CN108993378A - A kind of silane coupler modified galapectite/Fe3O4 composite material and preparation method - Google Patents
A kind of silane coupler modified galapectite/Fe3O4 composite material and preparation method Download PDFInfo
- Publication number
- CN108993378A CN108993378A CN201710423966.XA CN201710423966A CN108993378A CN 108993378 A CN108993378 A CN 108993378A CN 201710423966 A CN201710423966 A CN 201710423966A CN 108993378 A CN108993378 A CN 108993378A
- Authority
- CN
- China
- Prior art keywords
- galapectite
- composite material
- parts
- fe3o4
- hnts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of silane coupler modified galapectite/Fe3O4 composite material and preparation method, the weights of the composite material raw material are as follows: 20-40 parts of silane coupling agent, 100-120 parts of galapectite, 30-40 parts of iron chloride, 1-10 parts of ferrous sulfate.The composite material is to synthesize ferriferrous oxide particles on galapectite surface by situ synthesis.The composite material is good to heavy metal ion adsorbed effect, removal rate is high, facilitates the purpose of recycling and reusing, removes heavy metal ions in wastewater as adsorbent, has great social benefit and environmental benefit；The composite material preparation process is simple.
Description
Technical field
The present invention relates to field of composite material preparation, specifically a kind of silane coupler modified galapectite/Fe3O4 composite wood
Material and preparation method thereof.
Background technique
In recent decades, with the continuous development of China's industry, such as metal plating industry, mining, fertilizer industry, print
Dye-works, tannery, insecticide factory, paper mill, textile industry etc., more and more heavy metal wastewater therebies are directly or indirectly discharged into ring
In border, especially in some remote sites.Unlike organic pollutant, heavy metal cannot be degraded by biology, and be easy in life
Enrichment, can also convert into the bigger methyl compound of toxicity in object, more than will cause to seriously threaten to organism after a certain amount of.
For example lead can cause nervous system damage, can also damage kidney, liver and reproductive system and basic cell work and big
Brain function；Nickel is more than that its critical level may be brought other than digestive discomfort, also will cause serious lung and kidney problems, and
Skin dermatitis.Therefore, the concern which results in people to heavy metal pollution of water body.
Clay is referred to as " universal material ", is increasingly paid attention to by people.Exploitation in terms of purification of water quality and sewage treatment
With application oneself through having made some progress, but still need to that exploitation high efficiency low cost, physicochemical properties are stable and can industrialize
Adsorbent or flocculant.Modification to clay, and its it is more and more to the absorption research of pollutant, have become popular class
One of topic.
Summary of the invention
The purpose of the present invention is to provide a kind of silane coupler modified galapectite/Fe3O4 composite material and its preparation sides
Method, the composite material is good to heavy metal ion adsorbed effect, removal rate is high, facilitates the purpose of recycling and reusing, as suction
Attached dose of removal heavy metal ions in wastewater.
Realizing the technical solution of the object of the invention is:
A kind of silane coupler modified galapectite/Fe3O4 composite material, the weight of raw material are as follows:
20-40 parts of silane coupling agent；
100-120 parts of galapectite；
30-40 parts of iron chloride；
1-10 parts of ferrous sulfate.
A kind of preparation method of silane coupler modified galapectite/Fe3O4 composite material, specifically comprises the following steps:
1) galapectite surface functional group is activated
It takes galapectite (HNTs) powder of 100-200 parts of high-purities to be put into beaker, is added in appropriate HCI O.5mol/L, room temperature
Lower stirring for 24 hours, activate galapectite table and functional group, then distilled water repeated flushing, until supernatant is neutrality, centrifugation point
From spare after 50 DEG C of drying 12h；
2) active galapectite and FeCl3 solution after taking step 1) to be acidified are mixed 24 hours, and be centrifuged at a high speed 20min,
It outwells supernatant and rejoins FeCl3 solution, stirring for 24 hours, four times repeatedly, guarantees the cation exchange of halloysite clay
Site is by Fe3+Saturation；
3) saturation galapectite (Fe (III)-HNTs) is added to and has been dissolved in FeSO4 solution, returned in 70 DEG C of oil bath pan inner edges
Stream side is passed through N into suspension2, then inwards and NH3H2O is added dropwise in mixed liquor, make solution alkaline mixed liquor, 70
It is reacted 5 hours at DEG C, the sample finally obtained with deionized water repeated flushing, removes extra ferrous ion, 60 DEG C of vacuum
Dry 12 h obtain HNTs/Fe3O4；
4) modified for surface, HNTs/Fe3O4 powder is dispersed in dehydrated alcohol, silane coupling agent is subsequently added into, is mixed
383K is condensed back 24 h to liquid under magnetic stirring, and modified sample obtained by magnetic separation, with dehydrated alcohol mistake repeatedly
Filter flushing sample, to remove excessive modifying agent and may hydrolyze the by-product generated, the sample finally obtained is put into 40 DEG C very
In empty drying box, dry 12h；
5) additional that 20 h are extracted in Soxhlet extraction device to gained sample again, check in extract liquor whether there is residual substance,
12 h of last 40 DEG C of vacuum drying, obtain modified HNTs/Fe3O4 composite material.
In step 3), the alkaline mixed solution, pH 9-11.
The utility model has the advantages that a kind of silane coupler modified galapectite/Fe3O4 composite material provided by the invention, the composite wood
Expect that good to heavy metal ion adsorbed effect, removal rate is high, facilitates the purpose of recycling and reusing, removes waste water as adsorbent
Middle heavy metal ion has great social benefit and environmental benefit；The composite material preparation process is simple.
Specific embodiment
The present invention is further elaborated below with reference to embodiment, but is not limitation of the invention.
Embodiment:
(1) it takes galapectite (HNTs) powder of 20g high-purity to be put into beaker, is added in 200 m L 0.5mol/L HCl, room
Temperature is lower to stir 24 h, activates the functional group on galapectite surface, then distilled water repeated flushing, until supernatant is neutrality, centrifugation
It separates, it is spare after 50 DEG C of 12 h of drying；
(2) active galapectite and 200 m L, 0.1 mol L-1 Fe Cl3 solution after taking 10 g to be acidified are mixed 24
Hour, 20 min are centrifugated with the speed of 5000 rpm, supernatant is outwelled, rejoins 200 m L, 0.1 mol L-1 Fe
Cl3 solution stirs 24 h, four times repeatedly, guarantees that the cation exchange site point of halloysite clay is saturated by Fe3+.
(3) 1.0 g iron saturation galapectite (Fe (III)-HNTs), which is added to, has dissolved 0.2 g Fe SO47H2O's
In 200 m L solution, N2 is passed through into suspension on 70 °C of oil bath pan inner edge reflux side, then dropwise to the inside mixed liquor
1 NH3H2O of 8mol L is added, controls the p H of mixed liquor and is reacted 5 hours under 9-10,70 °C, finally use deionization
The sample that water repeated flushing obtains, removes extra ferrous ion, and 60 °C of 12 h of vacuum drying obtain HNTs/Fe3O4；
(4) modified for surface, 2.0 g HNTs/Fe3O4 powder are dispersed in 100 m L dehydrated alcohols, are subsequently added into
4.0 g silane coupling agents, 383K is condensed back 24 h to mixed liquor under magnetic stirring, and modified sample is obtained by magnetic separation
It arrives, is repeatedly filtered with dehydrated alcohol and rinse sample, to remove excessive modifying agent and the by-product generated may be hydrolyzed, finally
To sample be put into 40 °C of vacuum ovens, dry 12h；
(5) additional that 20 h are extracted in Soxhlet extraction device to gained sample again, check in extract liquor whether there is residual substance,
12 h of last 40 °C of vacuum drying, obtain modified HNTs/Fe3O4 composite material.
Claims (3)
1. a kind of silane coupler modified galapectite/Fe3O4 composite material, which is characterized in that the weight of its raw material are as follows:
20-40 parts of silane coupling agent；
100-120 parts of galapectite；
30-40 parts of iron chloride；
1-10 parts of ferrous sulfate.
2. a kind of preparation method of silane coupler modified galapectite/Fe3O4 composite material, which is characterized in that specifically include as
Lower step:
1) galapectite surface functional group is activated
It takes galapectite (HNTs) powder of 100-200 parts of high-purities to be put into beaker, is added in appropriate HCI O.5mol/L, room temperature
Lower stirring for 24 hours, activate galapectite table and functional group, then distilled water repeated flushing, until supernatant is neutrality, centrifugation point
From spare after 50 DEG C of drying 12h；
2) active galapectite and FeCl3 solution after taking step 1) to be acidified are mixed 24 hours, and be centrifuged at a high speed 20min,
It outwells supernatant and rejoins FeCl3 solution, stirring for 24 hours, four times repeatedly, guarantees the cation exchange of halloysite clay
Site is by Fe3+Saturation；
3) saturation galapectite (Fe (III)-HNTs) is added to and has been dissolved in FeSO4 solution, returned in 70 DEG C of oil bath pan inner edges
Stream side is passed through N into suspension2, then inwards and NH3H2O is added dropwise in mixed liquor, make solution alkaline mixed liquor, 70
It is reacted 5 hours at DEG C, the sample finally obtained with deionized water repeated flushing, removes extra ferrous ion, 60 DEG C of vacuum
Dry 12 h obtain HNTs/Fe3O4；
4) modified for surface, HNTs/Fe3O4 powder is dispersed in dehydrated alcohol, silane coupling agent is subsequently added into, is mixed
383K is condensed back 24 h to liquid under magnetic stirring, and modified sample obtained by magnetic separation, with dehydrated alcohol mistake repeatedly
Filter flushing sample, to remove excessive modifying agent and may hydrolyze the by-product generated, the sample finally obtained is put into 40 DEG C very
In empty drying box, dry 12h；
5) additional that 20 h are extracted in Soxhlet extraction device to gained sample again, check in extract liquor whether there is residual substance,
12 h of last 40 DEG C of vacuum drying, obtain modified HNTs/Fe3O4 composite material.
3. preparation method according to claim 1, which is characterized in that in step 3), the alkaline mixed solution, pH 9-
11。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710423966.XA CN108993378A (en) | 2017-06-07 | 2017-06-07 | A kind of silane coupler modified galapectite/Fe3O4 composite material and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710423966.XA CN108993378A (en) | 2017-06-07 | 2017-06-07 | A kind of silane coupler modified galapectite/Fe3O4 composite material and preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108993378A true CN108993378A (en) | 2018-12-14 |
Family
ID=64573112
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710423966.XA Pending CN108993378A (en) | 2017-06-07 | 2017-06-07 | A kind of silane coupler modified galapectite/Fe3O4 composite material and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108993378A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109351337A (en) * | 2018-12-18 | 2019-02-19 | 东北大学 | A kind of preparation method and applications of silane coupler modified zeolite |
| CN110860279A (en) * | 2019-11-07 | 2020-03-06 | 江苏大学 | Polyamide amine functionalized halloysite nanotube and preparation method and application thereof |
| CN113388132A (en) * | 2021-06-10 | 2021-09-14 | 合肥科天水性科技有限责任公司 | Magnetic polyurethane hydrogel and preparation method and application thereof |
| CN113773555A (en) * | 2021-09-17 | 2021-12-10 | 武汉工程大学 | Halloysite-based composite flame retardant and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006080895A1 (en) * | 2005-01-20 | 2006-08-03 | Agency For Science, Technology And Research | Water-soluble, surface-functionalized nanoparticle for bioconjugation via universal silane coupling |
| CN102580696A (en) * | 2012-02-20 | 2012-07-18 | 江苏大学 | Preparation method of temperature sensitive adsorbent of halloysite magnetic composite material surface blotting |
| US20120258051A1 (en) * | 2011-04-08 | 2012-10-11 | Bell Charleson S | Multistrata nanoparticles and methods for making multistrata nanoparticles |
| CN106111067A (en) * | 2016-07-27 | 2016-11-16 | 中国科学院新疆理化技术研究所 | A kind of preparation method and application of silane coupler modified magnetic halloysite material |
-
2017
- 2017-06-07 CN CN201710423966.XA patent/CN108993378A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006080895A1 (en) * | 2005-01-20 | 2006-08-03 | Agency For Science, Technology And Research | Water-soluble, surface-functionalized nanoparticle for bioconjugation via universal silane coupling |
| US20120258051A1 (en) * | 2011-04-08 | 2012-10-11 | Bell Charleson S | Multistrata nanoparticles and methods for making multistrata nanoparticles |
| CN102580696A (en) * | 2012-02-20 | 2012-07-18 | 江苏大学 | Preparation method of temperature sensitive adsorbent of halloysite magnetic composite material surface blotting |
| CN106111067A (en) * | 2016-07-27 | 2016-11-16 | 中国科学院新疆理化技术研究所 | A kind of preparation method and application of silane coupler modified magnetic halloysite material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109351337A (en) * | 2018-12-18 | 2019-02-19 | 东北大学 | A kind of preparation method and applications of silane coupler modified zeolite |
| CN110860279A (en) * | 2019-11-07 | 2020-03-06 | 江苏大学 | Polyamide amine functionalized halloysite nanotube and preparation method and application thereof |
| CN113388132A (en) * | 2021-06-10 | 2021-09-14 | 合肥科天水性科技有限责任公司 | Magnetic polyurethane hydrogel and preparation method and application thereof |
| CN113773555A (en) * | 2021-09-17 | 2021-12-10 | 武汉工程大学 | Halloysite-based composite flame retardant and preparation method thereof |
| CN113773555B (en) * | 2021-09-17 | 2022-06-14 | 武汉工程大学 | Halloysite-based composite flame retardant and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108993378A (en) | A kind of silane coupler modified galapectite/Fe3O4 composite material and preparation method | |
| Zhao et al. | Uranium (Ⅵ) adsorption from aqueous solutions by microorganism-graphene oxide composites via an immobilization approach | |
| Yuan et al. | Charge balanced anti-adhesive polyacrylamidoxime hydrogel membrane for enhancing uranium extraction from seawater | |
| CN104971697B (en) | Preparation and application methods for magnetic biochar material used for removing arsenic pollution in water body | |
| CN102989427B (en) | Enteromorpha absorbent and preparation technology thereof | |
| CN102887581B (en) | Flocculating agent for treating sewage in Chinese patent medicine production enterprises and preparation method thereof | |
| CN107935236A (en) | A kind of method of the processing containing surface active agent wastewater | |
| CN105107471B (en) | Sulfydryl lignocellulosic/montmorillonite Composite heavy metal absorbent and preparation and application | |
| CN105126742B (en) | A kind of method using modified kaolin sorbent treatment fluoride waste | |
| CN103041791B (en) | Preparation method of novel lead removal agent | |
| CN105771876B (en) | The preparation method of modified eggshell magnetic adsorbent and the method for removing heavy metal in water removal | |
| CN109261133A (en) | A kind of ferromagnetism composite balls and its application being easily recycled | |
| CN104587956A (en) | Preparation method of coated nano zero-valent iron taking multilayer activated-carbon-coated graphene oxide composite powder as carrier | |
| CN113842883B (en) | Lanthanum-loaded iron carbon nanotube film material for environmental remediation and preparation method and application thereof | |
| CN103877927A (en) | Preparation method of magnetic nano Fe3O4 particles by biological catalysis and application of particles to treatment of uranium-containing wastewater | |
| CN102774847A (en) | Preparation and application methods for novel magnetic molecular sieve adsorbent material | |
| Nguyen et al. | Preparation of Zn-doped biochar from sewage sludge for chromium ion removal | |
| CN103816903B (en) | The synthetic method of iron-base magnetic nanoneedle iron ore | |
| CN110560012A (en) | Method for removing phosphorus in water by using resin-loaded hydrated iron oxide | |
| CN104645932B (en) | A kind of composite modified zeolite of iron and manganese oxides and preparation method and application | |
| CN104353412A (en) | Iron hydroxide/sepiolite compound arsenic adsorbing agent as well as preparation method and application thereof | |
| CN105617980B (en) | A kind of bentonitic method and its application of biosurfactant modified magnetic | |
| Yang et al. | A novel La (OH) 3 decorated co-graft tannin and polyethyleneimine co-coating magnetic adsorbent for effective and selective phosphate removal from natural water and real wastewater | |
| CN105771918A (en) | Preparation method and application of magnetic anaerobic granular sludge-chitosan adsorbent | |
| CN107008230A (en) | Magnetic composite adsorbent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181214 |
|
| WD01 | Invention patent application deemed withdrawn after publication |