CN106669610A - Clay heavy metal adsorbent, and preparation method and application thereof - Google Patents

Clay heavy metal adsorbent, and preparation method and application thereof Download PDF

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Publication number
CN106669610A
CN106669610A CN201611243042.3A CN201611243042A CN106669610A CN 106669610 A CN106669610 A CN 106669610A CN 201611243042 A CN201611243042 A CN 201611243042A CN 106669610 A CN106669610 A CN 106669610A
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China
Prior art keywords
parts
clay
heavy metal
adsorbent
ethyl acetate
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CN201611243042.3A
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Chinese (zh)
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不公告发明人
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Henan Crystal Head Culture Media Co Ltd
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Henan Crystal Head Culture Media Co Ltd
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Priority to CN201611243042.3A priority Critical patent/CN106669610A/en
Publication of CN106669610A publication Critical patent/CN106669610A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/223Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Dispersion Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a clay heavy metal adsorbent, and a preparation method and application thereof. The adsorbent comprises the following raw materials in parts by weight: 27-35 parts of clay, 13-21 parts of ethyl acetate, 2-6 parts of titanium isopropylate and 5-12 parts of saligenol. The preparation method comprises the following steps: performing mixed grinding on the clay and the titanium isopropylate; adding the ethyl acetate solution, and performing ultrasonic treatment; and dropwisely adding the saligenol, stirring while heating in a sealed manner, then performing microwave treatment, stirring to dryness, and performing high-temperature calcination. The adsorbent prepared by the invention has very high heavy metal adsorption efficiency, and can be repeatedly used for more than 100 times. According to the invention, the clay heavy metal adsorbent has high adsorption capacity and high adsorption rate; the preparation method is simple; after use, heavy metal can be recovered by performing acid treatment, the adsorbent can be regenerated by performing high-temperature calcination at 450 DEG C, and the adsorbent can be repeatedly used for many times; the desorption is complete, and the recovery cost of the heavy metal is low; and the heavy metal treatment wastewater has the advantages of low treatment cost, simple process and no secondary pollution, thereby being suitable for industrial production.

Description

A kind of clay heavy metal absorbent and its preparation method and application
Technical field
The present invention relates to environment-friendly materials technical field, specifically a kind of clay heavy metal absorbent and preparation method thereof and should With.
Background technology
At present, process for treating heavy-metal waste water mainly has three classes:Chemical reaction removal method, Adsorption Concentration separate removal method with And microorganism or plant removal method.The first kind is that heavy metal ions in wastewater includes that neutralization is heavy by the method that chemical reaction is removed Shallow lake method, sulphide precipitation, ferrite coprecipitation, chemical reduction method, electrochemical reducing and high molecular heavy metals trapping agent Method etc.;Equations of The Second Kind be the heavy metal in waste water adsorbed under conditions of its chemical form is not changed, concentrated, detached side Method, including absorption, solvent extraction, evaporation and freezing method, ion exchange and membrance separation etc.;3rd class is by microorganism or plant The effect such as flocculation, absorption, accumulation, the enrichment method that removes heavy metal in waste water, including bioflocculation, biochemical process With plant ecological repair etc..The conventional processes generally existing high cost of heavy metal wastewater thereby, reaction is slow, easily cause secondary dirt The shortcomings of dye, difficult low concentration wastewater process.
Absorption method is a kind of effective ways for utilizing the unique texture of adsorbent toward removing heavy metals ion.At absorption method The active charcoal of conventional adsorbent, humic acidss, meerschaum, polysaccharide resins of reason electroplated heavy metals waste water etc..An absorption method process huge sum of money Category waste water have efficiently, easy and good selective, particularly strong to low concentration, contaminative, additive method is difficult to effectively The heavy metal wastewater thereby of process has unique using value.But the adsorbent for industrially using at present is expensive, extensively application It is restricted, the recovery of heavy metal, the regeneration and secondary pollution of adsorbent are also the difficult point in Heavymetal Wastewater Treatment by Adsorption. Conventional activated carbon of sorbent is widely used in waste water treatment, but regenerating active carbon efficiency is low, and water quality treatment is extremely difficult to back With requiring, the pretreatment of electroplating wastewater is typically only used for.Clay is to be piled up to form by volcanic ash, is with a kind of widest soil Earth medium.But individually clay adsorption heavy metal efficiency is low, it how is set to improve Adsorption of Heavy Metals efficiency to its simple process, It is problem that this patent need to be solved.
The content of the invention
It is an object of the invention to provide a kind of clay heavy metal absorbent and its preparation method and application, above-mentioned to solve The problem proposed in background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of clay heavy metal absorbent, is made up of the following raw material according to weight portion:Clay 27-35 parts, ethyl acetate 13-21 parts, isopropyl titanate 2-6 parts, saligenin 5-12 parts.
As further scheme of the invention:The clay heavy metal absorbent, by the following raw material group according to weight portion Into:Clay 29-33 parts, ethyl acetate 15-19 part, isopropyl titanate 3-5 parts, saligenin 7-10 parts.
As further scheme of the invention:The clay heavy metal absorbent, by the following raw material group according to weight portion Into:31 parts of clay, 17 parts of ethyl acetate, 4 parts of isopropyl titanate, 9 parts of saligenin.
Another object of the present invention is to provide a kind of preparation method of clay heavy metal absorbent, comprises the steps of:
1) deionized water of 4.8 times of ethyl acetate and its quality is mixed, ethyl acetate solution is obtained;
2) by clay and isopropyl titanate mixed grinding, 120 mesh sieves excessively, ethyl acetate solution is subsequently adding, is warming up to 72 DEG C And supersound process 32min at such a temperature, ultrasonic power is 1000W, then Deca saligenin, and 112 are warming up to after being added dropwise to complete DEG C and seal stir process 53min at such a temperature, then microwave treatment 20min again, microwave power is 800W, then in 99-101 Stir at a temperature of DEG C to dry, then 4h is calcined in 430 DEG C of Muffle furnace and obtain final product adsorbent.
Another object of the present invention is to provide application of the adsorbent in sewage disposal.
Compared with prior art, the invention has the beneficial effects as follows:
Clay and isopropyl titanate mixed grinding, recycle ethyl acetate supersound process, saligenin microwave treatment in the present invention Etc. adsorbent obtained in step, the adsorption efficiency of heavy metal is high, and reusable more than 100 times.Clay of the present invention The adsorption capacity of heavy metal absorbent is high, and adsorption rate is fast;Preparation method is simple, the use of rear acid treatment is recyclable heavy metal, Again 450 DEG C of high-temperature calcinations are renewable, are repeated high using number of times;Desorption is complete, heavy metal recovery low cost;Process a huge sum of money Category waste water has processing cost low, and process is simple does not have secondary pollution, and adsorbent can be repeatedly used, heavy metal recovery Easily, it is suitable to industrialized production.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, Obviously, described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based in the present invention Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of clay heavy metal absorbent is made up of the following raw material according to weight portion:Clay 27 Part, 13 parts of ethyl acetate, 2 parts of isopropyl titanate, 5 parts of saligenin.
4.8 times of deionized water of ethyl acetate and its quality is mixed, ethyl acetate solution is obtained.By clay and isopropanol Titanium mixed grinding, excessively 120 mesh sieves, are subsequently adding ethyl acetate solution, are warming up to 72 DEG C and at such a temperature supersound process 32min, ultrasonic power is 1000W, then Deca saligenin, 112 DEG C is warming up to after being added dropwise to complete and is sealed at such a temperature and stirred Process 53min is mixed, then microwave treatment 20min again, microwave power is 800W, then stirred at a temperature of 99 DEG C to dry, then 4h is calcined in 430 DEG C of Muffle furnace and obtains final product adsorbent.
Jing is tested and obtained repeatedly:The adsorption capacity of the adsorbent is 65-75mg/g;The adsorbent reuse 100 times with On still keep the adsorption capacity of 90-100%.
Embodiment 2
In the embodiment of the present invention, a kind of clay heavy metal absorbent is made up of the following raw material according to weight portion:Clay 35 Part, 21 parts of ethyl acetate, 6 parts of isopropyl titanate, 12 parts of saligenin.
4.8 times of deionized water of ethyl acetate and its quality is mixed, ethyl acetate solution is obtained.By clay and isopropanol Titanium mixed grinding, excessively 120 mesh sieves, are subsequently adding ethyl acetate solution, are warming up to 72 DEG C and at such a temperature supersound process 32min, ultrasonic power is 1000W, then Deca saligenin, 112 DEG C is warming up to after being added dropwise to complete and is sealed at such a temperature and stirred Process 53min is mixed, then microwave treatment 20min again, microwave power is 800W, then stirred at a temperature of 101 DEG C to dry, then 4h is calcined in 430 DEG C of Muffle furnace and obtains final product adsorbent.
Jing is tested and obtained repeatedly:The adsorption capacity of the adsorbent is 65-75mg/g;The adsorbent reuse 100 times with On still keep the adsorption capacity of 90-100%.
Embodiment 3
In the embodiment of the present invention, a kind of clay heavy metal absorbent is made up of the following raw material according to weight portion:Clay 29 Part, 15 parts of ethyl acetate, 3 parts of isopropyl titanate, 7 parts of saligenin.
4.8 times of deionized water of ethyl acetate and its quality is mixed, ethyl acetate solution is obtained.By clay and isopropanol Titanium mixed grinding, excessively 120 mesh sieves, are subsequently adding ethyl acetate solution, are warming up to 72 DEG C and at such a temperature supersound process 32min, ultrasonic power is 1000W, then Deca saligenin, 112 DEG C is warming up to after being added dropwise to complete and is sealed at such a temperature and stirred Process 53min is mixed, then microwave treatment 20min again, microwave power is 800W, then stirred at a temperature of 100 DEG C to dry, then 4h is calcined in 430 DEG C of Muffle furnace and obtains final product adsorbent.
Jing is tested and obtained repeatedly:The adsorption capacity of the adsorbent is 65-75mg/g;The adsorbent reuse 100 times with On still keep the adsorption capacity of 92-100%.
Embodiment 4
In the embodiment of the present invention, a kind of clay heavy metal absorbent is made up of the following raw material according to weight portion:Clay 33 Part, 19 parts of ethyl acetate, 5 parts of isopropyl titanate, 10 parts of saligenin.
4.8 times of deionized water of ethyl acetate and its quality is mixed, ethyl acetate solution is obtained.By clay and isopropanol Titanium mixed grinding, excessively 120 mesh sieves, are subsequently adding ethyl acetate solution, are warming up to 72 DEG C and at such a temperature supersound process 32min, ultrasonic power is 1000W, then Deca saligenin, 112 DEG C is warming up to after being added dropwise to complete and is sealed at such a temperature and stirred Process 53min is mixed, then microwave treatment 20min again, microwave power is 800W, then stirred at a temperature of 100 DEG C to dry, then 4h is calcined in 430 DEG C of Muffle furnace and obtains final product adsorbent.
Jing is tested and obtained repeatedly:The adsorption capacity of the adsorbent is 65-75mg/g;The adsorbent reuse 100 times with On still keep the adsorption capacity of 92-100%.
Embodiment 5
In the embodiment of the present invention, a kind of clay heavy metal absorbent is made up of the following raw material according to weight portion:Clay 31 Part, 17 parts of ethyl acetate, 4 parts of isopropyl titanate, 9 parts of saligenin.
4.8 times of deionized water of ethyl acetate and its quality is mixed, ethyl acetate solution is obtained.By clay and isopropanol Titanium mixed grinding, excessively 120 mesh sieves, are subsequently adding ethyl acetate solution, are warming up to 72 DEG C and at such a temperature supersound process 32min, ultrasonic power is 1000W, then Deca saligenin, 112 DEG C is warming up to after being added dropwise to complete and is sealed at such a temperature and stirred Process 53min is mixed, then microwave treatment 20min again, microwave power is 800W, then stirred at a temperature of 100 DEG C to dry, then 4h is calcined in 430 DEG C of Muffle furnace and obtains final product adsorbent.
Jing is tested and obtained repeatedly:The adsorption capacity of the adsorbent is 70-80mg/g;The adsorbent reuse 100 times with On still keep the adsorption capacity of 93-100%.
Comparative example 1
In addition to ethyl acetate is not contained, its material content and preparation process are consistent with embodiment 5.
Jing is tested, and the adsorption capacity of the adsorbent is 10-30mg/g, the adsorbent reuse 5 times after adsorption efficiency meeting Drop below the 50% of former adsorption capacity.
Comparative example 2
In addition to isopropyl titanate is not contained, its material content and preparation process are consistent with embodiment 5.
Jing is tested, and the adsorption capacity of the adsorbent is 10-30mg/g, the adsorbent reuse 5 times after adsorption efficiency meeting Drop below the 50% of former adsorption capacity.
Comparative example 3
In addition to ethyl acetate and isopropyl titanate is not contained, its material content and preparation process are consistent with embodiment 5.
Jing is tested, and the adsorption capacity of the adsorbent is 10-20mg/g, the adsorbent reuse 5 times after adsorption efficiency meeting Drop below the 50% of former adsorption capacity.
Result after adsorbent reactivation obtained in embodiment 1-5 and comparative example 1-3 5 times is as shown in table 1.
Table 1
Therefore, can be drawn by table 1, the adsorption capacity of the clay after other Feedstock treatings is big, reuse often.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be in other specific forms realized.Therefore, no matter From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped Containing an independent technical scheme, this narrating mode of description is only that for clarity those skilled in the art should Using description as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form those skilled in the art Understandable other embodiment.

Claims (5)

1. a kind of clay heavy metal absorbent, it is characterised in that be made up of the following raw material according to weight portion:Clay 27-35 parts, Ethyl acetate 13-21 part, isopropyl titanate 2-6 parts, saligenin 5-12 parts.
2. clay heavy metal absorbent according to claim 1, it is characterised in that by the following raw material group according to weight portion Into:Clay 29-33 parts, ethyl acetate 15-19 part, isopropyl titanate 3-5 parts, saligenin 7-10 parts.
3. clay heavy metal absorbent according to claim 1, it is characterised in that by the following raw material group according to weight portion Into:31 parts of clay, 17 parts of ethyl acetate, 4 parts of isopropyl titanate, 9 parts of saligenin.
4. a kind of preparation method of the clay heavy metal absorbent as described in claim 1-3 is arbitrary, it is characterised in that by following Step is constituted:
1) deionized water of 4.8 times of ethyl acetate and its quality is mixed, ethyl acetate solution is obtained;
2) by clay and isopropyl titanate mixed grinding, cross 120 mesh sieves, be subsequently adding ethyl acetate solution, be warming up to 72 DEG C and Supersound process 32min at this temperature, ultrasonic power is 1000W, then Deca saligenin, and 112 DEG C are warming up to after being added dropwise to complete simultaneously Stir process 53min is sealed at such a temperature, then microwave treatment 20min again, microwave power is 800W, then at 99-101 DEG C At a temperature of stir to dry, then 4h is calcined in 430 DEG C of Muffle furnace and obtains final product adsorbent.
5. application of the adsorbent as described in claim 1-3 is arbitrary in sewage disposal.
CN201611243042.3A 2016-12-29 2016-12-29 Clay heavy metal adsorbent, and preparation method and application thereof Pending CN106669610A (en)

Priority Applications (1)

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CN201611243042.3A CN106669610A (en) 2016-12-29 2016-12-29 Clay heavy metal adsorbent, and preparation method and application thereof

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Application Number Priority Date Filing Date Title
CN201611243042.3A CN106669610A (en) 2016-12-29 2016-12-29 Clay heavy metal adsorbent, and preparation method and application thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110201639A (en) * 2019-06-17 2019-09-06 周佳荣 A kind of molecular sieve for cigarette and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110201639A (en) * 2019-06-17 2019-09-06 周佳荣 A kind of molecular sieve for cigarette and preparation method thereof

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Application publication date: 20170517