CN102430395A - Preparation method of chitosan cross-linked vanillin adsorption film - Google Patents
Preparation method of chitosan cross-linked vanillin adsorption film Download PDFInfo
- Publication number
- CN102430395A CN102430395A CN201110303315XA CN201110303315A CN102430395A CN 102430395 A CN102430395 A CN 102430395A CN 201110303315X A CN201110303315X A CN 201110303315XA CN 201110303315 A CN201110303315 A CN 201110303315A CN 102430395 A CN102430395 A CN 102430395A
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- Prior art keywords
- solution
- vanillin
- adsorption film
- chitosan
- preparation
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- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 title abstract description 12
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 title abstract 5
- 235000012141 vanillin Nutrition 0.000 title abstract 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005266 casting Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000012153 distilled water Substances 0.000 claims abstract description 3
- 239000011521 glass Substances 0.000 claims abstract description 3
- 230000007935 neutral effect Effects 0.000 claims abstract description 3
- 230000005855 radiation Effects 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000001291 vacuum drying Methods 0.000 claims abstract description 3
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 2
- 235000021419 vinegar Nutrition 0.000 claims description 2
- 239000000052 vinegar Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 7
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000008929 regeneration Effects 0.000 abstract description 4
- 238000011069 regeneration method Methods 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract 3
- 238000005406 washing Methods 0.000 abstract 2
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- -1 amino, hydroxyl Chemical group 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000011868 grain product Nutrition 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A preparation method of a chitosan cross-linked vanillin adsorption film adopts the following process steps: respectively taking chitosan and vanillin for standby use, wherein the mass ratio of the chitosan to the vanillin is 1:2, the chitosan is dissolved in dilute acetic acid to prepare a 2% solution A, the vanillin is dissolved in ethanol to prepare a 10% solution B, the solution A and the solution B are heated by microwave radiation with the microwave power of 1000W and the heating temperature of 55 ℃, and after stirring for 13 minutes at the rotating speed of 480r/min, a casting solution is obtained for standby use; the generated casting solution is cast at a concentration of 0.20mL/cm by adopting a casting method2Spreading on glass test piece, vacuum drying at 80 deg.CThen, the solution is taken out and soaked for half an hour by 0.25mol/L NaOH solution to obtain an adsorption film. Washing with 95% ethanol solution, washing with distilled water to neutral, and drying to constant weight. The preparation method of the adsorption film has the advantages of rich raw materials, simple operation and low energy consumption. The microwave technology different from the common heating principle is adopted, the adsorption capacity of the obtained adsorption film to heavy metal is greatly improved, and the adsorption film is easy to separate from waste water and can be recycled after regeneration.
Description
Technical field
The invention belongs to the waste water treatment field, relate to a kind of heavy metal ion water treatment agent, particularly a kind of preparation method of chitosan crosslinked vanillic aldehyde adsorbed film.
Background technology
The method of removing heavy metal ions in wastewater at present comprises methods such as chemical precipitation, membrane technology, counter-infiltration and electrochemistry.But most technology costs are higher, complicated operation, subsequent treatment difficulty.Wherein absorption method is that the technology cost is lower, simple to operate and by one of method that extensively adopts.Shitosan is a kind of wide material sources, the natural polymer of renewable degraded, and containing a large amount of amino, hydroxyl in its molecule can complexation of metal ions, is a kind of adsorbent new raw material.But shitosan is prone to dissolving in acid medium runs off, and complexing power reduces, and has limited the extensive use of chitosan absorbent.It is little to prepare dissolubility, the shitosan water treatment agent that complexing power is strong.
Summary of the invention
The object of the invention provides the preparation method of a kind of natural, environmental protection, stable performance, high adsorption capacity, easily separated, reusable heavy metal ion adsorbed film, particularly a kind of preparation method of chitosan crosslinked vanillic aldehyde adsorbed film.
The technical scheme that adopts is:
A kind of preparation method of chitosan crosslinked vanillic aldehyde adsorbed film, adopt following processing step:
1, gets shitosan respectively and vanillic aldehyde is subsequent use; The mass ratio of shitosan and vanillic aldehyde is 1:2, and shitosan is dissolved in and is made into 2% solution A in the spirit of vinegar, and vanillic aldehyde is dissolved in and is made into 10% solution B in the ethanol; With solution A and solution B employing microwave power is that 1000W, heating-up temperature are 55 ℃ carry out microwave radiation heating; By rotating speed is after 480r/min stirs 13 minutes, to get casting solution, subsequent use;
2, adopt the stream method of prolonging, with the casting solution that generates with 0.20mL/cm
2Be extended on the glass coupon, after 80 ℃ of vacuum drying, take out NaOH solution soaking half an hour, obtain adsorbed film with 0.25mol/L, extremely neutral with distilled water flushing more earlier with the flushing of 95% ethanolic solution, be dried to constant weight, promptly get.
The present invention introduces a kind of modification of chitosan adsorbed film and preparation method thereof.This adsorbed film is a primary raw material with shitosan, vanillic aldehyde, adopts microwave technology synthetic.
This adsorbed film is 200mg/g Cu to initial concentration
2+And Pb
2+Adsorption capacity be respectively 221.42mg/g and 245.04mg/g, be higher than the chitosan crosslinked vanillic aldehyde grain products of microwave method preparation, also be higher than other metal ion adsorbent.
Adsorbed film is prone to from waste water, separate behind the adsorbing metal ions.The NaOH that the chitosan crosslinked vanillic aldehyde adsorbed film that has adsorbed metal ion is put into EDTA and the 0.2mol/L of 0.1mol/L mixes and dissolves, and vibration 10min leaves standstill the back and filters, and dries naturally, can get the desorption and regeneration adsorbed film.Adsorbed film after will drying adsorbs once more, calculates its adsorbance, so reuses 7 times, and this adsorbed film is that the adsorption capacity of 200mg/g copper ion drops to 184mg/g from 223.4mg/g to concentration, only reduces by 17.6 %; Adsorption capacity to same concentration lead ion drops to 200mg/g from 246mg/g, only reduces 18.6%.Explain that chitosan crosslinked vanillic aldehyde adsorbed film has good desorption and regeneration ability, regenerate and still can effectively use for 7 times.
The invention has the advantages that:
This adsorbed film preparation method abundant raw material, simple to operate, energy consumption is low.Employing is different from the microwave technology of common heating principle, has not only significantly improved reaction efficiency, also obtains the sorbing material of more excellent performance; The gained adsorbed film improves the adsorption capacity of heavy metal greatly, is easy to from waste water, separate, and can be recycled after the regeneration; Cost is low, is difficult for causing secondary pollution.
Claims (1)
1. the preparation method of a chitosan crosslinked vanillic aldehyde adsorbed film is characterized in that, adopts following processing step:
1), gets shitosan respectively and vanillic aldehyde is subsequent use; The mass ratio of shitosan and vanillic aldehyde is 1:2, and shitosan is dissolved in and is made into 2% solution A in the spirit of vinegar, and vanillic aldehyde is dissolved in and is made into 10% solution B in the ethanol; With solution A and solution B employing microwave power is that 1000W, heating-up temperature are 55 ℃ carry out microwave radiation heating; By rotating speed is after 480r/min stirs 13 minutes, to get casting solution, subsequent use;
2), adopt the stream method of prolonging, with the casting solution that generates with 0.20mL/cm
2Be extended on the glass coupon, after 80 ℃ of vacuum drying, take out NaOH solution soaking half an hour, obtain adsorbed film with 0.25mol/L, extremely neutral with distilled water flushing more earlier with the flushing of 95% ethanolic solution, be dried to constant weight, promptly get.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110303315XA CN102430395A (en) | 2011-10-10 | 2011-10-10 | Preparation method of chitosan cross-linked vanillin adsorption film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110303315XA CN102430395A (en) | 2011-10-10 | 2011-10-10 | Preparation method of chitosan cross-linked vanillin adsorption film |
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| CN102430395A true CN102430395A (en) | 2012-05-02 |
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| CN201110303315XA Pending CN102430395A (en) | 2011-10-10 | 2011-10-10 | Preparation method of chitosan cross-linked vanillin adsorption film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104475048A (en) * | 2014-11-05 | 2015-04-01 | 华玉叶 | Preparation method of crosslinking membrane for water processing |
| CN110314639A (en) * | 2019-07-11 | 2019-10-11 | 沈阳理工大学 | A kind of modified birnessite and its preparation method and application |
| CN112064334A (en) * | 2020-09-14 | 2020-12-11 | 湖南科力嘉纺织股份有限公司 | Method for carrying out anti-radiation pretreatment on cotton yarn |
| CN112619613A (en) * | 2020-12-01 | 2021-04-09 | 仲恺农业工程学院 | Powdery vanillin modified chitosan schiff base decolorant and preparation method thereof |
| CN113736472A (en) * | 2021-09-23 | 2021-12-03 | 湖南国重环境科技有限责任公司 | Slow-release arsenic fixing agent, preparation method thereof and application thereof in arsenic-contaminated soil remediation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215384A (en) * | 2008-01-11 | 2008-07-09 | 大连理工大学 | Method for preparing adsorbent recombination chitosan micro-sphere crosslinked resin |
| CN101220176A (en) * | 2007-10-18 | 2008-07-16 | 四川大学 | Blended degradable membrane of chitosan/xylogen and method for producing the same |
-
2011
- 2011-10-10 CN CN201110303315XA patent/CN102430395A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220176A (en) * | 2007-10-18 | 2008-07-16 | 四川大学 | Blended degradable membrane of chitosan/xylogen and method for producing the same |
| CN101215384A (en) * | 2008-01-11 | 2008-07-09 | 大连理工大学 | Method for preparing adsorbent recombination chitosan micro-sphere crosslinked resin |
Non-Patent Citations (2)
| Title |
|---|
| RICCARDO A. A., ET AL.: "Chitosans carrying the methoxyphenyl functions typical of lignin", 《CARBOHYDRATE POLYMERS》 * |
| 郑大锋等: "香草醛接枝壳聚糖的微波辐射制备及其吸附性能", 《华南理工大学学报（自然科学版）》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104475048A (en) * | 2014-11-05 | 2015-04-01 | 华玉叶 | Preparation method of crosslinking membrane for water processing |
| CN110314639A (en) * | 2019-07-11 | 2019-10-11 | 沈阳理工大学 | A kind of modified birnessite and its preparation method and application |
| CN110314639B (en) * | 2019-07-11 | 2022-03-11 | 沈阳理工大学 | Modified birnessite and preparation method and application thereof |
| CN112064334A (en) * | 2020-09-14 | 2020-12-11 | 湖南科力嘉纺织股份有限公司 | Method for carrying out anti-radiation pretreatment on cotton yarn |
| CN112619613A (en) * | 2020-12-01 | 2021-04-09 | 仲恺农业工程学院 | Powdery vanillin modified chitosan schiff base decolorant and preparation method thereof |
| CN113736472A (en) * | 2021-09-23 | 2021-12-03 | 湖南国重环境科技有限责任公司 | Slow-release arsenic fixing agent, preparation method thereof and application thereof in arsenic-contaminated soil remediation |
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Application publication date: 20120502 |