CN108854262A - A kind of preparation method of Perlite filter agent - Google Patents
A kind of preparation method of Perlite filter agent Download PDFInfo
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- CN108854262A CN108854262A CN201810762458.9A CN201810762458A CN108854262A CN 108854262 A CN108854262 A CN 108854262A CN 201810762458 A CN201810762458 A CN 201810762458A CN 108854262 A CN108854262 A CN 108854262A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/02—Loose filtering material, e.g. loose fibres
- B01D39/06—Inorganic material, e.g. asbestos fibres, glass beads or fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0407—Additives and treatments of the filtering material comprising particulate additives, e.g. adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0442—Antimicrobial, antibacterial, antifungal additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/12—Special parameters characterising the filtering material
- B01D2239/1208—Porosity
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Abstract
The invention discloses a kind of preparation methods of Perlite filter agent, belong to material for water treatment technical field.By perlite through silica dioxide gel and modifier modification, pre- modified pearl rock is made, by pre- modified pearl rock and carbon nanotube mixture in mass ratio 1：10~1：20 mixing, and the graphene oxide solution of 3~5 times of pre- modified pearl rock quality is added, it is stirred, adjusts pH to 7.8~8.8, pre- modified pearl rock mixture is obtained, by pre- modified pearl rock mixture and polyethylene polyamine in mass ratio 8：1~12：1 mixing, and aqueous solution of ester in the glucose sugar β of 0.05~0.08 times of pre- modified pearl rock mixture quality is added, it after being stirred, filters, stands, freeze-drying obtains modified pearl rock；By modified pearl rock and sodium hydroxide solution in mass ratio 1：8~1：10 mixing, impregnate, filtering, and being washed to cleaning solution is neutrality, dry, obtain Perlite filter agent.Has the characteristics that excellent filter effect.
Description
Technical field
The invention discloses a kind of preparation methods of Perlite filter agent, belong to material for water treatment technical field.
Background technique
Sanitary sewage comparison of ingredients is fixed, and the organic matters such as carbohydrate, protein, amino acid, fat are mainly contained, than
It is more suited to the growth of bacterium, becomes the place of bacterium, viral life breeding；But sanitary sewage be generally free of it is toxic, and have
There is certain fertilizer efficiency, can be used to irrigated farmland.The ingredient of agricultural effluent is then varied, different seasons, different places, no
With the villages and small towns of developing goal, waste water is needed with different processing methods.When handling sewage, for reduce quantity of wastewater effluent and its
Complexity, should in conjunction with wideling popularize methane-generating pit construction, by domestic water flushing supply (Heisui River) and other give birth to
Water (buck) is applied flexibly to separate.Buck is handled with self-purification system, and Heisui River and human and animal excreta are handled through anaerobic biogas generating pit, not only
The discharge amount, complexity and processing cost of sewage can be reduced, and to rural area cleaning new energy is developed, protection people occupies ring
Border, the sustainable development for promoting rural economy society etc. have great importance.Printing and dyeing sludge is that textile printing and dyeing factory gives birth in weaving
The sanitary sewage for producing living area discharge in the industrial wastewater that generates and factory in dyeing process, by sewage treatment plant using physics,
A kind of hybrid solid waste separated after chemical method processing；The ingredient origin of printing and dyeing sludge is more complicated, wherein
Contain the heavy metals such as a large amount of cadmium, mercury, lead, chromium, arsenic, nickel, zinc, copper, cyanide, pathogen, parasitic ovum, organic pollutant
Element and poisonous and harmful substance belong to one of dangerous solid waste of national regulation；Textile printing and dyeing enterprises quantity increases year by year,
Scale is increasing, and the discharge amount of the sanitary sewage in printing and dyeing industrial waste water and employee living area is increasing, the production of printing and dyeing sludge
Raw amount also increases sharply；The printing and dyeing sludge largely accumulated will not only occupy a large amount of soil, but also harmful components therein such as weight
Metal；Copper, chromium, arsenic, mercury, cadmium, lead, nickel, zinc, pathogen, parasitic ovum, organic pollutant and foul smell, which will become, influences city
The big public hazards of the one of environmental sanitation；It is mainly handled using burying method, to reduce the pollution to environment；But printing and dyeing are dirty
The comparison of ingredients of mud is complicated, and moisture content is high, especially heavy metal, if unprocessed direct landfill, it will contaminated soil and underground
Water resource is easy to produce secondary pollution, causes to seriously endanger to environment.And the traditional Perlite filter agent used when filtering is also
There is a problem of that filter effect is bad, therefore, how to improve the bad disadvantage of the filter effect of traditional Perlite filter agent, in the hope of
It is problem to be solved that the Perlite filter agent with good comprehensive performance is developed in exploration.
Summary of the invention
The present invention solves the technical problem of：For the bad disadvantage of traditional Perlite filter agent filter effect, mention
A kind of preparation method of Perlite filter agent is supplied.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
A kind of preparation method of Perlite filter agent, specific preparation step are：
（1）By ethyl orthosilicate and water in mass ratio 1：8~1：10 mixing, and 2~5 times of ethyl orthosilicate quality anhydrous is added
Ethyl alcohol and 1~2 times of ethyl orthosilicate quality of hydrochloric acid, after being stirred, obtain silica precursor, by silica precursor
With ethanol water in mass ratio 1：8~1：12 mixing, and 2~4 times of silica precursor quality of perlite and two is added
The ammonium hydroxide that 1~3 times of siliconoxide precursor quality, is stirred, and filtering must pre-process perlite blank；
（2）Pretreatment perlite blank is calcined, cooling discharge obtains pretreatment perlite；Pretreatment perlite is pressed with toluene
Mass ratio 1：20~1：30 mixing, and the modifying agent of 0.3~0.6 times of perlite quality of pretreatment, after being stirred, mistake is added
Filter is washed, dry, obtains pre- modified pearl rock；
（3）By pre- modified pearl rock and carbon nanotube mixture in mass ratio 1：10~1：20 mixing, and pre- modified pearl is added
The graphene oxide solution that 3~5 times of rock quality, is stirred, and adjusts pH to 7.8~8.8, obtains pre- modified pearl rock mixture,
By pre- modified pearl rock mixture and polyethylene polyamine in mass ratio 8：1~12：1 mixing, and pre- modified pearl rock mixing is added
Aqueous solution of ester in 0.05~0.08 times of amount of substance of glucose sugar β, after being stirred, filters, stands, and freeze-drying must be modified treasure
Zhu Yan；
（4）By modified pearl rock and sodium hydroxide solution in mass ratio 1：8~1：10 mixing, impregnate, and filtering is washed to cleaning solution
It is dry for neutrality, obtain Perlite filter agent.
Step（1）The perlite partial size is 1~10 μm.
Step（2）The modifying agent is any one in aminopropyl triethoxysilane or trimethoxy γ-aminopropylsilane.
Step（3）The preparation method of the carbon nanotube mixture is by carbon nanotube and sulfuric acid in mass ratio 1：3~1：5
Mixing, and 3~6 times of carbon nanotube mass of nitric acid is added, after being stirred, filtering, being washed to cleaning solution is neutrality, it is dry,
Carbon nanotube must be pre-processed, by pretreatment carbon nanotube and Nanometer Copper in mass ratio 1：1~1：2 mixing, and pretreatment carbon is added
The ethylene glycol that 10~20 times of Nanotube quality after ultrasonic disperse, adjusts pH to 9.0~9.2, and be stirred, is centrifuged, filtering,
Washing, obtains modified carbon nano-tube, by modified carbon nano-tube and water in mass ratio 1：It is mixed to obtain carbon nanotube for 100 mixing, ultrasonic disperse
Close object.
Step（3）The graphene oxide solution is by graphene oxide and water in mass ratio 1：200~1：300 mixing,
Ultrasonic disperse obtains graphene oxide solution.
Step（3）The polyethylene polyamine is diethylenetriamine, any one in tetraethylenepentamine or diethylenetriamine.
The beneficial effects of the invention are as follows：
（1）The present invention mixes perlite with silica precursor when preparing Perlite filter agent, and it is solidifying that silica is made
Glue perlite mixture, and calcined silica dioxide gel perlite mixture is modified with modifying agent, on the one hand, it will
After silica precursor is mixed with perlite, silica dioxide granule can be adhered to inside perlite, to increase in perlite
The contact site in portion, and then increase perlite in modifying process to the adsorbance of graphene oxide and carbon nanotube, it improves
Porosity inside perlite, and then the filter effect of product is improved, on the other hand, with modifying agent to calcined silica
Gel perlite mixture, which is modified, can make the silica surface inside perlite with amino group, so as to receive with carbon
Mitron and graphene oxide generate Electrostatic Absorption, improve the content of modified perlite inner carbon nanotube and graphite oxide, into
And the porosity of interiors of products is improved, the filter effect of product improves, and the silica being added can be dipped in later period alkali
It is removed in journey, so that the porosity of interiors of products be made to further increase, improves the filter effect of product；
（2）The present invention uses carbon nanotube and graphene oxide when preparing Perlite filter agent, and modified with polyethylene polyamine,
On the one hand, carbon nanotube and graphene oxide being added can be adsorbed in abstract under the action of electrostatic force, and inside perlite
Network structure is formed, to make the filter effect of product improve, also, since carbon nano tube surface carries Nanometer Copper, not only
It can guarantee the hole inside perlite, and can make product that there is certain bactericidal effect, on the other hand, using polyethylene polyamine
Modified, the two-dimensional network structure that carbon nanotube and graphene oxide can be made to be formed becomes three-dimensional net structure, thus in product
Portion forms increasingly complex network structure, further increases the filter effect of product.
Specific embodiment
The sulfuric acid in mass ratio 1 for being 65~68% by carbon nanotube and mass fraction：3~1：5 are mixed in beaker, and to
The nitric acid that the mass fraction that 3~6 times of carbon nanotube mass are added in beaker is 65~68% is 70~80 DEG C in temperature, and revolving speed is
After being stirred 4~6h under conditions of 300~400r/min, filtering must pre-process carbon nanotube blank, will pre-process carbon nanometer
Blank is washed to cleaning solution as neutrality, and must pre-process carbon after 1~3h of vacuum drying under conditions of 70~80 DEG C of temperature and receive
Mitron, by pretreatment carbon nanotube and Nanometer Copper in mass ratio 1：1~1：2 are mixed in flask, and pre- place is added into flask
The ethylene glycol of 10~20 times of carbon nanotube mass of reason, under conditions of frequency is 45~55kHz after 30~40min of ultrasonic disperse,
With mass fraction be 8~12% sodium hydroxide solution adjust flask in material pH to 9.0~9.2, and in temperature be 90 DEG C,
Revolving speed be 300~500r/min under conditions of be stirred 4~5h after, by material in flask in revolving speed be 3000~4000r/
After being centrifuged 10~20min under conditions of min, filtering obtains filter cake, after filter cake is washed with deionized 8~10 times, obtains modification
Carbon nanotube, by modified carbon nano-tube and water in mass ratio 1：100 mixing, the ultrasound point under conditions of frequency is 45~55kHz
After dissipating 10~20min, carbon nanotube mixture is obtained；By ethyl orthosilicate and water in mass ratio 1：8~1：In 10 mixing, and to just
The dehydrated alcohol and ethyl orthosilicate quality 1~2 of 2~5 times of ethyl orthosilicate quality are added in the mixture of silester and water
The hydrochloric acid that mass fraction again is 10~15% is 30~45 DEG C in temperature, and revolving speed stirs under conditions of being 300~400r/min
After mixing 1~2h, silica precursor is obtained, the ethanol water for being 40~65% by silica precursor and mass fraction
In mass ratio 1：8~1：12 mixing, and into the mixture of silica precursor and ethanol water before addition silica
The ammonium hydroxide that 2~4 times of weight of perlite and 1~3 times of silica precursor quality of mass fraction are 15~20% is driven, in
Temperature is 30~40 DEG C, and after revolving speed is stirred 40~60min under conditions of being 280~380r/min, filtering must pre-process treasure
Pearl rock blank；Pretreatment perlite blank is moved into Muffle furnace, calcines 1~2h under conditions of being 400~500 DEG C in temperature
Afterwards, temperature of charge in Muffle furnace is down to room temperature discharging, obtains pretreatment perlite；Perlite and toluene will be pre-processed in mass ratio
1：20~1：30 mixing, and 0.3~0.6 times of perlite quality of pretreatment is added into the mixture of pretreatment perlite and toluene
Modifying agent, in temperature be 110~115 DEG C, revolving speed be 300~400r/min under conditions of be stirred 10~12h after, mistake
Filter, obtains filter residue, and after filter residue is successively washed 5~8 times with deionization and ethyl alcohol respectively, vacuum is dry under conditions of being 50 DEG C in temperature
After dry 1~2h, pre- modified pearl rock is obtained；By pre- modified pearl rock and carbon nanotube mixture in mass ratio 1：10~1：20 mixing
In reaction kettle, and the graphene oxide solution of 3~5 times of pre- modified pearl rock quality is added into reaction kettle, in temperature be 60
~70 DEG C, after revolving speed is stirred 3~5h under conditions of being 400~600r/min, the hydroxide for being 10~12% with mass fraction
Sodium solution adjusts the pH to 7.8~8.8 of material in reactor, obtains pre- modified pearl rock mixture, pre- modified pearl rock is mixed
Object and polyethylene polyamine in mass ratio 8：1~12：1 is mixed in blender, and pre- modified pearl rock is added into blender and mixes
Close 0.05~0.08 times of amount of substance mass fraction be 20~30% glucose sugar β in aqueous solution of ester, in temperature be 30~40 DEG C,
After revolving speed is stirred 2~4h under conditions of being 600~800r/min, filtering obtains modified pearl rock blank, by modified pearl rock
Blank under room temperature stand 20~for 24 hours after, freeze-drying, obtain modified pearl rock；It is by modified pearl rock and mass fraction
10~18% sodium hydroxide solution in mass ratio 1：8~1：10 mixing, after impregnating 2~3h under room temperature, filtering is obtained precious
Perlite filter agent blank is washed to cleaning solution as neutrality by pearl rock filtering agent blank, and in temperature be under conditions of 60 DEG C it is true
After the dry 3~4h of sky, Perlite filter agent is obtained.The perlite partial size is 1~10 μm.The modifying agent is three ethoxy of aminopropyl
Any one in base silane or trimethoxy γ-aminopropylsilane.The graphene oxide solution is that graphene oxide and water are pressed matter
Measure ratio 1：200~1：300 mixing, ultrasonic disperse obtain graphene oxide solution.The polyethylene polyamine be diethylenetriamine, four
Any one in five amine of ethylene or diethylenetriamine.
Example 1
The sulfuric acid in mass ratio 1 for being 68% by carbon nanotube and mass fraction：5 are mixed in beaker, and carbon is added into beaker and receives
The nitric acid that the mass fraction that 6 times of mitron quality is 68% is 80 DEG C in temperature, and revolving speed is stirred under conditions of being 400r/min
After 6h, filtering must pre-process carbon nanotube blank, pretreatment carbon nanotube blank is washed to cleaning solution as neutrality, and in temperature
After being dried in vacuo 3h under conditions of 80 DEG C of degree, pretreatment carbon nanotube is obtained, in mass ratio with Nanometer Copper by pretreatment carbon nanotube
1：2 are mixed in flask, and are added into flask and pre-process 20 times of carbon nanotube mass of ethylene glycol, in frequency be 55kHz's
Under the conditions of after ultrasonic disperse 40min, the pH to 9.2 of material in flask is adjusted with the sodium hydroxide solution that mass fraction is 12%, and
In temperature be 90 DEG C, revolving speed be 500r/min under conditions of be stirred 5h after, by material in flask in revolving speed be 4000r/min
Under conditions of be centrifuged 20min after, filtering, obtain filter cake, after filter cake is washed with deionized 10 times, obtain modified carbon nano-tube, will
Modified carbon nano-tube and water in mass ratio 1：100 mixing obtain carbon and receive under conditions of frequency is 55kHz after ultrasonic disperse 20min
Nanotube mixture；By ethyl orthosilicate and water in mass ratio 1：In 10 mixing, and add into the mixture of ethyl orthosilicate and water
Enter the hydrochloric acid that 5 times of ethyl orthosilicate quality of dehydrated alcohol and 2 times of ethyl orthosilicate quality of mass fraction are 15%, in temperature
Be 45 DEG C, revolving speed be 400r/min under conditions of be stirred 2h after, obtain silica precursor, by silica precursor with
The ethanol water in mass ratio 1 that mass fraction is 65%：12 mixing, and to the mixed of silica precursor and ethanol water
Closing and 4 times of silica precursor quality of perlite and 3 times of silica precursor quality of mass fraction are added in object is 20%
Ammonium hydroxide, in temperature be 40 DEG C, revolving speed be 380r/min under conditions of be stirred 60min after, filtering, obtain pretreatment perlite
Blank；Pretreatment perlite blank is moved into Muffle furnace, it, will be in Muffle furnace after calcining 2h under conditions of being 500 DEG C in temperature
Temperature of charge is down to room temperature discharging, obtains pretreatment perlite；It will pretreatment perlite and toluene in mass ratio 1：1：30 mixing, and
Pre-process 0.6 times of perlite quality of modifying agent to being added in the mixture of pretreatment perlite and toluene, in temperature be 115
DEG C, after revolving speed is stirred 12h under conditions of being 400r/min, filtering obtains filter residue, and filter residue is successively used to deionization and ethyl alcohol point
After being dried in vacuo 2h under conditions of being 50 DEG C in temperature, pre- modified pearl rock Xi Di not be obtained after 8 times；By pre- modified pearl rock with
Carbon nanotube mixture in mass ratio 1：20 are mixed in reaction kettle, and 5 times of pre- modified pearl rock quality is added into reaction kettle
Graphene oxide solution, in temperature be 70 DEG C, revolving speed be 600r/min under conditions of be stirred 5h after, be with mass fraction
12% sodium hydroxide solution adjusts the pH to 8.8 of material in reactor, pre- modified pearl rock mixture is obtained, by pre- modified pearl
Rock mixture and polyethylene polyamine in mass ratio 12：1 is mixed in blender, and pre- modified pearl rock is added into blender and mixes
Close 0.08 times of amount of substance mass fraction be 30% glucose sugar β in aqueous solution of ester, in temperature be 40 DEG C, revolving speed 800r/min
Under conditions of be stirred 4h after, filtering obtains modified pearl rock blank, by modified pearl rock blank in standing under room temperature
After for 24 hours, freeze-drying obtains modified pearl rock；By modified pearl rock and mass fraction be 18% sodium hydroxide solution in mass ratio
1：10 mixing, after impregnating 3h under room temperature, filtering obtains Perlite filter agent blank, and Perlite filter agent blank is washed
To cleaning solution be neutrality, and in temperature be 60 DEG C under conditions of be dried in vacuo 4h after, obtain Perlite filter agent.The perlite grain
Diameter is 10 μm.The modifying agent is aminopropyl triethoxysilane.The graphene oxide solution is by graphene oxide and water
In mass ratio 1：300 mixing, ultrasonic disperse obtain graphene oxide solution.The polyethylene polyamine is diethylenetriamine.
Example 2
The sulfuric acid in mass ratio 1 for being 68% by carbon nanotube and mass fraction：5 are mixed in beaker, and carbon is added into beaker and receives
The nitric acid that the mass fraction that 6 times of mitron quality is 68% is 80 DEG C in temperature, and revolving speed is stirred under conditions of being 400r/min
After 6h, filtering must pre-process carbon nanotube blank, pretreatment carbon nanotube blank is washed to cleaning solution as neutrality, and in temperature
After being dried in vacuo 3h under conditions of 80 DEG C of degree, pretreatment carbon nanotube is obtained, in mass ratio with Nanometer Copper by pretreatment carbon nanotube
1：2 are mixed in flask, and are added into flask and pre-process 20 times of carbon nanotube mass of ethylene glycol, in frequency be 55kHz's
Under the conditions of after ultrasonic disperse 40min, the pH to 9.2 of material in flask is adjusted with the sodium hydroxide solution that mass fraction is 12%, and
In temperature be 90 DEG C, revolving speed be 500r/min under conditions of be stirred 5h after, by material in flask in revolving speed be 4000r/min
Under conditions of be centrifuged 20min after, filtering, obtain filter cake, after filter cake is washed with deionized 10 times, obtain modified carbon nano-tube, will
Modified carbon nano-tube and water in mass ratio 1：100 mixing obtain carbon and receive under conditions of frequency is 55kHz after ultrasonic disperse 20min
Nanotube mixture；By ethyl orthosilicate and water in mass ratio 1：In 10 mixing, and add into the mixture of ethyl orthosilicate and water
Enter the hydrochloric acid that 5 times of ethyl orthosilicate quality of dehydrated alcohol and 2 times of ethyl orthosilicate quality of mass fraction are 15%, in temperature
Be 45 DEG C, revolving speed be 400r/min under conditions of be stirred 2h after, obtain silica precursor, by silica precursor with
The ethanol water in mass ratio 1 that mass fraction is 65%：12 mixing, and to the mixed of silica precursor and ethanol water
Closing and 4 times of silica precursor quality of perlite and 3 times of silica precursor quality of mass fraction are added in object is 20%
Ammonium hydroxide, in temperature be 40 DEG C, revolving speed be 380r/min under conditions of be stirred 60min after, filtering, obtain pretreatment perlite
Blank；Pretreatment perlite blank is moved into Muffle furnace, it, will be in Muffle furnace after calcining 2h under conditions of being 500 DEG C in temperature
Temperature of charge is down to room temperature discharging, obtains pretreatment perlite；It will pretreatment perlite and carbon nanotube mixture in mass ratio 1：
20 are mixed in reaction kettle, and the graphene oxide solution of 5 times of perlite quality of pretreatment is added into reaction kettle, are in temperature
70 DEG C, after revolving speed is stirred 5h under conditions of being 600r/min, reaction is adjusted with the sodium hydroxide solution that mass fraction is 12%
The pH to 8.8 of material, obtains pretreatment perlite mixture in kettle, and pretreatment perlite mixture and polyethylene polyamine are pressed quality
Than 12：1 is mixed in blender, and the mass fraction of 0.08 times of perlite mixture quality of addition pretreatment is into blender
Aqueous solution of ester in 30% glucose sugar β, in temperature be 40 DEG C, revolving speed be 800r/min under conditions of be stirred 4h after, filtering,
Modified pearl rock blank is obtained, by modified pearl rock blank after standing for 24 hours under room temperature, freeze-drying obtains modified pearl rock；
The sodium hydroxide solution in mass ratio 1 for being 18% by modified pearl rock and mass fraction：10 mixing, in impregnating 3h under room temperature
Afterwards, filter, obtain Perlite filter agent blank, by Perlite filter agent blank be washed to cleaning solution for neutrality, and in temperature be 60
After being dried in vacuo 4h under conditions of DEG C, Perlite filter agent is obtained.The perlite partial size is 10 μm.The modifying agent is aminopropyl
Triethoxysilane.The graphene oxide solution is by graphene oxide and water in mass ratio 1：300 mixing, ultrasonic disperse,
Obtain graphene oxide solution.The polyethylene polyamine is diethylenetriamine.
Example 3
By ethyl orthosilicate and water in mass ratio 1：In 10 mixing, and positive silicic acid is added into the mixture of ethyl orthosilicate and water
The hydrochloric acid that the dehydrated alcohol and 2 times of ethyl orthosilicate quality of mass fraction that 5 times of ethyl ester quality are 15% is 45 DEG C in temperature, turns
After speed is stirred 2h under conditions of being 400r/min, silica precursor is obtained, by silica precursor and mass fraction
For 65% ethanol water in mass ratio 1：12 mixing, and add into the mixture of silica precursor and ethanol water
Enter the ammonium hydroxide that 4 times of silica precursor quality of perlite and 3 times of silica precursor quality of mass fraction are 20%,
It is 40 DEG C in temperature, after revolving speed is stirred 60min under conditions of being 380r/min, filtering must pre-process perlite blank；It will
It pre-processes perlite blank to move into Muffle furnace, after calcining 2h under conditions of being 500 DEG C in temperature, by temperature of charge in Muffle furnace
It is down to room temperature discharging, obtains pretreatment perlite；It will pretreatment perlite and toluene in mass ratio 1：1：30 mixing, and to pretreatment
The modifying agent of 0.6 times of perlite quality of pretreatment is added in the mixture of perlite and toluene, is 115 DEG C in temperature, revolving speed is
After being stirred 12h under conditions of 400r/min, filtering obtains filter residue, filter residue is successively washed 8 times with deionization and ethyl alcohol respectively
Afterwards, after being dried in vacuo 2h under conditions of being 50 DEG C in temperature, pre- modified pearl rock is obtained；Pre- modified pearl rock is mixed with carbon nanotube
Close object in mass ratio 1：20 are mixed in reaction kettle, and the graphite oxide of 5 times of pre- modified pearl rock quality is added into reaction kettle
Alkene solution, in temperature be 70 DEG C, revolving speed be 600r/min under conditions of be stirred 5h after, with mass fraction be 12% hydrogen-oxygen
Change the pH to 8.8 that sodium solution adjusts material in reactor, obtain pre- modified pearl rock mixture, is added into blender pre- modified precious
Aqueous solution of ester in the glucose sugar β that the mass fraction of 0.08 times of pearl rock mixture quality is 30% is 40 DEG C in temperature, and revolving speed is
After being stirred 4h under conditions of 800r/min, filtering obtains modified pearl rock blank, by modified pearl rock blank in room temperature condition
It is lower standing for 24 hours after, freeze-drying, obtain modified pearl rock；The sodium hydroxide solution that modified pearl rock is 18% with mass fraction is pressed
Mass ratio 1：10 mixing, after impregnating 3h under room temperature, filtering obtains Perlite filter agent blank, by Perlite filter agent base
Material be washed to cleaning solution for neutrality, and in temperature be 60 DEG C under conditions of be dried in vacuo 4h after, obtain Perlite filter agent.The treasure
Pearl rock partial size is 10 μm.The modifying agent is aminopropyl triethoxysilane.The graphene oxide solution is by graphite oxide
Alkene and water in mass ratio 1：300 mixing, ultrasonic disperse obtain graphene oxide solution.
Example 4
The sulfuric acid in mass ratio 1 for being 68% by carbon nanotube and mass fraction：5 are mixed in beaker, and carbon is added into beaker and receives
The nitric acid that the mass fraction that 6 times of mitron quality is 68% is 80 DEG C in temperature, and revolving speed is stirred under conditions of being 400r/min
After 6h, filtering must pre-process carbon nanotube blank, pretreatment carbon nanotube blank is washed to cleaning solution as neutrality, and in temperature
After being dried in vacuo 3h under conditions of 80 DEG C of degree, pretreatment carbon nanotube is obtained, in mass ratio with Nanometer Copper by pretreatment carbon nanotube
1：2 are mixed in flask, and are added into flask and pre-process 20 times of carbon nanotube mass of ethylene glycol, in frequency be 55kHz's
Under the conditions of after ultrasonic disperse 40min, the pH to 9.2 of material in flask is adjusted with the sodium hydroxide solution that mass fraction is 12%, and
In temperature be 90 DEG C, revolving speed be 500r/min under conditions of be stirred 5h after, by material in flask in revolving speed be 4000r/min
Under conditions of be centrifuged 20min after, filtering, obtain filter cake, after filter cake is washed with deionized 10 times, obtain modified carbon nano-tube, will
Modified carbon nano-tube and water in mass ratio 1：100 mixing obtain carbon and receive under conditions of frequency is 55kHz after ultrasonic disperse 20min
Nanotube mixture；By ethyl orthosilicate and water in mass ratio 1：In 10 mixing, and add into the mixture of ethyl orthosilicate and water
Enter the hydrochloric acid that 5 times of ethyl orthosilicate quality of dehydrated alcohol and 2 times of ethyl orthosilicate quality of mass fraction are 15%, in temperature
Be 45 DEG C, revolving speed be 400r/min under conditions of be stirred 2h after, obtain silica precursor, by silica precursor with
The ethanol water in mass ratio 1 that mass fraction is 65%：12 mixing, and to the mixed of silica precursor and ethanol water
Closing and 4 times of silica precursor quality of perlite and 3 times of silica precursor quality of mass fraction are added in object is 20%
Ammonium hydroxide, in temperature be 40 DEG C, revolving speed be 380r/min under conditions of be stirred 60min after, filtering, obtain pretreatment perlite
Blank；Pretreatment perlite blank is moved into Muffle furnace, it, will be in Muffle furnace after calcining 2h under conditions of being 500 DEG C in temperature
Temperature of charge is down to room temperature discharging, obtains pretreatment perlite；It will pretreatment perlite and toluene in mass ratio 1：1：30 mixing, and
Pre-process 0.6 times of perlite quality of modifying agent to being added in the mixture of pretreatment perlite and toluene, in temperature be 115
DEG C, after revolving speed is stirred 12h under conditions of being 400r/min, filtering obtains filter residue, and filter residue is successively used to deionization and ethyl alcohol point
After being dried in vacuo 2h under conditions of being 50 DEG C in temperature, pre- modified pearl rock Xi Di not be obtained after 8 times；By pre- modified pearl rock with
Carbon nanotube mixture in mass ratio 1：20 are mixed in reaction kettle, and 5 times of pre- modified pearl rock quality is added into reaction kettle
Graphene oxide solution, in temperature be 70 DEG C, revolving speed be 600r/min under conditions of be stirred 5h after, be with mass fraction
12% sodium hydroxide solution adjusts the pH to 8.8 of material in reactor, obtains pre- modified pearl rock mixture, adds into blender
Enter 0.08 times of pre- modified pearl rock mixture quality mass fraction be 30% glucose sugar β in aqueous solution of ester, in temperature be 40
DEG C, after revolving speed is stirred 4h under conditions of being 800r/min, filtering obtains modified pearl rock blank, by modified pearl rock blank
After standing for 24 hours under room temperature, freeze-drying obtains modified pearl rock；The hydrogen-oxygen for being 18% by modified pearl rock and mass fraction
Change sodium solution in mass ratio 1：10 mixing, after impregnating 3h under room temperature, filtering obtains Perlite filter agent blank, by pearl
Rock filtering agent blank be washed to cleaning solution for neutrality, and in temperature be 60 DEG C under conditions of be dried in vacuo 4h after, obtain perlite mistake
Filtering agent.The perlite partial size is 10 μm.The modifying agent is aminopropyl triethoxysilane.The graphene oxide solution is
By graphene oxide and water in mass ratio 1：300 mixing, ultrasonic disperse obtain graphene oxide solution.
Comparative example：The Perlite filter agent of packet header Chemical Co., Ltd. production.
The resulting Perlite filter agent of 1 to 4 example of example and comparative example product are subjected to performance detection, specific detection method
It is as follows：
The detection of printing and dyeing sludge filtering agent：Referring to HG/T2825-2009 People's Republic of China (PRC) chemical industry《Granular carclazyte》Standard
Detection.
Specific testing result is as shown in table 1：
1 Perlite filter agent performance test results of table
By 1 testing result of table it is found that the Perlite filter agent of technical solution of the present invention preparation has the spy of excellent filter effect
Point has broad prospects in the development of material for water treatment technology industry.
Claims (6)
1. a kind of preparation method of Perlite filter agent, which is characterized in that specifically preparation step is：
（1）By ethyl orthosilicate and water in mass ratio 1：8~1：10 mixing, and 2~5 times of ethyl orthosilicate quality anhydrous is added
Ethyl alcohol and 1~2 times of ethyl orthosilicate quality of hydrochloric acid, after being stirred, obtain silica precursor, by silica precursor
With ethanol water in mass ratio 1：8~1：12 mixing, and 2~4 times of silica precursor quality of perlite and two is added
The ammonium hydroxide that 1~3 times of siliconoxide precursor quality, is stirred, and filtering must pre-process perlite blank；
（2）Pretreatment perlite blank is calcined, cooling discharge obtains pretreatment perlite；Pretreatment perlite is pressed with toluene
Mass ratio 1：20~1：30 mixing, and the modifying agent of 0.3~0.6 times of perlite quality of pretreatment, after being stirred, mistake is added
Filter is washed, dry, obtains pre- modified pearl rock；
（3）By pre- modified pearl rock and carbon nanotube mixture in mass ratio 1：10~1：20 mixing, and pre- modified pearl is added
The graphene oxide solution that 3~5 times of rock quality, is stirred, and adjusts pH to 7.8~8.8, obtains pre- modified pearl rock mixture,
By pre- modified pearl rock mixture and polyethylene polyamine in mass ratio 8：1~12：1 mixing, and pre- modified pearl rock mixing is added
Aqueous solution of ester in 0.05~0.08 times of amount of substance of glucose sugar β, after being stirred, filters, stands, and freeze-drying must be modified treasure
Zhu Yan；
（4）By modified pearl rock and sodium hydroxide solution in mass ratio 1：8~1：10 mixing, impregnate, and filtering is washed to cleaning solution
It is dry for neutrality, obtain Perlite filter agent.
2. a kind of preparation method of Perlite filter agent according to claim 1, it is characterised in that：Step（1）The treasure
Pearl rock partial size is 1~10 μm.
3. a kind of preparation method of Perlite filter agent according to claim 1, it is characterised in that：Step（2）It is described to change
Property agent be any one in aminopropyl triethoxysilane or trimethoxy γ-aminopropylsilane.
4. a kind of preparation method of Perlite filter agent according to claim 1, it is characterised in that：Step（3）The carbon
The preparation method of nanotube mixture is by carbon nanotube and sulfuric acid in mass ratio 1：3~1：5 mixing, and carbon nanotube matter is added
The nitric acid of 3~6 times of amount, after being stirred, filtering is washed to cleaning solution as neutrality, and drying obtains pretreatment carbon nanotube, will be pre-
Handle carbon nanotube and Nanometer Copper in mass ratio 1：1~1：2 mixing, and the second of 10~20 times of carbon nanotube mass of pretreatment is added
Glycol after ultrasonic disperse, adjusts pH to 9.0~9.2, and be stirred, is centrifuged, filters, and washing obtains modified carbon nano-tube, will
Modified carbon nano-tube and water in mass ratio 1：100 mixing, ultrasonic disperse obtain carbon nanotube mixture.
5. a kind of preparation method of Perlite filter agent according to claim 1, it is characterised in that：Step（3）The oxygen
Graphite alkene solution is by graphene oxide and water in mass ratio 1：200~1：300 mixing, ultrasonic disperse obtain graphene oxide
Solution.
6. a kind of preparation method of Perlite filter agent according to claim 1, it is characterised in that：Step（3）It is described more
Ethylene polyamine is diethylenetriamine, any one in tetraethylenepentamine or diethylenetriamine.
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