CN106698616B - A kind of method that citric acid reduction prepares active carbon loading silver - Google Patents
A kind of method that citric acid reduction prepares active carbon loading silver Download PDFInfo
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- CN106698616B CN106698616B CN201611173162.0A CN201611173162A CN106698616B CN 106698616 B CN106698616 B CN 106698616B CN 201611173162 A CN201611173162 A CN 201611173162A CN 106698616 B CN106698616 B CN 106698616B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
Abstract
The present invention relates to a kind of methods that citric acid reduction prepares active carbon loading silver, with silver nitrate and citric acid complex solution, then infiltrate active carbon, are made by heat resolve and reduction.First preparing molar ratio is 3.6~3:1, silver nitrate-citric acid complex liquid that Ag mass of ion concentration is 0.01~0.6%；The ratio of active carbon and complex liquid is that 0.25~1Kg/ rises immersion 6~24 hours；It is thermally decomposed under circulating nitrogen gas protection；Dry after clear water washing, gained nano silver partial size is 10 ~ 60nm；0.01~0.5wt.% of silver carrying amount.Present invention reduces process flows, reduce reaction temperature, improve the germicidal efficiency of active carbon loading silver, reduce silver consuming amount.
Description
Technical field
The present invention relates to a kind of methods of active carbon loading silver.It then is soaked by with silver nitrate and citric acid complex solution
Active carbon is seeped, obtains the work of high stability using the reaction heat of silver nitrate and citric acid complex by heat resolve and reduction
Property carbon surface adsorb nano silver, for pure water purification and sterilization etc..
Technical background
The invention belongs to the modified absorbent charcoal material of the nano particle silver in fields such as purify, sterilize.
Domestic and international drinking water deep purification active carbon (AC), usually based on load silver.The preparation of active carbon loading silver (AC/Ag)
Method mainly includes infusion process, doping method, electrochemical deposition method, reduction method, supercritical water infusion process etc., and industrial applications are more
Be infusion process and reduction method.
Infusion process be using the film containing silver particles aqueous solution soaking AC such as silver nitrate, silver acetate, adsorbed after dry silver from
Then the active carbon of son decomposes by heating and obtains silver oxide, then in 400~500 DEG C of calcining several hours, utilize silver oxide height
Temperature decomposes and obtains metallic silver.It is required that calcining under inert gas protection, there cannot be free air infiltration to enter in calcination process and temperature-fall period,
Once there is free air infiltration to enter, the metallic silver easily formed can be oxidized to silver oxide again, and end product quality is not easy to control.Infusion process
AC/Ag simple process and low cost is prepared, pollution-free, silver is distributed in the surface AC, is conducive to sterilize.But AC is mainly physics to silver
Absorption, silver are easy to be lost, cannot achieve the effect that persistently to sterilize.
Reduction method is that AC is immersed in a period of time in Ag-containing solution, then with a kind of reducing agent silver ion reduction Cheng Dan
The process of matter silver.With NaBH4For reduction preparation AC/Ag, when detailed process is that active carbon is activated, is long under the conditions of being protected from light
Between be impregnated into AgNO3In solution, it is washed with distilled water later until then impregnating above-mentioned AC without silver ion detection in cleaning solution
In NaBH4In solution for a long time, washing removes residue NaBH later4, dry for a long time in 70 DEG C of vacuum.AC may be implemented in the method
With the good combination of Argent grain.But reduction method process flow is long；It needs repeatedly to wash, water resource requires high；Use be protected from light, vacuum
Etc. techniques, equipment requirement it is high；And Argent grain is mainly distributed in the outer surface and hole of AC with reunion shape, the Argent grain ratio of load
It is larger, and germicidal efficiency is not high.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of active carbon loading silver with efficient, lasting bactericidal effect.
The technical solution adopted by the present invention to solve the technical problems is complexing to occur with silver particles using a kind of
Reducing agent, silver ion is adsorbed in the surface and micropore of active carbon with complex form, it is then fast at a lower temperature
Speed reduction is decomposed, the active carbon loading silver for obtaining good dispersion, not easily runing off.It is specific as follows:
(1) silver nitrate-citric acid complex liquid preparation: a certain amount of silver nitrate crystal and Citric acid crystal are weighed, with distillation
Water dissolution obtains silver-colored ammonium nitrate complex liquid.Wherein, the molar ratio of silver nitrate and citric acid is between 3.6~3:1, preparation
Ag mass of ion concentration is 0.01~0.6% in aqueous solution.
(2) silver ion immersion, dry activated carbon: by commercially available water purification active carbon, such as fruit shell carbon, coal quality charcoal, with distillation
Water is cleaned, dries, is cooled.With prepared silver nitrate-citric acid complex liquid shaken at room temperature, impregnate active carbon, soaking time 6
~24 hours；The ratio of active carbon and complex liquid is 0.25~1Kg/ liter when immersion；It is filtered after immersion in ventilated environment, light protected environment
It is dry；Then in hot wind, such as electric drying oven with forced convection, 40~90 DEG C of dryings to constant weight remove water and the crystallization water.
(3) pyrolysis: active carbon is warming up to 120-200 DEG C after impregnating drying, and soaking time is 0.5~6 small
When.It is protected when thermal decomposition using dry circulating nitrogen gas, can also be used when having ready conditions and decompose ammonia protection.Using pushing away boat furnace, mesh belt
The continuous furnaces such as formula drying oven or rotary furnace realize continuous production.Heating rate is controlled at 0.1~2 DEG C/min, avoids heat
Decomposition reaction excessively acutely influences nano silver dispersibility and the interface binding power with activated carbon surface.
(4) it washs: by above-mentioned active carbon with pure water washing 2~4 times, washing away remaining reactant.In order to avoid silver granuel
Son oxidation, the drying temperature after cleaning are controlled at 50~120 DEG C.Silver-colored remaining quantity≤10ppb(micrograms per litre of water after cleaning),
Reach the standard of drinking water.
(5) detect: every batch of uses sodium sulfocyanate standard solution titration determination silver carrying amount, scanning electron microscopic observation Argent grain
Morphology and size, and after 25 DEG C, 150 r/min, constant temperature oscillation 600 hours, with resisting for the swollen Spectrophotometric Determination of Silver of double sulphur
Flow and failure property, silver-colored turnover rate≤25%, silver carrying amount receptor 1 activity charcoal specific surface and absorption property, complex liquid silver content, soaking technology
Step (2) silver is repeated when silver carrying amount is lower than desired 0.01~0.50wt.% of section with the influence of the parameter of thermal decomposition process
Ion impregnates, dry activated carbon and step (3) pyrolysis are to increase silver carrying amount.
The molar ratio of the silver nitrate and citric acid is 3.5~3:1.
The Ag mass of ion concentration is 0.1~0.6%.
Dry activated carbon is warming up to 140-180 DEG C in the step (3).
By silver nitrate (AgNO3) as oxidant, citric acid (C6H8O7) as complexing reducing agent, it is configured to aqueous solution.Lemon
Lemon acid and Ag ion form stable chelate, and solution, which gradually evaporates, can form gel, be adsorbed on the micropore surface of active carbon.This
Kind gel can react rapidly at 120~200 DEG C, release bulk gas and heat, the nano level superfine metallic silver that can be dispersed
Powder.Citric acid (CH2COOH-C(OH)-COOHCH2COOH fusing point) only has 153 DEG C, and burning is formed rapidly under an oxygen-containing atmosphere
CO2And H2O, but in the case where anoxic, it is reacted with nitrate anion and silver ion, obtains nano silver and CO2、H2O、N2O、N2Equal gas
Body.
Reaction equation when silver nitrate and citric acid are in molar ratio 18:5 is as follows:
18AgNO3+ 5C6H8O7→18Ag+30CO2+20H2O+9N2O
Reaction equation when silver nitrate and citric acid are in molar ratio 3:1 is as follows:
6AgNO3+2C6H8O7→6Ag+12CO2+8H2O+N2
When silver nitrate excess, reaction will appear the oxide of silver；When reducing agent citric acid is further excessive, oxygen is needed
Gas participates in reaction, or releases ammonia.
The present invention has the characteristics that reaction temperature is low and high-efficient, usually at 120-200 DEG C for producing active carbon loading silver
Between, the heat of decomposition reaction release promotes reaction to carry out.Compared with conventional dipping and thermal decomposition process, technique stream is shortened
Journey, reduce reaction temperature, avoid the occurrence of as pyroreaction and caused by Ag particle loosely and easily occur in conjunction with carbon surface
The problem of silver oxide.Compared with conventional reduction method, reduce dipping time, and due to complexing Ag chemical combination of the present invention
Object, which decomposes, generates bulk gas such as H2O、CO2、N2, N2O etc. disperses the Ag nano particles to be formed, overcomes General N aBH4Reduction
The Ag particle agglomeration phenomenon for preparing AC/Ag improves the germicidal efficiency of active carbon loading silver, reduces silver-colored dosage.
Present invention process process is simple, easily operated, yield is high, easy to industrialized production, have it is clean, environmentally protective and
Characteristics of energy saving.Gained nano silver partial size is 10 ~ 60nm；0.01~0.5wt.% of silver carrying amount；Argent grain and active carbon binding force are high,
150r/min vibrates in 25 DEG C of thermostatted waters, after 600 hours, silver-colored turnover rate≤25%；Argent grain good dispersion, germicidal efficiency
It is high.
Specific embodiment
It elaborates below by way of specific embodiment to the present invention.
Embodiment 1
(1) silver nitrate-citric acid complex liquid preparation: 17g silver nitrate and 6.4g citric acid are weighed, is dissolved with distilled water, is obtained
Obtain 100 liters of silver-colored ammonium nitrate complex liquids.Wherein, the molar ratio of silver nitrate and citric acid is 3:1, Ag ion in the aqueous solution of preparation
Mass concentration is about 0.01%.
(2) silver ion immersion, dry activated carbon: commercially available coconut fruit shell carbon is cleaned with distilled water, dries, cool.With
Ag mass of ion concentration is about 0.01%, and molar ratio is active for silver nitrate-citric acid complex liquid shaken at room temperature of 3:1, immersion
Charcoal, soaking time are 6 hours；The ratio of active carbon and complex liquid is 1Kg/ liter when immersion；After immersion in ventilated environment, be protected from light ring
Border is filtered dry；In electric drying oven with forced convection, 40 DEG C of dryings to constant weight remove water and the crystallization water.
(3) pyrolysis: active carbon is warming up at 120 DEG C after impregnating drying, and soaking time is 6 hours.Thermal decomposition
Dry in Shi Caiyong dry circulating nitrogen gas protection tube furnace, heating rate is 2 DEG C/min.
(4) it washs: by above-mentioned active carbon with pure water washing 2 times, washing away remaining reactant.In electric heating drum after cleaning
Wind drying box, 50 DEG C of dryings to constant weight.
(5) detect: gained nano silver partial size is 10nm；Silver carrying amount 0.01%；Argent grain and active carbon binding force are high,
150r/min vibrates in 25 DEG C of thermostatted waters, and after 600 hours, silver-colored turnover rate is 9%.
Embodiment 2
(1) silver nitrate-citric acid complex liquid preparation: 17g silver nitrate and 6.4g citric acid are weighed, is dissolved with distilled water, is obtained
Obtain 18 liters of silver-colored ammonium nitrate complex liquids.Wherein, the molar ratio of silver nitrate and citric acid is 3:1, Ag ion in the aqueous solution of preparation
Mass concentration is about 0.6%.
(2) silver ion immersion, dry activated carbon: commercially available coal quality charcoal is cleaned with distilled water, dries, cool.With Ag ion
The silver nitrate that mass concentration is about 0.6%-citric acid complex liquid shaken at room temperature impregnates active carbon, and soaking time is 24 hours；Leaching
The ratio of active carbon and complex liquid is 1Kg/ liter when bubble；It is filtered dry after immersion in ventilated environment, light protected environment；In electric heating forced air drying
Case, 90 DEG C of dryings to constant weight remove water and the crystallization water.
(3) pyrolysis: active carbon is warming up at 200 DEG C after impregnating drying, and soaking time is 0.5 hour.Heat point
It is protected at 0.1 DEG C/min using dry circulating nitrogen gas when solution using net belt type drying oven, heating rate control.
(4) it washs: by above-mentioned active carbon with pure water washing 4 times, washing away remaining reactant.Mesh belt is used in after cleaning
In formula drying oven, 120 DEG C of dryings to constant weight.
(5) detect: gained nano silver partial size is 58nm；Silver carrying amount 0.49%；Argent grain and active carbon binding force are high,
150r/min vibrates in 25 DEG C of thermostatted waters, and after 600 hours, silver-colored turnover rate is 23%.
Embodiment 3
(1) silver nitrate-citric acid complex liquid preparation: 17g silver nitrate and 6.0g citric acid are weighed, is dissolved with distilled water, is obtained
Obtain 18 liters of silver-colored ammonium nitrate complex liquids.Wherein, the molar ratio of silver nitrate and citric acid is 18:5.5, in the aqueous solution of preparation Ag from
Protonatomic mass concentration is about 0.6%.
(2) silver ion immersion, dry activated carbon: commercially available fruit shell carbon is cleaned with distilled water, dries, cool.With Ag ion
Mass concentration is about 0.6%, silver nitrate-citric acid complex liquid shaken at room temperature, immersion active carbon of the molar ratio for 18:5.5, leaching
Steeping the time is 12 hours；The ratio of active carbon and complex liquid is 0.25Kg/ liter when immersion；After immersion in ventilated environment, be protected from light ring
Border is filtered dry；It is dry to constant weight in 80 DEG C of heated-air drying cylinders, remove water and the crystallization water.
(3) pyrolysis: active carbon is warming up at 180 DEG C after impregnating drying, and soaking time is 3 hours.Thermal decomposition
Shi Caiyong pushes away boat drying oven, heating rate control at 0.5 DEG C/min automatically, is protected using dry circulating nitrogen gas.
(4) it washs: by above-mentioned active carbon with pure water washing 3 times, washing away remaining reactant.It is used in after cleaning automatic
Push away boat drying oven, 110 DEG C of dryings to constant weight.
(5) detect: gained nano silver partial size is 50nm；Silver carrying amount 0.3%；Argent grain and active carbon binding force are high,
150r/min vibrates in 25 DEG C of thermostatted waters, and after 600 hours, silver-colored turnover rate is 12%.
Embodiment 4
(1) silver nitrate-citric acid complex liquid preparation: 17g silver nitrate and 6.4g citric acid are weighed, is dissolved with distilled water, is obtained
Obtain 36 liters of silver-colored ammonium nitrate complex liquids.Wherein, the molar ratio of silver nitrate and citric acid is 3:1, Ag ion in the aqueous solution of preparation
Mass concentration is about 0.3%.
(2) silver ion immersion, dry activated carbon: commercially available fruit shell carbon is cleaned with distilled water, dries, cool.With Ag ion
Mass concentration is about 0.3%, and silver nitrate-citric acid complex liquid shaken at room temperature that molar ratio is 3:1 impregnates active carbon, when immersion
Between be 12 hours；The ratio of active carbon and complex liquid is 0.5Kg/ liter when immersion；It is filtered after immersion in ventilated environment, light protected environment
It is dry；It is dry to constant weight in 100 DEG C of heated-air drying cylinders, remove water and the crystallization water.
(3) pyrolysis: active carbon is warming up at 180 DEG C after impregnating drying, and soaking time is 3 hours.Thermal decomposition
Shi Caiyong pushes away boat drying oven, heating rate control at 0.5 DEG C/min automatically, is protected using dry circulating nitrogen gas.
(4) it washs: by above-mentioned active carbon with pure water washing 2 times, washing away remaining reactant.It is used in after cleaning automatic
Push away boat drying oven, 120 DEG C of dryings to constant weight.
(5) detect: gained nano silver partial size is 30nm；Silver carrying amount 0.3%；Argent grain and active carbon binding force are high,
150r/min vibrates in 25 DEG C of thermostatted waters, and after 600 hours, silver-colored turnover rate is 14%.
Embodiment 5
(1) silver nitrate-citric acid complex liquid preparation: weighing 8.5g silver nitrate and 3.2g citric acid, dissolved with distilled water,
Obtain 36 liters of silver-colored ammonium nitrate complex liquids.Wherein, the molar ratio of silver nitrate and citric acid is 3:1, in the aqueous solution of preparation Ag from
Protonatomic mass concentration is about 0.15%.
(2) silver ion immersion, dry activated carbon: commercially available fruit shell carbon is cleaned with distilled water, dries, cool.With Ag ion
Mass concentration is about 0.15%, and silver nitrate-citric acid complex liquid shaken at room temperature, immersion active carbon of the molar ratio for 3:1 impregnate
Time is 9 hours；The ratio of active carbon and complex liquid is 0.25Kg/ liter when immersion；It is filtered after immersion in ventilated environment, light protected environment
It is dry；It is dry to constant weight in 80 DEG C of heated-air drying cylinders, remove water and the crystallization water.
(3) pyrolysis: active carbon is warming up at 160 DEG C after impregnating drying, and soaking time is 2 hours.Thermal decomposition
Shi Caiyong dry circulating nitrogen gas protects tube furnace, and heating rate is controlled at 1 DEG C/min.
(4) it washs: by above-mentioned active carbon with pure water washing 2 times, washing away remaining reactant.With 80 DEG C of drums after cleaning
Wind drying box is dry to constant weight.
(5) detect: gained nano silver partial size is 30nm；Silver carrying amount 0.03%；Argent grain and active carbon binding force are high,
150r/min vibrates in 25 DEG C of thermostatted waters, and after 600 hours, silver-colored turnover rate is 10%.
Claims (4)
1. a kind of method that citric acid reduction prepares active carbon loading silver, it is characterised in that the following steps are included:
(1) silver nitrate-citric acid complex liquid preparation: silver nitrate crystal and Citric acid crystal are weighed, is dissolved with distilled water, is obtained
The molar ratio of silver nitrate-citric acid complex liquid, silver nitrate and citric acid is 3.6~3:1, Ag ion matter in the aqueous solution of preparation
Measuring concentration is 0.01~0.6%；
(2) silver ion immersion, dry activated carbon: water purification active carbon distilled water is cleaned, drying, cooling, with prepared nitre
Sour silver-citric acid complex liquid shaken at room temperature impregnates active carbon, and soaking time is 6~24 hours；Active carbon and complex liquid when immersion
Ratio be 0.25~1Kg/ liter；It is filtered dry after immersion in ventilation, light protected environment；Then it dries in 40~90 DEG C of hot winds to perseverance
Weight removes water and the crystallization water；
(3) pyrolysis: active carbon is warming up to 120-200 DEG C after impregnating drying, the heat preservation heat point of progress in 0.5~6 hour
Solution is protected using dry circulating nitrogen gas when thermal decomposition, or using decomposing ammonia protection；Using push away boat furnace, net belt type drying oven or
Rotary furnace realizes continuous production；Heating rate is controlled at 0.1~2 DEG C/min, and pyrolysis is avoided excessively acutely to influence
Nano silver dispersibility and the interface binding power with activated carbon surface；
(4) it washs: by step (3) products therefrom with pure water washing 2~4 times, washing away remaining reactant；In order to avoid silver
Particle oxidation, the drying temperature after cleaning are controlled at 50~120 DEG C；Silver-colored remaining quantity≤10ppb of water after cleaning, reaches and drinks
The standard of water；
(5) detect: every batch of uses sodium sulfocyanate standard solution titration determination silver carrying amount, scanning electron microscopic observation Argent grain pattern
And size, and after 25 DEG C, 150 r/min, constant temperature oscillation 600 hours, it is lost with the anti-current of dithizone spectrophotometry measurement silver
Performance, silver-colored turnover rate≤25%, silver carrying amount receptor 1 activity charcoal specific surface and absorption property, complex liquid silver content, soaking technology and heat
The influence of the parameter of decomposition technique repeats the immersion of step (2) silver ion, dry activated carbon when silver carrying amount is lower than 0.01wt.%
With step (3) pyrolysis to increase silver carrying amount.
2. the method that citric acid reduction as described in claim 1 prepares active carbon loading silver, it is characterised in that the silver nitrate
Molar ratio with citric acid is 3.5~3:1.
3. the method that citric acid reduction as described in claim 1 prepares active carbon loading silver, it is characterised in that: the Ag ion
Mass concentration is 0.1~0.6%.
4. the method that citric acid reduction as described in claim 1 prepares active carbon loading silver, it is characterised in that: institute in step (3)
Dry activated carbon is warming up to 140-180 DEG C after the immersion stated is dry.
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| CN102908990A (en) * | 2012-10-15 | 2013-02-06 | 南京正森环保科技有限公司 | Preparation method of silver-loaded activated carbon |
| CN105431230A (en) * | 2013-08-01 | 2016-03-23 | 南洋理工大学 | Method for forming noble metal nanoparticles on a support |
| WO2016151454A1 (en) * | 2015-03-20 | 2016-09-29 | Basf Corporation | Pt and/or pd egg-shell catalyst and use thereof |
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| KR20120021385A (en) * | 2010-07-29 | 2012-03-09 | 한국과학기술원 | Method for one-pot synthesizing of catalyst for fuel cell having nano structure shape |
| CN102553579A (en) * | 2011-05-27 | 2012-07-11 | 中国科学院福建物质结构研究所 | Preparation method of high-dispersity supported nano metal catalyst |
| CN102908990A (en) * | 2012-10-15 | 2013-02-06 | 南京正森环保科技有限公司 | Preparation method of silver-loaded activated carbon |
| CN105431230A (en) * | 2013-08-01 | 2016-03-23 | 南洋理工大学 | Method for forming noble metal nanoparticles on a support |
| WO2016151454A1 (en) * | 2015-03-20 | 2016-09-29 | Basf Corporation | Pt and/or pd egg-shell catalyst and use thereof |
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