CN106423045B - A kind of modified montmorillonoid sorbent preparation method of Treatment of Zinc-containing Wastewater - Google Patents
A kind of modified montmorillonoid sorbent preparation method of Treatment of Zinc-containing Wastewater Download PDFInfo
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- CN106423045B CN106423045B CN201611037852.3A CN201611037852A CN106423045B CN 106423045 B CN106423045 B CN 106423045B CN 201611037852 A CN201611037852 A CN 201611037852A CN 106423045 B CN106423045 B CN 106423045B
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- montmorillonite
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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
Abstract
A kind of modified montmorillonoid sorbent preparation method of Treatment of Zinc-containing Wastewater, the steps include: the preparation of (1) montmorillonite suspension: being purified montmorillonite for fine-powdered material by pretreatment measure, and is configured to montmorillonite suspension with distilled water；(2) preparation of FN intercalator, (3) FN intercalator is inorganic modified, (4) purification of FN intercalated montmorillonite, (5) preparation of SDS intercalator, (6) SDS intercalator is organically-modified, (7) preparation of PAM flocculant, (8) purification of SDS intercalated montmorillonite, PAM flocculant is added dropwise in the twice-modified montmorillonite suspension obtained in step (6), high speed centrifugation, filtering are quickly carried out after mixing evenly, filter residue is cleaned with deionized water to neutrality, low temperature drying is carried out, obtains pure SDS intercalated montmorillonite powder；(9) SDS intercalated montmorillonite powder metallurgy made from step (8) is roasted, modified montmorillonoid adsorbent is made.
Description
Technical field
The present invention relates to the modified montmorillonoid adsorbent preparations that trade effluent administers field more particularly to Treatment of Zinc-containing Wastewater
Technology.
Background technique
In recent years, as industrial circle develops, people gradually increase the demand of water resource, while global water
Problem of environmental pollution also becomes further prominent.Human industry's activity causes sewage largely to discharge, and leads to weight in earth surface water body
Metallic contaminants concentration is gradually increased, and seriously threatens the existence and living environment of the mankind.Especially certain activity are higher heavy
Metal ion sewage, such as the processing problem of zinc-containing water cause society since its difficulty of governance is big, effect is poor, at high cost
The highest attention of the common people and numerous experts have become trade effluent and administer the big technical problem that field must be captured.
The zinc ion concentration of zinc-containing water has been in a lower level at present, and common removal zinc ion measure has
The methods of chemical precipitation method, ion-exchange, activated carbon adsorption, but that there are treatment effeciencies is low, economic benefit is low etc. for these technologies
Disadvantage.By many decades technology precipitate, the pollutant absorption property of mineral material gradually by it has been found that mineral adsorbent because
For its rich reserves, it is low in cost, effect on environment is small the advantages that be concerned, related mineral adsorbent is at sewage containing zinc
The research of reason control has gradually become a hot spot.Wherein, montmorillonite is because of its higher specific surface area, biggish porosity and property
Matter is stable, the characteristics such as low in cost, is widely studied as a kind of excellent adsorbent material.The zinc of montmorillonite itself
Ionic adsorption performance is not high, but after being specifically modified to it, zinc ion absorption property can be significantly increased.At present
It is inorganic, organically-modified very extensive to the research of specific pollutants absorption property to increase it in relation to montmorillonite, still
For realizing that its promotes the processing capacity of zinc-containing water by modified, there is not too many research also, therefore by montmorillonite application
In zinc-containing water processing, the treatment effect reached is tended not to.It employs new technology and montmorillonite is subjected to modification appropriate, to mention
Its high zinc ion absorption property, can play a significant role for the processing of zinc-containing water.
Summary of the invention
The object of the present invention is to provide a kind of modified montmorillonoid sorbent preparation methods of Treatment of Zinc-containing Wastewater.
The present invention is a kind of modified montmorillonoid sorbent preparation method of Treatment of Zinc-containing Wastewater, including following operating procedure:
(1) preparation of montmorillonite suspension: montmorillonite is purified by the pretreatments measure such as flushing, drying, crushing, sieving
It for 100~150 targeted fine powder shape materials, and is 0.1~0.2 to be configured to montmorillonite suspension by solid-liquid mass ratio with distilled water；
(2) preparation of FN intercalator: 1mol/L iron nitrate solution, 1mol/L sodium hydroxide solution are mixed in the following proportions
It is uniform: 10~12mL of 1mol/L iron nitrate solution, 20~25mL of 1mol/L sodium hydroxide solution；
(3) FN intercalator is inorganic modified: under 60~80 DEG C of constant temperatures, the montmorillonite prepared in step (1) is outstanding
The FN intercalator prepared in turbid and step (2) is uniformly mixed in the ratio of 5:1~3:1, be sufficiently stirred and ultrasonic disperse 15~
20 minutes, keep montmorillonite suspension sufficiently modified；
(4) purification of FN intercalated montmorillonite: FN intercalation modifying montmorillonite suspension obtained in step (3) is centrifuged,
After precipitating, using washes of absolute alcohol, centrifugation, precipitating, cleaning process is repeated several times until solution pH value is lower than 8.0, Zhi Houyu
Low temperature drying is carried out at 60~80 DEG C, obtains pure FN intercalated montmorillonite powder；
(5) preparation of SDS intercalator: under normal temperature conditions, by lauryl sodium sulfate (SDS), 1mol/L nitric acid and nothing
Water-ethanol is uniformly mixed in the following proportions: lauryl sodium sulfate 20~25g, 1mol/L 10~12mL of nitric acid, dehydrated alcohol 10
~12mL；
(6) SDS intercalator is organically-modified: by the FN intercalated montmorillonite powder and distilled water that purification obtains in step (4)
It is configured to FN intercalated montmorillonite suspension for 0.1~0.2 by solid-liquid mass ratio, and is pressed with the SDS intercalator prepared in step (5)
The ratio of 8:1~5:1 is uniformly mixed, and is sufficiently stirred simultaneously ultrasonic disperse 15~20 minutes, is kept FN intercalated montmorillonite suspension secondary
It is modified；
(7) preparation of PAM flocculant: under normal temperature conditions by polyacrylamide, 1mol/L nitric acid and distilled water, by following
Ratio is uniformly mixed: polyacrylamide 5~10g, 1mol/L 10~12mL of nitric acid, 100~120mL of distilled water；
(8) it the purification of SDS intercalated montmorillonite: is added dropwise in the SDS intercalation modifying montmorillonite suspension obtained in step (6)
0.5%~0.8% PAM flocculant quickly carries out high speed centrifugation, filtering, by the filter residue deionized water of filtering after mixing evenly
Cleaning carries out low temperature drying at 60~80 DEG C later, obtains pure SDS intercalated montmorillonite powder to neutrality；
(9) by SDS intercalated montmorillonite powder made from step (8) at 450~550 DEG C high-temperature roasting 30~45 minutes,
Modified montmorillonoid adsorbent is made.
The present invention can reach comparable technical progress and practicability, and with the extensive utility value in industry, until
It has the advantage that less
(1) the present invention provides a kind of modified montmorillonoid sorbent preparation method of Treatment of Zinc-containing Wastewater, it is with montmorillonite
Base adsorbent passes through modification twice, modified montmorillonoid adsorbent is obtained, to the zinc ion of zinc-containing water in industrial wastewater
Adsorptivity with higher.
(2) raw material of the present invention is extensive, the feature of environmental protection is good, low in cost, and preparation process is simple, can be substantially reduced industry at
This, meets waste water control industry development requirement, value of industrial utilization with higher.
Specific embodiment
The present invention provides a kind of modified montmorillonoid sorbent preparation method of Treatment of Zinc-containing Wastewater, technically have obvious
Progressive, and have significant beneficial effect, be a kind of novel, progressive, effective new technology.It is addressed before for the present invention
Other technologies contents, features and effects will be illustrated in detail below.By the explanation of specific embodiment, when can be to this
Invention is able to more deeply and specifically understand to reach the technical means and efficacy that predetermined purpose is taken, however appended implementation
Example is only to provide reference and description and is used, and is not intended to limit the present invention.
The present invention provides a kind of modified montmorillonoid sorbent preparation methods of Treatment of Zinc-containing Wastewater, based on montmorillonite
Adsorbent, it is first inorganic modified to montmorillonite progress, FN intercalated montmorillonite is obtained, then carry out organically-modified and flocculation, purification, obtained
Modified montmorillonoid adsorbent is made after high-temperature roasting in pure SDS intercalated montmorillonite powder.It is obtained using this method
Modified montmorillonoid adsorbent can reach 88.0% or more to the removal rate of zinc ion in zinc-containing water.
A kind of modified montmorillonoid sorbent preparation method of Treatment of Zinc-containing Wastewater of the present invention, including following operating procedure:
(1) preparation of montmorillonite suspension: montmorillonite is purified by the pretreatments measure such as flushing, drying, crushing, sieving
It for 100~150 targeted fine powder shape materials, and is 0.1~0.2 to be configured to montmorillonite suspension by solid-liquid mass ratio with distilled water；
(2) preparation of FN intercalator: 1mol/L iron nitrate solution, 1mol/L sodium hydroxide solution are mixed in the following proportions
It is uniform: 10~12mL of 1mol/L iron nitrate solution, 20~25mL of 1mol/L sodium hydroxide solution；
(3) FN intercalator is inorganic modified: under 60~80 DEG C of constant temperatures, the montmorillonite prepared in step (1) is outstanding
The FN intercalator prepared in turbid and step (2) is uniformly mixed in the ratio of 5:1~3:1, be sufficiently stirred and ultrasonic disperse 15~
20 minutes, keep montmorillonite suspension sufficiently modified；
(4) purification of FN intercalated montmorillonite: FN intercalation modifying montmorillonite suspension obtained in step (3) is centrifuged,
After precipitating, using washes of absolute alcohol, centrifugation, precipitating, cleaning process is repeated several times until solution pH value is lower than 8.0, Zhi Houyu
Low temperature drying is carried out at 60~80 DEG C, obtains pure FN intercalated montmorillonite powder；
(5) preparation of SDS intercalator: under normal temperature conditions, by lauryl sodium sulfate (SDS), 1mol/L nitric acid and nothing
Water-ethanol is uniformly mixed in the following proportions: lauryl sodium sulfate 20~25g, 1mol/L 10~12mL of nitric acid, dehydrated alcohol 10
~12mL；
(6) SDS intercalator is organically-modified: by the FN intercalated montmorillonite powder and distilled water that purification obtains in step (4)
It is configured to FN intercalated montmorillonite suspension for 0.1~0.2 by solid-liquid mass ratio, and is pressed with the SDS intercalator prepared in step (5)
The ratio of 8:1~5:1 is uniformly mixed, and is sufficiently stirred simultaneously ultrasonic disperse 15~20 minutes, is kept FN intercalated montmorillonite suspension secondary
It is modified；
(7) preparation of PAM flocculant: under normal temperature conditions by polyacrylamide, 1mol/L nitric acid and distilled water, by following
Ratio is uniformly mixed: polyacrylamide 5~10g, 1mol/L 10~12mL of nitric acid, 100~120mL of distilled water；
(8) it the purification of SDS intercalated montmorillonite: is added dropwise in the SDS intercalation modifying montmorillonite suspension obtained in step (6)
0.5%~0.8% PAM flocculant quickly carries out high speed centrifugation, filtering, by the filter residue deionized water of filtering after mixing evenly
Cleaning carries out low temperature drying at 60~80 DEG C later, obtains pure SDS intercalated montmorillonite powder to neutrality；
(9) by SDS intercalated montmorillonite powder made from step (8) at 450~550 DEG C high-temperature roasting 30~45 minutes,
Modified montmorillonoid adsorbent is made.
Preferably, FN intercalator is at the uniform velocity added in 5 minutes during the preparation process, by iron nitrate solution in step (2)
It into sodium hydroxide solution, and stirs, temperature when control is added is 60~80 DEG C；
Preferably, SDS intercalator is slowly added into nitre during the preparation process, by lauryl sodium sulfate in step (5)
In acid, after being uniformly dissolved, the mixed solution of the two is at the uniform velocity added in dehydrated alcohol in 5 minutes, and is stirred,
Temperature when control is added is 20~25 DEG C；
Preferably, PAM flocculant is slowly added into distilled water during the preparation process, by polyacrylamide in step (7)
In, after being uniformly dissolved, the temperature when mixed solution of the two being at the uniform velocity added in nitric acid in 5 minutes, and controlling addition is
20~25 DEG C.
Embodiment 1:
Montmorillonite is cleaned, dried, crushed, is sieved, the montmorillonite fine materials of 140~150 mesh of partial size are selected,
The suspension that solid-liquid mass ratio is 0.1~0.2 is made with distilled water in the montmorillonite；With iron nitrate solution, sodium hydroxide solution
Prepare FN intercalator, under 60 DEG C of constant temperatures, be added in montmorillonite suspension carry out it is inorganic modified；FN intercalation modifying is covered
De- soil suspension is configured to FN by solid-liquid mass ratio with distilled water for 0.1~0.2 and inserts after centrifugation, precipitating, cleaning are purified
Layer montmorillonite suspension；SDS intercalator is prepared with lauryl sodium sulfate, nitric acid and dehydrated alcohol, it is de- to be added to FN intercalation illiteracy
It is modified that Secondary Organic is carried out in native suspension；PAM flocculant is prepared with polyacrylamide, nitric acid and distilled water, SDS is added to and inserts
In layer modified montmorillonoid suspension, quickly stirring, centrifugation, filtering, and it is cleaned, dry after at 500 DEG C high-temperature roasting 45 divide
Modified montmorillonoid adsorbent is made in clock.
The solution of zinc sulfate that waste water in the present embodiment is formulated using zinc sulfate and deionized water, after detection,
Its zinc ion content is 465.14 mgL-1。
The modified montmorillonoid adsorbent obtained using this method is to zinc ion in above-mentioned zinc-containing water (solution of zinc sulfate)
Removal rate is 88.0%.
Embodiment 2:
Montmorillonite is cleaned, dried, crushed, is sieved, the montmorillonite fine materials of 100~115 mesh of partial size are selected,
The suspension that solid-liquid mass ratio is 0.1~0.2 is made with distilled water in the montmorillonite；With iron nitrate solution, sodium hydroxide solution
Prepare FN intercalator, under 60 DEG C of constant temperatures, be added in montmorillonite suspension carry out it is inorganic modified；FN intercalation modifying is covered
De- soil suspension is configured to FN by solid-liquid mass ratio with distilled water for 0.1~0.2 and inserts after centrifugation, precipitating, cleaning are purified
Layer montmorillonite suspension；SDS intercalator is prepared with lauryl sodium sulfate, nitric acid and dehydrated alcohol, it is de- to be added to FN intercalation illiteracy
It is modified that Secondary Organic is carried out in native suspension；PAM flocculant is prepared with polyacrylamide, nitric acid and distilled water, SDS is added to and inserts
In layer modified montmorillonoid suspension, quickly stirring, centrifugation, filtering, and it is cleaned, dry after at 500 DEG C high-temperature roasting 45 divide
Modified montmorillonoid adsorbent is made in clock.
The solution of zinc sulfate that waste water in the present embodiment is formulated using zinc sulfate and deionized water, after detection,
Its zinc ion content is 465.14 mgL-1。
The modified montmorillonoid adsorbent obtained using this method is to zinc ion in above-mentioned zinc-containing water (solution of zinc sulfate)
Removal rate is 92.5%.
Embodiment 3:
Montmorillonite is cleaned, dried, crushed, is sieved, the montmorillonite fine materials of 100~115 mesh of partial size are selected,
The suspension that solid-liquid mass ratio is 0.1~0.2 is made with distilled water in the montmorillonite；With iron nitrate solution, sodium hydroxide solution
Prepare FN intercalator, under 80 DEG C of constant temperatures, be added in montmorillonite suspension carry out it is inorganic modified；FN intercalation modifying is covered
De- soil suspension is configured to FN by solid-liquid mass ratio with distilled water for 0.1~0.2 and inserts after centrifugation, precipitating, cleaning are purified
Layer montmorillonite suspension；SDS intercalator is prepared with lauryl sodium sulfate, nitric acid and dehydrated alcohol, it is de- to be added to FN intercalation illiteracy
It is modified that Secondary Organic is carried out in native suspension；PAM flocculant is prepared with polyacrylamide, nitric acid and distilled water, SDS is added to and inserts
In layer modified montmorillonoid suspension, quickly stirring, centrifugation, filtering, and it is cleaned, dry after at 550 DEG C high-temperature roasting 45 divide
Modified montmorillonoid adsorbent is made in clock.
The solution of zinc sulfate that waste water in the present embodiment is formulated using zinc sulfate and deionized water, after detection,
Its zinc ion content is 465.14 mgL-1。
The modified montmorillonoid adsorbent obtained using this method is to zinc ion in above-mentioned zinc-containing water (solution of zinc sulfate)
Removal rate is 95.3%.
The preparation method of aforementioned present invention can use it with more for the technical staff of sewage treatment industry now
Place, is a kind of technological innovation, has technical progress really.
The above is only to disclose presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, appoints
What those skilled in the art, without departing from the scope of the present invention, when in the technology using the disclosure above
Hold the equivalent embodiment for making a little variation or modification equivalent variations, but anything that does not depart from the technical scheme of the invention content, according to
According to technical spirit any simple modification, equivalent change and modification to the above embodiments of the invention, this hair is still fallen within
In the range of bright technical solution.
Claims (2)
1. a kind of application of modified montmorillonoid adsorbent in Treatment of Zinc-containing Wastewater, which is characterized in that the modified montmorillonoid is inhaled
Attached dose of preparation method specifically includes the following steps:
(1) preparation of montmorillonite suspension: being purified montmorillonite by flushing, drying, crushing, sieving pretreatment measure is 100
~150 targeted fine powder shape materials, and montmorillonite suspension is configured to for 0.1~0.2 by solid-liquid mass ratio with distilled water；
(2) preparation of FN intercalator: 1mol/L iron nitrate solution, 1mol/L sodium hydroxide solution are mixed in the following proportions
It is even: 10~12mL of 1mol/L iron nitrate solution, 20~25mL of 1mol/L sodium hydroxide solution；
(3) FN intercalator is inorganic modified:, will the middle montmorillonite suspension prepared of step (1) under 60~80 DEG C of constant temperatures
It is uniformly mixed with FN intercalator in the ratio of 5:1~3:1, is sufficiently stirred simultaneously ultrasonic disperse 15~20 minutes, keeps montmorillonite suspended
Liquid is sufficiently modified；
(4) it the purification of FN intercalated montmorillonite: after modified montmorillonoid suspension obtained in step (3) is centrifuged, is precipitated, uses
Washes of absolute alcohol, and centrifugation, precipitating, cleaning process is repeated several times until solution ph is lower than 8.0, later at 60~80 DEG C
Low temperature drying is carried out, pure FN intercalated montmorillonite powder is obtained；
(5) preparation of SDS intercalator: under normal temperature conditions, by lauryl sodium sulfate (SDS), 1mol/L nitric acid and anhydrous second
Alcohol is uniformly mixed in the following proportions: lauryl sodium sulfate 20~25g, 1mol/L 10~12mL of nitric acid, and dehydrated alcohol 10~
12mL；During the preparation process, lauryl sodium sulfate is slowly added into nitric acid, it is after being uniformly dissolved, the mixing of the two is molten
Liquid is at the uniform velocity added in dehydrated alcohol in 5 minutes, and is stirred, and temperature when control is added is 20~25 DEG C；
(6) SDS intercalator is organically-modified: obtained FN intercalated montmorillonite powder and distilled water will be purified in step (4) by solid
Liquid mass ratio is configured to FN intercalated montmorillonite suspension for 0.1~0.2, and the ratio uniform of 8:1~5:1 is pressed with SDS intercalator
It mixes, be sufficiently stirred simultaneously ultrasonic disperse 15~20 minutes, keep FN intercalated montmorillonite suspension twice-modified；
(7) preparation of PAM flocculant: under normal temperature conditions by polyacrylamide, 1mol/L nitric acid and distilled water, in the following proportions
It is uniformly mixed: polyacrylamide 5~10g, 1mol/L 10~12mL of nitric acid, 100~120mL of distilled water；
(8) purification of SDS intercalated montmorillonite: in the twice-modified montmorillonite suspension obtained in step (6) be added dropwise 0.5%~
0.8% PAM flocculant quickly carries out high speed centrifugation, filtering after mixing evenly, filter residue is cleaned with deionized water to neutrality, it
Low temperature drying is carried out at 60~80 DEG C afterwards, obtains pure SDS intercalated montmorillonite powder；
(9) by SDS intercalated montmorillonite powder made from step (8) at 450~550 DEG C high-temperature roasting 30~45 minutes, be made
Modified montmorillonoid adsorbent.
2. application of the modified montmorillonoid adsorbent according to claim 1 in Treatment of Zinc-containing Wastewater, which is characterized in that
During the preparation process, polyacrylamide is slowly added into distilled water for PAM flocculant, after being uniformly dissolved, by the mixing of the two
Solution is at the uniform velocity added in nitric acid in 5 minutes, and controlling temperature when addition is 20~25 DEG C.
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| CN109046256A (en) * | 2018-08-30 | 2018-12-21 | 湖南金旅环保股份有限公司 | The preparation method of organic improving montmorillonite |
| CN110876921B (en) * | 2018-09-06 | 2022-08-12 | 中国石油化工股份有限公司 | Preparation method of desulfurization and denitrification wastewater adsorbent |
| CN110876919B (en) * | 2018-09-06 | 2022-08-12 | 中国石油化工股份有限公司 | Preparation method of high-salinity wastewater nitrate radical adsorbent |
| CN109133308A (en) * | 2018-10-10 | 2019-01-04 | 江苏京牧生物技术有限公司 | A kind of formula of compound wastewater inorganic agent |
| CN112390337B (en) * | 2020-10-30 | 2022-01-28 | 西南科技大学 | Preparation method of modified montmorillonite, product and application thereof |
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| CN1887705A (en) * | 2005-06-30 | 2007-01-03 | 中国科学院生态环境研究中心 | Prepn process of organic pillared interlayered clay material |
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| CN1887705A (en) * | 2005-06-30 | 2007-01-03 | 中国科学院生态环境研究中心 | Prepn process of organic pillared interlayered clay material |
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