CN106390930A - Method for preparing silver-loaded activated carbon through glycine and silver nitrate complexation - Google Patents
Method for preparing silver-loaded activated carbon through glycine and silver nitrate complexation Download PDFInfo
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- CN106390930A CN106390930A CN201611173171.XA CN201611173171A CN106390930A CN 106390930 A CN106390930 A CN 106390930A CN 201611173171 A CN201611173171 A CN 201611173171A CN 106390930 A CN106390930 A CN 106390930A
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- silver
- activated carbon
- glycine
- silver nitrate
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 159
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 96
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 72
- 239000004332 silver Substances 0.000 title claims abstract description 72
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910001961 silver nitrate Inorganic materials 0.000 title claims abstract description 32
- 239000004471 Glycine Substances 0.000 title claims abstract description 28
- 238000010668 complexation reaction Methods 0.000 title abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000001035 drying Methods 0.000 claims abstract description 26
- 150000002500 ions Chemical class 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 14
- 230000000536 complexating effect Effects 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000000197 pyrolysis Methods 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 238000007654 immersion Methods 0.000 claims description 37
- 239000007788 liquid Substances 0.000 claims description 30
- 238000002360 preparation method Methods 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 11
- 238000011068 loading method Methods 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 8
- 230000007306 turnover Effects 0.000 claims description 8
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 238000000354 decomposition reaction Methods 0.000 claims description 7
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000003610 charcoal Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- 235000004279 alanine Nutrition 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000010924 continuous production Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 claims description 2
- 238000002798 spectrophotometry method Methods 0.000 claims description 2
- 238000004448 titration Methods 0.000 claims description 2
- 239000002384 drinking water standard Substances 0.000 claims 1
- 238000009413 insulation Methods 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 238000009423 ventilation Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 19
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 230000009467 reduction Effects 0.000 abstract description 6
- 230000001954 sterilising effect Effects 0.000 abstract description 4
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract 1
- 238000001149 thermolysis Methods 0.000 abstract 1
- 206010013786 Dry skin Diseases 0.000 description 10
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 8
- 230000014759 maintenance of location Effects 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 235000013399 edible fruits Nutrition 0.000 description 5
- 238000001802 infusion Methods 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 229910001923 silver oxide Inorganic materials 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- 238000007605 air drying Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 239000012279 sodium borohydride Substances 0.000 description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 description 3
- 239000003245 coal Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 230000002070 germicidal effect Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- -1 fruit shell carbon Chemical compound 0.000 description 1
- 150000002333 glycines Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 1
- 229940071536 silver acetate Drugs 0.000 description 1
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Inorganic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Plant Pathology (AREA)
- Pest Control & Pesticides (AREA)
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- General Health & Medical Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Analytical Chemistry (AREA)
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Abstract
The invention relates to a method for preparing silver-loaded activated carbon through glycine and silver nitrate complexation. A silver nitrate and glycine complexing solution is used, then activated carbon is infiltrated, and the silver-loaded activated carbon is prepared through pyrolysis and reduction. The method comprises the following steps: firstly preparing the silver nitrate and glycine complexing solution with a mol proportion of (2 to 1.5): 1, wherein the mass concentration of Ag ions is 0.01% to 0.6%; soaking for 6 to 24 hours in the solution in which the proportion of activated carbon to the complexing solution is 0.25 to 1 Kg/liter, and then dewatering and drying at the temperature of 50 to 100 DEG C; preserving the temperature of 160 to 260 DEG C under the protection of circulating nitrogen for 0.5 to 6 hours for thermolysis; and drying after washing with clean water. The grain diameter of nano silver obtained in the invention is 10 to 60 nm; the amount of loaded silver is 0.01 to 0.45 wt%; the binding force of silver particles and the activated carbon is high, the dispersity of the silver particles is good, the technological process is short, the reaction temperature is low, the sterilization efficiency of the silver-loaded activated carbon is improved, and the using amount of silver is reduced.
Description
Technical field
The present invention relates to a kind of method of active carbon loading silver.It is by preparing silver nitrate and complexing of glycin solution, then
Infiltration activated carbon, through heat resolve and reduction, using the reaction heat of silver nitrate and glycine complexes, obtains high stability
Activated carbon surface adsorbs nano-Ag particles, for aspects such as pure water purification and sterilization.
Technical background
The invention belongs to the modified absorbent charcoal material of the nano particle silver in the field such as purification, sterilization.
Drinking water deep purification activated carbon (AC) both at home and abroad, generally based on load silver.The preparation of active carbon loading silver (AC/Ag)
Method mainly includes infusion process, doping method, electrochemical deposition method, reducing process, supercritical water infusion process etc., and industrial applications are more
Be infusion process and reducing process.
Infusion process is using film containing silver particles aqueous solution soaking AC such as silver nitrate, silver acetate, obtain after being dried having adsorbed silver from
The activated carbon of son, is then passed through intensification decomposition and obtains silver oxide, then calcines some hours at 400～500 DEG C, high using silver oxide
Temperature is decomposed and is obtained argent.Require to calcine under inert gas shielding, free air infiltration can not be to enter in calcination process and temperature-fall period,
Once there being free air infiltration to enter, the argent easily being formed can be oxidized to silver oxide again, and its end product quality is wayward.Infusion process
Preparation AC/Ag process is simple, low cost, pollution-free, silver is distributed in AC surface, is conducive to sterilization.But the load silver that the method obtains
In activated carbon, AC and the combination of silver are mainly physical absorption, and silver easily runs off it is impossible to reach persistently sterilized effect.
Reducing process is AC to be 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 NaBH4Reduction preparation AC/Ag as a example, detailed process be activated carbon activation process, long under the conditions of lucifuge when
Between be impregnated into AgNO3In solution, afterwards with distillation water washing until no silver ion detection in cleaning solution, then above-mentioned AC is impregnated
In NaBH4Long-time in solution, washing afterwards removes remaining NaBH4, it is dried for a long time in 70 DEG C of vacuum.This method can realize AC
Good combination with Argent grain.But reducing process process flow is long；Need repeatedly to wash, water consumption is big, water resource purity requirement is high；
Need the techniques such as lucifuge, vacuum, equipment requirement 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 is larger, and germicidal efficiency is not high.
Content of the invention
It is an object of the invention to provide a kind of preparation method of the active carbon loading silver with efficient, lasting bactericidal action.
The technical solution adopted for the present invention to solve the technical problems is with silver particles, complexing to occur using one kind
Reducing agent, by silver ion with complex form adsorb in the surface and micropore of activated carbon, then fast at a lower temperature
Speed reduction, decomposition, the active carbon loading silver obtain good dispersion, not easily runing off.Specific as follows：
(1) silver nitrate-complexing of glycin liquid preparation：Weigh a certain amount of silver nitrate crystal and Glycine crystals, water-soluble with distilling
Solution, obtains silver-colored ammonium nitrate complex liquid.Wherein, silver nitrate and the molar ratio of glycine are 2～1.5:1, in the aqueous solution of preparation
Ag mass of ion concentration is 0.01～0.6%.
(2) silver ion immersion, dry activated carbon：By water purification active carbon, such as fruit shell carbon, ature of coal charcoal etc., with distillation washing
Only, dry, cool.With prepare silver nitrate-complexing of glycin liquid shaken at room temperature, soak activated carbon, soak time be 6～24
Hour；During immersion, the ratio of activated carbon and complex liquid is 0.25～1Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；
Then in hot blast, such as electric drying oven with forced convection, 50～100 DEG C of dryings, to constant weight, remove water and the crystallization water.
(3) pyrolysis：After immersion is dried, activated carbon is warming up at 160-260 DEG C, and temperature retention time is little for 0.5～6
When.Using dry circulating nitrogen gas protection during thermal decomposition, may also be employed when having ready conditions decomposing ammonia protection.Using pushing away boat stove, guipure
The continuous furnaces such as formula drying oven, rotary furnace can achieve continuous production.Programming rate controls at 0.1～2 DEG C/min, it is to avoid heat
Decomposition reaction excessively acutely affects Nano Silver dispersiveness and the interface binding power with activated carbon surface.
(4) wash：By above-mentioned activated carbon pure water washing 2～4 times, wash away the reactant of remnants.In order to avoid silver granuel
Son oxidation, the baking temperature after cleaning controls at 50～120 DEG C.Silver-colored remaining quantity≤the 10ppb of the water after cleaning（Micrograms per litre),
Reach the standard of drinking water.
(5) detect：Every batch adopts sodium sulfocyanate standard liquid titration determination silver carrying amount, scanning electron microscopic observation Argent grain shape
Looks and size, and in 25 DEG C, 150 r/min, constant temperature oscillation is after 600 hours, the anti-current of the Spectrophotometric Determination of Silver that swollen with double sulphur
Lose performance, turnover rate≤20% of silver, silver carrying amount receptor 1 activity charcoal specific surface and absorption property, complex liquid silver content, soaking technology and
The impact of the parameter of thermal decomposition process, when silver carrying amount is less than the interval 0.01～0.45wt.% requiring, repeat step（2）Silver from
Son immersion, dry activated carbon and step（3）Pyrolysis are to increase silver carrying amount.
Described silver nitrate is 1.8～1.5 with the mol ratio of alanine:1.
Described Ag mass of ion concentration is 0.1～0.6%.
Described dry activated carbon heats up as 180-250 DEG C.
By silver nitrate (AgNO3) as oxidant, glycine (C2H5NO2) as complexing reducing agent, it is configured to the aqueous solution；
Solution is gradually evaporated and can form gel.This gel can react rapidly, release a large amount of gases and heat at 160～260 DEG C, can
Obtain scattered nano level superfine silver powder.Glycine (H is there occurs first during this2N-CH2- COOH) hydrolysis anti-
Should, NH occurs4 +.With the carrying out of heating, water evaporation, the NH in solution4 +And NO3 -Ion is then with NH4NO3The form analysis of crystal
Go out, finally give AgOH, Ag2O and NH4NO3The mixture of crystal.Above-mentioned mixed crystal heat further it may occur that multiple
Miscellaneous decomposition reaction, obtains Nano Silver and CO2、H2O、N2O、N2Deng gas.
When silver nitrate and glycine are 2 in molar ratio:Reaction equation when 1 is as follows：
4AgNO3+2C2H5NO2→4Ag+4CO2+5H2O+3N2O
When silver nitrate and glycine are 3 in molar ratio:Reaction equation when 2 is as follows：
6AgNO3+4C2H5NO2→6Ag+8CO2+10H2O+5N2
When silver nitrate is excessive, reaction occurs the oxide of silver, but due to exothermic heat of reaction, local temperature raises, the oxidation of silver
Decomposition product and obtain elemental silver；When reducing agent glycine is excessive further, needs oxygen to participate in reaction, or discharge ammonia
Gas.
The present invention is used for producing active carbon loading silver, has the characteristics that reaction temperature is low and efficiency high, generally at 160-260 DEG C
Between, the heat of decomposition reaction release promotes reaction to carry out.Compared with conventional dipping and thermal decomposition process, shorten technique stream
Journey, is reduced reaction temperature, avoids the occurrence of the Ag particle being caused due to pyroreaction and be combined with carbon surface loosely and easy occur
The problem of silver oxide.Compared with conventional reduction method, decrease dipping number of times, and due to complexing Ag chemical combination of the present invention
Thing decomposes generation a large amount of gases such as NH3、H2O、CO2、N2, N2O etc., makes the Ag nano particles of formation disperse, overcomes General N aBH4
The Ag particle agglomeration phenomenon of AC/Ag is prepared in reduction, improves the germicidal efficiency of active carbon loading silver, reduces silver-colored consumption.
Present invention process process is simple, easily operated, yield is high, be easy to industrialized production, have cleaning, environmental protection and
Characteristics of energy saving.Gained Nano Silver particle diameter is 10 ~ 60nm；Silver carrying amount 0.01～0.45wt.%；Argent grain and activated carbon adhesion
Height, 150r/min, vibrate in 25 DEG C of thermostatted waters, after 600 hours, turnover rate≤25% of silver；Argent grain good dispersion, sterilized effect
Rate is high.
Specific embodiment
Below by way of specific embodiment, the present invention is elaborated.
Embodiment 1
(1) silver nitrate-complexing of glycin liquid preparation：Weigh 17g silver nitrate and 5.0g glycine, with distilling water dissolves, obtain
100 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate and the molar ratio of glycine are 3:2, Ag ion matter in the aqueous solution of preparation
Amount concentration is about 0.01%.
(2) silver ion immersion, dry activated carbon：Commercially available coconut fruit shell carbon distilled water is cleaned, dries, cooled.With
Ag mass of ion concentration is about 0.01%, and molar ratio is 3:2 silver nitrate-complexing of glycin liquid shaken at room temperature, immersion activity
Charcoal, soak time is 6 hours；During immersion, the ratio of activated carbon and complex liquid is 1Kg/ liter；In ventilated environment, lucifuge ring after immersion
Border is filtered dry；In electric drying oven with forced convection, 50 DEG C of dryings, to constant weight, remove water and the crystallization water.
(3) pyrolysis：After immersion is dried, activated carbon is warming up at 160 DEG C, and temperature retention time is 6 hours.Thermal decomposition
It is dried in the circulating nitrogen gas protection tube furnace that Shi Caiyong is dried, programming rate is 2 DEG C/min.
(4) wash：By above-mentioned activated carbon pure water washing 2 times, wash away the reactant of remnants.In electric heating air blast after cleaning
Drying box, 50 DEG C of dryings are to constant weight.
(5) detect：Gained Nano Silver particle diameter is 25nm；Silver carrying amount 0.01%；Argent grain is high with activated carbon adhesion,
150r/min, vibrates in 25 DEG C of thermostatted waters, and after 600 hours, the turnover rate of silver is 12%.
Embodiment 2
(1) silver nitrate-complexing of glycin liquid preparation：Weigh 17g silver nitrate and 5.0g glycine, with distilling water dissolves, obtain 18
Rise silver-colored ammonium nitrate complex liquid.Wherein, silver nitrate and the molar ratio of glycine are 3:2, Ag mass of ion in the aqueous solution of preparation
Concentration is about 0.6%.
(2) silver ion immersion, dry activated carbon：Commercially available ature of coal charcoal distilled water is cleaned, dries, cooled.Use Ag ion
Mass concentration is about 0.6%, and molar ratio is 3:2 silver nitrate-complexing of glycin liquid shaken at room temperature, immersion activated carbon, during immersion
Between be 24 hours；During immersion, the ratio of activated carbon and complex liquid is 1Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；
In electric drying oven with forced convection, 100 DEG C of dryings, to constant weight, remove water and the crystallization water.
(3) pyrolysis：After immersion is dried, activated carbon is warming up at 260 DEG C, and temperature retention time is 0.5 hour.Heat point
Controlled at 0.1 DEG C/min using net belt type drying oven, programming rate during solution, using the circulating nitrogen gas protection being dried.
(4) wash：By above-mentioned activated carbon pure water washing 4 times, wash away the reactant of remnants.It is used in net belt type after cleaning
In drying oven, 120 DEG C of dryings are to constant weight.
(5) detect：Gained Nano Silver particle diameter is 58nm；Silver carrying amount 0.44%；Argent grain is high with activated carbon adhesion, 150r/
Min, vibrates in 25 DEG C of thermostatted waters, and after 600 hours, the turnover rate of silver is 24%.
Embodiment 3
(1) silver nitrate-complexing of glycin liquid preparation：Weigh 17g silver nitrate and 3.8g glycine, with distilling water dissolves, obtain 18
Rise silver-colored ammonium nitrate complex liquid.Wherein, silver nitrate and the molar ratio of glycine are 2:1, Ag mass of ion in the aqueous solution of preparation
Concentration is about 0.6%.
(2) silver ion immersion, dry activated carbon：Commercially available fruit shell carbon distilled water is cleaned, dries, cooled.Use Ag ion
Mass concentration is about 0.6%, and molar ratio is 2:1 silver nitrate-complexing of glycin liquid shaken at room temperature, immersion activated carbon, during immersion
Between be 12 hours；During immersion, the ratio of activated carbon and complex liquid is 0.25Kg/ liter；Filter in ventilated environment, light protected environment after immersion
Dry；In 80 DEG C of heated-air drying cylinder dryings to constant weight, remove water and the crystallization water.
(3) pyrolysis：After immersion is dried, activated carbon is warming up at 200 DEG C, and temperature retention time is 3 hours.Thermal decomposition
Shi Caiyong pushes away boat drying oven automatically, programming rate controls at 0.5 DEG C/min, using the circulating nitrogen gas protection being dried.
(4) wash：By above-mentioned activated carbon pure water washing 3 times, wash away the reactant of remnants.It is used in automatically after cleaning
Push away boat drying oven, 110 DEG C of dryings are to constant weight.
(5) detect：Gained Nano Silver particle diameter is 60nm；Silver carrying amount 0.32%；Argent grain is high with activated carbon adhesion,
150r/min, vibrates in 25 DEG C of thermostatted waters, and after 600 hours, the turnover rate of silver is 14%.
Embodiment 4
(1) silver nitrate-complexing of glycin liquid preparation：Weigh 17g silver nitrate and 4.68g glycine, with distilling water dissolves, obtain
36 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate and the molar ratio of glycine are 1.6:1, 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 distilled water is cleaned, dries, cooled.Use Ag ion
Mass concentration is about 0.3%, and molar ratio is 1.6:1 silver nitrate-complexing of glycin liquid shaken at room temperature, immersion activated carbon, soak
Time is 12 hours；During immersion, the ratio of activated carbon and complex liquid is 0.5Kg/ liter；Filter in ventilated environment, light protected environment after immersion
Dry；In 100 DEG C of heated-air drying cylinder dryings to constant weight, remove water and the crystallization water.
(3) pyrolysis：After immersion is dried, activated carbon is warming up at 220 DEG C, and temperature retention time is 3 hours.Thermal decomposition
Shi Caiyong pushes away boat drying oven automatically, programming rate controls at 0.5 DEG C/min, using the circulating nitrogen gas protection being dried.
(4) wash：By above-mentioned activated carbon pure water washing 2 times, wash away the reactant of remnants.It is used in automatically after cleaning
Push away boat drying oven, 120 DEG C of dryings are to constant weight.
(5) detect：Gained Nano Silver particle diameter is 30nm；Silver carrying amount 0.3%；Argent grain is high with activated carbon adhesion,
150r/min, vibrates in 25 DEG C of thermostatted waters, and after 600 hours, the turnover rate of silver is 14%.
Embodiment 5
(1) silver nitrate-complexing of glycin liquid preparation：Weigh 8.5g silver nitrate and 4.4g glycine, with distilling water dissolves, obtain
36 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate and the molar ratio of glycine are 1.7:1, Ag ion in the aqueous solution of preparation
Mass concentration is about 0.15%.
(2) silver ion immersion, dry activated carbon：Commercially available fruit shell carbon distilled water is cleaned, dries, cooled.Use Ag ion
Mass concentration is about 0.15%, and molar ratio is 1.7:1 silver nitrate-complexing of glycin liquid shaken at room temperature, immersion activated carbon, leaching
The bubble time is 9 hours；During immersion, the ratio of activated carbon and complex liquid is 0.25Kg/ liter；In ventilated environment, light protected environment after immersion
It is filtered dry；In 90 DEG C of heated-air drying cylinder dryings to constant weight, remove water and the crystallization water.
(3) pyrolysis：After immersion is dried, activated carbon is warming up at 200 DEG C, and temperature retention time is 2 hours.Thermal decomposition
The circulating nitrogen gas protection tube furnace that Shi Caiyong is dried, programming rate controls at 1 DEG C/min,.
(4) wash：By above-mentioned activated carbon pure water washing 2 times, wash away the reactant of remnants.With 90 DEG C of drums after cleaning
Wind drying box drying is to constant weight.
(5) detect：Gained Nano Silver particle diameter is 25nm；Silver carrying amount 0.03%；Argent grain is high with activated carbon adhesion,
150r/min, vibrates in 25 DEG C of thermostatted waters, and after 600 hours, the turnover rate of silver is 9%.
Claims (4)
1. a kind of glycine prepares the method for active carbon loading silver it is characterised in that comprising the following steps with silver nitrate complexing：
(1) silver nitrate-complexing of glycin liquid preparation：Weigh silver nitrate crystal and Glycine crystals, with distilling water dissolves, obtain
Silver-colored ammonium nitrate complex liquid, silver nitrate is 2～1.5 with the molar ratio of glycine:1, in the aqueous solution of preparation, Ag mass of ion is dense
Spend for 0.01～0.6%；
(2) silver ion immersion, dry activated carbon：Water purification active carbon is cleaned with distilled water, dry, cool down, with the nitre preparing
Sour silver-complexing of glycin liquid shaken at room temperature, immersion activated carbon, soak time is 6～24 hours；Activated carbon and complex liquid during immersion
Ratio be 0.25～1Kg/ liter；It is filtered dry in ventilation, light protected environment after immersion；Then it is dried extremely in 50～100 DEG C of hot blast
Constant weight, removing water and the crystallization water；
(3) pyrolysis：After immersion is dried, activated carbon is warming up to 160-260 DEG C, and insulation carries out heat point for 0.5～6 hour
Solution, adopts dry circulating nitrogen gas protection, or is protected using decomposing ammonia during thermal decomposition；Using push away boat stove, net belt type drying oven or
Rotary furnace continuous furnace, realizes continuous production；Programming rate controls at 0.1～2 DEG C/min；
(4) wash：By above-mentioned activated carbon pure water washing 2～4 times, wash away the reactant of remnants；In order to avoid silver particles
Oxidation, the baking temperature after cleaning controls at 50～120 DEG C；Silver-colored remaining quantity≤the 10ppb of the water after cleaning, reaches drinking water
Standard；
(5) detect：Every batch adopts sodium sulfocyanate standard liquid titration determination silver carrying amount, scanning electron microscopic observation Argent grain pattern
And size, and in 25 DEG C, 150 r/min, constant temperature oscillation, after 600 hours, is lost with the anti-current of the swollen Spectrophotometric Determination of Silver of double sulphur
Performance, turnover rate≤20%, silver carrying amount receptor 1 activity charcoal specific surface and absorption property, complex liquid silver content, soaking technology and the heat of silver
The impact of the parameter of decomposition technique, when silver carrying amount is less than the 0.01～0.45wt.% requiring, repeat step（2）Silver ion soaks
Bubble, dry activated carbon and step（3）Pyrolysis are to increase silver carrying amount.
2. glycine as claimed in claim 1 and silver nitrate complexing prepare active carbon loading silver method it is characterised in that：Described
The mol ratio of silver nitrate and alanine be 1.8～1.5:1.
3. glycine as claimed in claim 1 and silver nitrate complexing prepare active carbon loading silver method it is characterised in that：Described
Ag mass of ion concentration be 0.1～0.6%.
4. glycine as claimed in claim 1 or 2 and silver nitrate complexing prepare active carbon loading silver method it is characterised in that：
Described dry activated carbon heats up as 180-250 DEG C.
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