CN106824132B - A kind of water treatment chromium adsorption material and preparation method thereof - Google Patents
A kind of water treatment chromium adsorption material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 31
- 239000011651 chromium Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical class CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 29
- 239000003463 adsorbent Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000002105 nanoparticle Substances 0.000 claims abstract description 18
- 239000004695 Polyether sulfone Substances 0.000 claims abstract description 14
- 229920006393 polyether sulfone Polymers 0.000 claims abstract description 14
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 14
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 14
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 14
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229920001568 phenolic resin Polymers 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims 2
- 238000007306 functionalization reaction Methods 0.000 claims 1
- 239000011159 matrix material Substances 0.000 claims 1
- 229920001342 Bakelite® Polymers 0.000 abstract description 11
- 239000004637 bakelite Substances 0.000 abstract description 11
- 238000001914 filtration Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 description 10
- 238000013019 agitation Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000011257 shell material Substances 0.000 description 3
- -1 Ether sulfone Chemical class 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000001174 sulfone group Chemical group 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
-
- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic 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
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of water process chromium adsorbent materials and preparation method thereof, in parts by weight, the material includes bakelite resin nano particle, 3 ~ 4 parts of polyvinylpyrrolidones of 7 ~ 12 parts of amino functionals, 10 ~ 12 parts of polyethersulfone resins and 70 ~ 75 parts of dimethylformamides；Its preparation step are as follows: be mixed bakelite resin nano particle, polyethersulfone resin, polyvinylpyrrolidone, the dimethylformamide of amino functional to obtain product A, product A is injected in syringe, water phase is instilled with given pace, solution is stood at room temperature and is collected by filtration afterwards for 24 hours, baking oven low temperature drying is put into and obtains chromium adsorbent material.Material diameter prepared by the present invention is 2-3mm, has stable structure, for Cr6+Adsorption effect it is good.
Description
Technical field
The present invention relates to a kind of nanocomposite and preparation method thereof, especially a kind of water process chromium adsorbent material and its
Preparation method belongs to material for water treatment preparation field.
Background technique
With human society and industrialized high speed development, water environment pollution problem gets worse, has injured
The existence of the mankind, the problem of becoming whole mankind institute general concern.There is heavy metal chromium toxicity to be not easy by generation greatly, in the environment
It thanks, be easily bioaccumulation and have the features such as biological amplification, seriously threaten the existence of the mankind and aquatic animals and plants.Therefore,
Seeking the further treatment technique for effectively removing heavy metal chromium has important Significance for Environment.
In numerous water treatment applications materials, nano material is because it is with huge specific surface area, high chemical activity energy,
To have good reduction and absorption property, the heavy metal contaminants in water body can be effectively removed.Therefore function nano material
Material has become an important research direction of water treatment field.Although nano material is solving water environment pollution and heavy metal
There is excellent performance in the advanced treating field of substance.However, nano material face it is 1. easy to reunite, it is difficult to recycle.2. easily
Cause secondary pollution, it is difficult to the problem of practical engineering application, constrain nano material in the practical application of water treatment field.Cause
This, the immobilization forming technique of nano material becomes the key point for being difficult to actual application problem for solving nano material.Pan etc.
[Liang Chen,Xin Zhao,Bingcai Pan；Journal of Hazardous Materials,284(2015)35–
42] utilize the method being prepared in situ by nano oxidized particulate zirconia growth in situ inside ion exchange resin ball pearl, it is obtained
Composite material has good removal effect to phosphate in water body.But growth in situ preparation method limitation is big, is only applicable to
The cladding of specific nano particle, most of nano particles can not growth in situ in material internal.[the H.- such as Kwang-Ho Choo
S.Park et al.Journal of Hazardous Materials286 (2015) 315-324] infusion process is utilized, it will be active
Charcoal is impregnated in nanometer Fe particle solution, prepares the composite material for having high absorption property to Natural Organic Pollutants.However, leaching
Stain method there is a problem of nano material be lost and stability difference.
In conclusion, by nano adsorption material immobilization, being easy to run off to solve nano material about using forming technique
The relevant report of problem is less, and the technique of existing synthesis immobilization nanometer moulding material is relatively cumbersome, severe reaction conditions,
Resulting materials stability is poor.
Summary of the invention
The object of the present invention is to provide a kind of water process chromium adsorbent materials and preparation method thereof.
Realizing the technical solution of the object of the invention is: a kind of water process chromium adsorbent material, in parts by weight, including 7
The bakelite resin nano particle of~12 parts of amino functionals, 3~4 parts of polyvinylpyrrolidones, 10~12 parts of polyethersulfone resins and
70~75 parts of dimethylformamides.
It is furthermore preferred that the weight of the bakelite resin nano particle of amino functional, polyvinylpyrrolidone, polyethersulfone resin
Proportion is respectively 10 parts, 3 parts and 10 parts.
Further, the adsorbent material is shell structurre.
The preparation method of above-mentioned adsorbent material, using polyethersulfone resin as basis material, the phenolic resin of amino functional is received
Rice corpuscles is adsorbent material, is included the following steps:
(1) bakelite resin nano particle, 3~4 parts of polyvinylpyrrolidones of 7~12 parts of amino functional are weighed, 10
~12 parts of polyethersulfone resins are added in 70~75 parts of dimethylformamides and dissolution reaction are mixed, mixed solution A obtained, by A
Solution ultrasonic disperse is uniform；
(2) finely dispersed solution A syringe is instilled into pure water with the rate of 1ml/min~4ml/min, at room temperature
It is collected by filtration after standing more than for 24 hours, is dried at 25 ± 5 DEG C, obtain the chromium adsorbent material.
In above-mentioned steps (1), the bakelite resin nano particle of the amino functional is made by the steps:
10~13 mass parts ethyl alcohol, 35~40 mass parts water are weighed, 15-25 is mixed in 0.5~0.6 mass parts ethylenediamine
Minute, it is added 0.4 part of resorcinol into solution at 30 DEG C, 0.6 part of formaldehyde stirs 24 hours or more, it is collected by centrifugation, in 100
It is dry at ± 10 DEG C.
In above-mentioned steps (1), stirring and dissolving reacts 6~8h；Reaction temperature is 30 ± 5 DEG C.
Compared with prior art, the present invention its remarkable advantage is: (1) adsorption material fixed-type by polyethersulfone resin
Material has good absorption property, can effectively remove heavy metal chromium in water；(2) water process chromium adsorbent material produced by the present invention
It is with good stability；(3) scantling prepared is uniform, can control scantling by changing specification of syringe, makes
Preparation Method is simple, easy to industrialized production.
Detailed description of the invention
Fig. 1 is the cross-sectional scanning electron microscope photo of chromium adsorbent material made from embodiment 1.
Fig. 2 is (a is embodiment 1, and b is comparative example 1) of chromium adsorbent material made from the embodiment of the present invention 1 and comparative example 1.
Specific embodiment
Insight of the invention is that using polyethersulfone resin as Shell Materials by the bakelite resin nano grain of amino functional
Son is encapsulated in inside Shell Materials, so that solving the problems, such as that nano material is easy to run off generates secondary pollution.
Embodiment 1
Step 1: weighing the bakelite resin nano particle of 1g amino functional, 0.3g polyvinylpyrrolidone and 1g polyethers
Sulphone resin is added in 6.3ml dimethylformamide and is mixed and is dissolved in beaker, and magnetic agitation is to dissolution under 30 DEG C of oil baths
(6-8h)。
Step 2: acquired solution is placed in ultrasonic disperse 2h in 200kw ultrasonic wave, uniform mixed solution is obtained.
Step 3: the solution after ultrasound is instilled pure water with 2ml syringe with the rate of 1ml/min, obtaining partial size is
Brownish red ball is stood in 25 DEG C of pure water and is collected by filtration afterwards for 24 hours, dried, obtain at room temperature by the brownish red ball of 2mm-3mm
To chromium adsorbent material.
The performance test results of water process chromium adsorbent material obtained are as shown in table 1.
Embodiment 2
Step 1: it is poly- to weigh the bakelite resin nano particle of 0.8g amino functional, 0.3g polyvinylpyrrolidone and 1g
Ether sulfone resin is added in 6.3ml dimethylformamide and is mixed and is dissolved in beaker, and magnetic agitation is to molten under 30 DEG C of oil baths
It solves (6-8h).
Step 2: acquired solution is placed in ultrasonic disperse 2h in 200kw ultrasonic wave, uniform mixed solution is obtained.
Step 3: the solution after ultrasound is instilled pure water with 2ml syringe with the rate of 1ml/min, obtaining partial size is
Brownish red ball is stood in 25 DEG C of pure water and is collected by filtration afterwards for 24 hours, dried, obtain at room temperature by the brownish red ball of 2mm-3mm
To chromium adsorbent material.
The performance test results of water process chromium adsorbent material obtained are as shown in table 1.
Embodiment 3
Step 1: it is poly- to weigh the bakelite resin nano particle of 0.6g amino functional, 0.3g polyvinylpyrrolidone and 1g
Ether sulfone resin is added in 6.3ml dimethylformamide and is mixed and is dissolved in beaker, and magnetic agitation is to molten under 30 DEG C of oil baths
It solves (6-8h).
Step 2: acquired solution is placed in ultrasonic disperse 2h in 200kw ultrasonic wave, uniform mixed solution is obtained.
Step 3: the solution after ultrasound is instilled pure water with 2ml syringe with the rate of 1ml/min, obtaining partial size is
Brownish red ball is stood in 25 DEG C of pure water and is collected by filtration afterwards for 24 hours, dried, obtain at room temperature by the brownish red ball of 2mm-3mm
To chromium adsorbent material.
The performance test results of water process chromium adsorbent material obtained are as shown in table 1.
Embodiment 4
Step 1: weighing the bakelite resin nano particle of 1g amino functional, 0.3g polyvinylpyrrolidone and 1g polyethers
Sulphone resin is added in 6.3ml dimethylformamide and is mixed and is dissolved in beaker, and magnetic agitation is to dissolution under 30 DEG C of oil baths
(6-8h)。
Step 2: acquired solution is placed in ultrasonic disperse 2h in 200kw ultrasonic wave, uniform mixed solution is obtained.
Step 3: the solution after ultrasound is instilled pure water with 5ml syringe with the rate of 2.5ml/min, obtaining partial size is
Brownish red ball is stood in 25 DEG C of pure water and is collected by filtration afterwards for 24 hours, dried, obtain at room temperature by the brownish red ball of 3mm-4mm
To chromium adsorbent material.
The performance test results of water process chromium adsorbent material obtained are as shown in table 1.
Comparative example 1
0.3g polyvinylpyrrolidone and 1g polyethersulfone resin are weighed, is added in 6.3ml dimethylformamide and is mixed
It is dissolved in beaker, the magnetic agitation extremely dissolution (6-8h) under 30 DEG C of oil baths.
Step 2: acquired solution is placed in ultrasonic disperse 2h in 200kw ultrasonic wave, uniform mixed solution is obtained.
Step 3: the solution after ultrasound is instilled pure water with 2ml syringe with the rate of 1ml/min, obtaining partial size is
White ball is stood in 25 DEG C of pure water and is collected by filtration afterwards for 24 hours, dried at room temperature, obtain chromium by the white ball of 2mm-3mm
Adsorbent material.
The performance test results of water process chromium adsorbent material obtained are as shown in table 1.
Table 1
The chromium adsorbent material of embodiment 1-3 and comparative example 1 are used for chromate waste water processing: being used for pH is 2, chromium ion
When content is in the waste water of 100mg/L, chromium adsorbent material dosage is 0.5g/L, that is, can reach good treatment effect.To each
Known to the chromium adsorbent material synthesized in embodiment and comparative example is characterized: polymer drops bead diameter homogeneous diameter obtained is about
2mm；Meanwhile as Fig. 1-2 it is found that made from include finger-like pore structure inside polymer ball, pass through the quasi- of adsorption isotherm
It closes result and illustrates that adsorption process belongs to Lang Gemiao single layer reversible adsorption.
Claims (6)
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| CN107511125A (en) * | 2017-09-06 | 2017-12-26 | 南京理工大学 | Load the preparation method of hollow Nano hydrous zirconium oxide(HZO) grade polymer drops |
| CN118307112B (en) * | 2024-06-07 | 2024-08-20 | 安徽农业大学 | Sewage treatment flocculant and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554547A (en) * | 2013-10-12 | 2014-02-05 | 上海师范大学 | Amino functionalized mesoporous macromolecular small nanosphere and preparation method thereof |
| CN104058401A (en) * | 2014-07-11 | 2014-09-24 | 北京科技大学 | Preparation method of porous carbon microspheres |
| CN105566589A (en) * | 2015-12-08 | 2016-05-11 | 上海师范大学 | Amino-functionalization ordered mesopore phenolic resin material and preparing method thereof |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554547A (en) * | 2013-10-12 | 2014-02-05 | 上海师范大学 | Amino functionalized mesoporous macromolecular small nanosphere and preparation method thereof |
| CN104058401A (en) * | 2014-07-11 | 2014-09-24 | 北京科技大学 | Preparation method of porous carbon microspheres |
| CN105566589A (en) * | 2015-12-08 | 2016-05-11 | 上海师范大学 | Amino-functionalization ordered mesopore phenolic resin material and preparing method thereof |
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