CN104324700A - Preparation method of high-amino porous chitosan resin - Google Patents
Preparation method of high-amino porous chitosan resin Download PDFInfo
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- CN104324700A CN104324700A CN201410511294.4A CN201410511294A CN104324700A CN 104324700 A CN104324700 A CN 104324700A CN 201410511294 A CN201410511294 A CN 201410511294A CN 104324700 A CN104324700 A CN 104324700A
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- chitosan resin
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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- Chemical & Material Sciences (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)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of high-amino porous chitosan resin in the field of environmental protection. The preparation method includes following steps: (1) dissolving chitosan in an acetic acid solution of which a mass fraction is 2% for preparing a chitosan solution and stirring the chitosan solution until the chitosan is dissolved completely; (2) through a reverse suspension method, adding liquid paraffin and a pore-forming agent with fully stirring to enable the reaction system to be in an emulsion status; (3) adding a formaldehyde solution to the mixed system and performing pre-crosslinking at 60 DEG C for 40-60 min; (4) adjusting the pH value of the solution to 10-13 with sodium hydroxide, adding an epichlorohydrin solution and carrying out a reaction at 80 DEG C for 3h; (5) performing filtration, a washing operation with water and an extraction process, and then performing a washing process with acetone and ethanol fully to obtain a product; and (6) adding the product to a 0.5mol/L hydrochloric acid solution, stirring and filtering the product, and finally soaking the product in a 1.0mol/L sodium hydroxide solution and washing the product to neutralization to obtain the high-amino porous chitosan resin. The high-amino porous chitosan resin is good in adsorption effect and can be utilized repeatedly.
Description
Technical field
The invention belongs to field of Environment Protection, be specifically related to a kind of preparation method of high amino porous chitosan resin.
Background technology
China is the first big country of textile printing and dyeing industry, and textile printing and dyeing industry is the discharge rich and influential family of industrial wastewater, and in each industrial trade of China, textile printing and dyeing industry wastewater discharge accounts for the 5th of national industrial wastewater statistics discharge capacity.Dyeing waste water has that the water yield is large, water quality is complicated, content of organics is high, raised path between farm fields biochemical is poor, alkalescence is large, colourity high, and directly discharge will cause serious water environment pollution.The processing method of dyeing waste water is a lot, but treatment effect is different.Absorption method is the common technique of decolorizing printing and dyeing waste water process.In recent years, people have developed various sorbing material, and the process of dyeing waste water achieves good effect.
Containing a large amount of active group in chitosan molecule, it has good absorption property to many inorganic acids, organic acid and acid compound, but due to Powdered shitosan particle diameter too little Yi be scattered in solution, cause adsorbent and solution separation difficulty, or blocking fixed bed.Shitosan easily runs off in weakly acidic solution simultaneously, and these make it be restricted as the application of adsorbent.
Summary of the invention
In order to overcome the above problems, the invention provides a kind of preparation method of high amino porous chitosan resin.
A preparation method for high amino porous chitosan resin, described preparation method comprises the following steps:
(1) 10-20 part shitosan being dissolved in mass fraction is in the acetic acid solution of 2%, is mixed with chitosan solution, is stirred to and dissolves completely at 50 DEG C;
(2) adopt inverse phase suspension to add atoleine, pore-foaming agent, fully stir and make reaction system become emulsion form;
(3) in mixed system, formalin is added in 60 DEG C of precrosslink 40-60min;
(4) with NaOH, pH value of solution is modulated 10-13, add epoxychloropropane solution, at 80 DEG C, react 3h;
(5) reacted rear filtration, washing, with apparatus,Soxhlet's extracting 12-24h, then fully washs with acetone and ethanol, removing residual organic matter;
(6) be then placed in 0.5 mol/L hydrochloric acid solution agitation and filtration, finally soak with 1.0 mol/L sodium hydroxide solutions, be washed to neutrality, obtain high amino porous chitosan resin.
Further, described in step (2), pore-foaming agent is polyethylene glycol.
Further, it is characterized in that, in step (2), stir speed (S.S.) is 600r/min-1000r/min.
Further, the amino porous chitosan resin of described height is used for the absorption of waste water from dyestuff.
Beneficial effect of the present invention is: the amino porous chitosan resin of described height as dye wastewater adsorbent, advantages of good adsorption effect, the rate of adsorption is fast; Use NaOH as parsing agent, the amino porous chitosan resin of described height can recycle, and improves the utilization rate of high amino porous chitosan resin.
Detailed description of the invention
Embodiment 1
A preparation method for high amino porous chitosan resin, described preparation method comprises the following steps:
(1) 10 parts of shitosans being dissolved in mass fraction is in the acetic acid solution of 2%, is mixed with chitosan solution, is stirred to and dissolves completely at 50 DEG C;
(2) adopt inverse phase suspension to add atoleine, pore-foaming agent polyethylene glycol, fully stir and make reaction system become emulsion form, wherein stir speed (S.S.) is 600r/min;
(3) in mixed system, formalin is added in 60 DEG C of precrosslink 40-60min;
(4) with NaOH, pH value of solution is modulated 10-13, add epoxychloropropane solution, at 80 DEG C, react 3h;
(5) reacted rear filtration, washing, with apparatus,Soxhlet's extracting 12h, then fully washs with acetone and ethanol, removing residual organic matter;
(6) be then placed in 0.5 mol/L hydrochloric acid solution agitation and filtration, finally soak with 1.0 mol/L sodium hydroxide solutions, be washed to neutrality, obtain high amino porous chitosan resin.
Embodiment 2
A preparation method for high amino porous chitosan resin, described preparation method comprises the following steps:
(1) 20 parts of shitosans being dissolved in mass fraction is in the acetic acid solution of 2%, is mixed with chitosan solution, is stirred to and dissolves completely at 50 DEG C;
(2) adopt inverse phase suspension to add atoleine, pore-foaming agent polyethylene glycol, fully stir and make reaction system become emulsion form, wherein stir speed (S.S.) is 1000r/min;
(3) in mixed system, formalin is added in 60 DEG C of precrosslink 60min;
(4) with NaOH, pH value of solution is modulated 10-13, add epoxychloropropane solution, at 80 DEG C, react 3h;
(5) reacted rear filtration, washing, with apparatus,Soxhlet's extracting 12-24h, then fully washs with acetone and ethanol, removing residual organic matter;
(6) be then placed in 0.5 mol/L hydrochloric acid solution agitation and filtration, finally soak with 1.0 mol/L sodium hydroxide solutions, be washed to neutrality, obtain high amino porous chitosan resin.
Embodiment 3
A preparation method for high amino porous chitosan resin, described preparation method comprises the following steps:
(1) 18 parts of shitosans being dissolved in mass fraction is in the acetic acid solution of 2%, is mixed with chitosan solution, is stirred to and dissolves completely at 50 DEG C;
(2) adopt inverse phase suspension to add atoleine, pore-foaming agent polyethylene glycol, fully stir and make reaction system become emulsion form, wherein stir speed (S.S.) is 800r/min;
(3) in mixed system, formalin is added in 60 DEG C of precrosslink 60min;
(4) with NaOH, pH value of solution is modulated 10-13, add epoxychloropropane solution, at 80 DEG C, react 3h;
(5) reacted rear filtration, washing, with apparatus,Soxhlet's extracting 20h, then fully washs with acetone and ethanol, removing residual organic matter;
(6) be then placed in 0.5 mol/L hydrochloric acid solution agitation and filtration, finally soak with 1.0 mol/L sodium hydroxide solutions, be washed to neutrality, obtain high amino porous chitosan resin.
Claims (4)
1. a preparation method for high amino porous chitosan resin, is characterized in that, comprise the following steps:
(1) 10-20 part shitosan being dissolved in mass fraction is in the acetic acid solution of 2%, is mixed with chitosan solution, is stirred to and dissolves completely at 50 DEG C;
(2) adopt inverse phase suspension to add atoleine, pore-foaming agent, fully stir and make reaction system become emulsion form;
(3) in mixed system, formalin is added in 60 DEG C of precrosslink 40-60min;
(4) with NaOH, pH value of solution is modulated 10-13, add epoxychloropropane solution, at 80 DEG C, react 3h;
(5) reacted rear filtration, washing, with apparatus,Soxhlet's extracting 12-24h, then fully washs with acetone and ethanol, removing residual organic matter;
(6) be then placed in 0.5 mol/L hydrochloric acid solution agitation and filtration, finally soak with 1.0 mol/L sodium hydroxide solutions, be washed to neutrality, obtain high amino porous chitosan resin.
2. the preparation method of a kind of high amino porous chitosan resin according to claim 1, it is characterized in that, described in step (2), pore-foaming agent is polyethylene glycol.
3. the preparation method of a kind of high amino porous chitosan resin according to claim 1, is characterized in that, in step (2), stir speed (S.S.) is 600 r/min-1000 r/min.
4. the preparation method of a kind of high amino porous chitosan resin according to claim 1, is characterized in that, the amino porous chitosan resin of described height is used for the absorption of waste water from dyestuff.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410511294.4A CN104324700A (en) | 2014-09-29 | 2014-09-29 | Preparation method of high-amino porous chitosan resin |
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| CN201410511294.4A CN104324700A (en) | 2014-09-29 | 2014-09-29 | Preparation method of high-amino porous chitosan resin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104826608A (en) * | 2015-05-19 | 2015-08-12 | 湖南大学 | Method for degrading orange II in wastewater by using porous chitosan gel beads prepared by using amino protection-modification-release method |
| CN105001614A (en) * | 2015-06-30 | 2015-10-28 | 苏州博利迈新材料科技有限公司 | Heavy metal filtering nanometer membrane for waste water and preparation method thereof |
| CN108993430A (en) * | 2018-08-14 | 2018-12-14 | 济南大学 | A kind of preparation method of chitosan-houghite nano composite material |
| CN113198426A (en) * | 2021-04-22 | 2021-08-03 | 孝感市光源电力集团有限责任公司 | Chitosan resin production system and production method |
| CN115672281A (en) * | 2022-09-16 | 2023-02-03 | 苏州博进生物技术有限公司 | Preparation method of mercury ion adsorption resin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698711A (en) * | 2009-10-22 | 2010-04-28 | 国家海洋局天津海水淡化与综合利用研究所 | Method for preparing chitosan resin for extracting noble metals from bittern |
| CN102989421A (en) * | 2011-09-08 | 2013-03-27 | 王然 | Preparation method of cross-linked chitosan resin |
-
2014
- 2014-09-29 CN CN201410511294.4A patent/CN104324700A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698711A (en) * | 2009-10-22 | 2010-04-28 | 国家海洋局天津海水淡化与综合利用研究所 | Method for preparing chitosan resin for extracting noble metals from bittern |
| CN102989421A (en) * | 2011-09-08 | 2013-03-27 | 王然 | Preparation method of cross-linked chitosan resin |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104826608A (en) * | 2015-05-19 | 2015-08-12 | 湖南大学 | Method for degrading orange II in wastewater by using porous chitosan gel beads prepared by using amino protection-modification-release method |
| CN105001614A (en) * | 2015-06-30 | 2015-10-28 | 苏州博利迈新材料科技有限公司 | Heavy metal filtering nanometer membrane for waste water and preparation method thereof |
| CN108993430A (en) * | 2018-08-14 | 2018-12-14 | 济南大学 | A kind of preparation method of chitosan-houghite nano composite material |
| CN108993430B (en) * | 2018-08-14 | 2021-08-27 | 济南大学 | Preparation method of chitosan-hydrotalcite nano composite material |
| CN113198426A (en) * | 2021-04-22 | 2021-08-03 | 孝感市光源电力集团有限责任公司 | Chitosan resin production system and production method |
| CN115672281A (en) * | 2022-09-16 | 2023-02-03 | 苏州博进生物技术有限公司 | Preparation method of mercury ion adsorption resin |
| CN115672281B (en) * | 2022-09-16 | 2024-02-09 | 苏州博进生物技术有限公司 | Preparation method of mercury ion adsorption resin |
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Application publication date: 20150204 |