CN106582509A - Heavy metal ion porous adsorbing material and preparation method thereof - Google Patents
Heavy metal ion porous adsorbing material and preparation method thereof Download PDFInfo
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- CN106582509A CN106582509A CN201611015926.3A CN201611015926A CN106582509A CN 106582509 A CN106582509 A CN 106582509A CN 201611015926 A CN201611015926 A CN 201611015926A CN 106582509 A CN106582509 A CN 106582509A
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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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
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention relates to the technical field of new environmental friendly materials for heavy metal ion adsorption, in particular to a heavy metal ion porous adsorbing material and a preparation method thereof. According to the invention, the technical problems of difficulty in separation and recovery of a water body, high preparation cost and low regeneration efficiency of an existing porous adsorbing material after heavy metal wastewater is treated. Compared with the prior art, the preparation method of the heavy metal ion porous adsorbing material has the advantages of simple preparation process, low cost, high repeatability and the like. The porous adsorbing material prepared by using the preparation method presents an excellent absorbing performance when treating heavy metal wastewater containing lead, copper and cadmium. After treating the wastewater, the porous adsorbing material can be directly taken out for recovery due to high molding strength, and the initial regeneration efficiency of the adsorbing material can exceed 85% through regenerated liquid treatment after reaching adsorption and saturation.
Description
Technical field
The present invention relates to heavy metal ion adsorbing material technical field, and in particular to a kind of heavy metal ion porous adsorption material
Material and preparation method thereof.
Background technology
Heavy metal pollution is referred to and is more than 4.5 g/cm by relative density3And have the metal or metalloid of obvious murder by poisoning to human body
The environmental pollution that element is produced.Heavy metal in environment directly can enter human body by skin, oral cavity, also can be inhaled by animals and plants
Enrichment is received, enters internal by way of food chain.When the Accumulation of heavy metals amount in human body excessively can affect nerve system of human body,
Digestive system and immune normal activity, cause bodily fuctions' organ failure, induction cardiovascular disease, cutaneum carcinoma, cancer of the stomach
Etc. disease, the production and life to people produces serious influence.
China's industry and mining are flourishing, and substantial amounts of heavy metal contaminants are discharged in water body and cause serious environmental problem, weight
The situation is tense for metallic pollution improvement.Currently, the processing method of heavy metal pollution of water body includes bioanalysis, ion-exchange, chemistry
The precipitation method and absorption method, wherein bioanalysis are to rely on the method that microorganism and plant reduce Heavy Metals in Waters content, the method
Environmental protection non-secondary pollution, but have the shortcomings that to remove that speed is slow and excessive cycle；Ion-exchange is current research heat
Point, but input processes greatly costly so that the method is difficult to effectively be promoted；Chemical precipitation method method is simple and processes fast
Degree is fast, but easily causes secondary pollution；Absorption method be using sorbing material to the suction-operated of Heavy Metals in Waters ion incite somebody to action
The method that heavy metal is removed, has the advantages that strong adaptability, easy to operate and recyclable, and prospect is more optimistic, but long action time,
Adsorption capacity difference becomes the bottleneck of its Developing Extension.In a word, the processing method of current heavy metal pollution of water body is all subject to each not
The restriction of sufficient feature, it is difficult to obtain and promote on a large scale, therefore, the new heavy metal pollution of research and development processes material and technology just seems
It is highly desirable to.
Heavy metal contaminants in water body are processed using absorption method, it is critical only that the preparation cost of adsorbent, adsorptivity
Energy and power of regeneration.The patent application of Publication No. CN105771933A discloses a kind of heavy metal in water sorbing material and its system
Preparation Method and application, the patent application to dacron fabric by dopamine by self assembled monolayer technology carrying out surface
Modification, obtains preferably adsorbing the bionical composite adsorbing material of the heavy metal in waste water, although the technical method is to a water body huge sum of money
Category pollution has a preferable absorption property, but the method is the shortcomings of have high cost, complex process and poor repeatability, and prepare
Sorbing material there are problems that being not easily recycled recycling and, therefore it is difficult to obtain large-scale practical application.
The content of the invention
Present invention aims to prior art weak point, there is provided a kind of heavy metal ion porous adsorbing material and
Its preparation method, in guarantee, its porous material heavy metal ion prepared has the same of preferable adsorption capacity to the preparation method
When, and with environmental protection non-secondary pollution, easy regeneration and regeneration efficiency（Regeneration efficiency）High the advantages of, the method
Also have the advantages that low cost, preparation process is simple and repeatability are strong.
To solve above-mentioned technical problem, the technical solution used in the present invention is：
A kind of preparation method of heavy metal ion porous adsorbing material, comprises the following steps：
1）By weight, 60～80 parts of diatomite, 10～20 parts of sintering aid, 3～15 parts of pore former, 1～5 part of dispersant are mixed
Merge ball milling into powder；
2）By step 1）Obtained powder crosses 80 ~ 160 mesh sieves, adds and ball up and dry after appropriate deionized water；
3）By step 2）Obtained ball was obtained porous material just body in 750～950 DEG C of high-temperature calcinations 2～4 hours；
4）By step 3）Just body is added in hydrochloric acid solution obtained porous material, stirring immersion 0.5-2 hours；
5）By step 4）Just body is added in ferrimanganic salting liquid the porous material that process is obtained, and is slowly stirred immersion 1-3 hours；
6）By step 5）Just body is added in aqueous slkali the porous material that process is obtained, and is slowly stirred immersion 1～2 hour；
7）By step 6）Just body thermostatic crystallization in 60-100 DEG C of water bath reacts 8-12 hours to the porous material that process is obtained；
8）By step 7）Just soma is dry for the porous material that process is obtained, and obtains final product the heavy metal ion porous adsorbing material.
Further, the step 1）Middle diatomite is by 35%～55%wt of 45～65%wt of bio-diatomite and calcined diatomite
Composition.
Further, the step 1）Middle sintering aid be bentonite, kaolin, clay, silica flour, it is talcous at least
It is a kind of.
Further, the step 1）Middle pore former be calcium carbonate, magnesium carbonate, wood chip, bamboo carbon powder, PP GRANULES extremely
Few one kind.
Further, the step 1）Middle dispersant is sodium silicate aqueous solution.
Further, the step 2）In, the appropriate water of addition is the deionized water for accounting for the powder 35%-55%wt.
Further, the step 5）Middle ferrimanganic salting liquid is by deionized water, MnCl2·4H2O and FeCl3·6H2O is pressed
Quality compares deionized water：MnCl2·4H2O：FeCl3·6H2O=11～14：1.5～3.0：1 is blended.
Further, the step 6）Middle aqueous slkali is by deionized water, NaOH and Na2CO3Deionized water in mass ratio：
NaOH：Na2CO3=9～11：1.0～1.5：1 is blended.
Further, the step 8）Specially：By step 7）Just body is first under the conditions of 70 ~ 80 DEG C for obtained porous material
1-3 hours are dried, then are dried under the conditions of 100 ~ 140 DEG C to the moisture in porous material less than 1%wt, obtain final product the heavy metal
Ion porous sorbing material.
The present invention also provides a kind of using heavy metal ion porous adsorbing material obtained in above-mentioned preparation method.
A kind of preparation principle of the preparation method of heavy metal ion porous adsorbing material of the present invention is：Nanometer ferrimanganic bimetallic
Oxide heavy metal has very strong adsorption capacity, and ceramsite material is based on concrete dynamic modulus, large specific surface area, it may have certain
Heavy metal adsorption, while ceramsite material easily reclaimed after adsorption saturation is reached and regeneration process, the present invention system
Preparation Method has complementary advantages, greatly by the way that nanometer ferrimanganic particle is embedded in porous ceramic grain using nano-particle and porous material
The removal ability and the rate of adsorption that improve porous material heavy metal, adsorption capacity significantly improves.
Beneficial effects of the present invention：
A kind of preparation method of heavy metal ion porous adsorbing material of the present invention, compared with prior art, with preparation technology letter
The advantages of single, low cost and strong repeatability.
A kind of heavy metal ion porous adsorbing material of the present invention, compared with prior art, has the following technical effect that：
1）The density of porous material of the present invention is little, porosity is high, high mechanical strength, has to the heavy metal ion in water body very strong
Adsorption capacity；
2）Porous material of the present invention, by the way that nanometer ferrimanganic bimetallic oxide is embedded in porous material, overcomes nanoparticle
Son is difficult to the shortcoming for recycling during heavy metal is processed, and further increases the absorption of porous material heavy metal ion
Ability；
3）Porous material of the present invention has the advantages that shaping strength is high, therefore profit again can be directly taken out after adsorption saturation is reached
With, Jing after regenerated liquid first treated, regeneration efficiency（Regeneration efficiency）Up to more than 85%；
4）Porous material of the present invention also has the advantages that environmental protection and non-secondary pollution.
Specific embodiment
Embodiment 1
A kind of preparation method of the heavy metal ion porous adsorbing material in the present embodiment, comprises the following steps：
1）Weigh diatomite, the bentonite of 4.3g, the feldspar powder of 2.6g of 27.0g, the bamboo carbon powder of 3.8g and the sodium metasilicate of 0.7g
For raw material, mix and be placed in ball milling 20 minutes in ball grinder, obtain powder；
2）By step 1）Obtained powder crosses 120 mesh sieves, and adding deionized water makes powder moisture content reach 46%, balls up simultaneously
It is placed in 105 DEG C of drying in baking oven；
3）By step 2）Obtained ball is placed in resistance box 850 DEG C of high-temperature calcinations 3 hours, and porous material just body is obtained；
4）By step 3）Just body is added in the hydrochloric acid solution that concentration is 0.5mol/L the porous material for obtaining, and stirring immersion 1 is little
When；
5）Weigh the MnCl of 16.8g2·4H2The FeCl of O and 8.2g3·6H2O be added in the deionized water of 100ml make it is standby
Ferrimanganic salting liquid；By step 4）Just body is added in ferrimanganic salting liquid the porous material for obtaining, and is slowly stirred immersion 2 hours；
6）Weigh the Na of the NaOH and 9.6g of 10.9g2CO3In being added to the deionized water of 100ml, standby aqueous slkali is made；Will
Step 5）Just body is added in aqueous slkali the porous material for obtaining, and is slowly stirred immersion 1 hour；
7）With glass plate by step 6）Just body is placed in thermostatic crystallization reaction 10 hours in 80 DEG C of water bath to the porous material for obtaining；
8）By step 7）The first body of porous material for obtaining is placed in baking oven and is dried, and obtains final porous material.
Embodiment 2
1）First, diatomite, the bentonite of 4.8g, the feldspar powder of 3.0g of 24.3g, the bamboo carbon powder of 5.8g and the silicon of 0.7g are weighed
Sour sodium is raw material, and mixing is placed in ball milling 30 minutes in ball grinder, obtains powder；
2）By step 1）Obtained powder crosses 80 mesh sieves, and adding deionized water makes powder moisture content reach 55%, and ball up juxtaposition
95 in baking ovenoC is dried；
3）By step 2）Obtained ball is placed in resistance box 950 DEG C of high-temperature calcinations 2 hours, and porous material just body is obtained；
4）By step 3）Just body is added in the hydrochloric acid solution that concentration is 0.5mol/L the porous material for obtaining, and is slowly stirred immersion
1 hour；
5）Weigh the MnCl of 11.4g2·4H2The FeCl of O and 7.2g3·6H2O be added in the deionized water of 100ml make it is standby
Ferrimanganic salting liquid；By step 4）Just body is added in ferrimanganic salting liquid the porous material for obtaining, and is slowly stirred immersion 2 hours；
6）Weigh the Na of the NaOH and 9.0g of 12.1g2CO3In being added to the deionized water of 100ml, standby aqueous slkali is made；Will
Step 5）Just body is added in aqueous slkali the porous material for obtaining, and is slowly stirred immersion 1.5 hours；
7）With glass plate by step 6）Just body is placed in thermostatic crystallization reaction 12 hours in 80 DEG C of water bath to the porous material for obtaining；
8）By step 7）The first body of porous material for obtaining is placed in baking oven and is dried, and obtains final porous material.
Embodiment 3
1）First, diatomite, the bentonite of 3.8g, the feldspar powder of 2.1g of 29.2g, the bamboo carbon powder of 3.1g and the silicon of 1.1g are weighed
Sour sodium is raw material, and mixing is placed in ball milling 40 minutes in ball grinder, obtains powder；
2）By step 1）The compound that ball milling is crossed crosses 160 mesh sieves, and adding deionized water makes powder moisture content reach 35%, spin
Shaping, is placed in 135 in baking ovenoC is dried；
3）By step 2）Obtained raw material is placed in resistance box 750 DEG C of high-temperature calcinations 4 hours, and porous material just body is obtained；
4）By step 3）Just body is added in the hydrochloric acid solution that concentration is 0.5mol/L the porous material for obtaining, and is slowly stirred immersion
1 hour；
5）Weigh the MnCl of 20.0g2·4H2The FeCl of O and 9.1g3·6H2O be added in the deionized water of 100ml make it is standby
Ferrimanganic salting liquid；By step 4）Just body is added in ferrimanganic salting liquid the porous material for obtaining, and is slowly stirred immersion 2 hours；
6）Weigh the Na of the NaOH and 10.5g of 11.6g2CO3In being added to the deionized water of 100ml, standby aqueous slkali is made；Will
Step 5）Just body is added in aqueous slkali the porous material for obtaining, and is slowly stirred immersion 2 hours；
7）With glass plate by step 6）Just body is placed in thermostatic crystallization reaction 8 hours in 80 DEG C of water bath to the porous material for obtaining；
8）By step 7）The first body of porous material for obtaining is placed in baking oven and is dried, and obtains final porous material.
The using method of porous material of the present invention is：A certain amount of porous adsorption material is added in heavy metal-containing waste water
Material, slowly vibrating for a period of time after, centrifugation, determine solution in each concentration of heavy metal ion；
Wherein, concentration of heavy metal ion is determined using inductive coupling plasma emission spectrograph（ICP）.
Porous adsorbing material is as follows to the computing formula of the Adsorption efficiency of heavy metal ions in wastewater：
R(%)=（1-Ct/Co）×100
Wherein R be heavy metal removing rate, CoFor the initial concentration of heavy metal in waste water, CtFor a huge sum of money in water body after the reaction t times
The residual concentration of category, unit is mg/L.
The porous adsorbing material that adsorption saturation is reached after waste water is processed, is soaked with the hydrochloric acid solution that concentration is 0.1mol/L
Bubble desorption 1 hour, deionized water soaking and washing, then immersion 1 hour is carried out with the NaOH solution of 0.3mol/L, 105oC conditions
Lower drying, finally gives regeneration porous adsorbing material, then processes the waste water containing heavy metal with regeneration porous adsorbing material.
Using the gained sample of embodiment 1,2,3 as adsorbent, Pb is prepared respectively2+、Cu2+And Cd2+Volumetric concentration is respectively
The simulation heavy metal pollution water sample of 1000mg/L, 1000mg/L and 500mg/L, using activated carbon as control sorbing material, at it
Adsorption test and regeneration test are carried out under the conditions of its condition identical, the absorption of porous adsorbing material heavy metal of the present invention is determined
Removal capacity and coefficient of recovery, as a result as shown in table 1.
The absorption property and regeneration efficiency of the porous adsorbing material heavy metal ion of the present invention of table 1
As can be seen from the above table, the porous material of embodiment of the present invention 1-3 processes leaded, copper, cadmium heavy metal wastewater thereby and can show
Go out excellent absorption property, process the porous material after waste water because it has higher shaping strength, therefore can directly take out
Recycling；Sorbing material after adsorption saturation is reached by regenerated liquid process, first regeneration efficiency can reach 85% with
On.
Claims (10)
1. a kind of preparation method of heavy metal ion porous adsorbing material, it is characterised in that comprise the following steps：
1）By weight, 60～80 parts of diatomite, 10～20 parts of sintering aid, 3～15 parts of pore former, 1～5 part of dispersant are mixed
Merge ball milling into powder；
2）By step 1）Obtained powder crosses 80 ~ 160 mesh sieves, adds and ball up and dry after appropriate deionized water；
3）By step 2）Obtained ball was obtained porous material just body in 750～950 DEG C of high-temperature calcinations 2～4 hours；
4）By step 3）Just body is added in hydrochloric acid solution obtained porous material, stirring immersion 0.5-2 hours；
5）By step 4）Just body is added in ferrimanganic salting liquid the porous material that process is obtained, and is slowly stirred immersion 1-3 hours；
6）By step 5）Just body is added in aqueous slkali the porous material that process is obtained, and is slowly stirred immersion 1～2 hour；
7）By step 6）The first body of porous material that process is obtained is in 60-100oThermostatic crystallization reaction 8-12 hours in the water bath of C；
8）By step 7）Just soma is dry for the porous material that process is obtained, and obtains final product the heavy metal ion porous adsorbing material.
2. the preparation method of heavy metal ion porous adsorbing material as claimed in claim 1, it is characterised in that the step 1）In
Diatomite is made up of 45～65%wt of bio-diatomite and 35%～55%wt of calcined diatomite.
3. the preparation method of heavy metal ion porous adsorbing material as claimed in claim 1, it is characterised in that the step 1）In
Sintering aid is bentonite, kaolin, clay, silica flour, talcous at least one.
4. the preparation method of heavy metal ion porous adsorbing material as claimed in claim 1, it is characterised in that the step 1）In
Pore former is calcium carbonate, magnesium carbonate, wood chip, bamboo carbon powder, at least one of PP GRANULES.
5. the preparation method of heavy metal ion porous adsorbing material as claimed in claim 1, it is characterised in that the step 1）In
Dispersant is sodium silicate aqueous solution.
6. the preparation method of heavy metal ion porous adsorbing material as claimed in claim 1, it is characterised in that the step 2）In
The appropriate water for adding is the deionized water for accounting for the powder 35%-55%wt.
7. the preparation method of heavy metal ion porous adsorbing material as claimed in claim 1, it is characterised in that the step 5）In
Ferrimanganic salting liquid is by deionized water, MnCl2·4H2O and FeCl3·6H2O deionized waters in mass ratio：MnCl2·4H2O：
FeCl3·6H2O=11～14：1.5～3.0：1 is blended.
8. the preparation method of heavy metal ion porous adsorbing material as claimed in claim 1, it is characterised in that the step 6）In
Aqueous slkali is by deionized water, NaOH and Na2CO3Deionized water in mass ratio：NaOH：Na2CO3=9～11：1.0～1.5：1 mixes
System is formed.
9. the preparation method of heavy metal ion porous adsorbing material as claimed in claim 1, it is characterised in that the step 8）Tool
Body is：By step 7）Just body is first dried 1-3 hours to obtained porous material under the conditions of 70 ~ 80 DEG C, then in 100 ~ 140 DEG C of conditions
Lower drying to the moisture in porous material is less than 1%wt, obtains final product the heavy metal ion porous adsorbing material.
10. it is a kind of to adopt heavy metal ion porous adsorbing material obtained in preparation method described in any one of claim 1～9.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106994329A (en) * | 2017-06-07 | 2017-08-01 | 浙江工业大学 | A kind of application of the Mn oxide carried magnetic bentonite and preparation method thereof with adsorbing heavy metal in water cadmium |
| CN107617422A (en) * | 2017-09-13 | 2018-01-23 | 铜陵市业永兴工贸有限责任公司 | A kind of copper-containing wastewater inorganic agent and preparation method thereof |
| CN107841629A (en) * | 2017-11-07 | 2018-03-27 | 长沙埃比林环保科技有限公司 | A kind of method of porous mineral processing lead waste water |
| CN109174065A (en) * | 2018-10-22 | 2019-01-11 | 管敏富 | The preparation and the application in processing waste water from dyestuff that iron magnesium compound coats bentonite composite granule adsorbent |
| CN112875969A (en) * | 2021-04-14 | 2021-06-01 | 铜陵瑞莱科技有限公司 | Method for treating wastewater from iron oxide pigment production |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106994329A (en) * | 2017-06-07 | 2017-08-01 | 浙江工业大学 | A kind of application of the Mn oxide carried magnetic bentonite and preparation method thereof with adsorbing heavy metal in water cadmium |
| CN107617422A (en) * | 2017-09-13 | 2018-01-23 | 铜陵市业永兴工贸有限责任公司 | A kind of copper-containing wastewater inorganic agent and preparation method thereof |
| CN107841629A (en) * | 2017-11-07 | 2018-03-27 | 长沙埃比林环保科技有限公司 | A kind of method of porous mineral processing lead waste water |
| CN109174065A (en) * | 2018-10-22 | 2019-01-11 | 管敏富 | The preparation and the application in processing waste water from dyestuff that iron magnesium compound coats bentonite composite granule adsorbent |
| CN112875969A (en) * | 2021-04-14 | 2021-06-01 | 铜陵瑞莱科技有限公司 | Method for treating wastewater from iron oxide pigment production |
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