CN107540081A - A kind of preparation method of biochemical wastewater treatment composite biological packing - Google Patents
A kind of preparation method of biochemical wastewater treatment composite biological packing Download PDFInfo
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- CN107540081A CN107540081A CN201710958489.7A CN201710958489A CN107540081A CN 107540081 A CN107540081 A CN 107540081A CN 201710958489 A CN201710958489 A CN 201710958489A CN 107540081 A CN107540081 A CN 107540081A
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- diatomite
- crystalline flake
- flake graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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Abstract
The present invention relates to a kind of preparation method of biochemical wastewater treatment composite biological packing, it mainly carries out impregnation to commodity diatomite, then slurries are prepared with the diatomite after impregnation and ozone pre-oxidation and the crystalline flake graphite of chemical oxidation intercalation processing, phosphoric acid and aluminium hydroxide, expanded graphite diatomite aluminum phosphate composite biological packing is prepared by granulation and calcination process to slurries again.The present invention is simple to operate, cost is cheap, safety and environmental protection, the composite biological packing of preparation have the advantages that quality is light, chemical stability is good, intensity is high, it is resistance to rinse, be not easily blocked, surface area it is big, it is suitable for attachment and the flourish of microorganism, then can guarantee that efficient, the stable operation of biofilter biochemical wastewater treatment.
Description
Technical field
The invention belongs to technical field of sewage, more particularly to a kind of preparation side of the compounded mix of sewage disposal
Method.
Background technology
Sanitary sewage and municipal sewage have the advantages of yield is big, biochemical treatment characteristic is good, if but not appropriately processed
After be discharged into river, lake, reservoir and ocean water environment, the self-purification capacity of natural water can be reduced, and water quality can be caused to dislike
Change, then endanger aquatile system health, and health can be jeopardized.Therefore, sanitary sewage and municipal sewage are suitably located
Discharge or reuse are fwaater resources protections and the core content that utilizes after reason.The innovation and application of biomembrane sewage disposal technology at present
Receive much concern, for biomembrane sewage disposal technology, compared with catalytic oxidation and biological rotating disk, biofilter can be effectively real
Existing saprobia two stage treatment and tertiary treatment, it has fully used for reference the mentality of designing of bio-contact oxidation and the rapid filter that feeds water,
The features such as integrating aeration and biological oxidation, suspension retention, periodically backwash, save second pond；It is simultaneously aerobic, scarce in it
Oxygen area simultaneously deposits, and can effectively realize the efficiency of simultaneous nitrification and denitrification denitrogenation.Biological filtering tank process as a kind of new bio at
Reason technology, it is widely used to the fields such as sanitary sewage, municipal sewage, micro-polluted water, Industrial Wastewater Treatment and Treated sewage reusing.
In being constructed in biofilter, filler is its core component, and research shows, particle diameter, material, adsorpting characteristic, the hole of filler
The physicochemical characteristics such as rate have a major impact to the apposition growth of microorganism and sewage purification, and filler provides growth in microorganism and is situated between
While matter, also pollutant can be directly removed by the effect such as precipitating, filtering, adsorbing and intercepting, its sewage to biofilter
Treatment efficiency plays vital effect.The filler used at present in biofilter mainly have quartz sand, haydite, anthracite,
Shale, vermiculite, cordierite, gravel, slag, ceramic ring, resilient bristles, volcanic rock etc., but filtering and absorption be present in these fillers
The defects of acting on low, dirt-carrying ability.Thus, research and develop strong novel microbial adhesive ability, filtering, retention and good adsorption performance
Biologic packing material, be lifting biofilter biochemical sewage disposal efficiency, further expand its application important measure.
Therefore, in terms of carrier performance lifting and new packing research and development, domestic and foreign scholars and engineers and technicians carry out
Fruitful work.Studies have reported that using paper white sludge, flyash and other additives as raw material, using balling-up and calciner
Skill, ceramic filter material is prepared for, its essential mineral is mutually anorthite and cacoclasite.Its is light porous, and handles ammonia nitrogen waste water
Excellent effect, but its density is small, is easy to outflow with water.Also studies have reported that using flyash as primary raw material, clay, dehydration are dirty
Mud, desulfurated plaster etc. are auxiliary material, are prepared for flyash ceramic particulate filler, and the surface roughness of the flyash ceramic particulate filler is big, hole
Rate is high, specific surface area is big, bio-film colonization performance it is good in addition, and also studies have reported that using diatomite, flyash, clay, bentonite as
Raw material, by adding binding agent and pore creating material, filled out through sintered at high temperature Diatomite Ceramsite filler and light haydite of powdered coal ash
Material, the filler can ensure the excellent Sewage Biological Treatment efficiency in biofilter.But above-mentioned paper white sludge ceramic filter material, diatomite
The defects of there is sintering temperature height in the preparation of ceramics filling and light haydite of powdered coal ash filler, energy consumption is big.Publication No. CN
103951044A patent is referred to sepiolite, medical stone, cement, polyvinyl alcohol, sodium alginate, hydrogen peroxide, iron chloride, sulphur
Sour manganese, cobalt chloride and agar are primary raw material, prepare polyvinyl alcohol, silicon mosanom and hydrogen peroxide liquid mixture first, so
This liquefied mixture is mixed into system with materials such as sepiolite, medical stone, cement, iron chloride, manganese sulfate, cobalt chloride and agar afterwards
Grain, after the process processing such as room temperature, drying screening, high pressure low temperature maintenance, steam-cured and normal temperature cooling, it is prepared for one kind
Biologic packing material, the filler are advantageous to microorganism growth and propagation for biochemical wastewater treatment process, and the biofilm time is short, effluent quality
It is good.But the filler preparation section is relatively cumbersome, and contents of many kinds of heavy metal ion is applied, potential hazard be present to environment.Publication number
A kind of high efficiency packing preparation method for sewage disposal is referred to for CN 104671402A patent, it is first by equal proportion
PPG, fertile soil, silicone surfactant and diatomite add water mixing, stirring, mixed liquor is prepared, then to mixing
Activated carbon is added in liquid and is stirred, is finally adding appropriate anaerobic digestion bacterium and microbial germ powder.The technology is made to fill out
Expect that there is good biomembrane fixation performance, filler not conglomeration in sewage disposal process, and water permeability is good.But prepared by the filler
Cost is higher, and its bad mechanical strength, is easily lost because of immersion, so engineer applied efficiency is not good enough.
The content of the invention
To overcome the shortcomings of the prior art, effectively lift the microorganism attachment of filler used in biofilter, retained
Filter and absorption property, then realize that biofilter biochemical sewage is efficiently disposed, and a kind of quality of present invention offer is light, chemical stability
It is good, intensity is high, it is resistance to rinse, be not easily blocked, the preparation method for the biochemical wastewater treatment composite biological packing that surface area is big.This hair
It is bright that impregnation mainly is carried out to commodity diatomite, then with the diatomite after impregnation and ozone pre-oxidation and chemical oxygen
The crystalline flake graphite, phosphoric acid and aluminium hydroxide for changing intercalation processing prepare slurries, then slurries are prepared for by granulation and calcination process
Expanded graphite-diatomite-aluminum phosphate composite biological packing.
The preparation method of the present invention is as follows：
(1) ozone pre-oxidation of crystalline flake graphite and chemical oxidation intercalation processing：
1. the ozone pre-oxidation processing of crystalline flake graphite：
It is 1 by crystalline flake graphite and the mass ratio of deionized water:1.5 ratio, deionized water is added in container, and will
The container for filling deionized water is placed on magnetic stirring apparatus, is then added to average grain diameter in container for the crystalline flake graphite of 80 mesh
And open the mixing control switch of magnetic stirring apparatus；Ozone generator generating tube is inserted into beaker bottom afterwards, opens ozone hair
Raw appliance mains switch, source of the gas used in ozone generator is pure oxygen, is 10mg/L by the ozone amount that solution is passed into generating tube, room
20~30min of ozone oxidation is carried out to crystalline flake graphite under temperature；After ozone oxidation terminates, solution is carried out crystalline flake graphite is collected by filtration
Powder, is washed with deionized crystalline flake graphite 3 times, afterwards by the crystalline flake graphite after ozone Oxidation Treatment at a temperature of 80~90 DEG C
Dry 8h；
2. the chemical oxidation intercalation processing of crystalline flake graphite：
By perchloric acid：Crystalline flake graphite：Potassium permanganate：The mass ratio of potassium dihydrogen phosphate aqueous solution is 8.33~11.7:1:0.5
~0.67:16.67:Perchloric acid, is added in container by 20 ratio first, and the container for filling perchloric acid is placed in into magnetic force and stirred
Mix on device, the crystalline flake graphite and potassium permanganate solid for then successively 1. preparing step are added in container and are used preservative film
Sealing, stirring and the heater switch of magnetic stirring apparatus are opened, it is 75~85 DEG C to control solution temperature, after stirring reaction 30min again
Saturation potassium dihydrogen phosphate aqueous solution is added in container, and solution temperature in container is adjusted to 35~45 by 75~85 DEG C
DEG C, 60~90min of stirring reaction at a temperature of this；Reaction after terminating carries out that chemical oxidation intercalation processing is collected by filtration to mixed solution
Crystalline flake graphite powder afterwards, and with the abundant washing powder of deionized water until the pH of washings is neutral；Afterwards by washes clean
Powder be placed in baking oven at a temperature of 60~70 DEG C and dry 24h, the crystalline flake graphite after chemical oxidation intercalation processing is made；
(2) diatomaceous impregnation：
Commodity diatomite is subjected to Screening Treatment with the standard inspection sieve of 120 mesh first, sieving is collected, after weighing sieving
Diatomite, prepare the slurries that diatomite mass content is 30%~40% with deionized water；Then it is 5% to prepare mass concentration
~8% Polyaluminium Sulfate Chloride aqueous solution, and diatomite slurries are mixed in equal volume with the Polyaluminium Sulfate Chloride aqueous solution, afterwards will mixing
20~the 30min of ultrasonic wave room temperature cavitation process of solution afterwards；After ultrasonic cavitation processing terminates, first by diatomite slurries with gathering
The mixed solution of sulphur aluminum chloride aqueous solution stands 3~5h, is then filtered after abandoning supernatant, and gleanings are washed with deionized
2 times, the gleanings after washing are placed in baking oven afterwards, 12h are dried at a temperature of 100~110 DEG C, finally by dried receipts
Collection thing is ground into the ultra-fine grain of 120 mesh, obtains the diatomite after impregnation；
(3) preparation of expanded graphite-diatomite-aluminum phosphate composite biological packing：
1. the preparation of slurry liquid：
By crystalline flake graphite：Diatomite：Phosphoric acid：Aluminium hydroxide：Deionized water：Mass ratio=0.7~1 of absolute ethyl alcohol：40
~45：35~45：12~15：35~45：Container, is placed on magnetic stirring apparatus by 5 ratio first, then successively that quality is dense
Spend the phosphoric acid for 85%, deionized water and absolute ethyl alcohol to be added in container, stirring makes it well mixed, then by aluminium hydroxide
It is added in beaker and stirs 20~30min, afterwards by mixed solution 10~15min of ultrasonic wave room temperature cavitation process；Ultrasound
After ripple room temperature cavitation process, crystalline flake graphite and the diatomite of impregnation prepared by step (1) are added in solution, water-bath control
The temperature of mixed solution processed is 70~80 DEG C, 45~60min of stirring reaction；Mixed solution is finally naturally cooled into room temperature, i.e.,
Obtain expanded graphite-diatomite-slurry liquid used in the preparation of aluminum phosphate composite biological packing；
2. the granulation process of composite biological packing：
Above-mentioned slurry liquid is added in granulating disc, it is 10~20r/min to control rotating speed, is carried out at ambient temperature
It is granulated, the spherical composite biological packing average diameter of preparation is 5mm；
3. drying and the sintering processes of composite biological packing：
Above-mentioned spherical composite biological packing is placed in drying box first processing is dried, drying temperature is 100~110
DEG C, 6~8h of drying time, then the filler after drying process is placed in crucible, then crucible is put into Muffle furnace to filler
It is sintered, muffle furnace hearth temperature is increased to 500~550 DEG C with 10 DEG C/min heating rate by room temperature, insulation 30
~60min, Muffle furnace power switch is closed afterwards, muffle furnace hearth temperature is naturally cooled to room temperature, treat that fire box temperature cools down
To room temperature, the filler particles of sintering processes are taken out, that is, expanded graphite-diatomite-aluminum phosphate biochemical wastewater treatment has been made
Use composite biological packing.
The present invention has the following advantages that compared with prior art：
1st, preparation technology is simple to operate, cost is cheap, safety and environmental protection；
2nd, prepare composite biological packing have quality is light, chemical stability is good, intensity is high, it is resistance to rinse, be not easily blocked, table
The advantages that area is big, it can realize and the efficient absorption of polarity in water body and nonpolar organic pollutants is enriched with；
3rd, the composite biological packing prepared is suitable for attachment and the flourish of microorganism, can guarantee that biofilter biochemical sewage
Efficient, the stable operation of processing.
Brief description of the drawings
Fig. 1 is the internal morphology figure of composite biological packing prepared by the embodiment of the present invention 1.
Fig. 2 is composite biological packing internal morphology partial enlarged drawing prepared by the embodiment of the present invention 1.
Embodiment
Embodiment 1
1) ozone pre-oxidation of crystalline flake graphite and chemical oxidation intercalation processing：
1. the ozone pre-oxidation processing of crystalline flake graphite：
150g deionized waters are added in the beaker that volume is 500mL first, and the beaker for filling deionized water is put
In on magnetic stirring apparatus, then 100g average grain diameters are added in beaker for the crystalline flake graphite of 80 mesh and open magnetic stirring apparatus
Mixing control switch；Ozone generator generating tube is inserted into beaker bottom afterwards, opens ozonizer power supply switch, ozone
Source of the gas used in generator is pure oxygen, is 5mg/L by the ozone amount that solution is passed into generating tube, and crystalline flake graphite is carried out at room temperature
Ozone oxidation 20min；After ozone oxidation terminates, solution is carried out that crystalline flake graphite powder is collected by filtration first, be washed with deionized water
Wash crystalline flake graphite 3 times, the crystalline flake graphite after ozone Oxidation Treatment is dried into 8h at a temperature of 80 DEG C afterwards；
2. the chemical oxidation intercalation processing of crystalline flake graphite：
25g perchloric acid is added in the beaker that volume is 200mL first, and the beaker for filling perchloric acid is placed in magnetic force
On agitator, the crystalline flake graphite and 1.5g potassium permanganate solids that then successively 1. prepare 3g steps are added in beaker and will burnt
Rim of a cup is sealed with preservative film, opens stirring and the heater switch of magnetic stirring apparatus, and it is 75 DEG C to control solution temperature, stirring reaction
50g saturation potassium dihydrogen phosphate aqueous solutions are added in beaker again after 30min, and solution temperature in beaker is adjusted to by 75 DEG C
35 DEG C, stirring reaction 60min at a temperature of this；Reaction is carried out after chemical oxidation intercalation processing is collected by filtration after terminating to mixed solution
Crystalline flake graphite powder, and with the abundant washing powder of deionized water until the pH of washings is neutral；Afterwards by washes clean
Powder, which is placed in baking oven at a temperature of 60 DEG C, dries 24h, produces the crystalline flake graphite after chemical oxidation intercalation processing；
2) diatomaceous impregnation：
Commodity diatomite is subjected to Screening Treatment with the standard inspection sieve of 120 mesh first, sieving is collected, after weighing sieving
Diatomite, prepare the slurries that diatomite mass content is 30% with deionized water；Then the polysulfide that mass concentration is 5% is prepared
Aluminum chloride aqueous solution, and 25mL diatomite slurries are mixed with the 25mL Polyaluminium Sulfate Chloride aqueous solution, afterwards by mixed solution
With ultrasonic wave room temperature cavitation process 20min；It is first that diatomite slurries and Polyaluminium Sulfate Chloride are water-soluble after ultrasonic cavitation processing terminates
The mixed solution of liquid stands 3h, is then filtered after abandoning supernatant, and gleanings is washed with deionized 2 times, afterwards will washing
Gleanings afterwards are placed in baking oven, and 12h is dried at a temperature of 100 DEG C, dried gleanings finally are ground into 120 purposes and surpassed
Fine grained, obtain the diatomite after impregnation；
3) preparation of expanded graphite-diatomite-aluminum phosphate composite biological packing：
1. the preparation of slurry liquid：
500mL beaker is placed on magnetic stirring apparatus first, then successively by 35g mass concentrations be 85% phosphoric acid,
35g deionized waters and 5g absolute ethyl alcohols are added in beaker, and stirring makes it well mixed, is then added to 12g aluminium hydroxides
In beaker and 20min is stirred, afterwards by mixed solution ultrasonic wave room temperature cavitation process 10min；Ultrasonic wave room temperature cavitation process
Afterwards, the diatomite after the crystalline flake graphite prepared by 0.7g steps (1) and 40g impregnations is added in solution, and water-bath control is mixed
The temperature for closing solution is 70 DEG C, stirring reaction 45min；Mixed solution is finally naturally cooled into room temperature, slurry liquid is made；
2. the granulation process of composite biological packing：
The above-mentioned slurry liquid of 500mL is added in granulating disc, it is 10r/min to control rotating speed, is entered at ambient temperature
Row is granulated, and the spherical composite biological packing average diameter of preparation is 5mm；
3. drying and the sintering processes of composite biological packing：
Above-mentioned spherical composite biological packing is placed in drying box first processing is dried, drying temperature is 100 DEG C, is dried
Time is 6h, then the filler after drying process is placed in crucible, then crucible is put into Muffle furnace filler is sintered
Processing, muffle furnace hearth temperature are increased to 500 DEG C with 10 DEG C/min heating rate by room temperature, are incubated 30min, close horse afterwards
Not stove power switch, muffle furnace hearth temperature is naturally cooled to room temperature, the filler particles of sintering processes are taken out, that is, dirt is made
Water biochemical treatment expanded graphite-diatomite-aluminum phosphate composite biological packing.
According to the composite biological packing performance indications prepared by embodiment 1 as shown in appendix 1, the compounded mix performance indications
Meet ceramic grain filter (QB/T 4383-2012) demand of technical standard in national light industry professional standard；With one kind with flyash
Compared with clay for the commercially available ceramic grain filter of key component, composite biological packing quality manufactured in the present embodiment is lighter, there have to be higher
Voidage and large specific surface area, and its cylindrical compress strength is bigger.
As shown in figure 1, it can be clearly apparent inside haydite with the presence of a large amount of microcellular structures；As shown in Figure 2, it can be seen that, through smelly
After oxygen oxidation pre-treatment and chemical graft processing, the crystalline flake graphite added becomes expanded graphite after 500 DEG C of heat treatment, its shape
State is vermiform, and the presence of the vermicular expanded graphite ensure that compounded mix has good adsorbent performance, and the vermiform is swollen
Swollen graphite can play a part of assisting pore-creating in forming process, then ensure that composite biological packing has the inner hole structure of prosperity.
The performance indications of subordinate list 1 compare
Embodiment 2
1) ozone pre-oxidation of crystalline flake graphite and chemical oxidation intercalation processing：
1. the ozone pre-oxidation processing of crystalline flake graphite：
150g deionized waters are added in the beaker that volume is 500mL first, and the beaker for filling deionized water is put
In on magnetic stirring apparatus, then 100g average grain diameters are added in beaker for the crystalline flake graphite of 80 mesh and open magnetic stirring apparatus
Mixing control switch；Ozone generator generating tube is inserted into beaker bottom afterwards, opens ozonizer power supply switch, ozone
Source of the gas used in generator is pure oxygen, is 5mg/L by the ozone amount that solution is passed into generating tube, and crystalline flake graphite is carried out at room temperature
Ozone oxidation 23min；After ozone oxidation terminates, solution is carried out that crystalline flake graphite powder is collected by filtration first, be washed with deionized water
Wash crystalline flake graphite 3 times, the crystalline flake graphite after ozone Oxidation Treatment is dried into 8h at a temperature of 83 DEG C afterwards；
2. the chemical oxidation intercalation processing of crystalline flake graphite：
28g perchloric acid is added in the beaker that volume is 200mL first, and the beaker for filling perchloric acid is placed in magnetic force
On agitator, the crystalline flake graphite and 1.7g potassium permanganate solids that then successively 1. prepare 3g steps are added in beaker and will burnt
Rim of a cup is sealed with preservative film, opens stirring and the heater switch of magnetic stirring apparatus, and it is 78 DEG C to control solution temperature, stirring reaction
53g saturation potassium dihydrogen phosphate aqueous solutions are added in beaker again after 30min, and solution temperature in beaker is adjusted to by 78 DEG C
38 DEG C, stirring reaction 70min at a temperature of this；Reaction is carried out after chemical oxidation intercalation processing is collected by filtration after terminating to mixed solution
Crystalline flake graphite powder, and with the abundant washing powder of deionized water until the pH of washings is neutral；Afterwards by washes clean
Powder, which is placed in baking oven at a temperature of 63 DEG C, dries 24h, produces the crystalline flake graphite after chemical oxidation intercalation processing；
2) diatomaceous impregnation：
Commodity diatomite is subjected to Screening Treatment with the standard inspection sieve of 120 mesh first, sieving is collected, after weighing sieving
Diatomite, prepare the slurries that diatomite mass content is 33% with deionized water；Then the polysulfide that mass concentration is 6% is prepared
Aluminum chloride aqueous solution, and 25mL diatomite slurries are mixed with the 25mL Polyaluminium Sulfate Chloride aqueous solution, afterwards by mixed solution
With ultrasonic wave room temperature cavitation process 23min；It is first that diatomite slurries and Polyaluminium Sulfate Chloride are water-soluble after ultrasonic cavitation processing terminates
The mixed solution of liquid stands 4h, is then filtered after abandoning supernatant, and gleanings is washed with deionized 2 times, afterwards will washing
Gleanings afterwards are placed in baking oven, and 12h is dried at a temperature of 103 DEG C, dried gleanings finally are ground into 120 purposes and surpassed
Fine grained, obtain the diatomite after impregnation；
3) preparation of expanded graphite-diatomite-aluminum phosphate composite biological packing：
1. the preparation of slurry liquid：
500mL beaker is placed on magnetic stirring apparatus first, then successively by 38g mass concentrations be 85% phosphoric acid, 38g
Deionized water and 5g absolute ethyl alcohols are added in beaker, and stirring makes it well mixed, and 13g aluminium hydroxides then are added into beaker
In and stir 23min, afterwards by mixed solution ultrasonic wave room temperature cavitation process 12min；, will after ultrasonic wave room temperature cavitation process
Diatomite after the crystalline flake graphite of 0.8g steps (1) preparation and 42g impregnations is added in solution, water-bath control mixed solution
Temperature be 73 DEG C, stirring reaction 50min；Mixed solution is finally naturally cooled into room temperature, produce expanded graphite-diatomite-
Slurry liquid used in the preparation of aluminum phosphate composite biological packing；
2. the granulation process of composite biological packing：
The above-mentioned slurry liquid of 500mL is added in granulating disc, it is 13r/min to control rotating speed, is entered at ambient temperature
Row is granulated, and the spherical composite biological packing average diameter of preparation is 5mm；
3. drying and the sintering processes of composite biological packing：
Above-mentioned spherical composite biological packing is placed in drying box first processing is dried, drying temperature is 104 DEG C, is dried
Time is 7h, then the filler after drying process is placed in crucible, then crucible is put into Muffle furnace filler is sintered
Processing, muffle furnace hearth temperature are increased to 510 DEG C by room temperature with 10 DEG C/min heating rate, lower insulation 40min, closed afterwards
Muffle furnace power switch, muffle furnace hearth temperature is naturally cooled to room temperature, the filler particles of sintering processes are taken out, dirt is made
Water biochemical treatment expanded graphite-diatomite-aluminum phosphate composite biological packing.
Embodiment 3
1) ozone pre-oxidation of crystalline flake graphite and chemical oxidation intercalation processing：
1. the ozone pre-oxidation processing of crystalline flake graphite：
150g deionized waters are added in the beaker that volume is 500mL first, and the beaker for filling deionized water is put
In on magnetic stirring apparatus, then 100g average grain diameters are added in beaker for the crystalline flake graphite of 80 mesh and open magnetic stirring apparatus
Mixing control switch；Ozone generator generating tube is inserted into beaker bottom afterwards, opens ozonizer power supply switch, ozone
Source of the gas used in generator is pure oxygen, is 5mg/L by the ozone amount that solution is passed into generating tube, and crystalline flake graphite is carried out at room temperature
Ozone oxidation 26min；After ozone oxidation terminates, solution is carried out that crystalline flake graphite powder is collected by filtration first, be washed with deionized water
Wash crystalline flake graphite 3 times, the crystalline flake graphite after ozone Oxidation Treatment is dried into 8h at a temperature of 86 DEG C afterwards；
2. the chemical oxidation intercalation processing of crystalline flake graphite：
31g perchloric acid is added in the beaker that volume is 200mL first, and the beaker for filling perchloric acid is placed in magnetic force
On agitator, the crystalline flake graphite and 1.9g potassium permanganate solids that then successively 1. prepare 3g steps are added in beaker and will burnt
Rim of a cup is sealed with preservative film, opens stirring and the heater switch of magnetic stirring apparatus, and it is 81 DEG C to control solution temperature, stirring reaction
56g saturation potassium dihydrogen phosphate aqueous solutions are added in beaker again after 30min, and solution temperature in beaker is adjusted to by 81 DEG C
41 DEG C, stirring reaction 80min at a temperature of this；Reaction is carried out after chemical oxidation intercalation processing is collected by filtration after terminating to mixed solution
Crystalline flake graphite powder, and with the abundant washing powder of deionized water until the pH of washings is neutral；Afterwards by washes clean
Powder, which is placed in baking oven at a temperature of 66 DEG C, dries 24h, produces the crystalline flake graphite after chemical oxidation intercalation processing；
2) diatomaceous impregnation：
Commodity diatomite is subjected to Screening Treatment with the standard inspection sieve of 120 mesh first, sieving is collected, after weighing sieving
Diatomite, prepare the slurries that diatomite mass content is 36% with deionized water；Then the polysulfide that mass concentration is 7% is prepared
Aluminum chloride aqueous solution, and 25mL diatomite slurries are mixed with the 25mL Polyaluminium Sulfate Chloride aqueous solution, afterwards by mixed solution
With ultrasonic wave room temperature cavitation process 26min；It is first that diatomite slurries and Polyaluminium Sulfate Chloride are water-soluble after ultrasonic cavitation processing terminates
The mixed solution of liquid stands 4.5h, is then filtered after abandoning supernatant, and gleanings is washed with deionized 2 times, will wash afterwards
Gleanings after washing are placed in baking oven, and 12h is dried at a temperature of 106 DEG C, dried gleanings finally are ground into 120 purposes
Ultra-fine grain, obtain the diatomite after impregnation；
3) preparation of expanded graphite-diatomite-aluminum phosphate composite biological packing：
1. the preparation of slurry liquid：
500mL beaker is placed on magnetic stirring apparatus first, then successively by 41g mass concentrations be 85% phosphoric acid, 41g
Deionized water and 5g absolute ethyl alcohols are added in beaker, and stirring makes it well mixed, and 14g aluminium hydroxides then are added into beaker
In and stir 26min, afterwards by mixed solution ultrasonic wave room temperature cavitation process 14min；, will after ultrasonic wave room temperature cavitation process
Diatomite after the crystalline flake graphite of 0.9g steps (1) preparation and 44g impregnations is added in solution, water-bath control mixed solution
Temperature be 76 DEG C, stirring reaction 55min；Mixed solution is finally naturally cooled into room temperature, produce expanded graphite-diatomite-
Slurry liquid used in the preparation of aluminum phosphate composite biological packing；
2. the granulation process of composite biological packing：
The above-mentioned slurry liquid of 500mL is added in granulating disc, it is 16r/min to control rotating speed, is entered at ambient temperature
Row is granulated, and the spherical composite biological packing average diameter of preparation is 5mm；
3. drying and the sintering processes of composite biological packing：
Above-mentioned spherical composite biological packing is placed in drying box first processing is dried, drying temperature is 107 DEG C, is dried
Time is 7h, then the filler after drying process is placed in crucible, then crucible is put into Muffle furnace filler is sintered
Processing, muffle furnace hearth temperature are increased to 530 DEG C with 10 DEG C/min heating rate by room temperature, are incubated 50min, close horse afterwards
Not stove power switch, muffle furnace hearth temperature is naturally cooled to room temperature, the filler particles of sintering processes are taken out, sewage is made
Biochemical treatment expanded graphite-diatomite-aluminum phosphate composite biological packing.
Embodiment 4
1) ozone pre-oxidation of crystalline flake graphite and chemical oxidation intercalation processing：
1. the ozone pre-oxidation processing of crystalline flake graphite：
150g deionized waters are added in the beaker that volume is 500mL first, and the beaker for filling deionized water is put
In on magnetic stirring apparatus, then 100g average grain diameters are added in beaker for the crystalline flake graphite of 80 mesh and open magnetic stirring apparatus
Mixing control switch；Ozone generator generating tube is inserted into beaker bottom afterwards, opens ozonizer power supply switch, ozone
Source of the gas used in generator is pure oxygen, is 5mg/L by the ozone amount that solution is passed into generating tube, and crystalline flake graphite is carried out at room temperature
Ozone oxidation 30min；After ozone oxidation terminates, solution is carried out that crystalline flake graphite powder is collected by filtration first, be washed with deionized water
Wash crystalline flake graphite 3 times, the crystalline flake graphite after ozone Oxidation Treatment is dried into 8h at a temperature of 90 DEG C afterwards；
2. the chemical oxidation intercalation processing of crystalline flake graphite：
35g perchloric acid is added in the beaker that volume is 200mL first, and the beaker for filling perchloric acid is placed in magnetic force
On agitator, the crystalline flake graphite and 2.0g potassium permanganate solids that then successively 1. prepare 3g steps are added in beaker and will burnt
Rim of a cup is sealed with preservative film, opens stirring and the heater switch of magnetic stirring apparatus, and it is 85 DEG C to control solution temperature, stirring reaction
60g saturation potassium dihydrogen phosphate aqueous solutions are added in beaker again after 30min, and solution temperature in beaker is adjusted to by 85 DEG C
45 DEG C, stirring reaction 90min at a temperature of this；Reaction is carried out after chemical oxidation intercalation processing is collected by filtration after terminating to mixed solution
Crystalline flake graphite powder, and with the abundant washing powder of deionized water until the pH of washings is neutral；Afterwards by washes clean
Powder, which is placed in baking oven at a temperature of 70 DEG C, dries 24h, produces the crystalline flake graphite after chemical oxidation intercalation processing；
2) diatomaceous impregnation：
Commodity diatomite is subjected to Screening Treatment with the standard inspection sieve of 120 mesh first, sieving is collected, after weighing sieving
Diatomite, prepare the slurries that diatomite mass content is 40% with deionized water；Then the polysulfide that mass concentration is 8% is prepared
Aluminum chloride aqueous solution, and 25mL diatomite slurries are mixed with the 25mL Polyaluminium Sulfate Chloride aqueous solution, afterwards by mixed solution
With ultrasonic wave room temperature cavitation process 30min；It is first that diatomite slurries and Polyaluminium Sulfate Chloride are water-soluble after ultrasonic cavitation processing terminates
The mixed solution of liquid stands 5h, is then filtered after abandoning supernatant, and gleanings is washed with deionized 2 times, afterwards will washing
Gleanings afterwards are placed in baking oven, and 12h is dried at a temperature of 110 DEG C, dried gleanings finally are ground into 120 purposes and surpassed
Fine grained, obtain the diatomite after impregnation；
3) preparation of expanded graphite-diatomite-aluminum phosphate composite biological packing：
1. the preparation of slurry liquid：
500mL beaker is placed on magnetic stirring apparatus first, then successively by 45g mass concentrations be 85% phosphoric acid, 45g
Deionized water and 5g absolute ethyl alcohols are added in beaker, and stirring makes it well mixed, and 15g aluminium hydroxides then are added into beaker
In and stir 30min, afterwards by mixed solution ultrasonic wave room temperature cavitation process 15min；, will after ultrasonic wave room temperature cavitation process
Diatomite after the crystalline flake graphite of 1g steps (1) preparation and 45g impregnations is added in solution, water-bath control mixed solution
Temperature is 80 DEG C, stirring reaction 60min；Mixed solution is finally naturally cooled into room temperature, produces expanded graphite-diatomite-phosphorus
Slurry liquid used in sour aluminium composite biological packing preparation；
2. the granulation process of composite biological packing：
The above-mentioned slurry liquid of 500mL is added in granulating disc, rotating speed position 20r/min is controlled, enters at ambient temperature
Row is granulated, and the spherical composite biological packing average diameter of preparation is 5mm；
3. drying and the sintering processes process of composite biological packing：
Above-mentioned spherical composite biological packing is placed in drying box first processing is dried, drying temperature is 110 DEG C, is dried
Time is 8h, then the filler after drying process is placed in crucible, then crucible is put into Muffle furnace filler is sintered
Processing, muffle furnace hearth temperature are increased to 550 DEG C by room temperature with 10 DEG C/min heating rate, lower insulation 60min, closed afterwards
Muffle furnace power switch, muffle furnace hearth temperature is set to naturally cool to room temperature, after fire box temperature is cooled to room temperature, at sintering
The filler particles of reason are taken out, and biochemical wastewater treatment expanded graphite-diatomite-aluminum phosphate composite biological packing is made.
Claims (1)
- A kind of 1. preparation method of biochemical wastewater treatment composite biological packing, it is characterised in that：The preparation method includes following Step：(1) ozone pre-oxidation of crystalline flake graphite and chemical oxidation intercalation processing：1. the ozone pre-oxidation processing of crystalline flake graphite：It is 1 by crystalline flake graphite and the mass ratio of deionized water:1.5 ratio, deionized water is added in container, and will be filled The container of deionized water is placed on magnetic stirring apparatus, and then average grain diameter is added in container and opened for the crystalline flake graphite of 80 mesh Open the mixing control switch of magnetic stirring apparatus；Ozone generator generating tube is inserted into beaker bottom afterwards, opens ozone generator Power switch, source of the gas used in ozone generator are pure oxygen, are 5mg/L by the ozone amount that solution is passed into generating tube, at room temperature 20~30min of ozone oxidation is carried out to crystalline flake graphite；After ozone oxidation terminates, solution is carried out crystalline graphite powder is collected by filtration End, is washed with deionized crystalline flake graphite 3 times, afterwards does the crystalline flake graphite after ozone Oxidation Treatment at a temperature of 80~90 DEG C Dry 8h；2. the chemical oxidation intercalation processing of crystalline flake graphite：By perchloric acid：Crystalline flake graphite：Potassium permanganate：The mass ratio of potassium dihydrogen phosphate aqueous solution is 8.33~11.7:1:0.5~ 0.67:16.67:Perchloric acid, is added in container by 20 ratio first, and the container for filling perchloric acid is placed in into magnetic agitation On device, the crystalline flake graphite and potassium permanganate solid that then successively 1. prepare step are added in container and use preservative film close it Envelope, stirring and the heater switch of magnetic stirring apparatus are opened, it is 75~85 DEG C to control solution temperature, again will after stirring reaction 30min Saturation potassium dihydrogen phosphate aqueous solution is added in container, and solution temperature in container is adjusted into 35~45 DEG C by 75~85 DEG C, 60~90min of stirring reaction at a temperature of this；Reaction is carried out after chemical oxidation intercalation processing is collected by filtration after terminating to mixed solution Crystalline flake graphite powder, and with the abundant washing powder of deionized water until the pH of washings is neutral；Afterwards by washes clean Powder, which is placed in baking oven at a temperature of 60~70 DEG C, dries 24h, and the crystalline flake graphite after chemical oxidation intercalation processing is made；(2) diatomaceous impregnation：Commodity diatomite is subjected to Screening Treatment with the standard inspection sieve of 120 mesh first, collects sieving, weighs the silicon after sieving Diatomaceous earth, the slurries that diatomite mass content is 30%~40% are prepared with deionized water；Then prepare mass concentration be 5%~ The 8% Polyaluminium Sulfate Chloride aqueous solution, and diatomite slurries are mixed in equal volume with the Polyaluminium Sulfate Chloride aqueous solution, after mixing afterwards Solution 20~30min of ultrasonic wave room temperature cavitation process；After ultrasonic cavitation processing terminates, first by diatomite slurries and polysulfide The mixed solution of aluminum chloride aqueous solution stands 3~5h, is then filtered after abandoning supernatant, and gleanings 2 are washed with deionized It is secondary, the gleanings after washing are placed in baking oven afterwards, 12h are dried at a temperature of 100~110 DEG C, finally by dried receipts Collection thing is ground into the ultra-fine grain of 120 mesh, obtains the diatomite after impregnation；(3) preparation of expanded graphite-diatomite-aluminum phosphate composite biological packing：1. the preparation of slurry liquid：By crystalline flake graphite：Diatomite：Phosphoric acid：Aluminium hydroxide：Deionized water：Mass ratio=0.7~1 of absolute ethyl alcohol：40~45： 35~45：12~15：35~45：Container, is placed on magnetic stirring apparatus by 5 ratio first, is then by mass concentration successively 85% phosphoric acid, deionized water and absolute ethyl alcohol is added in container, and stirring makes it well mixed, then adds aluminium hydroxide Into beaker and 20~30min is stirred, afterwards by mixed solution 10~15min of ultrasonic wave room temperature cavitation process；Sonication chamber After warm cavitation process, crystalline flake graphite and the diatomite of impregnation prepared by step (1) are added in solution, and water-bath control is mixed The temperature for closing solution is 70~80 DEG C, 45~60min of stirring reaction；Mixed solution is finally naturally cooled into room temperature, produced swollen Swollen graphite-diatomite-slurry liquid used in the preparation of aluminum phosphate composite biological packing；2. the granulation process of composite biological packing：Above-mentioned slurry liquid is added in granulating disc, it is 10~20r/min to control rotating speed, is made at ambient temperature Grain, the spherical composite biological packing average diameter of preparation is 5mm；3. drying and the sintering processes of composite biological packing：Above-mentioned spherical composite biological packing is placed in drying box first processing is dried, drying temperature is 100~110 DEG C, is done Filler after drying process, is then placed in crucible, then crucible is put into Muffle furnace filler is burnt by dry 6~8h of time Knot processing, muffle furnace hearth temperature are increased to 500~550 DEG C with 10 DEG C/min heating rate by room temperature, and insulation 30~ 60min, Muffle furnace power switch is closed afterwards, muffle furnace hearth temperature is naturally cooled to room temperature, treats that fire box temperature is cooled to After room temperature, the filler particles of sintering processes are taken out, that is, expanded graphite-diatomite-aluminum phosphate biochemical wastewater treatment has been made and has used Composite biological packing.
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| CN113072075A (en) * | 2021-03-30 | 2021-07-06 | 湖南三友环保科技有限公司 | Preparation method and application of sulfur-based diatomite powder material |
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| JP2001112463A (en) * | 1999-10-13 | 2001-04-24 | Kimiaki Hattori | Device for culturing microorganism contained in sludge |
| CN105064005A (en) * | 2015-07-23 | 2015-11-18 | 合肥众月健康科技有限公司 | Modified pumice-graphene oxide doped efficient polylactic acid-polypropylene biological film composite fiber carrier material and preparation method thereof |
| CN105540826A (en) * | 2015-12-16 | 2016-05-04 | 苏州捷宁模塑有限公司 | Filling material structure for rice factory sewage treatment |
| CN106867607A (en) * | 2017-03-28 | 2017-06-20 | 常州大学 | A kind of preparation method of modified composite biological packing |
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| JP2001112463A (en) * | 1999-10-13 | 2001-04-24 | Kimiaki Hattori | Device for culturing microorganism contained in sludge |
| CN105064005A (en) * | 2015-07-23 | 2015-11-18 | 合肥众月健康科技有限公司 | Modified pumice-graphene oxide doped efficient polylactic acid-polypropylene biological film composite fiber carrier material and preparation method thereof |
| CN105540826A (en) * | 2015-12-16 | 2016-05-04 | 苏州捷宁模塑有限公司 | Filling material structure for rice factory sewage treatment |
| CN106867607A (en) * | 2017-03-28 | 2017-06-20 | 常州大学 | A kind of preparation method of modified composite biological packing |
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| CN113072075A (en) * | 2021-03-30 | 2021-07-06 | 湖南三友环保科技有限公司 | Preparation method and application of sulfur-based diatomite powder material |
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