CN105921125A - Attapulgite clay/sodium alginate composite heavy metal absorbent and preparation method thereof - Google Patents
Attapulgite clay/sodium alginate composite heavy metal absorbent and preparation method thereof Download PDFInfo
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- CN105921125A CN105921125A CN201610432403.2A CN201610432403A CN105921125A CN 105921125 A CN105921125 A CN 105921125A CN 201610432403 A CN201610432403 A CN 201610432403A CN 105921125 A CN105921125 A CN 105921125A
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- attapulgite
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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Abstract
The invention relates to the field of environmental governance, in particular to a heavy metal absorbent and a preparation method thereof. The preparation method comprises the following steps: modifying attapulgite clay powder by using an aminosilane coupling agent to obtain attapulgite clay modified by a silane coupling agent; then dispersing the attapulgite clay in a glutaraldehyde solution, and fully stirring to obtain attapulgite clay modified by glutaraldehyde; and dropwise adding an acid solution of sodium alginate in suspension liquid of the attapulgite clay modified by the glutaraldehyde, heating and fully reacting to obtain a sodium alginate grafted and crosslinked attapulgite clay heavy metal absorbing material. By a mode of covalent bonds, the sodium alginate is grafted and crosslinked to the surface of the attapulgite clay, and in a using process, the sodium alginate cannot drop easily.
Description
Technical field
The present invention relates to field of environmental improvement, be specifically related to a kind of heavy metal absorbent and preparation method thereof.
Background technology
Along with global economy and the development of society, environmental pollution is day by day serious, and wherein industrial wastewater is as main environomental pollution source,
It it is a great problem perplexing countries in the world for a long time.Heavy metal ion in industrial wastewater has strong carcinogenic, teratogenesis, cause
Mutation effect, constitutes serious threat to health and ecological environment, the most strictly controls the pollution of heavy metal wastewater thereby to closing
Important.
Traditional process for treating heavy-metal waste water mainly has chemical precipitation method, ion exchange, membrane separation process etc., and these methods are led to
Being commonly present that investment is big, energy consumption high, operating cost is high, be easily generated secondary pollution problems, application is restricted.Absorption method is profit
With the pollutant in adsorbent water, thus the method purifying waste water, there is simple to operate, feature fast and effectively, obtain
It is widely applied.How to obtain adsorbent cheap, that high adsorption capacity, adsorptive selectivity are high, have become as research and development
Focus.
Summary of the invention
The present invention provides the adsorbing material of a kind of heavy metal ion, and component includes attapulgite, ammonium alginate, and attapulgite and
Ammonium alginate is connected by chemical bond,
Present invention also offers the preparation method of a kind of above-mentioned adsorbing material, concretely comprise the following steps:
(1) attapulgite powder body is scattered in organic solvent, dropping amino silicane coupling agent after being uniformly dispersed, 70～100 DEG C
Reaction 6～10h；Reaction is filtered after terminating, vacuum drying, obtains silane coupler modified attapulgite,
Wherein, attapulgite powder body is 1:10～1:30 with the mass ratio of organic solvent,
Organic solvent is toluene or dimethylbenzene,
The amino silicane coupling agent of dropping is 1:1 with the mass ratio of attapulgite powder body,
Amino silicane coupling agent be gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, N-β-(aminoethyl)-
γ-aminopropyltriethoxy dimethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-ammonia
Propyl-triethoxysilicane, γ-aminopropyltriethoxy diethoxy silane or γ-aminopropyltriethoxy dimethoxysilane；
(2) attapulgite modified it is scattered in what step (1) obtained in glutaraldehyde solution, filters after being sufficiently stirred for, washs,
Vacuum drying, obtains the attapulgite that glutaraldehyde is modified,
Wherein, the Solute mass fraction of glutaraldehyde solution is 5%,
Attapulgite modified and the glutaraldehyde solution mass ratio added is 1:10～1:25,
Whipping temp is 30～40 DEG C；
(3) sodium alginate joined in acid solution and stir, obtaining the acid solution of sodium alginate；Step (2) will be obtained
To the modified attapulgite of glutaraldehyde be made into suspension；The acid solution of sodium alginate is added drop-wise to the attapulgite that glutaraldehyde is modified
Suspension in, be stirred and heated to 30～45 DEG C after dropping, react 3～5h, centrifugation, fully wash, remove
The sodium alginate of non-covalent cross-linking, obtains the attapulgite heavy-metal adsorption material of sodium alginate graft crosslinking,
Wherein, acid solution be Solute mass fraction be the acetum of 1%, sodium alginate content in its acid solution be 0.5～
1.5g/100ml,
The attapulgite of glutaraldehyde modification concentration in its suspension is 1～2g/100ml,
During dropping, the weight ratio controlling the sodium alginate attapulgite modified with glutaraldehyde is 1:1～1:2.
The beneficial effects of the present invention is: present invention effect based on glutaraldehyde, by the way of covalent bond, sodium alginate is grafted
Being linked to attapulgite's surface, both adhesions are strong, and in use sodium alginate is difficult to come off from carrier surface and freely roll into a ball
Poly-, heavy metal is polluted and is embodied good absorption property.
Detailed description of the invention
Embodiment 1
(1) during 10g attapulgite is scattered in 100mL toluene, ultrasonic disperse 30min, under stirring condition, dropping 10g γ-
Aminopropyl triethoxysilane, after dripping, is heated to 70 DEG C, reacts 10h, and reaction is filtered after terminating, vacuum drying, i.e.
Obtain attapulgite modified by silane coupling agent；
(2) by molten for the glutaraldehyde that the attapulgite modified 150mL of being dispersed in Solute mass fraction is 5% that obtains in step (1)
In liquid, after 30 DEG C of reaction 3h, filter, after deionized water repeatedly washs, vacuum drying, obtain the attapulgite that glutaraldehyde is modified；
(3) sodium alginate joined in the acetum that Solute mass fraction is 1% and stir 3 hours, obtaining sodium alginate
Acid solution, wherein the content of sodium alginate is 0.5g/100ml,
The attapulgite that the glutaraldehyde obtained in step (2) is modified is made into the suspension that concentration is 1g/100ml,
It is 1:1 according to the weight ratio of sodium alginate with the attapulgite of glutaraldehyde modification, the acid solution of sodium alginate is added drop-wise to penta 2
In the suspension of the attapulgite that aldehyde is modified, after dropping, it is stirred and heated to 30 DEG C, reacts 5h, centrifugation, fully wash
Wash, obtain the attapulgite heavy-metal adsorption material of sodium alginate graft crosslinking.
Embodiment 2
(1) during 10g attapulgite is scattered in 200mL toluene, ultrasonic disperse 20min, under stirring condition, dropping 10g γ-
Aminopropyl trimethoxysilane, after dripping, is heated to 80 DEG C, reacts 8h, and reaction is filtered after terminating, and vacuum drying to obtain final product
Attapulgite modified by silane coupling agent；
(2) by molten for the glutaraldehyde that the attapulgite modified 100mL of being dispersed in Solute mass fraction is 5% that obtains in step (1)
In liquid, after 30 DEG C of reaction 4h, filter, after deionized water repeatedly washs, vacuum drying, obtain the attapulgite that glutaraldehyde is modified；
(3) sodium alginate joined in the acetum that Solute mass fraction is 1% and stir 3 hours, obtaining sodium alginate
Acid solution, wherein the content of sodium alginate is 1g/100ml,
The attapulgite that the glutaraldehyde obtained in step (2) is modified is made into the suspension that concentration is 1.5g/100ml,
It is 1:1.5 according to the weight ratio of sodium alginate with the attapulgite of glutaraldehyde modification, the acid solution of sodium alginate is added drop-wise to penta
In the suspension of the attapulgite of dialdehyde, after dropping, it is stirred and heated to 40 DEG C, reaction 4h, centrifugation, fully
Washing, obtains the attapulgite heavy-metal adsorption material of sodium alginate graft crosslinking.
Embodiment 3
(1) during 10g attapulgite is scattered in 250mL toluene, ultrasonic disperse 20min, under stirring condition, drip 10g N-
β-(aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, after dripping, is heated to 90 DEG C, reacts 7h, after reaction terminates
Filter, vacuum drying, obtain attapulgite modified by silane coupling agent；
(2) by molten for the glutaraldehyde that the attapulgite modified 200mL of being dispersed in Solute mass fraction is 5% that obtains in step (1)
In liquid, after 30 DEG C of reaction 3h, filter, after deionized water repeatedly washs, vacuum drying, obtain the attapulgite that glutaraldehyde is modified；
(3) sodium alginate joined in the acetum that Solute mass fraction is 1% and stir 3 hours, obtaining sodium alginate
Acid solution, wherein the content of sodium alginate is 1g/100ml,
The attapulgite that the glutaraldehyde obtained in step (2) is modified is made into the suspension that concentration is 1g/100ml,
It is 1:1.5 according to the weight ratio of sodium alginate with the attapulgite of glutaraldehyde modification, the acid solution of sodium alginate is added drop-wise to penta
In the suspension of the attapulgite of dialdehyde, after dropping, it is stirred and heated to 35 DEG C, reaction 4h, centrifugation, fully
Washing, obtains the attapulgite heavy-metal adsorption material of sodium alginate graft crosslinking.
Comparative example 1
(1) during 10g attapulgite is scattered in 200mL toluene, ultrasonic disperse 20min, under stirring condition, dropping 10g γ-
Aminopropyl trimethoxysilane, after dripping, is heated to 80 DEG C, reacts 8h, and reaction is filtered after terminating, and vacuum drying to obtain final product
Attapulgite modified by silane coupling agent；
(2) sodium alginate joined in the acetum that Solute mass fraction is 1% and stir 3 hours, obtaining sodium alginate
Acid solution, wherein the content of sodium alginate is 1g/100ml,
Attapulgite modified it is made into the suspension that concentration is 1.5g/100ml by what step (1) obtained,
It is 1:1.5 according to sodium alginate and attapulgite modified weight ratio, the acid solution of sodium alginate is added drop-wise to modified attapulgite
In the suspension of soil, after dropping, it is stirred and heated to 40 DEG C, reacts 4h, centrifugation, fully wash, obtain alginic acid
The attapulgite heavy-metal adsorption material that sodium is modified.
Taking each 0.5g of the compound adsorbent in the various embodiments described above, comparative example, the heavy metal copper ion concentration joining 1L is
In the water of 0.1g/L, after adsorbing 1h under room temperature (25 DEG C), detect the concentration of residual copper ion in solution and calculate absorption
Amount, concrete detection data are as shown in table 1:
Table 1
| Embodiment | Embodiment 2 | Embodiment 3 | Comparative example 1 | |
| Adsorbance (mg/g) | 86.4 | 85.2 | 82.6 | 67.8 |
Claims (9)
1. attapulgite clay/sodium alginate Compound Heavy Metals adsorbent, it is characterised in that: described absorbent component includes attapulgite
Soil, ammonium alginate, and attapulgite and ammonium alginate connected by chemical bond.
2. the preparation method of attapulgite clay/sodium alginate Compound Heavy Metals adsorbent as claimed in claim 1, it is characterised in that: institute
The step stating preparation method is,
(1) attapulgite powder body is scattered in organic solvent, dropping amino silicane coupling agent after being uniformly dispersed, 70～100 DEG C
Reaction 6～10h；Reaction is filtered after terminating, vacuum drying, obtains silane coupler modified attapulgite；
(2) attapulgite modified it is scattered in what step (1) obtained in glutaraldehyde solution, filters after being sufficiently stirred for, washs,
Vacuum drying, obtains the attapulgite that glutaraldehyde is modified；
(3) sodium alginate joined in acid solution and stir, obtaining the acid solution of sodium alginate；Step (2) will be obtained
To the modified attapulgite of glutaraldehyde be made into suspension；The acid solution of sodium alginate is added drop-wise to the attapulgite that glutaraldehyde is modified
Suspension in, be stirred and heated to 30～45 DEG C after dropping, react 3～5h, centrifugation, fully wash, obtain
The attapulgite heavy-metal adsorption material of sodium alginate graft crosslinking.
3. the preparation method of attapulgite clay/sodium alginate Compound Heavy Metals adsorbent as claimed in claim 2, it is characterised in that: step
Suddenly the organic solvent described in (1) is toluene or dimethylbenzene, and attapulgite powder body is 1:10～1 with the mass ratio of organic solvent:
30。
4. the preparation method of attapulgite clay/sodium alginate Compound Heavy Metals adsorbent as claimed in claim 2, it is characterised in that: step
Suddenly the amino silicane coupling agent described in (1) is gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, N-β
-(aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-ammonia second
Base)-gamma-aminopropyl-triethoxy-silane, γ-aminopropyltriethoxy diethoxy silane or γ-aminopropyltriethoxy dimethoxysilane,
The amino silicane coupling agent of dropping is 1:1 with the mass ratio of attapulgite powder body.
5. the preparation method of attapulgite clay/sodium alginate Compound Heavy Metals adsorbent as claimed in claim 2, it is characterised in that: step
Suddenly the Solute mass fraction of the glutaraldehyde solution described in (2) is 5%.
6. the preparation method of attapulgite clay/sodium alginate Compound Heavy Metals adsorbent as claimed in claim 2, it is characterised in that: step
Suddenly, in (2), the mass ratio of the attapulgite modified and glutaraldehyde solution of addition is 1:10～1:25.
7. the preparation method of attapulgite clay/sodium alginate Compound Heavy Metals adsorbent as claimed in claim 2, it is characterised in that: step
Suddenly the acid solution described in (3) be Solute mass fraction be the acetum of 1%, sodium alginate is content in described acid solution
It is 0.5～1.5g/100ml.
8. the preparation method of attapulgite clay/sodium alginate Compound Heavy Metals adsorbent as claimed in claim 2, it is characterised in that: step
Suddenly, in (3), the attapulgite of glutaraldehyde modification concentration in its suspension is 1～2g/100ml.
9. the preparation method of attapulgite clay/sodium alginate Compound Heavy Metals adsorbent as claimed in claim 2, it is characterised in that: step
Suddenly, in (3), during dropping, the weight ratio controlling the sodium alginate attapulgite modified with glutaraldehyde is 1:1～1:2.
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Cited By (9)
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|---|---|---|---|---|
| CN106630131A (en) * | 2016-10-25 | 2017-05-10 | 南京大学宜兴环保研究院 | Preparation method of modified attapulgite particles and method for accelerating granulation of anaerobic sludge by modified attapulgite particles |
| CN106732445A (en) * | 2016-11-30 | 2017-05-31 | 无锡龙盈环保科技有限公司 | A kind of silica modified heavy metal wastewater thereby adsorbent and preparation method thereof |
| CN106987306A (en) * | 2017-06-05 | 2017-07-28 | 蚌埠市江淮粮油有限公司 | It is a kind of to reduce the rape oil-pressing method of water content |
| CN107022411A (en) * | 2017-06-05 | 2017-08-08 | 蚌埠市江淮粮油有限公司 | A kind of preparation method of giving off a strong fragrance rapeseed oil |
| CN107583600A (en) * | 2017-10-18 | 2018-01-16 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of improved silica hydrogel and products thereof and application |
| CN109012621A (en) * | 2016-12-07 | 2018-12-18 | 天津市金鳞水处理科技有限公司 | A kind of heavy metal ion adsorbed and detection type compound water congealing glue fiber |
| CN109289788A (en) * | 2016-12-07 | 2019-02-01 | 天津市金鳞水处理科技有限公司 | Heavy metal ion adsorbed and detection type composite hydrogel |
| CN110841609A (en) * | 2019-12-11 | 2020-02-28 | 广西科技大学 | Preparation method of high-molecular-weight heavy metal adsorbent |
| CN112007617A (en) * | 2019-05-29 | 2020-12-01 | 西南科技大学 | Preparation method of shaddock peel/attapulgite composite material |
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Cited By (11)
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| CN106630131A (en) * | 2016-10-25 | 2017-05-10 | 南京大学宜兴环保研究院 | Preparation method of modified attapulgite particles and method for accelerating granulation of anaerobic sludge by modified attapulgite particles |
| CN106732445A (en) * | 2016-11-30 | 2017-05-31 | 无锡龙盈环保科技有限公司 | A kind of silica modified heavy metal wastewater thereby adsorbent and preparation method thereof |
| CN109012621A (en) * | 2016-12-07 | 2018-12-18 | 天津市金鳞水处理科技有限公司 | A kind of heavy metal ion adsorbed and detection type compound water congealing glue fiber |
| CN109289788A (en) * | 2016-12-07 | 2019-02-01 | 天津市金鳞水处理科技有限公司 | Heavy metal ion adsorbed and detection type composite hydrogel |
| CN106987306A (en) * | 2017-06-05 | 2017-07-28 | 蚌埠市江淮粮油有限公司 | It is a kind of to reduce the rape oil-pressing method of water content |
| CN107022411A (en) * | 2017-06-05 | 2017-08-08 | 蚌埠市江淮粮油有限公司 | A kind of preparation method of giving off a strong fragrance rapeseed oil |
| CN107583600A (en) * | 2017-10-18 | 2018-01-16 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of improved silica hydrogel and products thereof and application |
| CN112007617A (en) * | 2019-05-29 | 2020-12-01 | 西南科技大学 | Preparation method of shaddock peel/attapulgite composite material |
| CN112007617B (en) * | 2019-05-29 | 2022-03-04 | 西南科技大学 | Preparation method of shaddock peel/attapulgite composite material |
| CN110841609A (en) * | 2019-12-11 | 2020-02-28 | 广西科技大学 | Preparation method of high-molecular-weight heavy metal adsorbent |
| CN110841609B (en) * | 2019-12-11 | 2023-04-11 | 广西科技大学 | Preparation method of high-molecular-weight heavy metal adsorbent |
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