CN110523371A - It is a kind of attapulgite modified and its preparation method and application - Google Patents
It is a kind of attapulgite modified and its preparation method and application Download PDFInfo
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- CN110523371A CN110523371A CN201910852716.7A CN201910852716A CN110523371A CN 110523371 A CN110523371 A CN 110523371A CN 201910852716 A CN201910852716 A CN 201910852716A CN 110523371 A CN110523371 A CN 110523371A
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- attapulgite
- coupling agent
- silane coupling
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- chelating agent
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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Abstract
The invention discloses a kind of attapulgite modified, chelating agent is acted on by silane coupling agent and being connected in the surface and hole of attapulgite.Also disclose preparation method: (1) by attapulgite and hydrochloric acid solution ultrasonic mixing, filtering is washed to neutrality, and drying obtains pretreated attapulgite；(2) pretreated attapulgite and silane coupling agent are added in ethanol solution, oscillating reactions after ultrasound, filtration washing, drying obtains the attapulgite of silane coupling agent processing；(3) chelating agent is added to the water, is configured to chelating agent solution, then the attapulgite of silane coupling agent processing is added in chelating agent solution and is reacted, washing and drying obtains the modified attapulgite of chelating agent.The present invention is modified attapulgite using chelating agent, and method of modifying is simple, environmentally friendly, will not generate secondary pollution；It is attapulgite modified to can be realized to heavy metal ions in wastewater (Cu2+And Cr6+) efficient absorption.
Description
Technical field
The present invention relates to a kind of attapulgite modified and its preparation method and application more particularly to modified a kind of chelating agent
Attapulgite and preparation method thereof and the attapulgite modified application at heavy metal ion adsorbed aspect.
Background technique
Heavy metal ion harm to the human body is serious, mainly has ion exchange to the processing method of effluent containing heavy metal ions at present
Method, membrane separation process, electrochemical deposition method, absorption method etc..Wherein, absorption method to the removal rate height of heavy metal ion, large amount of adsorption,
The rate of adsorption is fast, easy to operate.But it is generally used for heavy metal ion adsorbed adsorbent price costly.
Attapulgite is also known as palygorskite, is a kind of aqueous rich magnesium aluminium silicon salt clay mineral with link layer structure.Concave convex rod
Stone ore object almost various regions all over the world, it is cheap and easy to get and enjoys the laudatory title of " thousand with soil ", " kings of ten thousand soil ", has wider
Wealthy application prospect.Attapulgite is played important with its unique multi-pore channel structure and high surface area in environmental pollution treatment
Effect, especially in decoloring dye waste water and water in terms of heavy metal ion-containing waste water processing, there is high utility value.But it
There is certain mineralogy limitations to weaken whole because of the symbiosis impurity in mineral containing significant proportion for right palygorskite
Physical and chemical performance, so that the adsorptivity of attapulgite be made to be greatly affected in industrial application.
Summary of the invention
Goal of the invention: in view of the above problems, the present invention propose it is a kind of with the attapulgite modified of preferable absorption property.This
The another object of invention is to provide the attapulgite modified preparation method.It is a still further object of the present invention to provide the modification is recessed
Application of the convex stick soil at heavy metal ion adsorbed aspect.
Technical solution: of the present invention attapulgite modified, chelating agent is connected to bumps by silane coupling agent effect
In the surface and hole of stick soil.
It is of the present invention to prepare above-mentioned attapulgite modified method, comprising the following steps:
(1) by attapulgite and hydrochloric acid solution ultrasonic mixing, filtering is washed to neutrality, and drying obtains pretreated bumps
Stick soil；
(2) pretreated attapulgite and silane coupling agent are added in ethanol solution, diafiltration is crossed in oscillating reactions after ultrasound
It washs, dries, obtain the attapulgite of silane coupling agent processing；
(3) chelating agent is added to the water, is configured to chelating agent solution, then the attapulgite of silane coupling agent processing is added
It is reacted in chelating agent solution, washing and drying obtains the modified attapulgite of chelating agent.
Wherein, the concentration of hydrochloric acid solution is 1~9mol/L in the step (1), the attapulgite and hydrochloric acid solution
Solid-to-liquid ratio is 1:10~1:20, and acid processing can remove the dirts such as carbonate, together with the poly- attapulgite stick crystalline substance beam of decomposed
When H+The Mg contained in attapulgite can be replaced2+、Al3+And Fe3+Equal metal ions, the cation for improving attapulgite are commutative
Property, improve the adsorptivity of attapulgite；Ultrasonic time be 10~30min, drying temperature be 70~110 DEG C, drying time be 8~
12h。
Silane coupling agent in the step (2) is 3- aminopropyl triethoxysilane, γ-aminopropyl trimethoxy silicon
One of alkane, N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane are a variety of；The volume of silane coupling agent is that ethyl alcohol is molten
The solid-to-liquid ratio of the 1%~10% of liquid product, the pretreated attapulgite and ethanol solution is 1:5~1:10；Ultrasonic time
For 10~30min, oscillating reactions temperature is 60~80 DEG C, and duration of oscillation is 5~8h, and drying temperature is 60~120 DEG C, when drying
Between be 8~12h.
Chelating agent in the step (3) is carboxylic acid quasi-chelate compound, selected from four sodium of iminodisuccinic acid, sodium citrate,
Sodium tartrate or sodium gluconate, the concentration of chelating agent solution are 0.05~0.20mol/L, the concave convex rod of silane coupling agent processing
The solid-to-liquid ratio of soil and chelating agent solution is 1:10~1:20；Reaction time be 12~for 24 hours, drying temperature be 60~80 DEG C, drying
Time is 10~14h.
By the above-mentioned attapulgite modified absorption applied to heavy metal ion.
Attapulgite modified preparation method of the invention is using attapulgite as matrix, and silane coupling agent hydrolysis generates silicon
Dehydration condensation occurs for hydroxyl and attapulgite's surface hydroxyl, makes attapulgite's surface grafted amino group, thus amino and chelating
Electrostatic interaction occurs for the carboxyl on agent surface, and chelating agent modification to attapulgite's surface improves the suction-operated to heavy metal.
The utility model has the advantages that compared with prior art, remarkable advantage of the invention is: the present invention is chelated using biodegradation type
Agent is modified attapulgite, and method of modifying is simple, environmentally friendly, will not generate secondary pollution；Attapulgite modified energy
Enough efficient absorptions realized to heavy metal ions in wastewater, to Cu2+And Cr6+Adsorbance respectively be up to 35.23mg/g and
7.39mg/g。
Detailed description of the invention
Fig. 1 is attapulgite and attapulgite modified infrared spectrogram；
Fig. 2 is attapulgite and attapulgite modified scanning electron microscope sem figure.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples.
Embodiment 1
(1) it by attapulgite and 1mol/L hydrochloric acid solution ultrasound 10min, filters, is washed with deionized into after standing
Property, drying 8h obtains pretreated attapulgite under the conditions of 70 DEG C, and wherein the solid-to-liquid ratio of attapulgite and hydrochloric acid solution is 1:10
(g:mL)；
(2) pretreated attapulgite and silane coupling agent 3- aminopropyl triethoxysilane are added sequentially to ethanol solution
In (volume ratio of ethyl alcohol and water is 2:3), 5h is reacted in constant temperature oscillation shaking table 60 DEG C after ultrasonic 10min, after cooling and standings
Filtering, is successively washed with dehydrated alcohol, deionized water, dries 8h under the conditions of 60 DEG C, obtains the concave convex rod of silane coupling agent processing
Soil, wherein silane coupling agent volume is the 1% of volumes of aqueous ethanol, and the solid-to-liquid ratio of pretreated attapulgite and ethanol solution is
1:5；
(3) four sodium of chelating agent iminodisuccinic acid is added to the water, is configured to the chelating agent solution of 0.05mol/L, room
Under temperature, the attapulgite of silane coupling agent processing is added in chelating agent solution, 12h is reacted, is washed after terminating through deionized water
Wash, under the conditions of 60 DEG C dry 10h obtain modified attapulgite, wherein silane coupling agent processing attapulgite and chelating agent it is molten
The solid-to-liquid ratio of liquid is 1:10.
Fig. 1 is the infrared spectrogram of rear attapulgite before modified, and modified attapulgite is in 2941cm-1Characteristic peak enhancing,
For the stretching vibration characteristic peak of-OH；In 1406cm-1The symmetrical stretching vibration peak for locating appearance-COOH, illustrates that chelating agent is successfully modified
To the surface of attapulgite.
Fig. 2 be attapulgite before modification after SEM figure, modified attapulgite is distributed relative distribution, and surface is by chela
Mixture surrounds.
Embodiment 2
(1) it by attapulgite and 9mol/L hydrochloric acid solution ultrasound 30min, filters, is washed with deionized into after standing
Property, drying 12h obtains pretreated attapulgite under the conditions of 110 DEG C, and wherein the solid-to-liquid ratio of attapulgite and hydrochloric acid solution is 1:
20；
(2) pretreated attapulgite and silane coupling agent 3- aminopropyl triethoxysilane are added sequentially to ethanol solution
In, 8h is reacted after ultrasonic 30min in constant temperature oscillation shaking table 80 DEG C, is filtered after cooling and standings, successively with dehydrated alcohol, go from
Sub- water washing dries 12h under the conditions of 120 DEG C, obtains the attapulgite of silane coupling agent processing, and wherein silane coupling agent volume is
The solid-to-liquid ratio of the 10% of volumes of aqueous ethanol, pretreated attapulgite and ethanol solution is 1:10；
(3) four sodium of chelating agent iminodisuccinic acid is added to the water, is configured to the chelating agent solution of 0.20mol/L, room
Under temperature, the attapulgite of silane coupling agent processing is added in chelating agent solution, reaction for 24 hours, is washed after terminating through deionized water
Wash, under the conditions of 80 DEG C dry 14h obtain modified attapulgite, wherein silane coupling agent processing attapulgite and chelating agent it is molten
The solid-to-liquid ratio of liquid is 1:20.
Embodiment 3
(1) by attapulgite and 4.5mol/L hydrochloric acid solution ultrasound 15min, filtered after standing, be washed with deionized to
Neutrality, drying 10h obtains pretreated attapulgite under the conditions of 90 DEG C, and wherein the solid-to-liquid ratio of attapulgite and hydrochloric acid solution is 1:
15；
(2) pretreated attapulgite and silane coupling agent 3- aminopropyl triethoxysilane are added sequentially to ethanol solution
In, 6.5h is reacted after ultrasonic 15min in constant temperature oscillation shaking table 70 DEG C, is filtered after cooling and standings, successively with dehydrated alcohol, go
Ion water washing dries 10h under the conditions of 90 DEG C, obtains the attapulgite of silane coupling agent processing, wherein silane coupling agent volume
It is the 5% of volumes of aqueous ethanol, the solid-to-liquid ratio of pretreated attapulgite and ethanol solution is 1:7.5；
(3) four sodium of chelating agent iminodisuccinic acid is added to the water, is configured to the chelating agent solution of 0.10mol/L, room
Under temperature, the attapulgite of silane coupling agent processing is added in chelating agent solution, 18h is reacted, is washed after terminating through deionized water
Wash, under the conditions of 70 DEG C dry 12h obtain modified attapulgite, wherein silane coupling agent processing attapulgite and chelating agent it is molten
The solid-to-liquid ratio of liquid is 1:15.
Embodiment 4
(1) it by attapulgite and 1mol/L hydrochloric acid solution ultrasound 30min, filters, is washed with deionized into after standing
Property, drying 8h obtains pretreated attapulgite under the conditions of 70 DEG C, and wherein the solid-to-liquid ratio of attapulgite and hydrochloric acid solution is 1:10；
(2) pretreated attapulgite and silane coupling agent 3- aminopropyl triethoxysilane, γ-aminopropyl trimethoxy
Silane is added sequentially in ethanol solution, reacts 5h, mistake after cooling and standings after ultrasonic 10min in constant temperature oscillation shaking table 60 DEG C
Filter, is successively washed with dehydrated alcohol, deionized water, dries 12h under the conditions of 60 DEG C, obtains the concave convex rod of silane coupling agent processing
Soil, wherein silane coupling agent volume is the 1% of volumes of aqueous ethanol, and the solid-to-liquid ratio of pretreated attapulgite and ethanol solution is
1:10；
(3) four sodium of chelating agent iminodisuccinic acid is added to the water, is configured to the chelating agent solution of 0.05mol/L, room
Under temperature, the attapulgite of silane coupling agent processing is added in chelating agent solution, 12h is reacted, is washed after terminating through deionized water
Wash, under the conditions of 60 DEG C dry 10h obtain modified attapulgite, wherein silane coupling agent processing attapulgite and chelating agent it is molten
The solid-to-liquid ratio of liquid is 1:10.
Embodiment 5
(1) it by attapulgite and 1mol/L hydrochloric acid solution ultrasound 10min, filters, is washed with deionized into after standing
Property, drying 8h obtains pretreated attapulgite under the conditions of 70 DEG C, and wherein the solid-to-liquid ratio of attapulgite and hydrochloric acid solution is 1:10；
(2) pretreated attapulgite and silane coupling agent 3- aminopropyl triethoxysilane are added sequentially to ethanol solution
In, 5h is reacted after ultrasonic 10min in constant temperature oscillation shaking table 60 DEG C, is filtered after cooling and standings, successively with dehydrated alcohol, go from
Sub- water washing dries 8h under the conditions of 60 DEG C, obtains the attapulgite of silane coupling agent processing, and wherein silane coupling agent volume is second
The solid-to-liquid ratio of the 1% of alcoholic solution volume, pretreated attapulgite and ethanol solution is 1:10；
(3) chelator acid citrate sodium is added to the water, is configured to the chelating agent solution of 0.10mol/L, at room temperature, by silane
The attapulgite of coupling agent treatment is added in chelating agent solution, reacts 12h, through deionized water washing, 60 DEG C of conditions after terminating
Lower drying 10h obtains modified attapulgite, wherein the solid-to-liquid ratio of the attapulgite and chelating agent solution of silane coupling agent processing
For 1:10.
Embodiment 6
(1) it by attapulgite and 9mol/L hydrochloric acid solution ultrasound 30min, filters, is washed with deionized into after standing
Property, drying 12h obtains pretreated attapulgite under the conditions of 110 DEG C, and wherein the solid-to-liquid ratio of attapulgite and hydrochloric acid solution is 1:
20；
(2) pretreated attapulgite and silane coupling agent 3- aminopropyl triethoxysilane are added sequentially to ethanol solution
In, 8h is reacted after ultrasonic 10min in constant temperature oscillation shaking table 80 DEG C, is filtered after cooling and standings, successively with dehydrated alcohol, go from
Sub- water washing dries 12h under the conditions of 120 DEG C, obtains the attapulgite of silane coupling agent processing, and wherein silane coupling agent volume is
The solid-to-liquid ratio of the 10% of volumes of aqueous ethanol, pretreated attapulgite and ethanol solution is 1:20；
(3) chelating agent sodium tartrate is added to the water, is configured to the chelating agent solution of 0.20mol/L, at room temperature, by silane
The attapulgite of coupling agent treatment is added in chelating agent solution, and reaction for 24 hours, is washed after terminating through deionized water, 80 DEG C of conditions
Lower drying 14h obtains modified attapulgite, wherein the solid-to-liquid ratio of the attapulgite and chelating agent solution of silane coupling agent processing
For 1:20.
Heavy metal ion adsorbed performance test
By the attapulgite of Examples 1 to 6, silane coupling agent processing attapulgite and attapulgite modified press respectively
The dosage of 0.8g/L is added to Cu2+、Cr6+Initial concentration is to vibrate 12h at room temperature in the waste water of 1mmol/L, after standing
Filtering measures Cu using inductively coupled plasma atomic mass spectrometry, spectrophotometry2+、Cr6+Concentration calculates adsorbance, absorption
Data are shown in Table 1.
Adsorbance of each embodiment of table 1 to heavy metal ions in wastewater
As shown in Table 1, attapulgite modified to Cu compared to attapulgite2+、Cr6+Adsorbance significantly improve, compare
Several embodiments, wherein embodiment 2 is to Cu2+、Cr6+Adsorbance is up to 35.23mg/g and 7.39mg/g, has been respectively increased 3.3 times
With 1.8 times, adsorption effect is apparently higher than other embodiments.It should be noted that the concentration of chelating agent solution of the present invention is 0.05
~0.20mol/L, if excessive concentration can block the duct of attapulgite to influence adsorption effect, if concentration it is too low will lead to it is recessed
The chelator connected on convex stick soil is too low, and adsorption effect is also undesirable.
Claims (10)
1. a kind of attapulgite modified, which is characterized in that chelating agent is connected to the table of attapulgite by silane coupling agent effect
In face and hole.
2. a kind of prepare attapulgite modified method as described in claim 1, which comprises the following steps:
(1) by attapulgite and hydrochloric acid solution ultrasonic mixing, filtering is washed to neutrality, and drying obtains pretreated concave convex rod
Soil；
(2) pretreated attapulgite and silane coupling agent are added in ethanol solution, oscillating reactions after ultrasound, filtration washing,
Drying obtains the attapulgite of silane coupling agent processing；
(3) chelating agent is added to the water, is configured to chelating agent solution, then chelating is added in the attapulgite of silane coupling agent processing
It is reacted in agent solution, washing and drying obtains the modified attapulgite of chelating agent.
3. attapulgite modified preparation method according to claim 1, which is characterized in that hydrochloric acid in the step (1)
The concentration of solution is 1~9mol/L, and the solid-to-liquid ratio of the attapulgite and hydrochloric acid solution is 1:10~1:20.
4. attapulgite modified preparation method according to claim 1, which is characterized in that super in the step (1)
The sound time is 10~30min, and drying temperature is 70~110 DEG C, and drying time is 8~12h.
5. attapulgite modified preparation method according to claim 1, which is characterized in that the silicon in the step (2)
Alkane coupling agent is 3- aminopropyl triethoxysilane, γ-aminopropyltrimethoxysilane, N- (β-aminoethyl)-γ-aminopropyl three
One of methoxy silane is a variety of.
6. attapulgite modified preparation method according to claim 1, which is characterized in that silane in the step (2)
The volume of coupling agent is the 1%~10% of volumes of aqueous ethanol, the solid-to-liquid ratio of the pretreated attapulgite and ethanol solution
For 1:5~1:10.
7. attapulgite modified preparation method according to claim 1, which is characterized in that super in the step (2)
The sound time is 10~30min, and oscillating reactions temperature is 60~80 DEG C, and duration of oscillation is 5~8h, and drying temperature is 60~120 DEG C,
Drying time is 8~12h.
8. attapulgite modified preparation method according to claim 1, which is characterized in that the chela in the step (3)
Mixture is carboxylic acid quasi-chelate compound, is selected from four sodium of iminodisuccinic acid, sodium citrate, sodium tartrate or sodium gluconate, chelating
The concentration of agent solution is 0.05~0.20mol/L, and the attapulgite of silane coupling agent processing and the solid-to-liquid ratio of chelating agent solution are
1:10~1:20.
9. attapulgite modified preparation method according to claim 1, which is characterized in that reaction in the step (3)
Time be 12~for 24 hours, drying temperature be 60~80 DEG C, drying time be 10~14h.
10. a kind of attapulgite modified application in heavy metal ion adsorbed described in claim 1.
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Cited By (6)
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| CN115155513A (en) * | 2022-07-08 | 2022-10-11 | 两山生态科技(山东)有限公司 | Preparation method and application of modified volcanic ash |
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| CN115350681A (en) * | 2022-08-16 | 2022-11-18 | 青海师范大学 | Carboxylated attapulgite composite material and preparation method and application thereof |
| CN115350682A (en) * | 2022-08-16 | 2022-11-18 | 青海师范大学 | Attapulgite composite material rich in carboxyl and preparation method and application thereof |
| CN116116377A (en) * | 2023-01-10 | 2023-05-16 | 中国铁工投资建设集团有限公司 | Preparation method and application of attapulgite adsorbent loaded with bimetallic oxide |
| CN117625200A (en) * | 2023-11-01 | 2024-03-01 | 山东智土生态环境研究院有限公司 | Preparation method and application of contaminated soil heavy metal passivation material |
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| CN109225143A (en) * | 2018-10-22 | 2019-01-18 | 成都新柯力化工科技有限公司 | A kind of attapulgite modified filtrate and preparation method for heavy metal containing wastewater treatment |
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| CN115155513A (en) * | 2022-07-08 | 2022-10-11 | 两山生态科技(山东)有限公司 | Preparation method and application of modified volcanic ash |
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| CN115304961A (en) * | 2022-09-23 | 2022-11-08 | 广东宝克文具有限公司 | Color paste containing functional crosslinking assistant capable of promoting stability of color paste system, preparation method thereof and application thereof in neutral ink |
| CN116116377A (en) * | 2023-01-10 | 2023-05-16 | 中国铁工投资建设集团有限公司 | Preparation method and application of attapulgite adsorbent loaded with bimetallic oxide |
| CN117625200A (en) * | 2023-11-01 | 2024-03-01 | 山东智土生态环境研究院有限公司 | Preparation method and application of contaminated soil heavy metal passivation material |
| CN117625200B (en) * | 2023-11-01 | 2024-05-03 | 山东智土生态环境研究院有限公司 | Preparation method and application of contaminated soil heavy metal passivation material |
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