CN109014244A - A method of silver powder is prepared with environment-friendly metal silver salt - Google Patents
A method of silver powder is prepared with environment-friendly metal silver salt Download PDFInfo
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- CN109014244A CN109014244A CN201810886036.2A CN201810886036A CN109014244A CN 109014244 A CN109014244 A CN 109014244A CN 201810886036 A CN201810886036 A CN 201810886036A CN 109014244 A CN109014244 A CN 109014244A
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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
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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Abstract
The invention discloses a kind of methods for preparing silver powder with environment-friendly metal silver salt, belong to conductive metal Preparation Technique of Powders field, include the following steps: that the preparation of silver citrate and thermal decomposition method prepare silver powder.The present invention prepares environment-friendly metal silver salt silver citrate by raw material of silver nitrate；9-12 μm of super fine silver powder is prepared by thermally decomposing；It is generated in silver powder preparation process of the invention without the waste water containing ammonia nitrogen, simple production process, environmental protection is at low cost, can be realized industrialized production.
Description
Technical field
It is specifically a kind of to prepare silver powder with environment-friendly metal silver salt the invention belongs to conductive metal Preparation Technique of Powders field
Method.
Background technique
Being constantly progressive and develop with social industry, simultaneously because people expect industrial negative effect
Not enough, it is unfavorable to prevent, and results in the big crisis of global three: shortage of resources, environmental pollution, ecological disruption.Wherein, environmental pollution
It can cause directly to destroy and influence to the ecosystem, such as: desertification, forest deterioration can also cause indirectly to human society
Harm, the hazard ratio of sometimes this indirect environmental benefit directly endangered bigger caused by that time, be also more difficult to eliminate.
With the globalization of economy and trade, industrial pollution becomes the main factor for causing environmental pollution, and industry is dirty
Dye mainly as caused by " three wastes " (waste water,waste gas and industrial residue) and various noises in industrial production, can be divided into contaminated wastewater,
Exhaust emission, residue contamination, noise pollution.Industrial pollution is very harmful to industrial or agricultural construction and people's health, is mainly manifested in:
First is that discharging the harmful wastes such as a large amount of raw waters, gas, slag in industrial production, the ecological balance of agricultural can be seriously destroyed
And natural resources, the development of agricultural production is caused great harm；Second is that harm of the Industrial " three Waste " to industrial production itself
Also very serious, toxic polluter meeting corrosion pipeline, damages equipment, influences the service life of workshop etc.；Third is that environmental pollution,
Public hazards are spread unchecked, and the health of broad masses of the people is directly endangered；Fourth is that some industrial pollution consequences are serious, it is difficult to it removes, some
Pollution is not easy to find, endanger caused by discovery later very serious.
The main preparation methods of super fine silver powder are to prepare silver powder by Liquid reduction reaction process using silver nitrate as raw material at present,
A large amount of high concentration silver-containing liquid waste can be generated in silver powder preparation process, in waste water silver in the form of ions and concentration it is non-
Chang Gao.If not removing silver and the reuse in waste water, it not only will affect environment, also will cause the waste of noble metal.Secondly as
Using silver nitrate as raw material, organic matter is added in reduction process and carries out reduction reaction, causes to contain a large amount of ammonia in silver powder waste water
Nitrogen and large amount of complex organic matter, so that COD concentration height, bio-toxicity effect are strong in such waste water.Therefore for silver powder can
Sustainable development, and reduce environmental pollution, it is necessary to the exploratory development that silver powder prepares raw material is carried out, it is high using a kind of silver content,
Environmental pollution is few, and silver powder simple and easy to get prepares raw material to substitute the industrial production that silver nitrate carries out silver powder.Also, with
The hitting dynamics that country increasingly payes attention to environmental protection and environmental pollution is increasingly severe, novel environment friendly silver powder prepare raw material
Use more and more will be studied and be paid close attention in future.
Summary of the invention
The object of the present invention is to provide a kind of methods for preparing silver powder with environment-friendly metal silver salt, useless to solve the prior art
The problem of silver content is big in liquid, and contains a large amount of ammonia nitrogens and organic matter, pollutes environment and noble metal is caused to waste.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
A method of silver powder being prepared with environment-friendly metal silver salt, is included the following steps:
Step 1: the preparation of silver citrate:
A, at room temperature, sodium citrate is dissolved in deionized water, obtains sodium citrate solution；
B, silver nitrate is dissolved in deionized water, obtains silver nitrate solution；
C, sodium citrate solution is slowly dropped in silver nitrate solution, after being added dropwise, carries out strong mixing；Using strong mixing,
And using be added dropwise by the way of be in order to reaction process reduce reunite generation, and make solution be uniformly mixed；
D, after standing 2-4h, supernatant is removed, obtains precipitating to be washed with deionized water being washed with dehydrated alcohol, washes to finish and dry
To silver citrate solid；
Step 2: thermal decomposition method prepares silver powder:
A, dispersing agent, reducing agent are dissolved in solvent, obtain liquid A on earth；
B, the silver citrate for obtaining step 1 is added to stirring in the liquid A of bottom and obtains system B to dissolving；
C, system B is placed in 180-220 DEG C of constant temperature system and stands heating 30-50min taking-up, gone after being cooled to room temperature
Supernatant obtains silver powder precipitating；
D, obtained silver powder deionized water and dehydrated alcohol are washed, washes complete drying and obtains D50It is ultra-fine at 9-12 μm
Silver powder.
Sodium citrate solution mass concentration described in step 1 is 170-235g/L, and the mass concentration of silver nitrate solution is
The mass ratio of 305-425mol/L, silver nitrate and sodium citrate is 1.73-2.4:1.
The time of dropwise addition described in the step C of step 1 is 20-30min.
Mixing speed described in the step C of step 1 is 370-450rpm, mixing time 40-60min.
Deionization described in the step D of step 1 is washed 2-3 times, and dehydrated alcohol is washed 1-2 times.
Dispersing agent described in step 2 is polyethylene pyrrole network alkanone, Macrogol 4000, polyvinyl alcohol or Tween-80.
Reducing agent described in step 2 is ascorbic acid, formic acid or formaldehyde.
Solvent described in step 2 is deionized water or glycerol.
The mass ratio of dispersing agent and silver citrate is 0.08-0.2:1, dispersing agent in system B described in the step B of step 2
Mass concentration be 5-10g/L, the mass ratio of reducing agent and silver citrate is 1.15-1.6:1, and the mass concentration of reducing agent is
75-85g/L, the mass concentration of silver citrate are 65-75g/L.
It is because nothing contains in silver powder production process that the present invention, which prepares silver powder raw materials for production using silver citrate and silver nitrate,
The waste water of ammonia nitrogen generates, small pollution of the environment.
The selection of reducing agent of the present invention is the key that Control granularity uniform concentration, can be better by control in preparation
Silver powder forming core processed and growth rate obtain that crystallinity is high, silver powder product of homogeneous grain diameter to reach, the selection of dispersing agent be in order to
It prevents from reuniting in silver powder preparation process, influences the pattern and index of silver powder, the determination of the amount of dispersing agent is to guarantee
In subsequent laundering process after silver powder dispersibility and silver powder synthesize in silver powder synthesis process silver powder can be reduced with washes clean
The remaining of middle organic matter reduces scaling loss.
In the present invention determination of decomposition temperature be in order to guarantee that silver citrate can completely resolve into silver powder, rather than its
His Ag-containing compound.
The present invention having the beneficial effect that compared to the prior art
(1) present invention prepares environment-friendly metal silver salt silver citrate by raw material of silver nitrate；
(2) silver citrate of the invention prepares 9-12 μm of super fine silver powder by thermal decomposition；
(3) present invention prepares the method for silver powder and the maximum difference of ordinary electronic slurry silver powder preparation method is silver citrate
The main raw material(s) for becoming silver powder production that silver nitrate can be substituted, is a kind of environment-friendly materials；
(4) it is generated in silver powder preparation process of the invention without the waste water containing ammonia nitrogen, simple production process, environmental protection is at low cost, can
Realize industrialized production.
Specific embodiment
The present invention will be further described With reference to embodiment.
Step 1: the preparation of silver citrate:
A, at room temperature, sodium citrate is dissolved in deionized water, obtains sodium citrate solution；
B, silver nitrate is dissolved in deionized water, obtains silver nitrate solution；
C, sodium citrate solution is slowly dropped in silver nitrate solution, after being added dropwise, carries out strong mixing；
D, after standing 2-4h, supernatant is removed, obtains precipitating to be washed with deionized water being washed with dehydrated alcohol, washes to finish and dry
To silver citrate solid；
Step 2: thermal decomposition method prepares silver powder:
A, dispersing agent, reducing agent are dissolved in solvent, obtain liquid A on earth；
B, the silver citrate for obtaining step 1 is added to stirring in the liquid A of bottom and obtains system B to dissolving；
C, system B is placed in 180-220 DEG C of constant temperature system and stands heating 30-50min taking-up, gone after being cooled to room temperature
Supernatant obtains silver powder precipitating；
D, obtained silver powder deionized water and dehydrated alcohol are washed, washes and finishes drying to obtain D50 ultra-fine at 9-12 μm
Silver powder.
Sodium citrate solution mass concentration described in step 1 is 170-235g/L, and the mass concentration of silver nitrate solution is
The mass ratio of 305-425g/L, silver nitrate and sodium citrate is 1.73-2.4:1.
The time of dropwise addition described in the step C of step 1 is 20-30min.
Mixing speed described in the step C of step 1 is 370-450rpm, mixing time 40-60min.
Deionization described in the step D of step 1 is washed 2-3 times, and dehydrated alcohol is washed 1-2 times.
Dispersing agent described in step 2 is polyethylene pyrrole network alkanone, Macrogol 4000, polyvinyl alcohol or Tween-80.
Reducing agent described in step 2 is ascorbic acid, formic acid or formaldehyde.
Solvent described in step 2 is deionized water or glycerol.
The mass ratio of dispersing agent and silver citrate is 0.08-0.2:1, dispersing agent in system B described in the step B of step 2
Mass concentration be 5-10g/L, the mass ratio of reducing agent and silver citrate is 1.15-1.6:1, and the mass concentration of reducing agent is
75-85g/L, the mass concentration of silver citrate are 65-75g/L.
Embodiment 1:
A, the preparation of silver citrate
(1) at room temperature, sodium citrate 578g is dissolved in 2.7L deionized water, obtains sodium citrate solution；(2) silver nitrate is weighed
1000g is dissolved in 2.5L deionized water, obtains silver nitrate solution；(3) sodium citrate solution is slowly dropped to silver nitrate solution
In, time for adding 30min, after being added dropwise, the mixing speed strong mixing of 390rpm 60 minutes；(4) it after stirring, stands
Remove supernatant after 2h, gained precipitating be washed with deionized water 3 times, dehydrated alcohol wash 1 time, wash complete 60 DEG C of drying both white lemon
The silver-colored solid of lemon acid.
B, thermal decomposition method prepares silver powder
(1) weigh 8.5g polyethylene pyrrole network alkanone, 102g ascorbic acid is dissolved in 1.2L deionized water, obtain liquid A on earth；(2) claim
Silver citrate 85g after taking drying is added to stirring in the liquid A of bottom and obtains system B to dissolving；(3) system B is placed on 190 DEG C
Constant temperature Muffle furnace in stand heating 50 minutes after take out, remove supernatant after being cooled to room temperature, obtain silver powder precipitate；(4) will
Gained silver powder be washed with deionized water 3 times, dehydrated alcohol wash 2 times, wash it is complete 60 DEG C drying, both D50For 11.20 μm of super fine silver powder.
Embodiment 2:
A, the preparation of silver citrate
(1) at room temperature, sodium citrate 578g is dissolved in 3.4L deionized water, obtains sodium citrate solution；(2) silver nitrate is weighed
1000g is dissolved in 2.5L deionized water, obtains silver nitrate solution；(3) sodium citrate solution is slowly dropped to silver nitrate solution
In, time for adding 30min, after being added dropwise, the mixing speed strong mixing of 390rpm 60 minutes；(4) it after stirring, stands
Remove supernatant after 4h, gained precipitating be washed with deionized water 3 times, dehydrated alcohol wash 1 time, wash complete 60 DEG C of drying both white lemon
The silver-colored solid of lemon acid.
B, thermal decomposition method prepares silver powder
(1) weigh 20g polyethylene pyrrole network alkanone, 160g ascorbic acid is dissolved in 1.5L deionized water and is added 0.5L glycerol, obtain
Liquid A on earth；(2) the silver citrate 100g after weighing drying is added to stirring in the liquid A of bottom and obtains system B to dissolving；(3) by body
Be B be placed on heated 50 minutes in 200 DEG C of constant temperature system after take out, remove supernatant after being cooled to room temperature, it is heavy to obtain silver powder
It forms sediment；(4) by gained silver powder be washed with deionized water 3 times, dehydrated alcohol wash 2 times, wash it is complete 60 DEG C drying, both D50For 9.22 μm surpass
Thin silver powder.
Embodiment 3:
A, the preparation of silver citrate
(1) at room temperature, sodium citrate 416.67g is dissolved in 1.95L deionized water, obtains sodium citrate solution；(2) nitre is weighed
Acid silver 1000g is dissolved in 2.5L deionized water, obtains silver nitrate solution；(3) sodium citrate solution is slowly dropped to silver nitrate
In solution, time for adding 30min, after being added dropwise, the mixing speed strong mixing of 400rpm 50 minutes；(4) after stirring,
Remove supernatant after standing 3h, gained precipitating be washed with deionized water 3 times, dehydrated alcohol wash 1 time, wash complete 60 DEG C dry both it is white
Silver citrate solid.
B, thermal decomposition method prepares silver powder
(1) 5.6g Macrogol 4000 is weighed, 85g formic acid is dissolved in 1L deionized water and 0.3L glycerol is added, obtains liquid A on earth；
(2) the silver citrate 70g after weighing drying is added to stirring in the liquid A of bottom and obtains system B to dissolving；(3) system B is placed on
It heats in 190 DEG C of constant temperature system and takes out after forty minutes, remove supernatant after being cooled to room temperature, obtain silver powder precipitating；(4) by institute
Silver powder be washed with deionized water 3 times, dehydrated alcohol wash 2 times, wash complete 60 DEG C of drying, both D50 is 9.12 μm of super fine silver powder.
Embodiment 4:
A, the preparation of silver citrate
(1) at room temperature, sodium citrate 368.5g is dissolved in 1.5L deionized water, obtains sodium citrate solution；(2) nitric acid is weighed
Silver-colored 637.5g is dissolved in 1.5L deionized water, obtains silver nitrate solution；(3) that sodium citrate solution is slowly dropped to silver nitrate is molten
In liquid, time for adding 30min, after being added dropwise, the mixing speed strong mixing of 390rpm 60 minutes；(4) quiet after stirring
Set and remove supernatant after 2h, gained precipitating be washed with deionized water 3 times, dehydrated alcohol wash 1 time, wash complete 60 DEG C of drying both it is white
Silver citrate solid.
B, thermal decomposition method prepares silver powder
(1) 10g Tween-80 is weighed, 135g ascorbic acid is dissolved in 1.8L deionized water and 0.2L glycerol is added, obtains liquid A on earth；
(2) the silver citrate 120g after weighing drying is added to stirring in the liquid A of bottom and obtains system B to dissolving；(3) system B is placed on
It is taken out after being heated 50 minutes in 210 DEG C of constant temperature system, removes supernatant after being cooled to room temperature, obtain silver powder precipitating；(4) by institute
Silver powder be washed with deionized water 3 times, dehydrated alcohol wash 2 times, wash complete 60 DEG C of drying, both D50 is 11.45 μm of super fine silver powder.
Embodiment 5:
A, the preparation of silver citrate
(1) at room temperature, sodium citrate 578g is dissolved in 2.7L deionized water, obtains sodium citrate solution；(2) silver nitrate is weighed
1000g is dissolved in 2.5L deionized water, obtains silver nitrate solution；(3) sodium citrate solution is slowly dropped to silver nitrate solution
In, time for adding 30min, after being added dropwise, the mixing speed strong mixing of 410rpm 60 minutes；(4) it after stirring, stands
Remove supernatant after 2h, gained precipitating be washed with deionized water 3 times, dehydrated alcohol wash 1 time, wash complete 60 DEG C of drying both white lemon
The silver-colored solid of lemon acid.
B, thermal decomposition method prepares silver powder
(1) 12g polyvinyl alcohol is weighed, 150g ascorbic acid is dissolved in 2L deionized water and 0.3L glycerol is added, obtains liquid A on earth；
(2) the silver citrate 135g after weighing drying is added to stirring in the liquid A of bottom and obtains system B to dissolving；(3) system B is placed on
It heats in 220 DEG C of constant temperature system and takes out after forty minutes, remove supernatant after being cooled to room temperature, obtain silver powder precipitating；(4) by institute
Silver powder be washed with deionized water 3 times, dehydrated alcohol wash 2 times, wash complete 60 DEG C of drying, both D50 is 10.15 μm of super fine silver powder.
Embodiment 6:
A, the preparation of silver citrate
(1) at room temperature, sodium citrate 381.25g is dissolved in 1.9L deionized water, obtains sodium citrate solution；(2) nitre is weighed
Acid silver 762.5g is dissolved in 2.5L deionized water, obtains silver nitrate solution；(3) sodium citrate solution is slowly dropped to silver nitrate
In solution, time for adding 20min, after being added dropwise, the mixing speed strong mixing of 450rpm 40 minutes；(4) after stirring,
Remove supernatant after standing 3h, gained precipitating be washed with deionized water 3 times, dehydrated alcohol wash 1 time, wash complete 60 DEG C dry both it is white
Silver citrate solid.
B, thermal decomposition method prepares silver powder
(1) 12g polyvinyl alcohol is weighed, 144.5g formaldehyde is dissolved in 1.5L deionized water and 0.2L glycerol is added, obtains liquid A on earth；
(2) the silver citrate 125g after weighing drying is added to stirring in the liquid A of bottom and obtains system B to dissolving；(3) system B is placed on
It heats in 220 DEG C of constant temperature system and takes out after forty minutes, remove supernatant after being cooled to room temperature, obtain silver powder precipitating；(4) by institute
Silver powder be washed with deionized water 3 times, dehydrated alcohol wash 2 times, wash complete 60 DEG C of drying, both D50 is 9.15 μm of super fine silver powder.
Embodiment 7:
A, the preparation of silver citrate
(1) at room temperature, sodium citrate 578g is dissolved in 3.4L deionized water, obtains sodium citrate solution；(2) silver nitrate is weighed
1000g is dissolved in 2.5L deionized water, obtains silver nitrate solution；(3) sodium citrate solution is slowly dropped to silver nitrate solution
In, time for adding 30min, after being added dropwise, the mixing speed strong mixing of 370rpm 60 minutes；(4) it after stirring, stands
Remove supernatant after 4h, gained precipitating be washed with deionized water 3 times, dehydrated alcohol wash 1 time, wash complete 60 DEG C of drying both white lemon
The silver-colored solid of lemon acid.
B, thermal decomposition method prepares silver powder
(1) weigh 18g polyethylene pyrrole network alkanone, 155g ascorbic acid is dissolved in 1.5L deionized water and is added 0.5L glycerol, obtain
Liquid A on earth；(2) the silver citrate 100g after weighing drying is added to stirring in the liquid A of bottom and obtains system B to dissolving；(3) by body
Be B be placed on heated 50 minutes in 200 DEG C of constant temperature system after take out, remove supernatant after being cooled to room temperature, it is heavy to obtain silver powder
It forms sediment；(4) by gained silver powder be washed with deionized water 3 times, dehydrated alcohol wash 2 times, wash it is complete 60 DEG C drying, both D50For 9.67 μm surpass
Thin silver powder.
Claims (9)
1. a kind of method for preparing silver powder with environment-friendly metal silver salt, it is characterised in that include the following steps:
Step 1: the preparation of silver citrate:
A, at room temperature, sodium citrate is dissolved in deionized water, obtains sodium citrate solution；
B, silver nitrate is dissolved in deionized water, obtains silver nitrate solution；
C, sodium citrate solution is slowly dropped in silver nitrate solution, after being added dropwise, carries out strong mixing；
D, after standing 2-h, supernatant is removed, obtains precipitating to be washed with deionized water being washed with dehydrated alcohol, washes to finish and dry
To silver citrate solid；
Step 2: thermal decomposition method prepares silver powder:
A, dispersing agent, reducing agent are dissolved in solvent, obtain liquid A on earth；
B, the silver citrate for obtaining step 1 is added to stirring in the liquid A of bottom and obtains system B to dissolving；
C, system B is placed in 180-220 DEG C of constant temperature system and stands heating 30-50min taking-up, gone after being cooled to room temperature
Supernatant obtains silver powder precipitating；
D, obtained silver powder deionized water and dehydrated alcohol are washed, washes complete drying and obtains D50In 9-12 μm of ultra-fine silver
Powder.
2. the method for preparing silver powder with environment-friendly metal silver salt as described in claim 1, it is characterised in that: described in step 1
Sodium citrate solution mass concentration is 170-235g/L, and the mass concentration of silver nitrate solution is 305-425mol/L, silver nitrate with
The mass ratio of sodium citrate is 1.73-2.4:1.
3. the method for preparing silver powder with environment-friendly metal silver salt as described in claim 1, it is characterised in that: the step of step 1
The time of dropwise addition described in C is 20-30min.
4. the method for preparing silver powder with environment-friendly metal silver salt as described in claim 1, it is characterised in that: the step of step 1
Mixing speed described in C is 370-450rpm, mixing time 40-60min.
5. the method for preparing silver powder with environment-friendly metal silver salt as described in claim 1, it is characterised in that: the step of step 1
Deionization described in D is washed 2-3 times, and dehydrated alcohol is washed 1-2 times.
6. the method for preparing silver powder with environment-friendly metal silver salt as described in claim 1, it is characterised in that: described in step 2
Dispersing agent is polyethylene pyrrole network alkanone, Macrogol 4000, polyvinyl alcohol or Tween-80.
7. the method for preparing silver powder with environment-friendly metal silver salt as described in claim 1, it is characterised in that: described in step 2
Reducing agent is ascorbic acid, formic acid or formaldehyde.
8. the method for preparing silver powder with environment-friendly metal silver salt as described in claim 1, it is characterised in that: described in step 2
Solvent is deionized water or glycerol.
9. the method for preparing silver powder with environment-friendly metal silver salt as described in claim 1, it is characterised in that: the step of step 2
The mass ratio of dispersing agent and silver citrate is 0.08-0.2:1 in system B described in B, and the mass concentration of dispersing agent is 5-10g/L,
The mass ratio of reducing agent and silver citrate is 1.15-1.6:1, and the mass concentration of reducing agent is 75-85g/L, the matter of silver citrate
Amount concentration is 65-75g/L.
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| CN114260461A (en) * | 2021-12-28 | 2022-04-01 | 成都市天甫金属粉体有限责任公司 | Multi-fold spherical silver powder and preparation method and application thereof |
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Application publication date: 20181218 |