CN104096851B - The combine production method of a kind of super fine silver powder and CALCIUM PYRUVIC - Google Patents
The combine production method of a kind of super fine silver powder and CALCIUM PYRUVIC Download PDFInfo
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Abstract
The present invention is open a kind of with silver nitrate oxide acetylacetonate aldehyde in the basic conditions, prepares the clean preparation method of super fine silver powder and CALCIUM PYRUVIC simultaneously.Employing is in reactor and stream adds liquor argenti nitratis ophthalmicus, sodium hydroxide solution and pyroracemic aldehyde solution, redox reaction generates super fine silver powder and sodium pyruvate solution, react 0.5-1 hour under maintaining reacting liquid temperature 20-30 DEG C and pH9-11, be then warming up to 40-50 DEG C and reaction is carried out completely.Isolated by filtration super fine silver powder, adds calcium acetate solution after filter vacuum is concentrated again, and the CALCIUM PYRUVIC precipitation that isolated by filtration generates, washing, drying obtains the CALCIUM PYRUVIC crystallization meeting pharmaceutical quality standard.Super fine silver powder prepared by the present invention can be used as the raw material of solar cell or electronic touch screen conductive silver paste, and CALCIUM PYRUVIC product can be used as fat-reducing nutrient agent application.The present invention prepares two kinds of practical fine chemical products simultaneously, and raw material is fully used, and decreases discarded object, and production cost reduces, technical process safety and environmental protection.
Description
Technical field
The present invention relates to the combine production method of a kind of super fine silver powder and CALCIUM PYRUVIC; particularly with silver nitrate in the basic conditions oxide acetylacetonate aldehyde produce the clean preparation method of super fine silver powder and CALCIUM PYRUVIC simultaneously; raw material availability can be improved and reduce discarded object and produce, belong to new chemical materials and field of environment protection.
Background technology
Pyruvic acid and salt thereof are the important organic chemical industry's intermediates of a class, are widely used in organic synthesis industry.Pyruvic acid for the synthesis of several amino acids, as L-Trp, L-Leu, Cys, or synthetic vitamin B6 and B12, the acid of preparation hydrogenation atropine and the important source material of synthesizing ethylene polymer.Agriculturally can be used for producing bactericide, herbicide, also can be used as food additives, be applied to food and brewing industry.Pyruvic acid and salt thereof are also very extensive in the application of medical domain, can be used for the medicine producing sedative, antioxidant, antivirotic and synthesis Hypertension.In recent years, find that CALCIUM PYRUVIC has magical fat-reducing effect, be widely used as nutritional agents, its market demand increases severely.
The production method of pyruvic acid mainly contains chemical synthesis, enzyme transforming process and biological fermentation process.Wherein, chemical synthesis comprises again potassium tartrate method evaporation, lactic acid catalytic oxidation, pyroracemic aldehyde method oxidizing process etc.Conventional acetonate is Sodium Pyruvate and CALCIUM PYRUVIC, and they are obtained by reacting by pyruvic acid and sodium salt or calcium salt.The common drawback of pyruvic acid and the existing production method of salt thereof is that production yield is low, seriously polluted and production cost is too high, causes product price too high, have impact on the rapid expansion in products application market.
Silver powder is most widely used a kind of noble metal powder maximum with consumption in electronic industry, is the key function material producing the various electronic component products such as electronic touch screen, electronic connector.Developing rapidly of electronics and information industry, has driven the development in super fine silver powder and electrocondution slurry market.Silver powder is also the important component part of solar cell conductive silver slurry, and the fast development of solar cell industry further promotes the market demand of super fine silver powder.The key technical index such as the high conductivity after conductive silver paste film forming and compactness determine primarily of the performance of super fine silver powder, and super fine silver powder performance depends primarily on the morphological feature such as granularity and distribution thereof of its appearance structure feature, powder.For solar cell conductive silver slurry, the electrocondution slurry only meeting the silver powder preparation of specified conditions just possesses good serigraphy performance, could form the front silver electrode had compared with high square resistance and thin grid line after oversintering.
The preparation method of silver powder has high-energy ball milling method, spray heating decomposition (SP method), plasma evaporation condensation method, chemical liquid phase reducing process and microemulsion method etc., and wherein chemical liquid phase reducing process obtains extensive attention because of advantages such as production equipment is simple, technics comparing easily controls, low cost, low energy consumption.
CHEMET house journal of U.S. US4456474(1984-06-26) disclose the traditional handicraft of superfine silver powders preparing, silver nitrate aqueous solution is sprayed in the ammonium hydroxide aqueous solution containing trace copper ion, surfactant, hydrazine hydrate under high-speed stirred by high-pressure nozzle atomization, react 15-40 minute at normal temperatures, isolated by filtration precipitates, washing, drying, obtains 0.6-2.5 μm, specific area 0.6-2.0m
2high-purity silver powder of/g.The shortcoming that batch process and product quality are stable not for conventional method, Taiwan Kexue institute patent US5413617(1995-05-09) a kind of silver powder preparation technology controlling specific area is disclosed, first the aqueous solution and silver ammino solution that contain surfactant and hydrazine hydrate reduction agent are added low-temp reaction groove continuously, 7-60 minute is reacted at 5-20 DEG C, then pyroreaction groove is proceeded to, at 40-60 DEG C, continued reaction, isolated by filtration precipitates, and obtains micro aluminum powder.
Patent about silver powder preparation method is also a lot, Chinese patent CN102921944(2013-02-13) a kind of silver powder for conductive silver paste of solar battery electrode and preparation method thereof is disclosed, employing glucose, hydrazine hydrate, hydroquinones or ascorbic acid and composition thereof are reducing agent; Chinese patent CN102632248(2012-08-15) a kind of ball shape silver powder and preparation method thereof is disclosed, employing ascorbic acid is reducing agent, and polyvinylpyrrolidone is protective agent; Chinese patent CN101941078(2011-01-12) a kind of solar battery electrode slurry silver powder and preparation method thereof is disclosed, adopt hydrazine hydrate, formaldehyde, sodium thiosulfate or sodium borohydride to be reducing agent; Japan Patent JP2013189704(2013-09-26) open a kind of adopt formaldehyde to be reducing agent, stearic acid makes the protectant silver powder production method of dispersion; US Patent No. 5000928(1991-03-19) adopt sodium formate to be the silver powder production method of reducing agent; US Patent No. 4456473(1984-06-26) open a kind of adopt hydrazine hydrate to be reducing agent production high-purity silver powder method; Korean Patent KR20100100210(2010-09-15) open method of producing silver powder by inferior sodium phosphate; JP2001107101(2001-04-17) disclose a kind of high dispersive ball shape silver powder production method, employing quinhydrones is reducing agent, makes dispersion protective agent with gelatin; JPH06122905(1994-05-06) disclose a kind of ball shape silver powder production method, adopt sodium borohydride, formaldehyde, quinhydrones and polyvinylpyrrolidone to be reducing agent.
The deficiency that micro aluminum powder prepares reducing agent existence comprises: (1) reducing agent hydrazine hydrate, formaldehyde and quinhydrones are poisonous, and excitant is very strong, and environmental protection and safety problems are given prominence to; (2) borane reducing agent sodium hydride, quinhydrones high cost, affect silver powder productivity effect; (3) reducing agent ascorbic acid is to condition sensitives such as reduction system acidity, concentration and temperature, and working condition is wayward; (4) most of reducing agent need with a large amount of dispersant with the use of, cause follow-up silver powder separation difficulty; (5) rate of charge of conventional reducing agent is excessive, lacks the novel reducer of safety and stability.
In above super fine silver powder production technology, the discarded object that the oxidized generation of reducing agent is useless, the processing procedure of these pollutants is cumbersome.At present because the super fine silver powder high added value of producing and production scale less, the problem of environmental pollution in production is not also subject to enough attention.Along with the super fine silver powder market demand and production scale constantly expand, be badly in need of developing the process for cleanly preparing that reducing agent effectively can be utilized.
Summary of the invention
The object of this invention is to provide a kind of employing silver nitrate oxide acetylacetonate aldehyde in the basic conditions, produce the clean preparation method of super fine silver powder and CALCIUM PYRUVIC, reaction raw materials is fully used, and the technical scheme taked and production stage are simultaneously:
(1) by industrial acetone aldehyde solution dilution, add the organic dispersing agent of industrial acetone aldehyde quality 0-2%, the concentration obtaining containing organic dispersing agent is the pyroracemic aldehyde solution of 0.5-1.0mol/L;
(2) respectively silver nitrate and NaOH are dissolved in deionized water, being diluted to concentration after dissolving is the liquor argenti nitratis ophthalmicus of 0.5-1.0mol/L and the sodium hydroxide solution of 1.0mol/L;
(3) in the glass reactor of band stirring, also stream adds liquor argenti nitratis ophthalmicus, sodium hydroxide solution and pyroracemic aldehyde solution, reaction generates super fine silver powder and sodium pyruvate solution, control material molar ratio is: silver nitrate: pyroracemic aldehyde: NaOH=1:0.5-0.7:1-1.4, charging rate controls to be precipitated as canescence what keep generating in reactant liquor, reacts 0.5-1 hour under maintaining reacting liquid temperature 20-30 DEG C and pH9-11;
(4) fed intake rear raised temperature to 40-50 DEG C, continued stirring reaction 0.5-1 hour, make reaction carry out completely;
(5) silver powder of isolated by filtration generation, successively with deionized water and ethanol washing, at 80 DEG C, drying obtains super fine silver powder product, silver powder particles in closely spherical, smooth surface and glossy, narrow diameter distribution, average grain diameter 1.2-1.8 μm, tap density 4.5-5.0g/mL, specific area 0.4-0.8m
3/ g, quality meets silver paste of solar cells and prepares requirement, in the molar yield of silver nitrate for 99.1%-100%;
(6) by the volume of the filtrate Vacuum Concentration to original 1/3rd at 50-60 DEG C after separation silver powder, calcium acetate solution is added under stirring, reaction generates CALCIUM PYRUVIC precipitation, controls pyroracemic aldehyde and calcium acetate mol ratio 1:0.4-0.6, controls reaction temperature 20-40 DEG C;
(7) isolated by filtration CALCIUM PYRUVIC precipitation, deionized water is washed, drying obtains CALCIUM PYRUVIC crystallization, product appearance is faint yellow to white powder, pyruvic acid content >=66.0%, calcium content >=15.2%, water content≤17.5%, heavy metal (Pb)≤0.0001%, meets CALCIUM PYRUVIC pharmaceutical quality standard, in the molar yield of pyroracemic aldehyde for 70%-86%.
The raw material acetone aldehyde adopted in the present invention, has another name called methyl-glyoxal, nonpoisonous and tasteless, and in molecular structure, existing ketone group has aldehyde radical again, and pure material is very active, so commodity occur all as an aqueous solution, is mainly used in the synthesis of pharmaceutical intermediate.Current pyroracemic aldehyde mainly adopts propane diols to be raw material, and on silver catalyst, catalytic gas phase oxidation is produced.China's pyroracemic aldehyde annual production about 1.5 ten thousand tons, ample supply of commodities on the market, the market price is cheaper.
Raw pyroracemic aldehyde of the present invention is commercially available 40% industrial acetone aldehyde or 20%-30% industrial acetone aldehyde, and industrial acetone aldehyde contains propane diols and the hydroxypropanone-of 0.2%-2%, does not affect the invention process.
Raw silver nitrate of the present invention is reagent silver nitrate or industrial silver is dissolved in the obtained liquor argenti nitratis ophthalmicus of excess nitric acid, and a small amount of nitric acid adulterated in industrial nitric acid silver material implements not impact to invention.
The dispersant adopted in the present invention is the pyruvic acid that pyroracemic aldehyde oxidation reaction generates, the silver-colored grain surface that pyruvic acid is adsorbed on generation blocks it and too fastly to grow up, react rear easy washing removing, even without adding organic dispersing agent, also silver-colored crystallite dimension can be limited in micron or sub-micrometer range.
Silver nitrate oxide acetylacetonate aldehyde of the present invention prepares silver powder simultaneously and pyruvic acid carries out in the basic conditions, and reaction equation is as follows:
2AgNO
3+CH
3COCHO+2NaOH=2Ag+CH
3COCOOH+2NaNO
3+H
2O
Need in reaction constantly to add NaOH or potassium hydroxide solution control reactant liquor pH9-11, when reacting liquid basicity is too high, the disproportionation of pyroracemic aldehyde reduces side reaction aggravation, adds raw material acetone aldehyde consumption, the actual rate of charge of pyroracemic aldehyde should be greater than theoretical amount, and the disproportionated reaction formula of pyroracemic aldehyde is as follows:
2CH
3COCHO+NaOH=CH
3COCOONa+CH
3COCH
2OH
The incipient stage of the present invention's reaction, the raw material liquor argenti nitratis ophthalmicus added directly reacts with pyroracemic aldehyde and forms the silver-colored nucleus of black and pyruvic acid; In the subsequent reactions stage, first raw material liquor argenti nitratis ophthalmicus reacts with the pyruvic acid that contains in reactant liquor and generates pyruvic acid silver ligand, pyruvic acid silver generates silver atoms with pyroracemic aldehyde reaction again and generates pyruvic acid, and the silver atoms that reduction generates homoepitaxial on the silver-colored nucleus previously formed is the silver-colored crystal grain of several microns.
The reaction cycle that the formation of pyruvic acid silver ligand and reduction generate silver atoms and pyruvic acid is carried out, and reaction equation is as follows:
AgNO
3+CH
3COCOONa=CH
3COCOOAg+NaNO
3
CH
3COCHO+2CH
3COCOOAg+H
2O=2Ag+3CH
3COCOOH
Course of reaction more complicated of the present invention, actual not necessarily pyruvic acid silver ligand of participating in reduction reaction, it can be a small amount of silver ion that its dissociation is formed, concentration of silver ions determines primarily of pyruvic acid silver ligand stability constant, speed is added and reaction temperatures affect is less by silver nitrate, because concentration of silver ions is more stable, reduction reaction conditions easily controls.
In the present invention, the decomposition of pyroracemic aldehyde disproportionation and oxidation generation pyruvic acid adsorb at silver-colored grain surface as dispersant, the too fast of silver-colored nucleus can be effectively suppressed to be grown up, the dispersant adsorption layer of each silver-colored nucleating surface is in occupation of certain space simultaneously, make the silver-colored crystal grain formed cannot be coalescent, be in the state of fully dispersion, silver powder particle diameter is controlled.
In the present invention, leading portion reaction temperature is 20-30 DEG C, improve temperature by fast reaction speed, excessive temperature will make silver powder density reduce and particle diameter uneven, also increase pyroracemic aldehyde disproportionation decomposition rate simultaneously, back segment reaction temperature is 40-50 DEG C, silver ion in solution is reacted completely, in order to avoid content of beary metal is too high in product CALCIUM PYRUVIC.
For making silver powder surface topography and even particle size distribution, can also coordinate and add organic dispersing agent, but organic dispersing agent add the CALCIUM PYRUVIC product quality that can not affect coproduction, oleic acid, dodecyl sodium sulfate, low molecular poly (PE600) or polyvinylpyrrolidone (PVP) etc. can be selected, be convenient to reaction complete after employing water-washing method remove from product.
Advantage and the beneficial effect of invention are embodied in:
(1) the present invention reduces silver nitrate using pyroracemic aldehyde as reducing agent, and the silver powder product density obtained is high, narrow diameter distribution, can be used as solar cell or electronic touch screen conductive silver paste raw material;
(2) the present invention is using pyroracemic aldehyde product pyruvic acid as dispersant component, can wash removing after having reacted, and greatly reduce organic dispersing agent consumption, product purity is high;
(3) the CALCIUM PYRUVIC product that the present invention obtains reaches pharmaceutical grade quality standard, can be used as fat-reducing nutrient agent application;
(4) the present invention can produce two kinds of practical fine chemical products simultaneously, and raw material is fully used, and decrease discarded object and produce, production cost reduces, production process safety and environmental protection.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1
12.6g40% industrial acetone aldehyde (0.07mol) 60mL deionized water is diluted to the pyroracemic aldehyde solution that concentration is 1.0mol/L; 5.9g chemical pure NaOH (0.14mol) is used 134mL deionized water dissolving, obtains the sodium hydroxide solution of 1.0mol/L; 17.0g silver nitrate reagent (0.1mol) is dissolved in 80mL deionized water, and dilution obtains 100mL1.0mol/L liquor argenti nitratis ophthalmicus.
In the 500mL glass reactor that band stirs, also stream drips pyroracemic aldehyde solution, sodium hydroxide solution and liquor argenti nitratis ophthalmicus simultaneously, black silver nucleus is had to produce at once, stop reinforced 10 minutes, when precipitation changes canescence gradually into, continue to add material liquid, rate of addition controls to be precipitated as grey what keep generating in reactant liquor, maintains reactant liquor pH10-11 and reaction temperature 25-30 DEG C, feeds in raw material and complete for about 30 minutes.Feed intake rear raised temperature to 40-50 DEG C, has continued stirring reaction 0.5 hour, generate linen silver-colored crystal grain.
The silver powder that isolated by filtration generates, successively with 20mL deionized water and ethanol washing, at 80 DEG C, drying obtains super fine silver powder product 10.8g, in the molar yield 100% of silver nitrate, silver powder particles in closely spherical, smooth surface and glossy, narrow diameter distribution, average grain diameter 1.5 μm, tap density 4.8g/mL, specific area 0.62m
3/ g.
Filtrate Vacuum Concentration at 50-60 DEG C after being separated silver powder, to 100mL, is added the calcium acetate solution 21mL (0.035mol) of mass percentage concentration 20% under stirring, reaction generates CALCIUM PYRUVIC precipitation, reaction temperature 20-40 DEG C.
Isolated by filtration CALCIUM PYRUVIC precipitates, and with the washing precipitation of 20mL deionized water, dry CALCIUM PYRUVIC crystallization 10.5g (0.049mol), quality meets pharmaceutical grade standard, in the molar yield of pyroracemic aldehyde for 70%.
Embodiment 2
By 10.8g40% industrial acetone aldehyde (0.06mol) 50mL deionized water dilution, add 0.1g oleic acid dispersant, the concentration obtaining containing dispersant is the pyroracemic aldehyde solution of 1.0mol/L; 5.1g chemical pure NaOH (0.12mol) is used 115mL deionized water dissolving, obtains the sodium hydroxide solution of 1.0mol/L; 17.0g silver nitrate reagent (0.1mol) is dissolved in 80mL deionized water, and dilution obtains 100mL1.0mol/L liquor argenti nitratis ophthalmicus.
In the 500mL glass reactor that band stirs, also stream drips pyroracemic aldehyde solution, sodium hydroxide solution and liquor argenti nitratis ophthalmicus simultaneously, black silver nucleus is had to produce at once, stop reinforced 5 minutes, when precipitation changes canescence gradually into, continue to add material liquid, rate of addition controls to be precipitated as canescence what keep generating in reactant liquor, maintains reactant liquor pH9-10 and reaction temperature 25-30 DEG C, feeds in raw material and complete for about 30 minutes.Feed intake rear raised temperature to 40-50 DEG C, has continued stirring reaction 0.5 hour, generate linen silver-colored crystal grain.Isolated by filtration silver powder, successively with 20mL deionized water and ethanol washing, at 80 DEG C, drying obtains super fine silver powder product 10.7g, in the molar yield 99.1% of silver nitrate, silver powder particles is in closely spherical, smooth surface and glossy, narrow diameter distribution, average grain diameter 1.7 μm, tap density 4.6g/mL, specific area 0.54m
3/ g.
Filtrate Vacuum Concentration at 50-60 DEG C after being separated silver powder, to 100mL, is added the calcium acetate solution 18mL (0.03mol) of mass percentage concentration 20% under stirring, reaction generates CALCIUM PYRUVIC precipitation, reaction temperature 20-40 DEG C.Isolated by filtration CALCIUM PYRUVIC precipitates, and with the washing precipitation of 20mL deionized water, dry CALCIUM PYRUVIC crystallization 10.1g (0.047mol), quality meets pharmaceutical grade standard, in the molar yield of pyroracemic aldehyde for 78%.
Embodiment 3
By 9.0g40% industrial acetone aldehyde (0.05mol) 50mL deionized water dilution, add 0.05g dodecyl sodium sulfate dispersant, the concentration obtaining containing dispersant is the pyroracemic aldehyde solution of 1.0mol/L; 5.1g chemical pure NaOH (0.12mol) is used 115mL deionized water dissolving, obtains the sodium hydroxide solution of 1.0mol/L; 17.0g silver nitrate reagent (0.1mol) is dissolved in 80mL deionized water, and dilution obtains 100mL1.0mol/L liquor argenti nitratis ophthalmicus.
In the 500mL glass reactor that band stirs, also stream drips pyroracemic aldehyde solution, sodium hydroxide solution and liquor argenti nitratis ophthalmicus simultaneously, rate of addition controls to be precipitated as canescence what keep generating in reactant liquor, maintain reactant liquor pH10-11 and reaction temperature 25-30 DEG C, feed in raw material and complete for about 20 minutes.Feed intake rear raised temperature to 40-50 DEG C, has continued stirring reaction 0.5 hour, generate linen silver-colored crystal grain.Isolated by filtration silver powder, successively with 20mL deionized water and ethanol washing, at 80 DEG C, drying obtains super fine silver powder product 10.7g, in the molar yield 99.1% of silver nitrate, silver powder particles in closely spherical, smooth surface and glossy, narrow diameter distribution, average grain diameter 1.7 μm, tap density 4.7g/mL, specific area 0.51m
3/ g.
Filtrate Vacuum Concentration at 50-60 DEG C after being separated silver powder, to 100mL, is added the calcium acetate solution 18mL (0.03mol) of mass percentage concentration 20% under stirring, reaction generates CALCIUM PYRUVIC precipitation, reaction temperature 20-40 DEG C.Isolated by filtration CALCIUM PYRUVIC precipitates, and with the washing precipitation of 20mL deionized water, dry CALCIUM PYRUVIC crystallization 9.0g (0.042mol), quality meets pharmaceutical grade standard, in the molar yield of pyroracemic aldehyde for 86%.
Claims (4)
1. the combine production method of a super fine silver powder and CALCIUM PYRUVIC, it is characterized in that adopting silver nitrate oxide acetylacetonate aldehyde in the basic conditions, prepare the clean preparation method of super fine silver powder and CALCIUM PYRUVIC simultaneously, reaction raw materials is fully used and decreases discarded object to produce, the technical scheme taked and production stage are:
(1) by industrial acetone aldehyde solution dilution, add the organic dispersing agent of industrial acetone aldehyde quality 0-2%, the concentration obtaining not containing or containing organic dispersing agent is the pyroracemic aldehyde solution of 0.5-1.0mol/L;
(2) respectively silver nitrate and NaOH are dissolved in deionized water, after dissolving, are diluted to the nitre that concentration is 0.5-1.0mol/L
The sodium hydroxide solution of the silver-colored solution of acid and 1.0mol/L;
(3) in the glass reactor of band stirring, also stream adds liquor argenti nitratis ophthalmicus, sodium hydroxide solution and pyroracemic aldehyde solution, instead
Should generate super fine silver powder and sodium pyruvate solution, controlling material molar ratio is: silver nitrate: pyroracemic aldehyde: NaOH=1:
0.5-0.7:1-1.4, charging rate controls to be precipitated as canescence what keep generating in reactant liquor, maintains reacting liquid temperature
0.5-1 hour is reacted under 20-30 DEG C and pH9-11;
(4) fed intake rear raised temperature to 40-50 DEG C, continued stirring reaction 0.5-1 hour, make reaction carry out completely;
(5) silver powder of isolated by filtration generation, successively with deionized water and ethanol washing, at 80 DEG C, drying obtains super fine silver powder product, and quality meets silver paste of solar cells and prepares requirement, in the molar yield of silver nitrate for 99.1%-100%;
(6) filtrate after silver powder will be separated, at 50-60 DEG C, Vacuum Concentration is to the volume of original 1/3rd, adds calcium acetate solution under stirring, and reaction generates CALCIUM PYRUVIC precipitation, control pyroracemic aldehyde and calcium acetate mol ratio l:0.4-0.6, control reaction temperature 20-40 DEG C;
(7) isolated by filtration CALCIUM PYRUVIC precipitation, deionized water is washed, and drying obtains the CALCIUM PYRUVIC crystallization meeting pharmaceutical quality standard, in the molar yield of pyroracemic aldehyde for 70%-86%.
2. the combine production method of super fine silver powder and CALCIUM PYRUVIC according to claim l, is characterized in that raw material acetone aldehyde
The pyroracemic aldehyde industrial goods of mass percentage concentration 40% or the pyroracemic aldehyde industrial goods of mass percentage concentration 20%-30%.
3. the combine production method of super fine silver powder and CALCIUM PYRUVIC according to claim l, is characterized in that raw material silver nitrate
Chemical reagent or the silver nitrate industrial goods containing a small amount of nitric acid.
4. the combine production method of super fine silver powder and CALCIUM PYRUVIC according to claim l, is characterized in that organic dispersing agent
Oleic acid, dodecyl sodium sulfate, low molecular poly (PE600) or polyvinylpyrrolidone (PVP).
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Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3219355A1 (en) * | 1982-05-22 | 1983-11-24 | Basf Ag, 6700 Ludwigshafen | Process for the preparation of pyruvic acid |
| JPS63133990A (en) * | 1986-11-21 | 1988-06-06 | Toyobo Co Ltd | Production of pyruvic acid |
| JP4839767B2 (en) * | 2005-10-14 | 2011-12-21 | 東洋インキＳｃホールディングス株式会社 | A method for producing a metal fine particle dispersion, a conductive ink using the metal fine particle dispersion produced by the method, and a conductive pattern. |
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