CN109759025A - A kind of preparation method of use in waste water treatment adsorbent - Google Patents
A kind of preparation method of use in waste water treatment adsorbent Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of use in waste water treatment adsorbent, belong to technical field of waste water processing.The present invention handles flyash acidleach, flyash can be significantly increased to the adsorption capacity of dyestuff, using chitosan composite fly ash, Powder ash adsorption is on chitosan surface in recombination process, change the electrical property of fine coal gray surface, and waste water from dyestuff is usually electronegative, flyash is thus set to have adsorption ability, enhance the treatment effect to waste water, the strontium carbonate extracted from celestine is doped in flyash, strontium carbonate can make titanium dioxide distortion of lattice, titanium dioxide forbidden band energy gap is set to narrow, make titanium dioxide that the light of more wide area wavelength can be absorbed, the medium body of the bacterium solution containing natto is prepared with soybean powder, wherein it is rich in gamma-polyglutamic acid, the space that gamma-polyglutamic acid reserves after being biodegradable provides space for the growth of subsequent microorganism, increase the amount of active microorganism on adsorbent, to improve adsorbent The biofilm amount of microorganism.
Description
Technical field
The invention discloses a kind of preparation methods of use in waste water treatment adsorbent, belong to technical field of waste water processing.
Background technique
With the development of economy, the chemical plant of various regions is more and more, the hot spot for being treated as all circles' concern of trade effluent,
Traditional plating, process hides, Treatment of Metal Surface, printing and dyeing, petrochemical industry and wastewater discharge containing other organic pollutants increasingly increases
Add.
Dyestuff is a class of pollutant common in waste water, mostlys come from weaving, leather, papermaking, rubber, plastics, makeup
In the production process of the industrial circles such as product, pharmacy and food.While being widely used in promotion economic development of dyestuff, also generates
A large amount of waste water from dyestuff is discharged into environment water, results in the pollution of natural water.Therefore, to the improvement of waste water from dyestuff oneself
One of research hotspot as water treatment field.In early days, common dye waste water treatment method mainly includes flocculent precipitation, changes
Learn oxidizing process, membrane separation process and biological degradation method.Although these methods can reduce dyestuff in waste water from dyestuff to a certain extent
Content, but still there is miscellaneous defects, for example, because adsorption rate is low, processing cost is excessively high and to waste water from dyestuff at
The bad adaptability of variation is divided in addition to be also possible to generate during processing toxic the result is that the removal effect to dyestuff is not good enough
Harmful side product or a large amount of sludge, so as to cause secondary pollution.
The dyeing process of textile can generate a large amount of waste water, and a certain amount of dyestuff is contained in these waste water.Dyeing waste water
Water quality it is complicated, high organic content, coloration is deep, and biological degradability is low, and processing method usually has absorption method, flocculence, oxygen
Change reduction method, biochemical method and membrane processing method etc..Absorption method is to utilize unique physical structure or chemical structure possessed by adsorbent,
By the effect of Van der Waals force and chemical bond, realization effectively removes pollutant in water body.Absorption method is used for organic pollutant
The processing of waste water, have many advantages, such as it is applied widely, do not generate secondary pollution, therefore widely answered in the treatment of waste water
With.The conventional active charcoal of adsorbent, coal ash, zeolite, diatomite etc..Activated carbon adsorptive capacity is strong and wide adaptation range, in recent years
In the wastewater treatment of a variety of pollution sources is paid attention to and applied, but active carbon price is high, service life is short, regeneration
This height.
Existing research report cationic starch and cation PVA can be used as dyestuff and dyeing waste water high-efficient decolorizing flocculant.
However the cationic starch and cation PVA with certain degree of substitution can meet water dissolution, therefore cannot be directly used as fixed bed suction
Attached dose of processing dyestuff and dyeing waste water.Even if making it lose water solubility by cross-linking reaction, but can still exist and meet water-swellable ask
Topic, using separately as adsorbent also can frequently result in fluid resistance larger problem when liquid passes through fixed bed.
Therefore, invent a kind of adsorption rate it is high, it is to fuel waste water removal effect high, organic pollutant can be explained
Use in waste water treatment adsorbent has positive effect to technical field of waste water processing.
Summary of the invention
Present invention mainly solves the technical issues of, for use in waste water treatment adsorbent act on it is single, adsorption rate is low, to dyestuff
Waste water removal effect is poor, cannot provide a kind of use in waste water treatment adsorbent to the defect that organic pollutant is degraded
Preparation method.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of use in waste water treatment adsorbent the preparation method comprises the following steps: agar, Bacillus natto powder, wheat bran, soybean powder is taken to be placed in fermentor,
Under the conditions of 40~45 DEG C, heat-preservation fermentation obtains medium body, will alkalize deacetylated flocculant and gel powder mixing is put into and is equipped with
In the fermentation ware of medium body, control fermentation biofilm temperature is 30~33 DEG C, and the fermentation biofilm time is 10~15 days, obtains waste water
Adsorbent is used in processing；
Alkalize deacetylated flocculant the preparation method comprises the following steps:
(1) flyash, celestine, coke are mixed, is placed in Muffle furnace, be heated to 400 DEG C~500 DEG C, roast 3~4h
High-temperature activation powder is obtained, according to parts by weight, 20~30 parts of high-temperature activation powder and 4~5 portions of mixing carburization agents are put into 80~100
In the hot water of 60~100 DEG C of part, wherein it is 5 ︰ 1 mixing system that mixing carburization agent is ammonium hydrogen carbonate and Strontia hydrate in mass ratio
It is standby to form, 2~3h is stood after stirring, removes upper liquid, collects lower sediment thing；
(2) above-mentioned lower sediment thing, phenol, furfural, sodium carbonate are mixed and are fitted into reaction kettle, be heated to 50~55 DEG C,
10~12h of insulation reaction obtains phenolic aldehyde gel, is aged 10~12h, obtains the gel of doping strontium carbonate, then be placed in cold in dry ice
Dry 2~3h is lyophilized, obtains aeroge, aeroge is put into retort, is carbonized in argon atmosphere, carbonization temperature is controlled
It is 300~350 DEG C, carbonization time is 20~25min, obtains activating fly ash containing strontium carbonate；
(3) above-mentioned activating fly ash containing strontium carbonate is separated by filtration to obtain acidleach with after 40~45min of sulfuric acid solution impregnation
Acidleach activating fly ash is then that 5 ︰ 1 are mixed with shrimp shell meal by activating fly ash in mass ratio, and being put into mass fraction is 30%
4~5h of impregnation in sodium hydroxide solution obtains the deacetylated flocculant that alkalizes；
Gel powder the preparation method comprises the following steps:
(1) addition 40~50mL dehydrated alcohol and the wooden nano-cellulose of 2~3g into ultrasonic disperse instrument, ultrasonic disperse 4~
6min obtains cellulose suspension, and cellulose suspension is placed in the conical flask with blender, with dropping funel with 1~
18~20mL butyl titanate is added into conical flask for the drop rate of 3mL/min, while starting blender, with 400~500r/
The revolving speed of min starts 10~15min of stirring and obtains presoma；
(2) glacial acetic acid that addition 20~25mL mass fraction is 98% in Xiang Shangshu presoma, 20~30mL silicon dioxide gel,
1~2h is stirred, complex sol is obtained, still aging 2~3 days, obtains dry colloidal sol, it is 60~70 that dry colloidal sol, which is placed in set temperature,
DEG C baking oven in, dry 10~12h obtains gel piece, and gel piece is put into 30~35min of grinding in mortar, 200 meshes is crossed and obtains
To gel powder.
Each ingredient in medium body, according to parts by weight, including 4~5 parts of agar, 2~4 parts of Bacillus natto powder, wheat bran 5~7
Part, 20~25 parts of soybean powder.
Soybean powder is made by cooked ground 200 mesh of soya bean.
Deacetylated flocculant and the gel powder mixing mass ratio of alkalizing are 1 ︰ 5.
Flyash, celestine, coke mixing mass ratio are 10 ︰, 4 ︰ 1 in the preparation method of deacetylated flocculant that alkalizes.
Lower sediment thing, phenol, furfural, sodium carbonate mixing mass ratio are 7 ︰ in the preparation method of deacetylated flocculant that alkalizes
8 ︰, 10 ︰ 1.
Sulfuric acid solution mass fraction is 80% in the preparation method of deacetylated flocculant that alkalizes, sodium hydroxide solution quality point
Number is 30%.
Ultrasonic disperse control supersonic frequency is 40~45kHz in the preparation method of gel powder.
The mass fraction of glacial acetic acid is 98% in the preparation method of gel powder.
The beneficial effects of the present invention are:
(1) present invention obtains high-temperature activation powder with reductive coke and calcination activation using flyash and celestine as raw material, then will be high
Temperature activation powder Hot water immersion, addition mixing carburization agent make its carbonization, and standing sedimentation collects lower sediment thing, by above-mentioned precipitating
Object, phenol, furfural, sodium carbonate mixing, insulation reaction obtain phenolic aldehyde gel under the alkalization catalytic action of sodium carbonate, and process is old
It is dried after change and carbonizes to obtain the activating fly ash containing strontium carbonate, then pass through acidleach processing, then mix with shrimp shell meal and be placed in alkali
Make shrimp shell meal dipping deacetylated in liquid, obtain the deacetylated flocculant that alkalizes, metatitanic acid is added in wooden nano-cellulose suspension
In ethyl ester, presoma is obtained, acetic acid, silicon dioxide gel are added dropwise into presoma, stirs to get complex sol, it is old by standing
Change, dry, grinding obtain gel powder, finally prepare medium body by raw material of soybean powder, the deacetylated flocculant that will alkalize is placed in
It ferments in medium body biofilm, obtains use in waste water treatment adsorbent, the present invention handles flyash acidleach, can significantly increase powder
Coal ash is to the adsorption capacity of dyestuff, and percent of decolourization is 96% or more, because of aluminium oxide, iron oxide, oxygen in high concentration strong acid and flyash
Change the reactive metal oxides such as calcium, generating sulfate, chloride of iron and aluminium etc. has stronger adsorption bleaching and cohesion
Inorganic salts its internal cavity has also on the other hand been got through by acidification, specific surface area is increased, at subsequent Re-boostering test
Reason one side alkaline matter can destroy the rigid shell on fly ash grain surface, make vitreous surface solable matter and alkaline oxygen
Compound reaction generates gelatinous mass, improves the flocculation activity of adsorbent, on the other hand can be deacetylated by chitin in shrimp shell meal
The chitosan of active hydroxyl and amino is generated, flyash itself is in alkalinity, is formed to iron hydroxide and alumine hydroxide colloid
Favorably, in addition, polysilicon acid Large molecule active dyestuff contains a large amount of active group, and contain a large amount of hydroxyl and amino in chitosan, this
A little active groups can in chitosan hydroxyl and amino covalent bond formed by chemical reaction, this contains chitosan in adsorbent
Amount plays very crucial effect for processing reactive dye, and using chitosan composite fly ash, flyash is inhaled in recombination process
It is attached to chitosan surface, changes the electrical property of fine coal gray surface, and waste water from dyestuff is usually electronegative, thus makes flyash
Not only there is adsorption ability, but also there is charge neutrality ability, the treatment effect to waste water is enhanced, with the compound fine coal of chitosan
After ash, the surface of compound is more uneven, and chitosan is partially retained in fine coal gray surface or even some enters powder
The pore interior of coal ash, fine coal gray surface are increased exponentially in loose webs structure specific surface area, and surface can enhance, and hydrophily increases
By force, and flyash plays the role of flocculation aid, is conducive to the increase and sedimentation of wadding body, and treated waste water is when shorter
It is interior to reach clarification, there is stronger adsorption bridging and net to catch ability, can make insoluble compound and fine particle that can also be adsorbed；
(2) primary attachment material of the invention is strontium carbonate activating fly ash, the complex sol of titanium dioxide and nano-cellulose
As organic pollutants assistant degradation agent, there is high-specific surface area by the flyash of acidleach and alkali process, to micro heavy
Metallic element and certain organic matters have very strong adsorption capacity, and receptor of the nano-cellulose as electronics is easy to receive dioxy
Change the light induced electron that titanium generates and improve the concentration of hydroxyl radical free radical to effectively inhibit the compound of light induced electron and hole,
Accelerate the progress of photocatalytic degradation, the strontium carbonate that the present invention is extracted from celestine is doped in flyash, and strontium carbonate can make
Titanium dioxide distortion of lattice makes titanium dioxide forbidden band energy gap narrow, and generates red shift, makes titanium dioxide that more wide area wavelength can be absorbed
Light, in addition strontium ion can absorb the luminous energy of higher energy, passes to titanium dioxide, help Titanium dioxide absorption luminous energy so that
Stronger catalytic activity is shown under visible light in titanium dioxide, and also the bacterium solution containing natto is prepared with soybean powder in the present invention
Medium body, wherein being rich in gamma-polyglutamic acid, it is poly- that gamma-polyglutamic acid can be complexed to obtain with ionizable metal salt in water pollutant γ-
Glutamate makes adsorbent have many advantages, such as biodegradability, good biocompatibility, high-moisture-retention, and gamma-polyglutamic acid is certainly
The physiological property of rich carboxyl and amino and microorganism is very much like in the polypeptide structure and strand of body, easily with micro- life
Object symbiosis, the space that gamma-polyglutamic acid reserves after being biodegradable provide space for the growth of subsequent microorganism, increase adsorbent
The amount of upper active microorganism improves the organic contamination of use in waste water treatment adsorbent to improve the biofilm amount of adsorbent microorganism
Object degradation capability, has a extensive future.
Specific embodiment
In mass ratio it is that 10 ︰, 4 ︰ 1 is mixed by flyash, celestine, coke, is placed in Muffle furnace, is heated to 400 DEG C
~500 DEG C, 3~4h of roasting obtains high-temperature activation powder, and according to parts by weight, 20~30 parts of high-temperature activation powder and 4~5 parts are mixed
Carburization agent is put into 80~100 parts 60~100 DEG C of hot water, wherein mixing carburization agent is that ammonium hydrogen carbonate and Strontia hydrate are pressed
Mass ratio is that 5 ︰ 1 are mixed with, and 2~3h is stood after stirring, removes upper liquid, collects lower sediment thing；By above-mentioned lower layer
Sediment, phenol, furfural, sodium carbonate are that 7 ︰, 8 ︰, 10 ︰ 1 mixing is fitted into reaction kettle in mass ratio, are heated to 50~55 DEG C,
10~12h of insulation reaction obtains phenolic aldehyde gel, is aged 10~12h, obtains the gel of doping strontium carbonate, then be placed in cold in dry ice
Dry 2~3h is lyophilized, obtains aeroge, aeroge is put into retort, is carbonized in argon atmosphere, carbonization temperature is controlled
It is 300~350 DEG C, carbonization time is 20~25min, obtains activating fly ash containing strontium carbonate；Powder is activated containing strontium carbonate by above-mentioned
After 40~45min of sulfuric acid solution impregnation that coal ash mass fraction is 80%, it is separated by filtration to obtain acidleach activating fly ash,
In mass ratio it is then that 5 ︰ 1 are mixed with shrimp shell meal by acidleach activating fly ash, is put into the sodium hydroxide solution that mass fraction is 30%
Middle 4~5h of impregnation obtains the deacetylated flocculant that alkalizes, spare；40~50mL dehydrated alcohol is added into ultrasonic disperse instrument
With the wooden nano-cellulose of 2~3g, control supersonic frequency is 40~45kHz, 4~6min of ultrasonic disperse, obtains cellulose suspension
Cellulose suspension is placed in the conical flask with blender by liquid, with dropping funel with the drop rate of 1~3mL/min to
18~20mL butyl titanate is added in conical flask, while starting blender, stirring 10 is started with the revolving speed of 400~500r/min
~15min obtains presoma；The glacial acetic acid that 20~25mL mass fraction is 98%, 20~30mL bis- are added into above-mentioned presoma
Silica sol stirs 1~2h, obtains complex sol, still aging 2~3 days, obtain dry colloidal sol, dry colloidal sol is placed in setting
Temperature is in 60~70 DEG C of baking oven, and dry 10~12h obtains gel piece, by gel piece be put into grinding 30 in mortar~
35min crosses 200 meshes and obtains gel powder；Cooked ground 200 mesh of soya bean is collected, obtains soybean powder, in parts by weight
Meter, takes 4~5 parts of agar, 2~4 parts of Bacillus natto powder, 5~7 parts of wheat bran, 20~25 parts of soybean powders to be placed in fermentor, 40~45
Under the conditions of DEG C, heat-preservation fermentation obtains medium body, is in mass ratio 1 ︰ 5, by the deacetylated flocculant of spare alkalization and above-mentioned gel
Powder mixing is put into the fermentation ware equipped with medium body, and control fermentation biofilm temperature is 30~33 DEG C, and the fermentation biofilm time is 10
~15 days, obtain use in waste water treatment adsorbent.
Example 1
It alkalizes the preparation of deacetylated flocculant:
In mass ratio it is that 10 ︰, 4 ︰ 1 is mixed by flyash, celestine, coke, is placed in Muffle furnace, is heated to 400 DEG C, roasting
It burns 3h and obtains high-temperature activation powder, according to parts by weight, 20 parts of high-temperature activation powder and 4 portions of mixing carburization agents are put into 80 parts 60 DEG C
In hot water, wherein it is that 5 ︰ 1 are mixed with that mixing carburization agent is ammonium hydrogen carbonate and Strontia hydrate in mass ratio, after stirring
2h is stood, upper liquid is removed, collects lower sediment thing；
In mass ratio it is that 7 ︰, 8 ︰, 10 ︰ 1 mixing is fitted into reaction kettle by above-mentioned lower sediment thing, phenol, furfural, sodium carbonate, heats
50 DEG C, insulation reaction 10h are warming up to, phenolic aldehyde gel is obtained, is aged 10h, obtains the gel of doping strontium carbonate, then be placed in dry ice
It is freeze-dried 2h, aeroge is obtained, aeroge is put into retort, carbonized in argon atmosphere, controls carbonization temperature
It is 300 DEG C, carbonization time 20min obtains activating fly ash containing strontium carbonate；
After the sulfuric acid solution impregnation 40min for being 80% by the above-mentioned mass fraction of activating fly ash containing strontium carbonate, it is separated by filtration
Acidleach activating fly ash is obtained, is in mass ratio then that 5 ︰ 1 are mixed with shrimp shell meal by acidleach activating fly ash, is put into mass fraction
For impregnation 4h in 30% sodium hydroxide solution, the deacetylated flocculant that alkalizes is obtained.
The preparation of gel powder:
40mL dehydrated alcohol and the wooden nano-cellulose of 2g are added into ultrasonic disperse instrument, control supersonic frequency is 40kHz, ultrasound
Disperse 4min, obtain cellulose suspension, cellulose suspension be placed in the conical flask with blender, with dropping funel with
18mL butyl titanate is added into conical flask for the drop rate of 1mL/min, while starting blender, with the revolving speed of 400r/min
Start stirring 10min and obtains presoma；
The glacial acetic acid that 20mL mass fraction is 98% is added into above-mentioned presoma, 20mL silicon dioxide gel stirs 1h, obtains
Complex sol still aging 2 days, obtains dry colloidal sol, dry colloidal sol is placed in the baking oven that set temperature is 60 DEG C, and dry 10h is obtained
To gel piece, gel piece is put into mortar and grinds 30min, crossed 200 meshes and obtain gel powder.
The preparation of use in waste water treatment adsorbent:
Cooked ground 200 mesh of soya bean is collected, soybean powder is obtained, according to parts by weight, takes 4 parts of agar, 2 parts of Bacillus nattos
Powder, 5 parts of wheat bran, 20 parts of soybean powders are placed in fermentor, and under the conditions of 40 DEG C, heat-preservation fermentation obtains medium body, in mass ratio
For 1 ︰ 5, the deacetylated flocculant of spare alkalization and above-mentioned gel powder are mixed and are put into the fermentation ware equipped with medium body, control hair
Ferment biofilm temperature is 30 DEG C, and the fermentation biofilm time is 10 days, obtains use in waste water treatment adsorbent.
Example 2
It alkalizes the preparation of deacetylated flocculant:
In mass ratio it is that 10 ︰, 4 ︰ 1 is mixed by flyash, celestine, coke, is placed in Muffle furnace, is heated to 450 DEG C, roasting
It burns 3.5h and obtains high-temperature activation powder, according to parts by weight, 20~30 parts of high-temperature activation powder and 4 portions of mixing carburization agents are put into 90 parts
In 80 DEG C of hot water, wherein it is that 5 ︰ 1 are mixed with that mixing carburization agent is ammonium hydrogen carbonate and Strontia hydrate in mass ratio,
2.5h is stood after stirring, removes upper liquid, collects lower sediment thing；
In mass ratio it is that 7 ︰, 8 ︰, 10 ︰ 1 mixing is fitted into reaction kettle by above-mentioned lower sediment thing, phenol, furfural, sodium carbonate, heats
52 DEG C, insulation reaction 11h are warming up to, phenolic aldehyde gel is obtained, ageing 11 obtains the gel of doping strontium carbonate, then is placed in dry ice
It is freeze-dried 2.5h, aeroge is obtained, aeroge is put into retort, carbonized in argon atmosphere, control charing temperature
Degree is 320 DEG C, and carbonization time 22min obtains activating fly ash containing strontium carbonate；
After the sulfuric acid solution impregnation 42min for being 80% by the above-mentioned mass fraction of activating fly ash containing strontium carbonate, it is separated by filtration
Acidleach activating fly ash is obtained, is in mass ratio then that 5 ︰ 1 are mixed with shrimp shell meal by acidleach activating fly ash, is put into mass fraction
For impregnation 4.5h in 30% sodium hydroxide solution, the deacetylated flocculant that alkalizes is obtained.
The preparation of gel powder:
42mL dehydrated alcohol and the wooden nano-cellulose of 2g are added into ultrasonic disperse instrument, control supersonic frequency is 42kHz, ultrasound
Disperse 5min, obtain cellulose suspension, cellulose suspension be placed in the conical flask with blender, with dropping funel with
19mL butyl titanate is added into conical flask for the drop rate of 2mL/min, while starting blender, with the revolving speed of 450r/min
Start stirring 12min and obtains presoma；
The glacial acetic acid that 22mL mass fraction is 98% is added into above-mentioned presoma, 25mL silicon dioxide gel stirs 1.5h, obtains
To complex sol, still aging 2 days, dry colloidal sol is obtained, dry colloidal sol is placed in the baking oven that set temperature is 65 DEG C, dry 11h,
Gel piece is obtained, gel piece is put into mortar and grinds 32min, 200 meshes is crossed and obtains gel powder.
The preparation of use in waste water treatment adsorbent:
Cooked ground 200 mesh of soya bean is collected, soybean powder is obtained, according to parts by weight, takes 4 parts of agar, 3 parts of Bacillus nattos
Powder, 6 parts of wheat bran, 22 parts of soybean powders are placed in fermentor, and under the conditions of 42 DEG C, heat-preservation fermentation obtains medium body, in mass ratio
For 1 ︰ 5, the deacetylated flocculant of spare alkalization and above-mentioned gel powder are mixed and are put into the fermentation ware equipped with medium body, control hair
Ferment biofilm temperature is 32 DEG C, and the fermentation biofilm time is 12 days, obtains use in waste water treatment adsorbent.
Example 3
It alkalizes the preparation of deacetylated flocculant:
In mass ratio it is that 10 ︰, 4 ︰ 1 is mixed by flyash, celestine, coke, is placed in Muffle furnace, is heated to 500 DEG C, roasting
It burns 4h and obtains high-temperature activation powder, according to parts by weight, 30 parts of high-temperature activation powder and 5 portions of mixing carburization agents are put into 100 parts 100 DEG C
Hot water in, wherein mixing carburization agent be ammonium hydrogen carbonate and Strontia hydrate is that 5 ︰ 1 are mixed in mass ratio, stirring
After stand 3h, remove upper liquid, collect lower sediment thing；
In mass ratio it is that 7 ︰, 8 ︰, 10 ︰ 1 mixing is fitted into reaction kettle by above-mentioned lower sediment thing, phenol, furfural, sodium carbonate, heats
55 DEG C, insulation reaction 12h are warming up to, phenolic aldehyde gel is obtained, is aged 12h, obtains the gel of doping strontium carbonate, then be placed in dry ice
It is freeze-dried 3h, aeroge is obtained, aeroge is put into retort, carbonized in argon atmosphere, controls carbonization temperature
It is 350 DEG C, carbonization time 25min obtains activating fly ash containing strontium carbonate；
After the sulfuric acid solution impregnation 45min for being 80% by the above-mentioned mass fraction of activating fly ash containing strontium carbonate, it is separated by filtration
Acidleach activating fly ash is obtained, is in mass ratio then that 5 ︰ 1 are mixed with shrimp shell meal by acidleach activating fly ash, is put into mass fraction
For impregnation 5h in 30% sodium hydroxide solution, the deacetylated flocculant that alkalizes is obtained.
The preparation of gel powder:
50mL dehydrated alcohol and the wooden nano-cellulose of 3g are added into ultrasonic disperse instrument, control supersonic frequency is 45kHz, ultrasound
Disperse 6min, obtain cellulose suspension, cellulose suspension be placed in the conical flask with blender, with dropping funel with
20mL butyl titanate is added into conical flask for the drop rate of 3mL/min, while starting blender, with the revolving speed of 500r/min
Start stirring 15min and obtains presoma；
The glacial acetic acid that 25mL mass fraction is 98% is added into above-mentioned presoma, 30mL silicon dioxide gel stirs 2h, obtains
Complex sol still aging 3 days, obtains dry colloidal sol, dry colloidal sol is placed in the baking oven that set temperature is 70 DEG C, and dry 12h is obtained
To gel piece, gel piece is put into mortar and grinds 35min, crossed 200 meshes and obtain gel powder.
The preparation of use in waste water treatment adsorbent:
Cooked ground 200 mesh of soya bean is collected, soybean powder is obtained, according to parts by weight, takes 5 parts of agar, 4 parts of Bacillus nattos
Powder, 7 parts of wheat bran, 25 parts of soybean powders are placed in fermentor, and under the conditions of 45 DEG C, heat-preservation fermentation obtains medium body, in mass ratio
For 1 ︰ 5, the deacetylated flocculant of spare alkalization and above-mentioned gel powder are mixed and are put into the fermentation ware equipped with medium body, control hair
Ferment biofilm temperature is 33 DEG C, and the fermentation biofilm time is 15 days, obtains use in waste water treatment adsorbent.
Comparative example 1: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking the deacetylated flocculant of alkalization.
Comparative example 2: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking gel powder.
Comparative example 3: the use in waste water treatment adsorbent of Wuxi company production.
Organic pollutant degradation is tested: taking the naphthalene solution of the adsorbent and 10ml in 10mg example 1~3 and comparative example
It is added in the sample bottle of 10ml with luxuriant and rich with fragrance solution, pyrene solution, alpha naphthol solution (Tu Shui ratio is about 1: 1000), it is small that 24 is vibrated at 25 DEG C
When (absorption reaches balance).The concentration range of naphthalene: 0.02~5 μ g/mL, luxuriant and rich with fragrance concentration range: 0.001~1.0 μ g/mL, pyrene
Concentration range: 0.001~0.1 μ g/mL, the concentration range of alpha naphthol: 0.02~17 μ g/mL, experiment measure naphthalene and phenanthrene, pyrene, first
The removal rate of naphthols and luxuriant and rich with fragrance and pyrene highest adsorbance, testing result are as shown in table 1.
Metal ion removal rate is tested: taking 200mL waste water into beaker, Cu in waste water2+、Cd2+And Pb2+It is initial dense
Degree is Absorbent to be added into waste water and takes supernatant after ultrasonic disperse 5min is placed on shaking table concussion 12h for 100mg/L
Liquid, with Cu in ICP measurement supernatant2+、Cd2+And Pb2+Absorption after concentration, the removal rate w=(of heavy metal ion is initially dense
Concentration after degree-absorption)/initial concentration, testing result is as shown in table 1.
Spend the test of waste water from dyestuff removal effect: by the adsorbent in example 1~3 and comparative example in direct light turquoise blue dyestuff
In waste water after 150min is adsorbed, dye decolored rate is measured.
1 use in waste water treatment performance of the adsorbent measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| The removal rate (%) of naphthalene | 94 | 94 | 95 | 82 | 75 | 85 |
| Luxuriant and rich with fragrance removal rate (%) | 97 | 98 | 99 | 80 | 76 | 86 |
| Luxuriant and rich with fragrance highest adsorbance (mg/g) | 7 | 8 | 8 | 4 | 3 | 5 |
| The removal rate (%) of pyrene | 98 | 99 | 99 | 80 | 72 | 85 |
| The highest adsorbance (mg/g) of pyrene | 6 | 7 | 7 | 3 | 2 | 4 |
| The removal rate (%) of alpha naphthol | 97 | 97 | 98 | 82 | 70 | 86 |
| Cu2+Removal rate (%) | 85.0 | 85.3 | 85.4 | 45.6 | 65.3 | 75.4 |
| Cd2+Removal rate (%) | 89.1 | 89.4 | 89.6 | 52.3 | 64.8 | 72.2 |
| Pb2+Removal rate (%) | 93.2 | 93.5 | 93.7 | 67.8 | 78.2 | 79.3 |
| Dye decolored rate (%) | 96 | 97 | 97 | 80 | 85 | 88 |
It is good to organic pollutant degradation according to above-mentioned detection data use in waste water treatment adsorbent of the invention, naphthalene and it is luxuriant and rich with fragrance,
Pyrene, the removal rate of alpha naphthol are high, all reach 94% or more, and high to metal ion removal rate, adsorption rate is high, remove to waste water from dyestuff
Effect is good, and dye decolored rate is high, 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 (9)
1. a kind of preparation method of use in waste water treatment adsorbent, it is characterised in that specific preparation step are as follows: take agar, Bacillus natto
Powder, wheat bran, soybean powder are placed in fermentor, and under the conditions of 40~45 DEG C, heat-preservation fermentation obtains medium body, and will alkalize de- second
Acyl flocculant and gel powder mixing are put into the fermentation ware equipped with medium body, and control fermentation biofilm temperature is 30~33 DEG C, hair
The ferment biofilm time is 10~15 days, obtains use in waste water treatment adsorbent；
The specific preparation step of the deacetylated flocculant of alkalization are as follows:
(1) flyash, celestine, coke are mixed, is placed in Muffle furnace, be heated to 400 DEG C~500 DEG C, roast 3~4h
High-temperature activation powder is obtained, according to parts by weight, 20~30 parts of high-temperature activation powder and 4~5 portions of mixing carburization agents are put into 80~100
In the hot water of 60~100 DEG C of part, wherein it is 5 ︰ 1 mixing system that mixing carburization agent is ammonium hydrogen carbonate and Strontia hydrate in mass ratio
It is standby to form, 2~3h is stood after stirring, removes upper liquid, collects lower sediment thing；
(2) above-mentioned lower sediment thing, phenol, furfural, sodium carbonate are mixed and are fitted into reaction kettle, be heated to 50~55 DEG C,
10~12h of insulation reaction obtains phenolic aldehyde gel, is aged 10~12h, obtains the gel of doping strontium carbonate, then be placed in cold in dry ice
Dry 2~3h is lyophilized, obtains aeroge, aeroge is put into retort, is carbonized in argon atmosphere, carbonization temperature is controlled
It is 300~350 DEG C, carbonization time is 20~25min, obtains activating fly ash containing strontium carbonate；
(3) above-mentioned activating fly ash containing strontium carbonate is separated by filtration to obtain acidleach with after 40~45min of sulfuric acid solution impregnation
Acidleach activating fly ash is then that 5 ︰ 1 are mixed with shrimp shell meal by activating fly ash in mass ratio, and being put into mass fraction is 30%
4~5h of impregnation in sodium hydroxide solution obtains the deacetylated flocculant that alkalizes；
The specific preparation step of the gel powder are as follows:
(1) addition 40~50mL dehydrated alcohol and the wooden nano-cellulose of 2~3g into ultrasonic disperse instrument, ultrasonic disperse 4~
6min obtains cellulose suspension, and cellulose suspension is placed in the conical flask with blender, with dropping funel with 1~
18~20mL butyl titanate is added into conical flask for the drop rate of 3mL/min, while starting blender, with 400~500r/
The revolving speed of min starts 10~15min of stirring and obtains presoma；
(2) glacial acetic acid that addition 20~25mL mass fraction is 98% in Xiang Shangshu presoma, 20~30mL silicon dioxide gel,
1~2h is stirred, complex sol is obtained, still aging 2~3 days, obtains dry colloidal sol, it is 60~70 that dry colloidal sol, which is placed in set temperature,
DEG C baking oven in, dry 10~12h obtains gel piece, and gel piece is put into 30~35min of grinding in mortar, 200 meshes is crossed and obtains
To gel powder.
2. a kind of preparation method of use in waste water treatment adsorbent according to claim 1, it is characterised in that: the culture
Each ingredient in matrix, according to parts by weight, including 4~5 parts of agar, 2~4 parts of Bacillus natto powder, 5~7 parts of wheat bran, soybean powder 20~
25 parts.
3. a kind of preparation method of use in waste water treatment adsorbent according to claim 1, it is characterised in that: the soya bean
Powder is made by cooked ground 200 mesh of soya bean.
4. a kind of preparation method of use in waste water treatment adsorbent according to claim 1, it is characterised in that: the alkalization
Deacetylated flocculant and gel powder mixing mass ratio are 1 ︰ 5.
5. a kind of preparation method of use in waste water treatment adsorbent according to claim 1, it is characterised in that: described
The deacetylated flocculant of alkalization specific preparation step (1) in flyash, celestine, coke mixing mass ratio be 10 ︰, 4 ︰
1。
6. a kind of preparation method of use in waste water treatment adsorbent according to claim 1, it is characterised in that: described
The deacetylated flocculant of alkalization specific preparation step (2) in lower sediment thing, phenol, furfural, sodium carbonate mixing quality
Than for 7 ︰, 8 ︰, 10 ︰ 1.
7. a kind of preparation method of use in waste water treatment adsorbent according to claim 1, it is characterised in that: described
The deacetylated flocculant of alkalization specific preparation step (3) in sulfuric acid solution mass fraction be 80%, sodium hydroxide solution matter
Measuring score is 30%.
8. a kind of preparation method of use in waste water treatment adsorbent according to claim 1, it is characterised in that: the gel powder
Specific preparation step (1) in ultrasonic disperse control supersonic frequency be 40~45kHz.
9. a kind of preparation method of use in waste water treatment adsorbent according to claim 1, it is characterised in that: the gel powder
Specific preparation step (2) in glacial acetic acid mass fraction be 98%.
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Cited By (6)
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| CN111115849A (en) * | 2020-01-03 | 2020-05-08 | 王小龙 | Preparation method of microbial sewage purification treatment agent |
| CN111186895A (en) * | 2020-01-14 | 2020-05-22 | 龙岩绿合环保有限公司 | Polyacrylamide water purifying agent, preparation method thereof, storage method thereof and use method thereof |
| CN112374617A (en) * | 2020-10-26 | 2021-02-19 | 盐城工业职业技术学院 | Sewage treatment agent |
| CN113578249A (en) * | 2021-07-23 | 2021-11-02 | 国网内蒙古东部电力有限公司电力科学研究院 | Preparation method of fly ash-based adsorption material |
| CN113797895A (en) * | 2021-10-20 | 2021-12-17 | 中国科学院城市环境研究所 | Activated carbon/graphene composite material and preparation method and application thereof |
| CN115382511A (en) * | 2021-11-02 | 2022-11-25 | 浙江大学台州研究院 | Preparation method of multiwalled carbon nanotube crosslinked natural latex adsorbent and method for treating heavy metal leaching wastewater by using adsorbent |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111115849A (en) * | 2020-01-03 | 2020-05-08 | 王小龙 | Preparation method of microbial sewage purification treatment agent |
| CN111186895A (en) * | 2020-01-14 | 2020-05-22 | 龙岩绿合环保有限公司 | Polyacrylamide water purifying agent, preparation method thereof, storage method thereof and use method thereof |
| CN111186895B (en) * | 2020-01-14 | 2022-04-29 | 龙岩绿合环保有限公司 | Polyacrylamide water purifying agent, preparation method thereof, storage method thereof and use method thereof |
| CN112374617A (en) * | 2020-10-26 | 2021-02-19 | 盐城工业职业技术学院 | Sewage treatment agent |
| CN113578249A (en) * | 2021-07-23 | 2021-11-02 | 国网内蒙古东部电力有限公司电力科学研究院 | Preparation method of fly ash-based adsorption material |
| CN113578249B (en) * | 2021-07-23 | 2023-10-20 | 国网内蒙古东部电力有限公司电力科学研究院 | Preparation method of fly ash-based adsorption material |
| CN113797895A (en) * | 2021-10-20 | 2021-12-17 | 中国科学院城市环境研究所 | Activated carbon/graphene composite material and preparation method and application thereof |
| CN115382511A (en) * | 2021-11-02 | 2022-11-25 | 浙江大学台州研究院 | Preparation method of multiwalled carbon nanotube crosslinked natural latex adsorbent and method for treating heavy metal leaching wastewater by using adsorbent |
| CN115382511B (en) * | 2021-11-02 | 2023-07-11 | 浙江大学台州研究院 | Preparation method of multiwall carbon nanotube crosslinked natural latex adsorbent and method for treating heavy metal leaching wastewater by using adsorbent |
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