CN106955688A - A kind of method of preparation and use of attapulgite catalytic oxidant - Google Patents
A kind of method of preparation and use of attapulgite catalytic oxidant Download PDFInfo
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- CN106955688A CN106955688A CN201710244760.0A CN201710244760A CN106955688A CN 106955688 A CN106955688 A CN 106955688A CN 201710244760 A CN201710244760 A CN 201710244760A CN 106955688 A CN106955688 A CN 106955688A
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- attapulgite
- catalytic oxidant
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- waste water
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Classifications
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
-
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- 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
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
Abstract
The invention discloses a kind of method of preparation and use of attapulgite catalytic oxidant, belong to technical field of waste water processing.The present invention relates to content Concave-convex clay rod is first substantially modified processing, then again in its area load transition metal reagent, attapulgite catalytic oxidant is finally made, then the catalytic oxidant is applied to the wastewater treatment of dyestuff intermediate, preferable adsorption treatment is played a part of to the pollutant in waste water, the processing cost and intractability of waste water from dyestuff are greatly reduced, with preferable application value.
Description
Technical field
The present invention relates to technical field of waste water processing, and in particular to a kind of preparation of attapulgite catalytic oxidant and uses
Method.
Background technology
In the last thirty years, water body organism pollution becomes the new focus of countries in the world scientific circles and attention from government.It is organic
Although pollutant is most of, content is little in water, and the harm to the mankind is very big.Wherein, the discharge of dyeing waste water accounts for very big
Ratio, dyeing waste water is the waste water of printing and dyeing mill's discharge based on processing cotton, fiber crops, chemical fibre and its blending product, waste water water
It is larger, per 1 ton of dyeing and printing process, 100~200 tons of textile water consumption, wherein 80~90% turn into waste water.The notable spy of dyeing waste water
One of levy is to carry higher colourity.After biochemical treatment, effluent color dilution decreases, but still with deeper color and luster, it is difficult
To reach discharge standard.Therefore, decolouring is an important step in treatment of dyeing wastewater.The dyestuff product that the current whole world is used
Kind tens thousand of kinds are reached, wherein reactive dye are just used more and more widely because it is bright in colour, chromatogram is complete.But due to work
Property dyestuff physicochemical property become in dyeing waste water one of difficult dyestuff removed.In recent years, studied in decolorizing printing and dyeing waste water
In, micro-nano material gets most of the attention in the application of catalysis and absorption, and micro-nano material generally refers to material of the size in 1nm~10 μm
Expect, the peculiar performance such as small-size effect, skin effect and quantum effect of micro-nano material provides important material base.It is conventional
The active charcoal of the nano material for decolorizing printing and dyeing waste water, nano-metal-oxide etc., these materials have good decolouring
Effect, but all exist that cost of manufacture is high or reserves are limited, it is non-renewable the problem of.
Therefore, research and develop it is a kind of both there is preferable decolouring scavenging effect, and the oxide material of recoverable into
For the emphasis studied at present, it may have preferable application prospect and use value.
The content of the invention
For defect of the prior art, it is an object of the invention to provide a kind of preparation of attapulgite catalytic oxidant and
Application method, the attapulgite catalytic oxidant prepared not only has preferable adsorption effect, also with more aerobic
Dirty effect is eliminated, and the preparation method is simple and easy to apply, with preferable application value.
The present invention solves technical problem and adopted the following technical scheme that：
The present invention relates to a kind of preparation of attapulgite catalytic oxidant, comprise the following steps：
（1）A certain amount of attapulgite clay is weighed, is added in flask, 2mol/L watery hydrochloric acid is added, wherein, the addition of watery hydrochloric acid
Volume：Concave convex rod quality is 1mL：2g ~ 5g, is placed in 10 ~ 20min of ultrasound under 30 ~ 50 DEG C of Ultrasonic Conditions；
（2）Said mixture is subjected to vacuum filtration, and cleaned with distilled water, is then dried in vacuum drying chamber；
（3）Dried Concave-convex clay rod is placed in Muffle furnace 0.5 ~ 1h of roasting under the conditions of 300 ~ 500 DEG C, cooling is obtained
To modified Concave-convex clay rod；
（4）Modified Concave-convex clay rod is added in flask, transition metal salt solution is added, in 30 ~ 50 DEG C of ultrasonic waves
Under the conditions of 10 ~ 20min of ultrasound, then heating, drying；
（5）Concave-convex clay rod after drying is placed in Muffle 1 ~ 2h of kiln roasting, 200 ~ 300 mesh are then crushed to, institute is produced
State attapulgite catalytic oxidant.
Preferably, the step（2）In distillation water cleaning method include：Concave-convex clay rod after suction filtration is added and burnt
In cup, distilled water is added, ultrasound 5min under Ultrasonic Conditions is placed in, is repeated 2 times operation.
Preferably, the step（4）The middle modified Concave-convex clay rod used reacts with transition metal salt solution
The preceding ground processing of need, is ground to 100 ~ 200 mesh.
Preferably, the step（5）In Concave-convex clay rod roasting after be placed in drying box and be cooled to room temperature, Ran Houzai
Carry out pulverization process.
The present invention also designs a kind of method of attapulgite catalytic oxidant, comprises the following steps：
（1）200mL dye intermediate wastewaters are taken in there-necked flask, the pH value of regulation waste water is 6 ~ 8；
（2）Attapulgite catalytic oxidant is added into waste water, oxygen is led to while stirring, at room temperature 3 ~ 5h of stirring reaction, i.e.,
It can obtain the waste water of emission compliance.
Preferably, the step（2）In lead to oxygen speed control blebbing speed be 2 ~ 5/s.
Preferably, step（2）The addition quality of the attapulgite catalytic oxidant of middle addition need to be catalyzed oxygen for every liter of waste water
1 ~ 1.5g of agent.
Preferably, the step（2）In logical oxygen the step of be replaced by be added dropwise hydrogen peroxide.
Compared with prior art, the present invention has following beneficial effect：
（1）The attapulgite catalytic oxidant of the present invention prepared, because attapulgite specific surface area is big so that oxygen
Agent has higher adsorption bleaching activity；Due to attapulgite rich reserves, cost of manufacture is cheap；Further, since concave convex rod
Penus natural nano-material, environmental protection will not cause secondary pollution to environment, meet the requirement of environmentally friendly product, tool
There is preferable use value.
（2）Attapulgite catalytic oxidant of the present invention is applied to the processing of dye intermediate wastewater, can be effective
The COD value of waste water is reduced, the degradation rate of waste water is substantially increased, meanwhile, the processing cost and difficulty of waste water from dyestuff are reduced,
Ensure that waste water from dyestuff being capable of qualified discharge.
（3）The characteristics of attapulgite catalytic oxidant that the present invention is prepared also has repeatable utilize, substantially reduces
The use cost of oxidant, the raw material availability of raising is adapted to industrialization promotion, with preferable Practical significance.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.These embodiments be merely to illustrate the present invention and without
In limitation the scope of the present invention.
Embodiment 1：
A kind of method of preparation and use of attapulgite catalytic oxidant of the preferred embodiment of the present invention；
The preparation of attapulgite catalytic oxidant, comprises the following steps：
（1）A certain amount of attapulgite clay is weighed, is added in flask, 2mol/L watery hydrochloric acid is added, wherein, the addition of watery hydrochloric acid
Volume：Concave convex rod quality is 1mL：3g, is placed in ultrasound 15min under 40 DEG C of Ultrasonic Conditions；
（2）Said mixture is subjected to vacuum filtration, and cleaned with distilled water, is then dried in vacuum drying chamber；
（3）Dried Concave-convex clay rod is placed in Muffle furnace and is calcined 1h under the conditions of 400 DEG C, cools down, obtains modified
Concave-convex clay rod；
（4）Modified Concave-convex clay rod is added in flask, transition metal salt solution is added, in 40 DEG C of Ultrasonic Conditions
Lower ultrasonic 15min, then heating, drying；
（5）Concave-convex clay rod after drying is placed in the h of Muffle kiln roasting 1.5,300 mesh are then crushed to, produced described recessed
The native catalytic oxidant of convex rod.
Step（2）In distillation water cleaning method include：Concave-convex clay rod after suction filtration is added in beaker, adds and steams
Distilled water, is placed in ultrasound 5min under Ultrasonic Conditions, is repeated 2 times operation, the hydrochloric acid that will be attached on Concave-convex clay rod is washed.
Step（4）The middle modified Concave-convex clay rod used needs ground place before being reacted with transition metal salt solution
Reason, is ground to 200 mesh, and milled processed enables to the transition metal salt can be more uniformly adhered to Concave-convex clay rod
Surface, improve Concave-convex clay rod service efficiency.
Step（5）In Concave-convex clay rod roasting after be placed in drying box and be cooled to room temperature, then carry out again at crushing
Reason.
The application method of attapulgite catalytic oxidant, comprises the following steps：
（1）200mL dye intermediate wastewaters are taken in there-necked flask, the pH value of regulation waste water is 7；
（2）Attapulgite catalytic oxidant is added into waste water, oxygen is led to while stirring, at room temperature stirring reaction 4h, you can
Obtain the waste water of emission compliance.Wherein, wherein blebbing speed is 3/s, the addition matter of the attapulgite catalytic oxidant of addition
Measure needs catalytic oxidant 1.2g for every liter of waste water.
Embodiment 2：
A kind of method of preparation and use of attapulgite catalytic oxidant of the preferred embodiment of the present invention；
The preparation of attapulgite catalytic oxidant, comprises the following steps：
（1）A certain amount of attapulgite clay is weighed, is added in flask, 2mol/L watery hydrochloric acid is added, wherein, the addition of watery hydrochloric acid
Volume：Concave convex rod quality is 1mL：2g, is placed in ultrasound 10min under 50 DEG C of Ultrasonic Conditions；
（2）Said mixture is subjected to vacuum filtration, and cleaned with distilled water, is then dried in vacuum drying chamber；
（3）Dried Concave-convex clay rod is placed in Muffle furnace and is calcined 0.5h under the conditions of 500 DEG C, cools down, is modified
Concave-convex clay rod afterwards；
（4）Modified Concave-convex clay rod is added in flask, transition metal salt solution is added, in 50 DEG C of Ultrasonic Conditions
Lower ultrasonic 10min, then heating, drying；
（5）Concave-convex clay rod after drying is placed in Muffle kiln roasting 1h, 200 mesh are then crushed to, the bumps are produced
Rod soil catalytic oxidant.
Step（2）In distillation water cleaning method include：Concave-convex clay rod after suction filtration is added in beaker, adds and steams
Distilled water, is placed in ultrasound 5min under Ultrasonic Conditions, is repeated 2 times operation.
Step（4）The middle modified Concave-convex clay rod used needs ground place before being reacted with transition metal salt solution
Reason, is ground to 100 mesh.
Step（5）In Concave-convex clay rod roasting after be placed in drying box and be cooled to room temperature, then carry out again at crushing
Reason.
The application method of attapulgite catalytic oxidant, comprises the following steps：
（1）200mL dye intermediate wastewaters are taken in there-necked flask, the pH value of regulation waste water is 8；
（2）Attapulgite catalytic oxidant is added into waste water, oxygen is led to while stirring, at room temperature 3 ~ 5h of stirring reaction, i.e.,
It can obtain the waste water of emission compliance.Wherein, wherein blebbing speed is 2/s, the addition of the attapulgite catalytic oxidant of addition
Quality needs catalytic oxidant 1.5g for every liter of waste water.
Embodiment 3：
A kind of method of preparation and use of attapulgite catalytic oxidant of the preferred embodiment of the present invention；
The preparation method of attapulgite catalytic oxidant, comprises the following steps：
（1）A certain amount of attapulgite clay is weighed, is added in flask, 2mol/L watery hydrochloric acid is added, wherein, the addition of watery hydrochloric acid
Volume：Concave convex rod quality is 1mL：5g, is placed in ultrasound 20min under 30 DEG C of Ultrasonic Conditions；
（2）Said mixture is subjected to vacuum filtration, and cleaned with distilled water, is then dried in vacuum drying chamber；
（3）Dried Concave-convex clay rod is placed in Muffle furnace and is calcined 1h under the conditions of 300 DEG C, cools down, obtains modified
Concave-convex clay rod；
（4）Modified Concave-convex clay rod is added in flask, transition metal salt solution is added, in 30 DEG C of Ultrasonic Conditions
Lower ultrasonic 20min, then heating, drying；
（5）Concave-convex clay rod after drying is placed in Muffle kiln roasting 2h, 300 mesh are then crushed to, the bumps are produced
Rod soil catalytic oxidant.
Step（2）In distillation water cleaning method include：Concave-convex clay rod after suction filtration is added in beaker, adds and steams
Distilled water, is placed in ultrasound 5min under Ultrasonic Conditions, is repeated 2 times operation.
Step（4）The middle modified Concave-convex clay rod used needs ground place before being reacted with transition metal salt solution
Reason, is ground to 200 mesh.
Step（5）In Concave-convex clay rod roasting after be placed in drying box and be cooled to room temperature, then carry out again at crushing
Reason.
The application method of attapulgite catalytic oxidant, comprises the following steps：
（1）200mL dye intermediate wastewaters are taken in there-necked flask, the pH value of regulation waste water is 6；
（2）Attapulgite catalytic oxidant is added into waste water, oxygen is led to while stirring, at room temperature stirring reaction 5h, you can
Obtain the waste water of emission compliance.Wherein, wherein blebbing speed is 5/s, the addition matter of the attapulgite catalytic oxidant of addition
Measure needs catalytic oxidant 1g for every liter of waste water.
Embodiment 4：
A kind of method of preparation and use of attapulgite catalytic oxidant of the preferred embodiment of the present invention；
The preparation of attapulgite catalytic oxidant, comprises the following steps：
（1）A certain amount of attapulgite clay is weighed, is added in flask, 2mol/L watery hydrochloric acid is added, wherein, the addition of watery hydrochloric acid
Volume：Concave convex rod quality is 1mL：3g, is placed in ultrasound 15min under 40 DEG C of Ultrasonic Conditions；
（2）Said mixture is subjected to vacuum filtration, and cleaned with distilled water, is then dried in vacuum drying chamber；
（3）Dried Concave-convex clay rod is placed in Muffle furnace and is calcined 1h under the conditions of 400 DEG C, cools down, obtains modified
Concave-convex clay rod；
（4）Modified Concave-convex clay rod is added in flask, transition metal salt solution is added, in 40 DEG C of Ultrasonic Conditions
Lower ultrasonic 15min, then heating, drying；
（5）Concave-convex clay rod after drying is placed in Muffle kiln roasting 1.5h, 300 mesh are then crushed to, produced described recessed
The native catalytic oxidant of convex rod.
Step（2）In distillation water cleaning method include：Concave-convex clay rod after suction filtration is added in beaker, adds and steams
Distilled water, is placed in ultrasound 5min under Ultrasonic Conditions, is repeated 2 times operation.
Step（4）The middle modified Concave-convex clay rod used needs ground place before being reacted with transition metal salt solution
Reason, is ground to 200 mesh.
Step（5）In Concave-convex clay rod roasting after be placed in drying box and be cooled to room temperature, then carry out again at crushing
Reason.
The application method of attapulgite catalytic oxidant, comprises the following steps：
（1）200mL dye intermediate wastewaters are taken in there-necked flask, the pH value of regulation waste water is 7；
（2）Attapulgite catalytic oxidant is added into waste water, 10mL hydrogen peroxide is added dropwise while stirring, 1h, stirring reaction is added dropwise
3h, you can obtain the waste water of emission compliance.Wherein, the addition quality of the attapulgite catalytic oxidant of addition is that every liter of waste water is needed
Catalytic oxidant 1g.
The attapulgite catalytic oxidant prepared in summary not only has preferable adsorption effect, also with preferable
Decontamination effect is aoxidized, and the preparation method is simple and easy to apply, it is easy to use, with preferable application value.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substance of the present invention.
Claims (8)
1. a kind of preparation of attapulgite catalytic oxidant, it is characterised in that：Comprise the following steps：
（1）A certain amount of attapulgite clay is weighed, is added in flask, 2mol/L watery hydrochloric acid is added, wherein, the addition of watery hydrochloric acid
Volume：Concave convex rod quality is 1mL：2g ~ 5g, is placed in 10 ~ 20min of ultrasound under 30 ~ 50 DEG C of Ultrasonic Conditions；
（2）Said mixture is subjected to vacuum filtration, and cleaned with distilled water, is then dried in vacuum drying chamber；
（3）Dried Concave-convex clay rod is placed in Muffle furnace 0.5 ~ 1h of roasting under the conditions of 300 ~ 500 DEG C, cooling is obtained
To modified Concave-convex clay rod；
（4）Modified Concave-convex clay rod is added in flask, transition metal salt solution is added, in 30 ~ 50 DEG C of ultrasonic waves
Under the conditions of 10 ~ 20min of ultrasound, then heating, drying；
（5）Concave-convex clay rod after drying is placed in Muffle 1 ~ 2h of kiln roasting, 200 ~ 300 mesh are then crushed to, institute is produced
State attapulgite catalytic oxidant.
2. the preparation of attapulgite catalytic oxidant according to claim 1, it is characterised in that：The step（2）In
Distillation water cleaning method includes：Concave-convex clay rod after suction filtration is added in beaker, distilled water is added, is placed in Ultrasonic Conditions
Lower ultrasonic 5min, is repeated 2 times operation.
3. the preparation of attapulgite catalytic oxidant according to claim 1, it is characterised in that：The step（4）In make
Modified Concave-convex clay rod needs ground processing before being reacted with transition metal salt solution, it is ground to 100 ~
200 mesh.
4. the preparation of attapulgite catalytic oxidant according to claim 1, it is characterised in that：The step（5）In
It is placed in after Concave-convex clay rod roasting in drying box and is cooled to room temperature, pulverization process is then carried out again.
5. the method for the attapulgite catalytic oxidant that one kind is obtained using such as any one of claim 1 ~ 4 preparation method, it is special
Levy and be：Comprise the following steps：
（1）200mL dye intermediate wastewaters are taken in there-necked flask, the pH value of regulation waste water is 6 ~ 8；
（2）Attapulgite catalytic oxidant is added into waste water, oxygen is led to while stirring, at room temperature 3 ~ 5h of stirring reaction, i.e.,
It can obtain the waste water of emission compliance.
6. the application method of attapulgite catalytic oxidant according to claim 5, it is characterised in that：The step（2）
In lead to oxygen speed control blebbing speed be 2 ~ 5/s.
7. the application method of attapulgite catalytic oxidant according to claim 5, it is characterised in that：Step（2）In plus
The addition quality of the attapulgite catalytic oxidant entered needs 1 ~ 1.5g of catalytic oxidant for every liter of waste water.
8. the application method of attapulgite catalytic oxidant according to claim 5, it is characterised in that：The step（2）
In logical oxygen the step of be replaced by be added dropwise hydrogen peroxide.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108940258A (en) * | 2018-08-22 | 2018-12-07 | 润泰化学（泰兴）有限公司 | A kind of weak acid catalyst of the double isobutyrate esterifications of synthesis 2,2,4- trimethylpentanediol |
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| CN104193119A (en) * | 2014-09-25 | 2014-12-10 | 安徽江海环境工程有限公司 | Process for deeply treating printing and dyeing wastewater in presence of attapulgite catalyst |
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2017
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| CN102716735A (en) * | 2012-06-25 | 2012-10-10 | 常州大学 | Preparation method of ATP/ Ce-Ti sold soluble oxide composite material |
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| CN104193119A (en) * | 2014-09-25 | 2014-12-10 | 安徽江海环境工程有限公司 | Process for deeply treating printing and dyeing wastewater in presence of attapulgite catalyst |
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| CN108940258A (en) * | 2018-08-22 | 2018-12-07 | 润泰化学（泰兴）有限公司 | A kind of weak acid catalyst of the double isobutyrate esterifications of synthesis 2,2,4- trimethylpentanediol |
| CN108940258B (en) * | 2018-08-22 | 2020-12-25 | 润泰化学（泰兴）有限公司 | Weak acid catalyst for synthesizing 2,2, 4-trimethylpentanediol diisobutyrate |
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