CN106378087A - Preparation method of nano composite adsorbing material as well as adsorbent and treatment method used for treating trihydroxy triphenylmethane substance in wastewater - Google Patents
Preparation method of nano composite adsorbing material as well as adsorbent and treatment method used for treating trihydroxy triphenylmethane substance in wastewater Download PDFInfo
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- CN106378087A CN106378087A CN201611028903.6A CN201611028903A CN106378087A CN 106378087 A CN106378087 A CN 106378087A CN 201611028903 A CN201611028903 A CN 201611028903A CN 106378087 A CN106378087 A CN 106378087A
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- nano composite
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- triphenylmethane
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0296—Nitrates of compounds other than those provided for in B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
Abstract
The invention provides a preparation method of a nano composite adsorbing material as well as an adsorbent and a treatment method used for treating a trihydroxy triphenylmethane substance in wastewater. The nano composite adsorbing material is prepared by using SrCO3, Bi(NO3).5H2O and C3H6N6 as mixed raw materials and through the following steps of confecting the mixed raw materials to be an aqueous solution, drying the aqueous solution for 1h to 2h at 60 DEG C to 80 DEG C, calcining an obtained first product for 4h to 6h at 400 DEG C to 700 DEG C, then cooling and grinding an obtained second product, and the like. Components of the adsorbent used for treating the trihydroxy triphenylmethane substance in the wastewater comprise the nano composite adsorbing material; during specific treatment, the adsorbent used for treating the trihydroxy triphenylmethane substance in the wastewater is added into the wastewater to carry out the treatment. The nano composite adsorbing material provided by the invention is high in the selective adsorbability on the trihydroxy triphenylmethane substance in the wastewater, is further high in adsorption capacity, and has an adsorption rate, which is up to 93.85 percent, to crystal violet; an unexpected selective adsorption effect is acquired.
Description
Technical field
The invention belongs to sorbing material technical field is and in particular to the preparation method of nano composite adsorption material, be used for locating
The adsorbent of trihydroxy triphenylmethane material and processing method in reason waste water.
Background technology
Developing rapidly of social economy leads to water environment pollution to become increasingly conspicuous.It is presently used for the major technique of wastewater treatment
Active sludge, membrane separation process, electrochemical process etc..Absorption method wherein based on sorbing material is because processing pollutant efficiency
High, operating cost is few, processing speed is fast, strong adaptability the features such as be still widely used so far.
Mainly active charcoal, activated alumina, diatomite, zeolite, diatomite, shitosan, the absorption of traditional sorbing material
Resin etc..But these sorbing material generally existings absorption non-selectivity, regeneration difficulty, the low defect of adsorption capacity.Nano material
The big feature of specific surface area becomes the first-selection of novel absorption material, and nano material, with the reduction of particle diameter, compares table
Area increases sharply, and adsorption effect is better, and how to prepare the little nano material of particle diameter is that it becomes the key of sorbing material, nanometer
The Selective adsorption of material is also the important indicator determining its absorption property.But still there is no the nano adsorption material of excellent performance at present
Material exists, and therefore, researcher is still finding efficient, single-minded novel absorption material for above fault in material.
Content of the invention
For deficiencies of the prior art, the technical problem to be solved in the present invention is：Inhale in prior art
The low problem of enclosure material absorption non-selectivity, adsorption capacity, and the nano combined suction that a kind of adsorption capacity is high, selectivity is good is provided
The preparation method of enclosure material, for processing the adsorbent of trihydroxy triphenylmethane material and processing method in waste water.
In order to solve above-mentioned technical problem, the present invention adopts the following technical scheme that：A kind of system of nano composite adsorption material
Preparation Method, comprises the steps：
1）With SrCO3、Bi(NO3)3·5H2O and C3H6N6For mixed material, to be made into mixing molten by soluble in water for described mixed material
Liquid；Wherein, described SrCO3、Bi(NO3)3·5H2O and C3H6N6Mass ratio be 1 ~ 3：1~5：1~10；
2）By step 1）The mixed solution prepared is placed in drying 1 ~ 2 h at 60 ~ 80 DEG C, obtains drying mixing material；
3）By step 2）The drying mixing material obtaining calcines 4 ~ 6 h at 400 ~ 700 DEG C, obtains calcined materials；
4）To step 3）The calcined materials obtaining carry out pulverization process, obtain described nano composite adsorption material.
Class graphite type carbon nitride in prior art（Graphitic carbon nitride, g-C3N4）Polymer have with
Layer structure as graphite-like, layer is be made up of C3N3 ring or C6N7 ring, is connected to form one layer infinitely by N atom between ring
The plane of extension, is then to be combined by weak Van der Waals force between layers, most of inorganic compounds and inorganic metal from
Son can in conjunction with or be inserted into g-C3N4In matrix, change its intrinsic property, improve its use category in catalytic field, often
It is used as photochemical catalyst field.SrCO3It is widely used in the fields such as color television cathode ray tube, electromagnet, strontium ferrite, bismuth system
Compound has superior photocatalysis performance and is commonly used to research as photochemical catalyst by forefathers.Those skilled in the art so far
Be all pay close attention to above-mentioned be three kinds of materials photocatalysis performance）Do not had and adopted class graphite type carbon nitride, SrCO3With bismuth system
Compound prepares the correlative study of nano adsorption material, do not have in prior art yet correlative study prove class graphite type carbon nitride,
SrCO3Can serve as adsorbent preparing raw material with bismuth based compound for preparing the nano adsorption material with excellent adsorption function
Material.The present invention breaks through class graphite type carbon nitride, SrCO in prior art3It is only used as the normal of photochemical catalyst raw material with bismuth based compound
Rule understanding, in research class graphite type carbon nitride, SrCO3Accidental with during three kinds of Material claddings making catalysis materials of bismuth based compound
Find that the material being obtained does not have good photocatalysis performance, but there is prominent efficacy of adsorption, research finds to be based on g-C3N4's
Layer structure and SrCO3, the property that possesses of bismuth based compound, change the crystal formation knot of material by the method for calcining
Structure, surface group etc., so that this compound system has excellent adsorption capacity, especially have well to the organic dyestuff in waste water
Selection adsorption effect, achieve unexpected nano adsorption effect.
Further, step 1）Described in mixed material gross mass and described water mass volume ratio >=1:10.Such
Consumption, can both meet and make mixed material spread more evenly across the requirement being blended in water, and turn avoid water consumption and excessively lead to
Long problem of follow-up drying time.
Further, step 1）Middle by described mixed material be placed in water ultrasonic disperse process 10 ~ 20 min, be made into mixing molten
Liquid.The method being processed using ultrasonic disperse, can effectively improve dispersion efficiency, make solute more sufficiently thoroughly be dissolved in mixing
In solution, mixed performance is more preferable.
Further, step 1）Described in SrCO3、Bi(NO3)3·5H2O and C3H6N6Mass ratio be 1:1:3.Using so
Mass ratio so that the sorbing material arriving is to the adsorption effect of trihydroxy triphenylmethane material more preferably, to crystal violet
Adsorption effect, up to 93.85%, achieves excellent adsorption effect.
As optimization, step 3）In will dry mixing material and calcine 4 h at 550 DEG C.Using such calcination time and
Calcining heat, can make the crystalline structure after composite calcining be better able to meet the requirement of high adsorption effect.
A kind of adsorbent for processing trihydroxy triphenylmethane material in waste water, its component includes said method and is obtained
Nano composite adsorption material.Such use in waste water treatment adsorbent is inhaled compared to activated carbon of the prior art, diatomite etc.
Attached dose of Selective adsorption is higher, especially has high selection adsorptivity to the trihydroxy triphenylmethane material in waste water, to printing and dyeing
The trihydroxy triphenylmethane material adsorption capacity such as various crystal violets in waste water is high, and high treating effect, compared to existing printing and dyeing
In waste water, trihydroxy triphenylmethane material process adsorbent achieves unexpected adsorption treatment effect.
The processing method of trihydroxy triphenylmethane material in a kind of waste water, is used for processing trihydroxy three in waste water by described
The adsorbent of phenylmethane class material adds process 15 ~ 120 min in waste water；Wherein, the mass body of described adsorbent and waste water
Long-pending ratio is 0.2 ~ 1.0 g：1000 mL.According to such processing method, the trihydroxy triphenylmethane material in waste water is carried out
Adsorption treatment, both ensure that adsorption treatment effect was good, shortened the process of trihydroxy triphenylmethane material in existing waste water again
Time, there are good market prospects.
As optimization, described adsorbent is 1.0 g with the mass volume ratio of waste water：1000 mL, process time is 90
min.Under such treatment conditions, adsorption effect is best.
As optimization, described organic dyestuff is crystal violet.The inventive method is best to the removal effect of crystal violet, to crystallization
Purple adsorption efficiency is up to 93.85%.
Compared to existing technology, the present invention has the advantages that：The inventive method breaks through class graphite mould in prior art
Carbonitride, SrCO3It is only used as the conventional understanding of photochemical catalyst raw material with bismuth based compound, based on g-C3N4Layer structure and
SrCO3, the collaborative compatibility effect of bismuth based compound, calcining the nano adsorption material with high selectivity, high-adsorption-capacity has been obtained
Material, this nano adsorption material is strong to the trihydroxy triphenylmethane material Selective adsorption in waste water, advantages of good adsorption effect, especially right
The adsorption rate of crystal violet is up to 93.85%, achieves unexpected adsorption treatment effect.And the letter of the inventive method preparation process
Single, short for simple operation, process time during wastewater treatment, there is good industrialized production and market application foreground.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail.The implementation case with the technology of the present invention is being
Under the premise of implemented, now provide detailed embodiment and specific operating process be creative the present invention to be described, but
Protection scope of the present invention is not limited to below example.
Embodiment 1：
A kind of preparation method of nano composite adsorption material, comprises the steps：
1）Take 4.5 g SrCO respectively3、4.5g Bi(NO3)3·5H2O、9.0g C3H6N6As mixed material, by mixed material
It is dissolved in 15 mL deionized waters, then ultrasonic disperse 15 min makes it mix, and obtains mixed solution.
2）By step 1）The mixed solution obtaining is placed in 60 DEG C of baking ovens, dries 1.5 h, many in mixed solution to remove
Remaining moisture, obtains drying mixing material.
3）By step 2）Dry mixing material and be placed in calcining in Muffle furnace, temperature is set as 550 DEG C, calcination time is 4h,
Obtain calcined materials.
4）Treat step 3）After the calcined materials obtaining are cooled to room temperature, with mortar finely ground after, obtain final product the nano combined of preparation
Sorbing material.
The present embodiment additionally provides a kind of adsorbent for processing trihydroxy triphenylmethane material in waste water, its component
The nano composite adsorption material being obtained for the present embodiment said method.
The crystal violet that this adsorbent being used for processing trihydroxy triphenylmethane material in waste water is added into 10 mg/L is molten
Liquid（The waste water containing organic dyestuff for the simulation）In, described adsorbent is 1.0g with the mass volume ratio of crystal violet solution：1000
ML, carries out adsorption treatment 135 min at 25 DEG C to crystal violet solution, and result shows using such processing method, to crystallization
Purple adsorption efficiency may be up to 93.85%, achieves prominent Selective adsorption and high-adsorption-capacity effect.
Embodiment 2：
A kind of preparation method of nano composite adsorption material, comprises the steps：
1）Take 2.0 g SrCO respectively3、2.0 g Bi(NO3)3·5H2O、14.0 g C3H6N6As mixed material, will mix former
Material is dissolved in 20 mL deionized waters, and then ultrasonic disperse 20 min makes it mix, and obtains mixed solution.
2）By step 1）The mixed solution obtaining is placed in 80 DEG C of baking ovens, dries 2 h, unnecessary in mixed solution to remove
Moisture, obtains drying mixing material.
3）By step 2）Dry mixing material and be placed in calcining in Muffle furnace, temperature is set as 550 DEG C, calcination time is 4h,
Obtain calcined materials.
4）Treat step 3）After the calcined materials obtaining are cooled to room temperature, finely ground with mortar, obtain final product the nano combined suction of preparation
Enclosure material.
The present embodiment additionally provides a kind of adsorbent for processing trihydroxy triphenylmethane material in waste water, its component
The nano composite adsorption material being obtained for the present embodiment said method.
The crystal violet that this adsorbent being used for processing trihydroxy triphenylmethane material in waste water is added into 10 mg/L is molten
Liquid（The waste water containing organic dyestuff for the simulation）In, described adsorbent is 1.0g with the mass volume ratio of crystal violet solution：1000
ML, carries out adsorption treatment 135 min at 25 DEG C to crystal violet solution, and result shows using such processing method, to crystallization
Purple adsorption efficiency may be up to 85.24%, achieves prominent Selective adsorption and high-adsorption-capacity effect.
Finally illustrate, above example only in order to technical scheme to be described and unrestricted, although with reference to relatively
Good embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to the skill of the present invention
Art scheme is modified or equivalent, the objective without deviating from technical solution of the present invention and scope, and it all should be covered at this
In the middle of the right of invention.
Claims (9)
1. a kind of preparation method of nano composite adsorption material is it is characterised in that comprise the steps：
1）With SrCO3、Bi(NO3)3·5H2O and C3H6N6For mixed material, to be made into mixing molten by soluble in water for described mixed material
Liquid；Wherein, described SrCO3、Bi(NO3)3·5H2O and C3H6N6Mass ratio be 1 ~ 3：1~5：1~10；
2）By step 1）The mixed solution prepared is placed in drying 1 ~ 2 h at 60 ~ 80 DEG C, obtains drying mixing material；
3）By step 2）The drying mixing material obtaining calcines 4 ~ 6 h at 400 ~ 700 DEG C, obtains calcined materials；
4）To step 3）The calcined materials obtaining carry out pulverization process, obtain described nano composite adsorption material.
2. according to claim 1 the preparation method of nano composite adsorption material it is characterised in that step 1）Described in mix
The gross mass of raw material and mass volume ratio >=1 of described water:10.
3. according to claim 1 the preparation method of nano composite adsorption material it is characterised in that step 1）Middle will be described mixed
Close raw material and be placed in water ultrasonic disperse process 10 ~ 20 min, be made into mixed solution.
4. according to claim 1 the preparation method of nano composite adsorption material it is characterised in that step 1）Described in
SrCO3、Bi(NO3)3·5H2O and C3H6N6Mass ratio be 1:1:3.
5. according to claim 1 the preparation method of nano composite adsorption material it is characterised in that step 3）Middle mixed by drying
Condensation material calcines 4 h at 550 DEG C.
6. a kind of adsorbent for processing trihydroxy triphenylmethane material in waste water is it is characterised in that its component includes weighing
Profit requires the nano composite adsorption material that 1 ~ 5 arbitrary methods described is obtained.
7. in a kind of waste water the processing method of trihydroxy triphenylmethane material it is characterised in that will be used for described in claim 6
The adsorbent processing trihydroxy triphenylmethane material in waste water adds process 15 ~ 120 min in waste water；Wherein, described suction
The attached dose of mass volume ratio with waste water is 0.2 ~ 1.0 g：1000 mL.
8. according to claim 7 in waste water the processing method of trihydroxy triphenylmethane material it is characterised in that described suction
The attached dose of mass volume ratio with waste water is 1.0 g：1000 mL, process time is 90 min.
9. according to claim 7 in waste water the processing method of trihydroxy triphenylmethane material it is characterised in that described three
Hydroxyl triphenylmethane material is crystal violet.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993571A (en) * | 2018-08-08 | 2018-12-14 | 重庆工商大学 | g-C3N4Application in/alkali salt composite photocatalyst material and its wastewater by photocatalysis |
| CN110280207A (en) * | 2019-07-02 | 2019-09-27 | 重庆工商大学 | Alkali salt/g-C3N4The application of composite adsorbing material and its absorption degradation triphenylmethane dye waste water |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993571A (en) * | 2018-08-08 | 2018-12-14 | 重庆工商大学 | g-C3N4Application in/alkali salt composite photocatalyst material and its wastewater by photocatalysis |
| CN110280207A (en) * | 2019-07-02 | 2019-09-27 | 重庆工商大学 | Alkali salt/g-C3N4The application of composite adsorbing material and its absorption degradation triphenylmethane dye waste water |
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| CN106378087B (en) | 2018-07-20 |
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