CN107364922A - The method that porous silica silicon composite handles waste water - Google Patents
The method that porous silica silicon composite handles waste water Download PDFInfo
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- CN107364922A CN107364922A CN201710763552.1A CN201710763552A CN107364922A CN 107364922 A CN107364922 A CN 107364922A CN 201710763552 A CN201710763552 A CN 201710763552A CN 107364922 A CN107364922 A CN 107364922A
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- Prior art keywords
- waste water
- solution
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- porous silica
- silicon composite
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Classifications
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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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/302—Treatment of water, waste water, or sewage by irradiation with microwaves
-
- 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
- C02F2101/345—Phenols
Abstract
The invention belongs to the method for technical field of nano material, more particularly to porous silica silicon composite processing waste water, MTES, water, absolute ethyl alcohol are mixed to prepare solution A and ZrCl4, the solution B mixing that is mixed to prepare of the dicarboxylic acids of 2,2 ' bipyridyl 5,5 ' and DMF solution heating, hydrochloric acid and concentrated ammonia liquor is added dropwise, stands, drying is soaked in the molten obtained porous silica silicon composite of iron chloride again, for the phenol in microwave degradation waste water；The waste water that phenol content is more than 100mg/L can be handled, phenol degrading rate is up to more than 99%, and degradation speed only needs 5 10 minutes, energy-efficient, and waste water can directly carry out microwave degradation without specially treated；Reused after novel porous silicon dioxide composite material is renewable used by the method for the present invention, degradation rate maintains more than 98% substantially after recycling, cost-effective.
Description
Technical field
The invention belongs to the side of technical field of nano material, more particularly to porous silica silicon composite processing waste water
Method.
Background technology
Because the property that single material nanoparticle system has is limited, the nanostructured complex of several material assemblings
The embodied value of system is highlighted, and the compound applications to nanostructures of widening multiple material carried out on nanoscale is led
Domain.Porous silica internal surface area is big, and pore diameter range is larger, thus is widely used in catalyst and absorption carrier.
Phenol is the raw material and intermediate of the industry productions such as papermaking, coking, oil refining, plastics, agricultural chemicals, medicine synthesis, containing phenol
Harm of the waste water to the mankind is very serious；Phenol in wastewater processing method typically uses photocatalytic degradation or microbial degradation at present
Method, but there is complex disposal process in existing method, the defects such as phenol conversion is low.
The content of the invention
The present invention solves above-mentioned technical problem present in prior art, there is provided at a kind of porous silica silicon composite
The method for managing waste water.
To solve the above problems, technical scheme is as follows：
The method that porous silica silicon composite handles waste water, comprises the following steps：
S1, MTES, water, absolute ethyl alcohol be well mixed, obtained solution A；The methyl triethoxy
Silane, water, the volume ratio of absolute ethyl alcohol are 1-1.5:2:0.2；
S2, by ZrCl4, 2,2 '-bipyridyl 5,5 '-dicarboxylic acids and DMF solution stir 4-8 hours under the conditions of 80-90 DEG C,
Obtained solution B；ZrCl in the solution B4, 2,2 '-bipyridyl 5,5 '-dicarboxylic acids concentration be 0.005-0.01mmol/mL；
S3, after the solution A is well mixed in equal volume with solution B, be added dropwise salt acid for adjusting pH be 3-4, dropwise addition concentrated ammonia liquor,
After stirring, more than 4 hours are stood, dries and solid A is made；
S4, the solid A is immersed in ferric chloride solution more than 4 hours, dries and porous silica composite wood is made
Material；
S5, the waste water containing phenol is added filled in the container of porous silica silicon composite, be placed in microwave reactor
In, degraded removes the phenol in waste water.
Preferably, the drying procedure of the step 3 is that 2-4 hours are heated under the conditions of 40-60 DEG C；Switch to 80-100 DEG C
Under the conditions of heat 2-4 hours；2-4 hours are heated under the conditions of switching to 120-140 DEG C.
Preferably, the drying procedure of the step 4 is that 2-4 hours are heated under the conditions of 70-90 DEG C
Preferably, ferric chloride solution concentration is 0.8-2mol/L in the step 4.
Preferably, the condition of step 5 microwave reaction is：Power is 700-1000W, reaction time 5-10min.
Preferably, container described in step 5 is consistent with capsule internal shapes used in step 3 so that porous silica is compound
Material is filled up completely with container, and the waste water of addition obtains optimal drop completely into the hole of porous silica silicon composite
Solve efficiency.
Preferably, for renewable after wastewater treatment, the renovation process is the porous silica silicon composite：
Soaked more than 4 hours in ferric chloride solution, ferric chloride solution concentration is 0.8-2mol/L.
Preferably, phenol in wastewater content described in step 5 is more than 100mg/L.
Relative to prior art, advantages of the present invention is as follows,
The present invention can be handled phenol content and be more than using the phenol in novel porous silicon dioxide composite material processing waste water
100mg/L waste water, phenol degrading rate are up to more than 99%, and degradation speed only needs 5-10 minutes, energy-efficient, waste water without
Specially treated is crossed, can directly carry out microwave degradation；
Novel porous silicon dioxide composite material preparing raw material is green used by the method for the present invention, preparation method
Simply, mild condition, suitable for industrial production；
Reused after novel porous silicon dioxide composite material is renewable used by the method for the present invention, recycling
Degradation rate maintains more than 98% substantially afterwards, cost-effective；
The renovation process of novel porous silicon dioxide composite material is simple to operate used by the method for the present invention, soaks 4
It can be re-used again after hour, quickness and high efficiency.
Embodiment
Embodiment 1：
Phenol in porous silica silicon composite processing waste water, comprises the following steps：
S1, MTES, water, absolute ethyl alcohol be well mixed, obtained solution A；The methyl triethoxy
Silane, water, the volume ratio of absolute ethyl alcohol are 1.2:2:0.2；
S2, by ZrCl4, 2,2 '-bipyridyl 5,5 '-dicarboxylic acids and DMF solution stir 8 hours under the conditions of 80-90 DEG C, system
Obtain solution B；ZrCl in the solution B4, 2,2 '-bipyridyl 5,5 '-dicarboxylic acids concentration be 0.006mmol/mL；
S3, after the solution A is well mixed in equal volume with solution B, be added dropwise salt acid for adjusting pH be 3-4, dropwise addition concentrated ammonia liquor,
After stirring, more than 4 hours are stood, is heated 3 hours under the conditions of 40-60 DEG C；Heating 3 is small under the conditions of switching to 80-100 DEG C
When；Heated 3 hours under the conditions of switching to 120-140 DEG C, dry and solid A is made；
S4, the solid A is immersed in concentration for more than 4 hours in 1.4mol/L ferric chloride solutions, in 70-90 DEG C of condition
Lower heating 2-4 hours, dry and porous silica silicon composite is made；
S5, the waste water of the 176mg/L containing phenol added fill the container of porous silica silicon composite (i.e. step 3 is quiet
Put container used) in, it is placed in microwave reactor, the condition of microwave reaction is：Power is 800W, reaction time 7min, is dropped
Solution removes the phenol in waste water, and phenol content C in water is detected after the completion of reaction.
Embodiment 2：
Phenol in porous silica silicon composite processing waste water, step is with embodiment 1, except that changing step
MTES, water, the volume ratio of absolute ethyl alcohol are in 1：
A groups：1:2:0.2
B groups：1.5:2:0.2
C groups：0.5:2:0.2
D groups：2:2:0.2
Embodiment 3：
Phenol in porous silica silicon composite processing waste water, step is with embodiment 1, except that changing step
ZrCl in 24, 2,2 '-bipyridyl 5,5 '-dicarboxylic acids concentration be：
A groups：0.01mmol/mL
B groups：0.015mmol/mL
C groups：0.003mmol/mL
Embodiment 4：
Phenol in porous silica silicon composite processing waste water, step is with embodiment 1, except that changing step
ZrCl in 24Mixing time with 2,2 '-bipyridyl 5,5 '-dicarboxylic acids is：
A groups：4 hours
B groups：2 hours
C groups：16 hours
Embodiment 5：
Phenol in porous silica silicon composite processing waste water, step is with embodiment 1, except that changing step
Drying procedure is in 3：
A groups：Heated 9 hours under the conditions of 40-60 DEG C,
B groups：Heated 9 hours under the conditions of 80-100 DEG C,
C groups：Heated 9 hours under the conditions of 120-140 DEG C,
Embodiment 6：
Phenol in porous silica silicon composite processing waste water, step is with embodiment 1, except that changing step
The concentration of ferric chloride solution is in 4：
A groups：0.8mol/L；
B groups：2.0mol/L；
C groups：0.4mol/L；
D groups：2.8mol/L；
Embodiment 7：
Phenol in porous silica silicon composite processing waste water, step is with embodiment 1, except that changing step
Microwave reaction condition is in 5：
A groups：Power is 700W, reaction time 10min
B groups：Power is 1000W, reaction time 5min
C groups：Power is 500W, reaction time 10min
D groups：Power is 1300W, reaction time 5min
Embodiment 8：
The degradation rate of phenol after calculating blank control group and embodiment 1-6 waste water microwave treatments：
Phenol degrading rate=(176-C)/176*100%
Blank control group is：The waste water of the 176mg/L containing phenol is added into empty container and (stands appearance used with the step 3 of embodiment 1
Device) in, it is placed in microwave reactor, the condition of microwave reaction is：Power is 800W, reaction time 7min, is detected afterwards in water
Phenol content C.
| Group | Phenol degrading rate % | Group | Phenol degrading rate % |
| Blank control | 1.3 | Embodiment 5 (A groups) | 98.7 |
| Embodiment 1 | 99.5 | Embodiment 5 (B groups) | 14.2 |
| Embodiment 2 (A groups) | 99.2 | Embodiment 5 (C groups) | 11.4 |
| Embodiment 2 (B groups) | 98.9 | Embodiment 6 (A groups) | 98.6 |
| Embodiment 2 (C groups) | 35.7 | Embodiment 6 (B groups) | 99.6 |
| Embodiment 2 (D groups) | 45.4 | Embodiment 6 (C groups) | 78.4 |
| Embodiment 3 (A groups) | 99.1 | Embodiment 6 (D groups) | 99.6 |
| Embodiment 3 (B groups) | 25.1 | Embodiment 7 (A groups) | 99.1 |
| Embodiment 3 (C groups) | 31.2 | Embodiment 7 (B groups) | 99.3 |
| Embodiment 4 (A groups) | 99.0 | Embodiment 7 (C groups) | 65.2 |
| Embodiment 4 (B groups) | 52.1 | Embodiment 7 (D groups) | 99.3 |
| Embodiment 4 (C groups) | 41.9 |
Embodiment 8：
Regenerated after porous silica silicon composite used in embodiment 1 is used for into wastewater treatment, renovation process is：
Concentration is to be soaked more than 4 hours in 1.4mol/L ferric chloride solutions, and after being washed with clear water, injection is useless containing the 176mg/L containing phenol
Water is added in the container (i.e. step 3 stands container used) for filling porous silica silicon composite, is placed in microwave reactor,
The condition of microwave reaction is：Power is 800W, and reaction time 7min, phenol degrading rate is 98.7%.
It should be noted that above-described embodiment is only presently preferred embodiments of the present invention, it is not used for limiting the present invention's
Protection domain, the equivalent substitution or replacement made on the basis of the above belong to protection scope of the present invention.
Claims (7)
1. the method that porous silica silicon composite handles waste water, it is characterised in that comprise the following steps：
S1, MTES, water, absolute ethyl alcohol be well mixed, obtained solution A；The MTES,
Water, the volume ratio of absolute ethyl alcohol are 1-1.5:2:0.2；
S2, by ZrCl4, 2,2 '-bipyridyl 5,5 '-dicarboxylic acids and DMF solution stir 4-8 hours under the conditions of 80-90 DEG C, be made
Solution B；ZrCl in the solution B4, 2,2 '-bipyridyl 5,5 '-dicarboxylic acids concentration be 0.005-0.01mmol/mL；
S3, after the solution A is well mixed in equal volume with solution B, be added dropwise salt acid for adjusting pH be 3-4, be added dropwise concentrated ammonia liquor, stir
After uniformly, more than 4 hours are stood, dries and solid A is made；
S4, the solid A is immersed in ferric chloride solution more than 4 hours, dries and porous silica silicon composite is made；
S5, the waste water containing phenol is added filled in the container of porous silica silicon composite, be placed in microwave reactor, drop
Solution removes the phenol in waste water.
2. the method as described in claim 1, it is characterised in that the drying procedure of the step 3 is, under the conditions of 40-60 DEG C
Heat 2-4 hours；2-4 hours are heated under the conditions of switching to 80-100 DEG C；2-4 hours are heated under the conditions of switching to 120-140 DEG C.
3. the method as described in claim 1, it is characterised in that the drying procedure of the step 4 is, under the conditions of 70-90 DEG C
Heat 2-4 hours.
4. the method as described in claim 1, it is characterised in that ferric chloride solution concentration is 0.8-2mol/L in the step 4.
5. the method as described in claim 1, it is characterised in that the condition of step 5 microwave reaction is：Power is 700-
1000W, reaction time 5-10min.
6. the method as described in claim 1, it is characterised in that container described in step 5 and capsule internal shapes one used in step 3
Cause.
7. the method as described in claim 1, it is characterised in that after the porous silica silicon composite is used for wastewater treatment
Renewable, the renovation process is：Soaked more than 4 hours in ferric chloride solution.
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| CN201710763552.1A CN107364922A (en) | 2017-08-30 | 2017-08-30 | The method that porous silica silicon composite handles waste water |
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| CN201710763552.1A CN107364922A (en) | 2017-08-30 | 2017-08-30 | The method that porous silica silicon composite handles waste water |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008045948A2 (en) * | 2006-10-10 | 2008-04-17 | Steward Environmental Solutions, Llc | Adsorbent composition and method of making same |
| CN101633505A (en) * | 2009-08-25 | 2010-01-27 | 郑文芝 | SiO2 nanoscale porous material with aerogel property prepared by microwave reaction and preparation method thereof |
| CN102921466A (en) * | 2012-10-30 | 2013-02-13 | 上海师范大学 | Heterogeneous Au/Ze-MOF catalyst and preparation method and application thereof |
-
2017
- 2017-08-30 CN CN201710763552.1A patent/CN107364922A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008045948A2 (en) * | 2006-10-10 | 2008-04-17 | Steward Environmental Solutions, Llc | Adsorbent composition and method of making same |
| CN101633505A (en) * | 2009-08-25 | 2010-01-27 | 郑文芝 | SiO2 nanoscale porous material with aerogel property prepared by microwave reaction and preparation method thereof |
| CN102921466A (en) * | 2012-10-30 | 2013-02-13 | 上海师范大学 | Heterogeneous Au/Ze-MOF catalyst and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| LIJIN 等: "Preparation of Methyltrimethoxysilane Derived Silica Aerogel", 《RARE METAL MATERIALS AND ENGINEERING 》 * |
| 区泳聪等: "两个基于2，2′-联吡啶-5，5′-二羧酸配体构筑的碱土金属配合物的合成、晶体结构及其光致发光性质", 《无机化学学报》 * |
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