark.
Singulative includes that plural number discusses object, unless the context clearly dictates otherwise." optional " or " any one " refer to that the item described thereafter or event may or may not occur, and this description includes situation that event occurs and the situation that event does not occurs.
Approximation term in specification and claims is used for modifying quantity, represents that the present invention is not limited to this particular number, also includes close to this quantity acceptable without causing the part of the correction of the change of relevant basic function.Accordingly, modify a numerical value with " about ", " about " etc., mean and the invention is not restricted to this exact numerical.In some example, approximation term likely corresponds to measure the precision of the instrument of numerical value.In present specification and claims, scope limits and can combine and/or exchange, and these scopes include all subranges contained therebetween if not stated otherwise.
Additionally, the indefinite article " a kind of " before key element of the present invention or component and " one " quantitative requirement (i.e. occurrence number) unrestriction to key element or component.Therefore " one " or " a kind of " should be read as including one or at least one, and the key element of singulative or component also include plural form, unless the obvious purport of described quantity refers to singulative.
One aspect of the present invention provides the preparation method of a kind of argentum powder, including:
It is respectively configured water reaction system A of silver ion, reductant solution B, dispersant solution C；
A, B and C being injected in continuous conduit formula reactor, hybrid reaction, to deposit Argent grain；With dry described Argent grain, crush and screen and obtain.
The water reaction system of silver ion
A
Water reaction system as silver ion, it is possible to use containing silver nitrate, silver salt complex or silver intermediate
Aqueous solution or slurry.Silver salt complex can be formed by adding ammonia, ammonium salt, chelate compound etc..Silver intermediate can be prepared by adding sodium hydroxide, sodium chloride, sodium carbonate etc..In the water reaction system of the present invention, the concentration of silver ion is preferably 10-250g/L, more preferably 100-200 g/L, and most preferably 150
g/L。
In one embodiment, for the water reaction system of the silver ion of the present invention, silver-containing material and pure water are comprised.
At least one in the silver-containing material of the application is selected from lower group: silver chloride, silver nitrate, silver acetate, Disilver carbonate and silver sulfate；Preferably, described silver-containing material is silver nitrate.
In one embodiment, for the water reaction system of the silver ion of the present invention, comprise ammonia and PH regulator further.
In one embodiment, described PH regulator is sodium hydroxide.
The addition of PH regulator can effectively regulate the pH value of the water reaction system of silver ion so that it is is maintained between 7.5～13.5, it is preferable that the pH value of described water reaction system is 8～12, it is highly preferred that the pH value of described water reaction system is 12.
Reductant solution
B
In a kind of embodiment of the inventive method, described reductant solution B comprises reducing agent and pure water.
In a kind of embodiment of the inventive method, at least one in lower group of described reducing agent: formaldehyde, formic acid, vitamin C, hydrazine hydrate, oxammonium sulfate., glucose, sodium borohydride, alkanolamine and hydroquinone；Preferably, described reducing agent is vitamin C.
In a kind of embodiment of the inventive method, described reductant solution B comprises PH regulator further.
In one embodiment, described PH regulator is sodium hydroxide.
The addition of PH regulator can effectively regulate the pH value of reductant solution B, it is preferable that the pH value of described reductant solution B is 8.
Dispersant solution
C
In a kind of embodiment of the inventive method, described dispersant solution C comprises:
Dispersant；
At least one in pure water or ethanol.
In a kind of embodiment of the inventive method, at least one in lower group of described dispersant: fatty acid, soap, surfactant, organic metal, chelating agen, hydroxy polymer, ethyoxyl polymer and protecting colloid；Such as, typical dispersant can use oleic acid or PVA.
Injection mode
In the present invention, the mode that A, B and C inject continuous conduit formula reactor is not particularly limited, can be injected separately into, it is also possible to arbitrarily mix injection, preferably, the one during the described injection mode that A, B and C inject continuous conduit formula reactor is selected from lower group:
C with A is mixed, then A/C mixed liquor and B are injected separately into continuous conduit formula reactor；
C with B is mixed, then B/C mixed liquor and A are injected separately into continuous conduit formula reactor；
A, B, C are injected separately into continuous conduit formula reactor；
A Yu B is injected separately into continuous conduit formula reactor, and after the contact point of A Yu B, injects C；
It is highly preferred that the described injection mode of continuous conduit formula reactor of A, B and C being injected for being injected separately into continuous conduit formula reactor by A Yu B, and after the contact point of A Yu B, inject C.
Preferably, when selecting to be injected separately into A Yu B continuous conduit formula reactor, and after the contact point of A Yu B, when injecting C, A, B all inject continuous conduit formula reactor with the flow of 5L/Min, and after the contact point of A Yu B at 2 meters, injecting C with the flow of 1L/Min, implant angle is for flow to angle ＞ 90 ° with solution A, B mixed liquor.
Continuous conduit formula reactor
Continuous conduit formula reactor be a kind of in a tubular form, continuous manipulation reactor that draw ratio is the biggest.This reactor can be the longest, if the reactor pipe range of propylene dimerization is in terms of kilometer.It has the advantage that back-mixing is little, volumetric efficiency is high.
Continuous conduit formula reactor for the present invention is not particularly limited, it is preferred that the internal diameter of described continuous conduit formula reactor is 10mm-200mm, and a length of 10cm-10m；It is highly preferred that the internal diameter of described continuous conduit formula reactor is 50mm-180mm, a length of 3m-8m；Most preferably, the internal diameter of described continuous conduit formula reactor is 100mm, a length of 6m.
In order to improve the efficiency of continuous conduit formula reactor further, in one embodiment, the inside of described continuous conduit formula reactor equipped with in mechanical stirring device and ultrasound wave vibrating bar one or both；Preferably, the inside of described continuous conduit formula reactor is simultaneously equipped with mechanical stirring device and ultrasound wave vibrating bar, and the multi-layer oar blade formula stirring paddle that described built-in machines agitating device is driven by motor, mixing speed is at 1-10000RPM, and the ultrasonic power of described ultrasound wave vibrating bar is 0.1-5KW.
The present invention includes implementation below:
The preparation method of 1. 1 kinds of argentum powder of embodiment, including:
It is respectively configured water reaction system A of silver ion, reductant solution B, dispersant solution C；
A, B and C being injected in continuous conduit formula reactor, hybrid reaction, to deposit Argent grain；With
It is dried described Argent grain, crushes and screens and obtain.
The method of embodiment 2. embodiment 1, water reaction system A of wherein said silver ion comprises silver-containing material and pure water.
The method of embodiment 3. embodiment 2, at least one in lower group of wherein said silver-containing material:
Silver chloride, silver nitrate, silver acetate, Disilver carbonate and silver sulfate.
Method any one of embodiment 4. embodiment 2-3, water reaction system A of wherein said silver ion, comprise ammonia and PH regulator further.
Method any one of embodiment 5. embodiment 1-4, in wherein said water reaction system A, the concentration of silver ion is 10-250g/L.
Method any one of embodiment 6. embodiment 1-5, in wherein said water reaction system A, the concentration of silver ion is 150g/L.
Method any one of embodiment 7. embodiment 1-6, the pH value of wherein said water reaction system A is 7.5～13.5.
Method any one of embodiment 8. embodiment 1-7, the pH value of wherein said water reaction system A is 12.
Method any one of embodiment 9. embodiment 1-8, wherein said reductant solution B comprises reducing agent and pure water.
Method described in embodiment 10. embodiment 9, at least one in lower group of wherein said reducing agent: formaldehyde, formic acid, vitamin C, hydrazine hydrate, oxammonium sulfate., glucose, sodium borohydride, alkanolamine and hydroquinone.
The method of embodiment 11. embodiment any one of 9-10, wherein said reductant solution B comprises PH regulator further.
Method any one of embodiment 12. embodiment 1-11, wherein said dispersant solution C comprises:
Dispersant；With
At least one in pure water or ethanol.
The method of embodiment 13. embodiment 12, at least one in lower group of wherein said dispersant: fatty acid, soap, surfactant, organic metal, chelating agen, hydroxy polymer, ethyoxyl polymer and protecting colloid.
Method any one of embodiment 14. embodiment 1-13, the wherein said injection mode that A, B and C inject continuous conduit formula reactor is to be mixed by C with A, and then A/C mixed liquor and B are injected separately into continuous conduit formula reactor.
Method any one of embodiment 15. embodiment 1-13, the wherein said injection mode that A, B and C inject continuous conduit formula reactor is to be mixed by C with B, and then B/C mixed liquor and A are injected separately into continuous conduit formula reactor.
Method any one of embodiment 16. embodiment 1-13, the wherein said injection mode of continuous conduit formula reactor of A, B and C being injected for being injected separately into continuous conduit formula reactor by A, B, C.
Method any one of embodiment 17. embodiment 1-13, the wherein said injection mode of continuous conduit formula reactor of A, B and C being injected for being injected separately into continuous conduit formula reactor by A Yu B, and after the contact point of A Yu B, injects C.
The method of embodiment 18. embodiment 17, wherein A, B all inject continuous conduit formula reactor with the flow of 5L/Min, and after the contact point of A Yu B at 2 meters, injecting C with the flow of 1L/Min, implant angle is for flow to angle ＞ 90 ° with solution A, B mixed liquor.
Method any one of embodiment 19. embodiment 1-18, the internal diameter of wherein said continuous conduit formula reactor is 10mm-200mm, a length of 10cm-10m.
Method any one of embodiment 20. embodiment 1-19, the internal diameter of wherein said continuous conduit formula reactor is 100mm, a length of 6m.
Method any one of embodiment 21. embodiment 1-20, the inside of wherein said continuous conduit formula reactor equipped with in mechanical stirring device and ultrasound wave vibrating bar one or both.
Method any one of embodiment 22. embodiment 1-21, the inside of wherein said continuous conduit formula reactor is simultaneously equipped with mechanical stirring device and ultrasound wave vibrating bar, and the multi-layer oar blade formula stirring paddle that described built-in machines agitating device is driven by motor, mixing speed is at 1-10000RPM, and the ultrasonic power of described ultrasound wave vibrating bar is 0.1-5KW.
Embodiments of the present invention define in the following example further.
Embodiment 1
Adding 10.2L ammonia (wt%=28%) in 200L container, add pure water and 1.7Kg silver nitrate, stirring and dissolving, adding sodium hydrate regulator solution pH value is 12, is configured to the solution A of concentration of silver ions 10g/L, and temperature keeps 40 DEG C；Interpolation 10g oleic acid, to 20g ethanol, stirring and dissolving, obtains solution C；Adding solution C to solution A, stirring and keeping temperature is 40 DEG C.Commercially available for 8.5L CP level formalin (wt%=37%) being dissolved in 80L pure water and obtains solution B, constant temperature is in 40 DEG C；Solution A, the mixed liquor of C and solution B pump into pipeline reactor with the flow of 20L/Min respectively, after reaction, mixed liquor filters, and the deionized water of the argentum powder after filtration cleans to electrical conductivity less than 100 μ s/cm, with absolute ethanol washing once, filter cake dry, pulverize in 50 DEG C and sieves to obtain argentum powder；
The internal diameter of described continuous conduit formula reactor is 100mm, a length of 6m；The inside of described continuous conduit formula reactor is simultaneously equipped with mechanical stirring device and ultrasonic echography ripple vibrating head, and the multi-layer oar blade formula stirring paddle that described built-in machines agitating device is driven by motor, mixing speed is at 1-10000RPM, and the ultrasonic power of described ultrasound wave vibrating bar is 0.1-5KW.
Embodiment 2
Adding 10.2L ammonia (wt%=28%) in 50L container, add pure water and 1.7Kg silver nitrate, stirring and dissolving, adding sodium hydrate regulator solution pH value is 13, is configured to the solution A of concentration of silver ions 100g/L, and temperature keeps 40 DEG C.Commercially available for 0.5L CP level hydrazine hydrate solution (wt%=80%) being dissolved in 5L pure water and obtains solution B, constant temperature is in 40 DEG C；15gPVA stirring and dissolving is obtained solution C in 5.5L pure water.Solution A, B, C pump into pipeline reactor with the flow of 2L/Min, 1L/min respectively, after reaction, mixed liquor filters, and the deionized water of the argentum powder after filtration cleans to electrical conductivity less than 100 μ s/cm, with absolute ethanol washing once, filter cake dry, pulverize in 50 DEG C and sieves to obtain argentum powder；
The internal diameter of described continuous conduit formula reactor is 25mm, a length of 6m；The inside of described continuous conduit formula reactor is simultaneously equipped with mechanical stirring device and ultrasound wave vibrating bar, and the multi-layer oar blade formula stirring paddle that described built-in machines agitating device is driven by motor, mixing speed is at 1-10000RPM, and the ultrasonic power of described ultrasound wave vibrating bar is 0.1-5KW.
Embodiment 3
1.7Kg silver nitrate being dissolved in pure water, stirring and dissolving, is configured to the silver nitrate solution A of concentration of silver ions 150g/L, temperature keeps 40 DEG C.Add sodium hydroxide, 2000g vitamin C is dissolved in 8L pure water, is configured to the aqueous solution B that pH value is 8, and temperature keeps 40 DEG C.Solution A, B all pump into pipeline reactor with the flow of 5L/Min, inject the PVA aqueous solution C of 15g/L after reactor solution A, B contact point at 2 meters, inject flow 1L/Min, and implant angle is for flow to angle ＞ 90 ° with solution A, B mixed liquor.Mixed argentum powder filters, and the deionized water of the argentum powder after filtration cleans to electrical conductivity less than 100 μ s/cm, and with absolute ethanol washing once, filter cake dry, pulverize in 50 DEG C and sieves to obtain argentum powder；
The internal diameter of described continuous conduit formula reactor is 40mm, a length of 6m；The inside of described continuous conduit formula reactor is simultaneously equipped with mechanical stirring device and ultrasound wave vibrating bar, and the multi-layer oar blade formula stirring paddle that described built-in machines agitating device is driven by motor, mixing speed is at 1-10000RPM, and the ultrasonic power of described ultrasound wave vibrating bar is 0.1-5KW.
Comparative example 1
Adding 10.2L ammonia (wt%=28%) in 50L container, add pure water and 1.7Kg silver nitrate, stirring and dissolving, adding sodium hydrate regulator solution pH value is 13, is configured to the solution A of concentration of silver ions 50g/L, and temperature keeps 40 DEG C.Commercially available for 0.5L CP level hydrazine hydrate solution (wt%=80%) being dissolved in 21L pure water and obtains solution B, constant temperature is in 40 DEG C.Solution A, B all pump into pipeline reactor with the flow of 2L/Min, are filtered by mixed argentum powder, and the deionized water of the argentum powder after filtration cleans to electrical conductivity less than 100 μ s/cm, and with absolute ethanol washing once, filter cake dry, pulverize in 50 DEG C and sieves to obtain argentum powder；
The internal diameter of described continuous conduit formula reactor is 100cm, a length of 6m；The inside of described continuous conduit formula reactor is simultaneously equipped with mechanical stirring device and ultrasound wave vibrating bar, and the multi-layer oar blade formula stirring paddle that described built-in machines agitating device is driven by motor, mixing speed is at 1-10000RPM, and the ultrasonic power of described ultrasound wave vibrating bar is 0.1-5KW.
Comparative example 2
Adding 10.2L ammonia (wt%=28%) in 200L container, add pure water and 1.7Kg silver nitrate, stirring and dissolving, adding sodium hydrate regulator solution pH value is 12, adds 2g oleic acid stirring and dissolving, is configured to the solution A of concentration of silver ions 10g/L, and temperature keeps 40 DEG C.Commercially available for 8.5L CP level formalin (wt%=37%) being dissolved in 80L pure water and obtains solution B, constant temperature is in 40 DEG C；Under stirring, with the flow of 10L/Min, solution B being pumped into solution A, after reaction, mixed liquor filters, and the deionized water of the argentum powder after filtration cleans to electrical conductivity less than 100 μ s/cm, and with absolute ethanol washing once, filter cake dry, pulverize in 50 DEG C and sieves to obtain argentum powder.
Above-mentioned test result is shown in Table 1.
Table 1
Data above is it can be seen that the quality of gained argentum powder all can be produced a very large impact by the factor such as addition of the kind of reducing agent, the kind of dispersant and feed postition, feed way, system pH value and dispersant.By the adjustment of above-mentioned factor, the argentum powder specific surface area that the application obtains is less than 1.55
m2/ g, and there is dispersibility and the uniformity of excellence, it is thus provided that the Advantageous Effects of the present invention.
Aforesaid example is merely illustrative, for explaining some features of the feature of the disclosure.Appended claim is intended to the widest scope that requirement it is contemplated that, and embodiments as presented herein is only the explanation of embodiment of selection of combination according to all possible embodiment.Therefore, the purpose of applicant is that appended claim is not by the selectional restriction of the example of explanation inventive feature.And the progress in science and technology will form the possible equivalent not being presently considered due to the inaccurate reason of language performance or son replacement, and these changes also should be interpreted to be covered by appended claim in the conceived case.
Claims (10)
1. a preparation method for argentum powder, including:
It is respectively configured water reaction system A of silver ion, reductant solution B, dispersant solution C；
A, B and C being injected in continuous conduit formula reactor, hybrid reaction, to deposit Argent grain；With
It is dried described Argent grain, crushes and screens and obtain.
2. the process of claim 1 wherein that water reaction system A of described silver ion comprises silver-containing material and pure water.
3. the method for claim 2, at least one in lower group of wherein said silver-containing material: silver chloride, nitre
Acid silver, silver acetate, Disilver carbonate and silver sulfate.
4. the process of claim 1 wherein that described reductant solution B comprises reducing agent and pure water.
5. the method for claim 4, wherein, at least one in lower group of described reducing agent: formaldehyde, formic acid, vitamin C, hydrazine hydrate, oxammonium sulfate., glucose, sodium borohydride, alkanolamine and hydroquinone.
6. the process of claim 1 wherein that described dispersant solution C comprises:
Dispersant；With
At least one in pure water or ethanol.
7. the method for claim 6, at least one in lower group of wherein said dispersant: fatty acid, soap, surfactant, organic metal, chelating agen, hydroxy polymer, ethyoxyl polymer and protecting colloid.
8. the process of claim 1 wherein the described injection mode of continuous conduit formula reactor one in lower group of A, B and C being injected:
C with A is mixed, then A/C mixed liquor and B are injected separately into continuous conduit formula reactor；With
C with B is mixed, then B/C mixed liquor and A are injected separately into continuous conduit formula reactor；With
A, B, C are injected separately into continuous conduit formula reactor；With
A Yu B is injected separately into continuous conduit formula reactor, and after the contact point of A Yu B, injects C.
9. the method described in any one of claim 1～8, the internal diameter of wherein said continuous conduit formula reactor is 10mm-200mm, a length of 10cm-10m.
10. the method described in any one of claim 1～8, the inside of wherein said continuous conduit formula reactor equipped with in mechanical stirring device and ultrasound wave vibrating bar one or both.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106334802A (en) * | 2016-09-29 | 2017-01-18 | 清华大学深圳研究生院 | Metal powder of spongy microstructure, preparation method thereof, and conductive material |
| CN106493390A (en) * | 2016-11-29 | 2017-03-15 | 金川集团股份有限公司 | A kind of liquid phase slit interference synthesis device |
| CN107457411A (en) * | 2017-06-15 | 2017-12-12 | 昆明理工大学 | A kind of method for preparing super fine silver powder |
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| CN110102778A (en) * | 2019-06-14 | 2019-08-09 | 上海镭立激光科技有限公司 | A kind of preparation method of low-temperature sintering high-crystallinity silver powder |
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| CN106334802A (en) * | 2016-09-29 | 2017-01-18 | 清华大学深圳研究生院 | Metal powder of spongy microstructure, preparation method thereof, and conductive material |
| CN106334802B (en) * | 2016-09-29 | 2018-12-28 | 清华大学深圳研究生院 | Metal powder with spongy microstructure and preparation method thereof, conductive material |
| CN106493390A (en) * | 2016-11-29 | 2017-03-15 | 金川集团股份有限公司 | A kind of liquid phase slit interference synthesis device |
| CN108213455A (en) * | 2016-12-22 | 2018-06-29 | 富士康(昆山)电脑接插件有限公司 | The preparation method of nano metal colloidal sol |
| CN107457411A (en) * | 2017-06-15 | 2017-12-12 | 昆明理工大学 | A kind of method for preparing super fine silver powder |
| CN108941599A (en) * | 2018-07-03 | 2018-12-07 | 珠海市彩龙科技有限公司 | A kind of continuous preparation method of Nanometer Copper |
| CN108941599B (en) * | 2018-07-03 | 2021-06-08 | 珠海市彩龙科技有限公司 | Continuous preparation method of nano-copper |
| CN110102778A (en) * | 2019-06-14 | 2019-08-09 | 上海镭立激光科技有限公司 | A kind of preparation method of low-temperature sintering high-crystallinity silver powder |
| CN116372181A (en) * | 2023-06-07 | 2023-07-04 | 长春黄金研究院有限公司 | Rod-shaped silver powder and preparation method thereof |
| CN116372181B (en) * | 2023-06-07 | 2023-09-05 | 长春黄金研究院有限公司 | Rod-shaped silver powder and preparation method thereof |
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