CN109772264A - A kind of preparation method of flue gas desulfurization activated coke - Google Patents
A kind of preparation method of flue gas desulfurization activated coke Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of flue gas desulfurization activated coke, belong to technical field of absorbent.Chemical bronze plating liquid can produce reducibility gas carbon monoxide and hydrogen in a heated condition in the present invention, copper ion oxidation is precipitated on iron powder surface the reducibility gas slowly released, make activated coke with sulfuric acid reaction, not avoid being pierced, improves the sulfur capacity of activated charcoal；Activated coke of the invention passes through dual activation, after making hydrolysis of organic matter degradation in part in activated coke under the effect of the composite activating agent of zinc chloride and copper chloride first, forming oligomer, reaction dehydration, it can promote intermediate product to be condensed, aromatisation, form the microstructure of class graphite, and generate porous system, improve activated coke sulfur capacity, prepared green powder is also a kind of catalytic oxidant, it can be sulfur trioxide in conjunction with Oxygen Catalytic Oxidation hydrogen sulfide, sulfur dioxide in air etc., to make the desulfurization effect of activated coke improve, have broad application prospects.
Description
Technical field
The invention discloses a kind of preparation methods of flue gas desulfurization activated coke, belong to technical field of absorbent.
Background technique
The characteristics of activated coke is a kind of particulate matter with adsorbent and catalyst dual property, its active charcoal,
Absorption and catalytic performance are good, and stable chemical performance can regenerate, reusable.Meanwhile it overcomes active carbon price again
High, the disadvantages of mechanical strength is low, easy crushing.In ambient water, gas pollution control field, active carbon is replaced with activated coke, is had more
Actual meaning.
Activated coke is the Special adsorbent that pore structure is reasonable, specific surface area is moderate, compressive resistance is high, is mainly used for doing
Method desulfurization, and iterative regenerable in actual application.Activated coke type is few at present, by partial size difference can be divided into 5mm,
It is several can be also divided into column coke, spherical coke, capsule formed coke etc. from shape by 9mm etc..Determine activated coke performance superiority and inferiority because being known as
Raw material and processing, raw material proportioning, moulding process, charing, activating process and equipment.
The desulfurization principle of activated coke be made using the characterization of adsorption and catalysis characteristics of activated coke sulfur dioxide in flue gas,
Vapor occurs hair with oxygen and answers, and generates sulfuric acid, is adsorbed on the surface of activated coke.When a certain proportion of different material of addition or change
When learning drug, adjustable pore size and pore-size distribution, thus the performance of left and right activated coke.
How the Sulfur capacity and intensity of activated coke are improved, and the production cost for reducing activated coke is the emphasis studied at present and difficulty
Point.
Existing activated coke is a kind of particulate matter with adsorption function using lignite as primary raw material.Existing activated coke
Preparation mainly divide following steps: first by pretreated lignite destructive distillation, semicoke is made, then utilize semicoke, coking coal and
Binder mixing, and through the Viability coke of overactivation.Lignite is a kind of low-quality coal, has many advantages, such as abundance, inexpensive, simultaneously
Have the shortcomings that moisture and high, not viscous, the easy nature of fugitive constituent again and is not suitable for storage and transportation.It is existing using lignite as the preparation side of raw material
Method, because lignite lumpiness is not of uniform size, it is necessary to break process is carried out, to carry out acidleach processing and destructive distillation to it, and lignite partial size
It is selected activated coke performance is had a major impact, a large amount of ash contents in lignite, river organic matter shrinkage stress has in retort process
Difference causes non-uniform contraction, cracks activated coke, intensity decline, and makes that the production cost increases.Activated coke is answered at present
When for flue gas desulfurization, it is low that there is also Sulfur capacity, is oxidized easily, the defect of desulfurization effect difference.
Therefore, invent that a kind of desulfurization effect is good and the flue gas desulfurization activated coke that is not easy to be oxidized is to technical field of absorbent
With positive effect.
Summary of the invention
Present invention mainly solves the technical issues of, for current activated coke be applied to flue gas desulfurization when, Sulfur capacity is low, be easy quilt
Oxidation, the defect of desulfurization effect difference provide a kind of preparation method of flue gas desulfurization activated coke.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of flue gas desulfurization activated coke the preparation method comprises the following steps:
Coke powder, coal tar, spare green powder will be activated, copper-clad iron nano powder, distilled water mixing are put into single lead screw ex truding briquetting machine
It is extruded into striped blocks, drying is placed in activation furnace, under nitrogen protection, is passed through vapor, is heated to 700~750 DEG C, is protected
After 45~50min of temperature activation, cooled to room temperature obtains flue gas desulfurization activated coke；
Copper-clad iron process for preparing nm powder are as follows:
(1) by mass fraction be 40% copper ammon solution, coke, glyoxalic acid, sodium tartrate, polyurethane and sodium carbonate be put into from
Disperse in sub- water, 20~25min is dispersed with the revolving speed of 3000~3500r/min in high speed disperser, obtains chemical bronze plating liquid；
(2) 400~500mL chemical bronze plating liquid is put into beaker, is heated to 90~100 DEG C, into beaker launch 40~
50g iron powder, 40~50min of insulation reaction are separated by filtration to obtain filter residue, and filter residue is placed in the baking oven that set temperature is 70~80 DEG C
In, it is put into ammonolysis craft hydrogen furnace after dry 2~3h, continues to restore dry 40~50min, obtains copper-clad iron nano powder；
Green powder the preparation method comprises the following steps:
4~5g vanadic anhydride, 15~20mL isobutanol, 8~10mL benzyl alcohol are placed in three mouthfuls with condensation reflux unit
In flask, 80~90 DEG C are heated to, after being condensed back 12~13h, 10~12mL mass fraction is added into three-necked flask
For 80% phosphoric acid solution, continue 6~7h of condensing reflux, obtain light green product, light green product is put into Muffle furnace, is added
Heat is warming up to 400~450 DEG C, calcines 4~5h, obtains green powder；
Activate coke powder the preparation method comprises the following steps:
(1) the lignite powder for being 2~3mm of partial size by brown coal crushing, is placed in high-temperature closed furnace, under nitrogen protection heat temperature raising
To 350~500 DEG C, isothermal holding for a period of time, is continuously heating to 950~1000 DEG C, after 30~35min of isothermal holding, by institute
It obtains naturally dry after product is cleaned with petroleum ether and obtains lignite semi-coke powder；
(2) by isometric ZnCl than being 4.5mol/L by concentration2The CuCl that solution and concentration are 0.5mol/L2Solution mixing is made
For composite activating agent, lignite semi-coke powder is placed in 10~15min of impregnation in composite activating agent, impregnation is subsequently isolated out
Lignite semi-coke powder is placed in high temperature process furnances, under nitrogen protection, with 500~550 DEG C of 2~3h of temperature-activated, is activated
Coke powder.
Flue gas desulfurization activated coke each component, according to parts by weight, including 100~120 parts of coke powder of activation, 30 coal tar~
35 parts, 10~12 parts of green powder, 18~20 parts of copper-clad iron nano powder, 20~25 parts of distilled water.
Flue gas desulfurization can be controlled further with heat preservation activation temperature in activated coke preparation process at 720~725 DEG C.
It is 40% that chemical bronze plating liquid each component in copper-clad iron process for preparing nm powder includes mass fraction according to parts by weight
40~50 parts of copper ammon solution, 20~30 parts of coke, 15~20 parts of glyoxalic acid, 60~70 parts of sodium tartrate, polyurethane 40~50
Part, 20~25 parts of sodium carbonate be put into 400~500 parts of deionized water.
The controllable reduction drying temperature of the ammonolysis craft hydrogen furnace is 80~85 DEG C.
Can further improve reflux temperature when being condensed back after addition phosphoric acid solution in the specific preparation step of green powder is
100~105 DEG C.
Isothermal holding, Ying Zhizhi lignite powder are changed under the conditions of 350~500 DEG C of temperature in activation coke powder preparation method
Colloid substance, then heat up.
Lignite semi-coke powder in mass ratio 1: 5 is placed in impregnation in composite activating agent in activation coke powder preparation method.
The beneficial effects of the present invention are:
(1) by high temperature pyrolysis after the present invention crushes lignite, impurity oil is washed away with petroleum ether, obtains lignite semi-coke powder, it will be brown
Coal semi-coke powder ZnCl2Solution and CuCl2After the multiple and activator impregnation of solution mixing, high-temperature activation obtains activation coke powder,
Using vanadic anhydride and phosphoric acid solution as raw material, addition isobutanol, benzyl alcohol are obtained as solvent by being condensed back, calcining
Green powder disperses the substances such as polyurethane, copper sulphate, coke and sodium tartrate in deionized water, obtains chemical bronze plating liquid,
Finally reduced iron powder is disposably put into the chemical bronze plating liquid of heating, insulation reaction obtains sediment, after drying precipitate
It is put into ammonolysis craft hydrogen furnace and continues to restore drying, obtain copper-clad iron nano powder, it finally will activation coke powder, coal tar, spare
Green powder, copper-clad iron nano powder, distilled water mixing are extruded into striped blocks, and vapor activates again under nitrogen protection, obtains flue gas
Activated coke for desulfuration, the present invention in chemical bronze plating liquid can produce reducibility gas carbon monoxide and hydrogen in a heated condition, delay
Copper ion oxidation is precipitated on iron powder surface the reducibility gas that slow release is released, and obtains copper-clad iron nano powder, copper-clad iron nano powder
On the one hand it can be used as antioxidant, protection activity coke is not oxidized, lengthens the service life of activated coke, need not in the short time
Regeneration replacement, another aspect copper-clad iron nano powder can produce copper oxide and iron oxide after being oxidized, and iron oxide, which can be used as, to be contained
The catalytic oxidant of sulphur compound, and the sulfur capacity of activated charcoal is improved, copper oxide can make the hydroxyl hydroformylation in activated coke, make
Activated coke with sulfuric acid reaction, does not avoid being pierced, and improves the sulfur capacity of activated charcoal；
(2) activated coke of the invention passes through dual activation, makes to live under the effect of the composite activating agent of zinc chloride and copper chloride first
Property coke in part hydrolysis of organic matter degradation, formed oligomer, reaction dehydration after, can promote intermediate product is condensed, aromatisation,
The microstructure of class graphite is formed, and generates porous system, the zinc of high concentration, copper ion abundant residues are in virtue in acid condition
In structure organic matter, complex compound is formed, is adsorbed in the micropore of class graphite microcrystalline structure, zinc, copper ion can be with catalysis oxidation sulphur
Compound, after vapor re-activation, the pore structure of activated coke is become larger, and improves activated coke sulfur capacity, prepared
Green powder is also a kind of catalytic oxidant, can be three oxygen in conjunction with Oxygen Catalytic Oxidation hydrogen sulfide, sulfur dioxide in air etc.
Change sulphur to have broad application prospects so that the desulfurization effect of activated coke be made to improve.
Specific embodiment
The lignite powder for being 2~3mm of partial size by brown coal crushing, is placed in high-temperature closed furnace, and heating rises under nitrogen protection
For temperature to 350~500 DEG C, isothermal holding is changed into colloid substance up to lignite powder, is continuously heating to 950~1000 DEG C, heat preservation
After handling 30~35min, naturally dry obtains lignite semi-coke powder after products therefrom is cleaned with petroleum ether；By isometric than will be dense
Degree is the ZnCl of 4.5mol/L2The CuCl that solution and concentration are 0.5mol/L2Solution, which mixes, is used as composite activating agent, and in mass ratio 1
: 5, lignite semi-coke powder is placed in 10~15min of impregnation in composite activating agent, the lignite semi-coke of impregnation is subsequently isolated out
Powder is placed in high temperature process furnances, under nitrogen protection, with 500~550 DEG C of 2~3h of temperature-activated, obtains activation coke powder；By 4
~5g vanadic anhydride, 15~20mL isobutanol, 8~10mL benzyl alcohol are placed in the three-necked flask with condensation reflux unit,
80~90 DEG C are heated to, after being condensed back 12~13h, it is 80% that 10~12mL mass fraction is added into three-necked flask
Phosphoric acid solution continues 6~7h of condensing reflux, obtains light green product, and light green product is put into Muffle furnace, is heated to
400~450 DEG C, 4~5h is calcined, green powder is obtained；According to parts by weight, the cuprammonium for being 40% by 40~50 parts of mass fractions
Solution, 20~30 parts of coke, 15~20 parts of glyoxalic acids, 60~70 parts of sodium tartrates, 40~50 parts of polyurethane and 20~25 parts of carbon
Sour sodium, which is put into 400~500 parts of deionized waters, to be dispersed, and disperses 20 in high speed disperser with the revolving speed of 3000~3500r/min
~25min, obtains chemical bronze plating liquid；400~500mL chemical bronze plating liquid is put into beaker, is heated to 90~100 DEG C,
40~50g iron powder is launched into beaker, 40~50min of insulation reaction is separated by filtration to obtain filter residue, and filter residue is placed in set temperature
To be put into ammonolysis craft hydrogen furnace after dry 2~3h in 70~80 DEG C of baking ovens, continues to restore dry 40~50min, obtain copper-clad
Iron nano powder；According to parts by weight, by 100~120 parts of activation coke powders, 30~35 parts of coal tar, 10~12 parts of spare greens
Powder, 18~20 parts of copper-clad iron nano powders, 20~25 parts of distilled water mixing, is put into single lead screw ex truding briquetting machine and is extruded into striped blocks, dry
It is placed in activation furnace, under nitrogen protection, is passed through vapor, be heated to 700~750 DEG C, 45~50min of heat preservation activation
Afterwards, cooled to room temperature obtains flue gas desulfurization activated coke.
Activate the preparation of coke powder: the lignite powder for being partial size 2mm by brown coal crushing is placed in high-temperature closed furnace, in nitrogen
350 DEG C are heated under protection, isothermal holding is changed into colloid substance up to lignite powder, is continuously heating to 950 DEG C, heat preservation
After handling 30min, naturally dry obtains lignite semi-coke powder after products therefrom is cleaned with petroleum ether；
By isometric ZnCl than being 4.5mol/L by concentration2The CuCl that solution and concentration are 0.5mol/L2Solution mixing conduct
Lignite semi-coke powder is placed in impregnation 10min in composite activating agent, is subsequently isolated out and soaks by composite activating agent, in mass ratio 1: 5
The lignite semi-coke powder of stain processing is placed in high temperature process furnances, under nitrogen protection, with 500 DEG C of temperature-activated 2h, is activated
Coke powder.
The preparation of green powder: 4g vanadic anhydride, 15mL isobutanol, 8mL benzyl alcohol are placed in condensing reflux dress
In the three-necked flask set, 80 DEG C are heated to, after being condensed back 12h, it is 80% that 10mL mass fraction is added into three-necked flask
Phosphoric acid solution, continue be condensed back 6h, obtain light green product, light green product be put into Muffle furnace, is heated to
400 DEG C, 4h is calcined, green powder is obtained.
The preparation of copper-clad iron nano powder: according to parts by weight, copper ammon solution, 20 parts of cokes by 40 parts of mass fractions for 40%
Charcoal, 15 parts of glyoxalic acids, 60 parts of sodium tartrates, 40 parts of polyurethane and 20 parts of sodium carbonate, which are put into 400 parts of deionized waters, to be dispersed, in height
20min is dispersed with the revolving speed of 3000r/min in fast dispersion machine, obtains chemical bronze plating liquid；
400mL chemical bronze plating liquid is put into beaker, is heated to 90 DEG C, 40g iron powder, insulation reaction are launched into beaker
40min is separated by filtration to obtain filter residue, filter residue is placed in the baking oven that set temperature is 70 DEG C, is put into ammonolysis craft hydrogen after dry 2h
Steam stove continues to restore dry 40min, obtains copper-clad iron nano powder.
The preparation of flue gas desulfurization activated coke: according to parts by weight, by 100 parts of activation coke powders, 30 parts of coal tar, 10 parts it is standby
Green powder, 18 parts of copper-clad iron nano powders, 20 parts of distilled water mixing, is put into single lead screw ex truding briquetting machine and is extruded into striped blocks, dry
It is placed in activation furnace, under nitrogen protection, is passed through vapor, be heated to 700 DEG C, it is naturally cold after keeping the temperature activation 45min
But to room temperature, flue gas desulfurization activated coke is obtained.
Activate the preparation of coke powder: the lignite powder for being partial size 2mm by brown coal crushing is placed in high-temperature closed furnace, in nitrogen
400 DEG C are heated under protection, isothermal holding is changed into colloid substance up to lignite powder, is continuously heating to 970 DEG C, heat preservation
After handling 32min, naturally dry obtains lignite semi-coke powder after products therefrom is cleaned with petroleum ether；
By isometric ZnCl than being 4.5mol/L by concentration2The CuCl that solution and concentration are 0.5mol/L2Solution mixing conduct
Lignite semi-coke powder is placed in impregnation 12min in composite activating agent, is subsequently isolated out and soaks by composite activating agent, in mass ratio 1: 5
The lignite semi-coke powder of stain processing is placed in high temperature process furnances, under nitrogen protection, with 520 DEG C of temperature-activated 2.5h, is lived
Change coke powder.
The preparation of green powder: 4g vanadic anhydride, 17mL isobutanol, 9mL benzyl alcohol are placed in condensing reflux dress
In the three-necked flask set, 85 DEG C are heated to, after being condensed back 12.5h, 11mL mass fraction, which is added, into three-necked flask is
80% phosphoric acid solution continues to be condensed back 6.5h, obtains light green product, light green product is put into Muffle furnace, and heating rises
Temperature calcines 4.5h, obtains green powder to 425 DEG C.
The preparation of copper-clad iron nano powder: according to parts by weight, copper ammon solution, 25 parts of cokes by 45 parts of mass fractions for 40%
Charcoal, 17 parts of glyoxalic acids, 65 parts of sodium tartrates, 45 parts of polyurethane and 22 parts of sodium carbonate, which are put into 450 parts of deionized waters, to be dispersed, in height
22min is dispersed with the revolving speed of 3200r/min in fast dispersion machine, obtains chemical bronze plating liquid；
450mL chemical bronze plating liquid is put into beaker, is heated to 95 DEG C, 45g iron powder, insulation reaction are launched into beaker
45min is separated by filtration to obtain filter residue, filter residue is placed in the baking oven that set temperature is 75 DEG C, is put into ammonolysis craft after dry 2.5h
Hydrogen furnace continues to restore dry 45min, obtains copper-clad iron nano powder.
The preparation of flue gas desulfurization activated coke: according to parts by weight, by 110 parts of activation coke powders, 32 parts of coal tar, 11 parts it is standby
Green powder, 19 parts of copper-clad iron nano powders, 22 parts of distilled water mixing, is put into single lead screw ex truding briquetting machine and is extruded into striped blocks, dry
It is placed in activation furnace, under nitrogen protection, is passed through vapor, be heated to 720 DEG C, it is naturally cold after keeping the temperature activation 47min
But to room temperature, flue gas desulfurization activated coke is obtained.
Activate the preparation of coke powder: the lignite powder for being partial size 3mm by brown coal crushing is placed in high-temperature closed furnace, in nitrogen
500 DEG C are heated under protection, isothermal holding is changed into colloid substance up to lignite powder, is continuously heating to 1000 DEG C, protects
After temperature processing 35min, naturally dry obtains lignite semi-coke powder after products therefrom is cleaned with petroleum ether；
By isometric ZnCl than being 4.5mol/L by concentration2The CuCl that solution and concentration are 0.5mol/L2Solution mixing conduct
Lignite semi-coke powder is placed in impregnation 15min in composite activating agent, is subsequently isolated out and soaks by composite activating agent, in mass ratio 1: 5
The lignite semi-coke powder of stain processing is placed in high temperature process furnances, under nitrogen protection, with 550 DEG C of temperature-activated 3h, is activated
Coke powder.
The preparation of green powder: 5g vanadic anhydride, 20mL isobutanol, 10mL benzyl alcohol are placed in condensing reflux dress
In the three-necked flask set, 90 DEG C are heated to, after being condensed back 13h, it is 80% that 12mL mass fraction is added into three-necked flask
Phosphoric acid solution, continue be condensed back 7h, obtain light green product, light green product be put into Muffle furnace, is heated to
450 DEG C, 5h is calcined, green powder is obtained.
The preparation of copper-clad iron nano powder: according to parts by weight, copper ammon solution, 30 parts of cokes by 50 parts of mass fractions for 40%
Charcoal, 20 parts of glyoxalic acids, 70 parts of sodium tartrates, 50 parts of polyurethane and 25 parts of sodium carbonate, which are put into 500 parts of deionized waters, to be dispersed, in height
25min is dispersed with the revolving speed of 3500r/min in fast dispersion machine, obtains chemical bronze plating liquid；
500mL chemical bronze plating liquid is put into beaker, is heated to 100 DEG C, 50g iron powder, insulation reaction are launched into beaker
50min is separated by filtration to obtain filter residue, filter residue is placed in the baking oven that set temperature is 80 DEG C, is put into ammonolysis craft hydrogen after dry 3h
Steam stove continues to restore dry 50min, obtains copper-clad iron nano powder.
The preparation of flue gas desulfurization activated coke: according to parts by weight, by 120 parts of activation coke powders, 35 parts of coal tar, 12 parts it is standby
Green powder, 20 parts of copper-clad iron nano powders, 25 parts of distilled water mixing, is put into single lead screw ex truding briquetting machine and is extruded into striped blocks, dry
It is placed in activation furnace, under nitrogen protection, is passed through vapor, be heated to 750 DEG C, it is naturally cold after keeping the temperature activation 50min
But to room temperature, flue gas desulfurization activated coke is obtained.
Comparative example 1: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking copper-clad iron nano powder.
Comparative example 2: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking green powder.
Comparative example 3: the flue gas desulfurization activated coke of Changzhou company production.
Saturation sulfur capacity test is detected by MT/T998-2006 standard.
7702.4 standard detection of GB/T is pressed in bulk specific weight test.
GB/T7702.7-2008 standard detection is pressed in iodine number test.
Inoxidizability test: the flue gas desulfurization in example 1~3 and comparative example is placed in the cigarette for needing desulfurization with activated coke
In gas, after a period of use, see whether to be oxidized, if need replacing.
Table 1 flue gas desulfurization activated coke performance measurement result
| Test item | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| It is saturated sulfur capacity (mg/g) | 180 | 181 | 182 | 120 | 130 | 142 |
| Bulk specific weight | 520 | 540 | 545 | 420 | 435 | 460 |
| Iodine number (mg/g) | 593 | 595 | 599 | 415 | 423 | 456 |
| Desulfuration efficiency (%) | 98 | 98 | 99 | 85 | 84 | 90 |
| Inoxidizability | Not oxidized, no replacement is required | Not oxidized, no replacement is required | Not oxidized, no replacement is required | It is oxidized, needs replacing | It is oxidized, needs replacing | Slight oxidation does not need to replace |
It is saturated sulfur capacity height according to above-mentioned detection data flue gas desulfurization of the invention activated coke, bulk specific weight is moderate, resists
Oxidisability is good, long service life, and desulfurization effect is good, and desulfuration efficiency does not need after a period of use up to 99%, good in oxidation resistance
Replacement, has broad application prospects.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of flue gas desulfurization activated coke, it is characterised in that specific preparation step are as follows:
Coke powder, coal tar, spare green powder will be activated, copper-clad iron nano powder, distilled water mixing are put into single lead screw ex truding briquetting machine
It is extruded into striped blocks, drying is placed in activation furnace, under nitrogen protection, is passed through vapor, is heated to 700~750 DEG C, is protected
After 45~50min of temperature activation, cooled to room temperature obtains flue gas desulfurization activated coke；
The specific preparation step of copper-clad iron nano powder are as follows:
(1) by mass fraction be 40% copper ammon solution, coke, glyoxalic acid, sodium tartrate, polyurethane and sodium carbonate be put into from
Disperse in sub- water, 20~25min is dispersed with the revolving speed of 3000~3500r/min in high speed disperser, obtains chemical bronze plating liquid；
(2) 400~500mL chemical bronze plating liquid is put into beaker, is heated to 90~100 DEG C, into beaker launch 40~
50g iron powder, 40~50min of insulation reaction are separated by filtration to obtain filter residue, and filter residue is placed in the baking oven that set temperature is 70~80 DEG C
In, it is put into ammonolysis craft hydrogen furnace after dry 2~3h, continues to restore dry 40~50min, obtains copper-clad iron nano powder；
The specific preparation step of the green powder are as follows:
4~5g vanadic anhydride, 15~20mL isobutanol, 8~10mL benzyl alcohol are placed in three mouthfuls with condensation reflux unit
In flask, 80~90 DEG C are heated to, after being condensed back 12~13h, 10~12mL mass fraction is added into three-necked flask
For 80% phosphoric acid solution, continue 6~7h of condensing reflux, obtain light green product, light green product is put into Muffle furnace, is added
Heat is warming up to 400~450 DEG C, calcines 4~5h, obtains green powder；
The specific preparation step of activation coke powder are as follows:
(1) the lignite powder for being 2~3mm of partial size by brown coal crushing, is placed in high-temperature closed furnace, under nitrogen protection heat temperature raising
To 350~500 DEG C, isothermal holding for a period of time, is continuously heating to 950~1000 DEG C, after 30~35min of isothermal holding, by institute
It obtains naturally dry after product is cleaned with petroleum ether and obtains lignite semi-coke powder；
(2) by isometric ZnCl than being 4.5mol/L by concentration2The CuCl that solution and concentration are 0.5mol/L2Solution mixing is made
For composite activating agent, lignite semi-coke powder is placed in 10~15min of impregnation in composite activating agent, impregnation is subsequently isolated out
Lignite semi-coke powder is placed in high temperature process furnances, under nitrogen protection, with 500~550 DEG C of 2~3h of temperature-activated, is activated
Coke powder.
2. a kind of preparation method of flue gas desulfurization activated coke according to claim 1, it is characterised in that: the flue gas
Activated coke for desulfuration each component, according to parts by weight, including activation 100~120 parts of coke powder, 30 coal tar~35 part, green flour
10~12 parts of end, 18~20 parts of copper-clad iron nano powder, 20~25 parts of distilled water.
3. a kind of preparation method of flue gas desulfurization activated coke according to claim 1, it is characterised in that: the flue gas
Activation temperature is kept the temperature in activated coke for desulfuration preparation process can further control at 720~725 DEG C.
4. a kind of preparation method of flue gas desulfurization activated coke according to claim 1, it is characterised in that: the copper-clad
Chemical bronze plating liquid each component in the specific preparation step of iron nano powder (1) includes the cuprammonium that mass fraction is 40% according to parts by weight
40~50 parts of solution, 20~30 parts of coke, 15~20 parts of glyoxalic acid, 60~70 parts of sodium tartrate, 40~50 parts of polyurethane, carbonic acid
20~25 parts of sodium are put into 400~500 parts of deionized water.
5. a kind of preparation method of flue gas desulfurization activated coke according to claim 1, it is characterised in that: the ammonia point
Solving the controllable reduction drying temperature of hydrogen furnace is 80~85 DEG C.
6. a kind of preparation method of flue gas desulfurization activated coke according to claim 1, it is characterised in that: the green
Can further improve reflux temperature when being condensed back after addition phosphoric acid solution in the specific preparation step of powder is 100~105 DEG C.
7. a kind of preparation method of flue gas desulfurization activated coke according to claim 1, it is characterised in that: the activation
Isothermal holding, Ying Zhizhi lignite powder are changed into glue under the conditions of 350~500 DEG C of temperature in the specific preparation step of coke powder (1)
Substance, then heat up.
8. a kind of preparation method of flue gas desulfurization activated coke according to claim 1, it is characterised in that: the activation
Lignite semi-coke powder in mass ratio 1: 5 is placed in impregnation in composite activating agent in the specific preparation step of coke powder (2).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607407A (en) * | 2020-06-15 | 2020-09-01 | 云南中翼鼎东投资集团生物科技开发有限公司 | Lignite mineral source soil conditioner and preparation method thereof |
| CN115779859A (en) * | 2022-11-30 | 2023-03-14 | 黑龙江省建筑材料工业规划设计研究院 | Magnetic adsorbent, preparation method thereof and treatment method of oily sewage |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607407A (en) * | 2020-06-15 | 2020-09-01 | 云南中翼鼎东投资集团生物科技开发有限公司 | Lignite mineral source soil conditioner and preparation method thereof |
| CN115779859A (en) * | 2022-11-30 | 2023-03-14 | 黑龙江省建筑材料工业规划设计研究院 | Magnetic adsorbent, preparation method thereof and treatment method of oily sewage |
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Application publication date: 20190521 |