CN106622168A - Heavy metal adsorption material based on attapulgite and preparation method thereof - Google Patents
Heavy metal adsorption material based on attapulgite and preparation method thereof Download PDFInfo
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- CN106622168A CN106622168A CN201611123044.9A CN201611123044A CN106622168A CN 106622168 A CN106622168 A CN 106622168A CN 201611123044 A CN201611123044 A CN 201611123044A CN 106622168 A CN106622168 A CN 106622168A
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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
- B01J20/12—Naturally occurring clays or bleaching 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid 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
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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Abstract
The invention discloses a heavy metal adsorption material based on attapulgite. The heavy metal adsorption material is prepared from the following raw materials in parts by weight: 35 to 40 parts of attapulgite, 5 to 9 parts of epoxy chloropropane, 2 to 5 parts of sodium nitrate, 3 to 7 parts of ethylene glycol tetraacetic acid, 2 to 5 parts of tetrabutyl titanate, 1 to 3 parts of amino tri methylene phosphonic acid, 5 to 8 parts of polyethyleneimine and 3 to 6 parts of alkylphenol polyoxyethylene. The invention also discloses a preparation method of the heavy metal adsorption material based on the attapulgite. The adsorption material prepared by the method provided by the invention has the advantages that the adsorption effect on heavy metal ions is good; the use is convenient; the manufacturing cost is low; the production cost is low; the large-scale popularization and use can be realized; the development of the heavy metal treatment industry is facilitated.
Description
Technical field
The present invention relates to heavy metal processing technology field, specifically a kind of heavy-metal adsorption material based on attapulgite and
Its preparation method.
Background technology
Science and technology is a double-edged sword, and scientific and technical fast development, promotes expanding economy since 21 century, improves people
The living standard of the people, however, at the same time, the mankind have also paid the cost of heaviness.Due to Industrial " three Waste " motor-vehicle tail-gas
The use of discharge, sewage irrigation and pesticide, herbicide, chemical fertilizer etc. and the development of mining industry, seriously pollute soil, water quality and
Air.
Heavy metal pollution is a kind of pollution great to human health damage.At present for heavy metal containing sewage, mainly pass through
Chemical method, physisorphtion and bioanalysises are processed, and wherein physisorphtion is because easy to use, and processing cost is low, application compared with
For extensive.
Attapulgite is ideal adsorbent, food processing aid and food additive, may replace activated carbon.It is not
Be only capable of decolourize, can also deodorization taste removal, removing heavy metals ion and carcinogen, also with certain selectivity, this is just carried for production
Facility is supplied, it can make deodorant for refrigerator, sewage-treating agent, household water filter, oil and fat refining decolorising agent, effect is extremely obvious,
In filler, carrier, additive, the binding agent that can pharmaceutically make medicine.Using attapulgite to liquid glucose decolourize can by by
12 procedures of powder activity carbon purifying are reduced to ten procedures, and process cycle shortens 50 minutes, extremely have to developping production
Profit.The commerieal sugar purified with attapulgite clay, its color and luster, figure, concentration, content of reducing sugar, pH value, sulfur dioxide ion contain
Amount, chloride content, protein content, sugar cook temperature and calcium ions and magnesium ions content etc. reach existing industry standard, save and decolourize
Processing cost 60% or so, the filter cake after decolouring can make mixed fodder, reduce environmental pollution, reach comprehensive utilization.Either
In adsorption process, or in sewage disposal, attapulgite can regenerate, and it consumes energy less, highly beneficial to environmental conservation.
But in heavy metal process field, the adsorption effect of natural attapulgite heavy metal is unsatisfactory, if can
By the modified and raw material compounding to attapulgite, a kind of adsorbing material based on attapulgite is made, improve its heavy metal
Adsorption effect, undoubtedly by with important market value.
The content of the invention
It is an object of the invention to provide a kind of heavy-metal adsorption material based on attapulgite and preparation method thereof, to solve
The problem proposed in certainly above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of heavy-metal adsorption material based on attapulgite, is made up of the following raw material according to weight:Attapulgite 35-
40 parts, epoxychloropropane 5-9 parts, sodium nitrate 2-5 parts, ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) 3-7 parts, tetrabutyl titanate 2-5 parts,
ATMP 1-3 parts, polyethyleneimine 5-8 part, alkylphenol polyoxyethylene 3-6 part.
As further scheme of the invention:It is made up of the following raw material according to weight:Attapulgite 36-39 parts, epoxy
Chloropropane 6-8 parts, sodium nitrate 3-4 parts, ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) 4-6 parts, tetrabutyl titanate 3-4 parts, amino front three
Fork phosphonic acids 1.3-2.6 parts, polyethyleneimine 6-7 part, alkylphenol polyoxyethylene 4-5 part.
As further scheme of the invention:It is made up of the following raw material according to weight:38 parts of attapulgite, epoxy chlorine
7 parts of propane, 4 parts of sodium nitrate, 5 parts of ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA), 3 parts of tetrabutyl titanate, ATMP 1.8
Part, 7 parts of polyethyleneimine, 4 parts of alkylphenol polyoxyethylene.
The preparation method of the heavy-metal adsorption material based on attapulgite, step is as follows:
1) attapulgite is weighed, after micronizing, crosses 300-400 mesh sieves, obtain attapulgite micropowder;
2) attapulgite micropowder is placed in container, adds the deionized water of 3-4 times of weight, it is quiet after stirring mixing 2-3h
1h is put, the supernatant and lower sediment is discarded, attapulgite suspension is obtained;
3) sodium nitrate and ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) are weighed, is added to attapulgite suspension, at 75-80 DEG C
Stirring mixing 1-2h, obtains mixture A;
4) epoxychloropropane, alkylphenol polyoxyethylene and ATMP are weighed, is added into mixture A,
Stirring mixing 1-2h, then carries out ultrasonic Treatment 30-40min at 75-80 DEG C, obtains mixture B;
5) after mixture B is vacuum dried, conducting forging processing 30-40min at 600-650 DEG C, and the forging for obtaining is produced
Thing is crushed, and crosses 100-200 mesh sieves, obtains forging powder;
6) tetrabutyl titanate and polyethyleneimine are weighed, forging powder are merged with tetrabutyl titanate and polyethyleneimine,
Ball milling mixing 3-5h, obtains powder, by granulation for powders.
As further scheme of the invention:Step 4) in, ultrasonic Treatment temperature is 65-70 DEG C, and ultrasonic power is
1300W。
Compared with prior art, the invention has the beneficial effects as follows:
The advantages of good adsorption effect of adsorbing material heavy metal ion prepared by the present invention, its adsorption effect is concavo-convex better than routine
Rod soil.Adsorbing material prepared by the present invention is easy to use, low cost of manufacture, and low production cost, can promote the use of on a large scale,
Be conducive to the development of heavy metal treatment industry.
Specific embodiment
Technical scheme is described in more detail with reference to specific embodiment.
Embodiment 1
A kind of heavy-metal adsorption material based on attapulgite, is made up of the following raw material according to weight:Attapulgite 35
Part, 5 parts of epoxychloropropane, 2 parts of sodium nitrate, 3 parts of ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA), 2 parts of tetrabutyl titanate, the methene of amino three
1 part of phosphonic acids, 5 parts of polyethyleneimine, 3 parts of alkylphenol polyoxyethylene.
In the present embodiment, the preparation method of the heavy-metal adsorption material based on attapulgite, step is as follows:
1) attapulgite is weighed, after micronizing, crosses 300 mesh sieves, obtain attapulgite micropowder;
2) attapulgite micropowder is placed in container, adds the deionized water of 3 times of weight, after stirring mixing 2h, stand 1h,
The supernatant and lower sediment are discarded, attapulgite suspension is obtained;
3) sodium nitrate and ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) are weighed, is added to attapulgite suspension, stirred at 75 DEG C
Mixing 1h is mixed, mixture A is obtained;
4) epoxychloropropane, alkylphenol polyoxyethylene and ATMP are weighed, is added into mixture A,
Stirring mixing 1h, then carries out ultrasonic Treatment 30min at 75 DEG C, obtains mixture B, wherein, ultrasonic Treatment temperature is 65
DEG C, ultrasonic power is 1300W;
5) after mixture B is vacuum dried, conducting forging processing 30min at 600 DEG C, and the forging product for obtaining is crushed,
100 mesh sieves are crossed, forging powder is obtained;
6) tetrabutyl titanate and polyethyleneimine are weighed, forging powder are merged with tetrabutyl titanate and polyethyleneimine,
Ball milling mixing 3h, obtains powder, by granulation for powders.
Embodiment 2
A kind of heavy-metal adsorption material based on attapulgite, is made up of the following raw material according to weight:Attapulgite 36
Part, 6 parts of epoxychloropropane, 3 parts of sodium nitrate, 6 parts of ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA), 4 parts of tetrabutyl titanate, the methene of amino three
2.6 parts of phosphonic acids, 6 parts of polyethyleneimine, 5 parts of alkylphenol polyoxyethylene.
In the present embodiment, the preparation method of the heavy-metal adsorption material based on attapulgite, step is as follows:
1) attapulgite is weighed, after micronizing, crosses 350 mesh sieves, obtain attapulgite micropowder;
2) attapulgite micropowder is placed in container, adds the deionized water of 4 times of weight, after stirring mixing 2h, stand 1h,
The supernatant and lower sediment are discarded, attapulgite suspension is obtained;
3) sodium nitrate and ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) are weighed, is added to attapulgite suspension, stirred at 75 DEG C
Mixing 1h is mixed, mixture A is obtained;
4) epoxychloropropane, alkylphenol polyoxyethylene and ATMP are weighed, is added into mixture A,
Stirring mixing 1h, then carries out ultrasonic Treatment 35min at 78 DEG C, obtains mixture B, wherein, ultrasonic Treatment temperature is 70
DEG C, ultrasonic power is 1300W;
5) after mixture B is vacuum dried, conducting forging processing 33min at 620 DEG C, and the forging product for obtaining is crushed,
150 mesh sieves are crossed, forging powder is obtained;
6) tetrabutyl titanate and polyethyleneimine are weighed, forging powder are merged with tetrabutyl titanate and polyethyleneimine,
Ball milling mixing 3.5h, obtains powder, by granulation for powders.
Embodiment 3
A kind of heavy-metal adsorption material based on attapulgite, is made up of the following raw material according to weight:Attapulgite 38
Part, 7 parts of epoxychloropropane, 4 parts of sodium nitrate, 5 parts of ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA), 3 parts of tetrabutyl titanate, the methene of amino three
1.8 parts of phosphonic acids, 7 parts of polyethyleneimine, 4 parts of alkylphenol polyoxyethylene.
In the present embodiment, the preparation method of the heavy-metal adsorption material based on attapulgite, step is as follows:
1) attapulgite is weighed, after micronizing, crosses 400 mesh sieves, obtain attapulgite micropowder;
2) attapulgite micropowder is placed in container, adds the deionized water of 4 times of weight, after stirring mixing 2.5h, stood
1h, discards the supernatant and lower sediment, obtains attapulgite suspension;
3) sodium nitrate and ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) are weighed, is added to attapulgite suspension, stirred at 78 DEG C
Mixing 1.5h is mixed, mixture A is obtained;
4) epoxychloropropane, alkylphenol polyoxyethylene and ATMP are weighed, is added into mixture A,
Stirring mixing 1.5h, then carries out ultrasonic Treatment 35min at 77 DEG C, obtains mixture B, wherein, ultrasonic Treatment temperature is
68 DEG C, ultrasonic power is 1300W;
5) after mixture B is vacuum dried, conducting forging processing 35min at 630 DEG C, and the forging product for obtaining is crushed,
200 mesh sieves are crossed, forging powder is obtained;
6) tetrabutyl titanate and polyethyleneimine are weighed, forging powder are merged with tetrabutyl titanate and polyethyleneimine,
Ball milling mixing 4h, obtains powder, by granulation for powders.
Embodiment 4
A kind of heavy-metal adsorption material based on attapulgite, is made up of the following raw material according to weight:Attapulgite 39
Part, 8 parts of epoxychloropropane, 3 parts of sodium nitrate, 4 parts of ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA), 4 parts of tetrabutyl titanate, the methene of amino three
2.6 parts of phosphonic acids, 6 parts of polyethyleneimine, 4 parts of alkylphenol polyoxyethylene.
In the present embodiment, the preparation method of the heavy-metal adsorption material based on attapulgite, step is as follows:
1) attapulgite is weighed, after micronizing, crosses 300 mesh sieves, obtain attapulgite micropowder;
2) attapulgite micropowder is placed in container, adds the deionized water of 3 times of weight, after stirring mixing 3h, stand 1h,
The supernatant and lower sediment are discarded, attapulgite suspension is obtained;
3) sodium nitrate and ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) are weighed, is added to attapulgite suspension, stirred at 80 DEG C
Mixing 1h is mixed, mixture A is obtained;
4) epoxychloropropane, alkylphenol polyoxyethylene and ATMP are weighed, is added into mixture A,
Stirring mixing 2h, then carries out ultrasonic Treatment 30min at 75 DEG C, obtains mixture B, wherein, ultrasonic Treatment temperature is 67
DEG C, ultrasonic power is 1300W;
5) after mixture B is vacuum dried, conducting forging processing 40min at 630 DEG C, and the forging product for obtaining is crushed,
100 mesh sieves are crossed, forging powder is obtained;
6) tetrabutyl titanate and polyethyleneimine are weighed, forging powder are merged with tetrabutyl titanate and polyethyleneimine,
Ball milling mixing 4.5h, obtains powder, by granulation for powders.
Embodiment 5
A kind of heavy-metal adsorption material based on attapulgite, is made up of the following raw material according to weight:Attapulgite 40
Part, 9 parts of epoxychloropropane, 5 parts of sodium nitrate, 7 parts of ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA), 5 parts of tetrabutyl titanate, the methene of amino three
3 parts of phosphonic acids, 8 parts of polyethyleneimine, 6 parts of alkylphenol polyoxyethylene.
In the present embodiment, the preparation method of the heavy-metal adsorption material based on attapulgite, step is as follows:
1) attapulgite is weighed, after micronizing, crosses 400 mesh sieves, obtain attapulgite micropowder;
2) attapulgite micropowder is placed in container, adds the deionized water of 4 times of weight, after stirring mixing 3h, stand 1h,
The supernatant and lower sediment are discarded, attapulgite suspension is obtained;
3) sodium nitrate and ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) are weighed, is added to attapulgite suspension, stirred at 80 DEG C
Mixing 2h is mixed, mixture A is obtained;
4) epoxychloropropane, alkylphenol polyoxyethylene and ATMP are weighed, is added into mixture A,
Stirring mixing 2h, then carries out ultrasonic Treatment 40min at 80 DEG C, obtains mixture B, wherein, ultrasonic Treatment temperature is 70
DEG C, ultrasonic power is 1300W;
5) after mixture B is vacuum dried, conducting forging processing 40min at 650 DEG C, and the forging product for obtaining is crushed,
200 mesh sieves are crossed, forging powder is obtained;
6) tetrabutyl titanate and polyethyleneimine are weighed, forging powder are merged with tetrabutyl titanate and polyethyleneimine,
Ball milling mixing 5h, obtains powder, by granulation for powders.
The advantages of good adsorption effect of adsorbing material heavy metal ion prepared by the present invention, its adsorption effect is concavo-convex better than routine
Rod soil.Adsorbing material prepared by the present invention is easy to use, low cost of manufacture, and low production cost, can promote the use of on a large scale,
Be conducive to the development of heavy metal treatment industry.
The better embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula, in the ken that one skilled in the relevant art possesses, can be with the premise of without departing from present inventive concept
Various changes can be made.
Claims (5)
1. a kind of heavy-metal adsorption material based on attapulgite, it is characterised in that be made up of the following raw material according to weight:It is recessed
Convex rod soil 35-40 parts, epoxychloropropane 5-9 parts, sodium nitrate 2-5 parts, ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) 3-7 parts, metatitanic acid are just
Butyl ester 2-5 parts, ATMP 1-3 parts, polyethyleneimine 5-8 part, alkylphenol polyoxyethylene 3-6 part.
2. the heavy-metal adsorption material based on attapulgite according to claim 1, it is characterised in that by following according to weight
The raw material composition of amount:Attapulgite 36-39 parts, epoxychloropropane 6-8 parts, sodium nitrate 3-4 parts, ethylene glycol diethyl ether diamidogen tetrem
Sour 4-6 parts, tetrabutyl titanate 3-4 parts, ATMP 1.3-2.6 parts, polyethyleneimine 6-7 part, alkyl phenol polyoxy second
Alkene ether 4-5 parts.
3. the heavy-metal adsorption material based on attapulgite according to claim 2, it is characterised in that by following according to weight
The raw material composition of amount:38 parts of attapulgite, 7 parts of epoxychloropropane, 4 parts of sodium nitrate, 5 parts of ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA),
3 parts of tetrabutyl titanate, 1.8 parts of ATMP, 7 parts of polyethyleneimine, 4 parts of alkylphenol polyoxyethylene.
4. a kind of preparation method of the heavy-metal adsorption material based on attapulgite as described in claim 1-3 is arbitrary, it is special
Levy and be, step is as follows:
1) attapulgite is weighed, after micronizing, crosses 300-400 mesh sieves, obtain attapulgite micropowder;
2) attapulgite micropowder is placed in container, adds the deionized water of 3-4 times of weight, after stirring mixing 2-3h, stand 1h,
The supernatant and lower sediment are discarded, attapulgite suspension is obtained;
3) sodium nitrate and ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) are weighed, is added to attapulgite suspension, stirred at 75-80 DEG C
Mixing 1-2h, obtains mixture A;
4) epoxychloropropane, alkylphenol polyoxyethylene and ATMP are weighed, is added into mixture A, in 75-80
Stirring mixing 1-2h, then carries out ultrasonic Treatment 30-40min at DEG C, obtains mixture B;
5) after mixture B is vacuum dried, conducting forging processing 30-40min at 600-650 DEG C, and the forging product powder that will be obtained
It is broken, 100-200 mesh sieves are crossed, obtain forging powder;
6) tetrabutyl titanate and polyethyleneimine are weighed, forging powder is merged with tetrabutyl titanate and polyethyleneimine, ball milling
Mixing 3-5h, obtains powder, by granulation for powders.
5. the preparation method of the heavy-metal adsorption material based on attapulgite according to claim 4, it is characterised in that step
It is rapid 4) in, ultrasonic Treatment temperature be 65-70 DEG C, ultrasonic power is 1300W.
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Application publication date: 20170510 |