CN105968263A - 以羧甲基马铃薯淀粉与丙烯酰胺为原料合成吸附Co2+树脂的方法 - Google Patents
以羧甲基马铃薯淀粉与丙烯酰胺为原料合成吸附Co2+树脂的方法 Download PDFInfo
- Publication number
- CN105968263A CN105968263A CN201610480146.XA CN201610480146A CN105968263A CN 105968263 A CN105968263 A CN 105968263A CN 201610480146 A CN201610480146 A CN 201610480146A CN 105968263 A CN105968263 A CN 105968263A
- Authority
- CN
- China
- Prior art keywords
- acrylamide
- solution
- potato starch
- concentration
- resin
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- 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
-
- 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
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- 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)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明公开了以羧甲基马铃薯淀粉与丙烯酰胺为原料合成吸附Co2+离子树脂的方法,主要特征为首先以氢氧化钠溶液水解丙烯酰胺,然后在氮气的保护下水浴加热,使羧甲基马铃薯淀粉与部分水解的丙烯酰胺在30~60℃下接枝聚合制备吸附Co2+树脂。最佳条件下合成的产品在1000mlCo2+浓度为10ppm的溶液中对Co2+的吸附量为49.84mg/g,去除率为99.85%,在1000mlCo2+浓度为350ppm的溶液中对Co2+的吸附量为1012.13mg/g,去除率为95.70%。本发明吸附Co2+离子树脂的制备具有以下优势:母体羧甲基马铃薯淀粉可溶于水中,因而不需要糊化,工艺简单易行,接枝聚合反应温度低,实用性强,制得的吸附Co2+树脂对Co2+离子吸附量和去除率高。
Description
技术领域
本发明涉及一种用于环境治理领域的功能高分子材料——吸附Co2+离子树脂的制备方法,特别是指以羧甲基马铃薯淀粉、用氢氧化钠部分水解的丙烯酰胺为主要原料制备吸附Co2+离子树脂的方法。
背景技术
由于重金属具有富集性及稳定性,很难在环境中降解的特点,因此相对于其他污染,重金属污染已经成为威胁人类发展的重大环境问题。人摄入钴超过500mg就会中毒。钴在土壤溶液中浓度10mg/L时,可使农作物死亡。人喝的水中钴离子超标时会引起许多严重的健康问题,如低血压、瘫痪、腹泻和骨缺陷等,也会导致活细胞的基因突变。
发明内容
本发明提供了一种操作工艺简单、吸附Co2+能力强、吸附量高的树脂产品及其制备方法。
其方法及步骤如下:
将羧甲基马铃薯淀粉与一定量的去离子水混合;称取一定量的丙烯酰胺,与一定量的去离子水混合,配制氢氧化钠溶液按一定水解度将其与丙烯酰胺溶液反应;将上述羧甲基马铃薯淀粉与去离子水的混合液与用氢氧化钠部分水解的丙烯酰胺溶液在反应瓶中混合均匀,加入一定量的引发剂过硫酸钾溶液及一定量的交联剂N,N'-亚甲基双丙烯酰胺溶液,搅拌使之均匀,通入氮气,缓慢加热,使反应体系温度逐步升高,聚合反应发生在30-60℃之间,温度继续升高达到80℃时保温1.5h,然后取出产物,经烘干、粉碎即得吸附Co2+树脂。上述使用的引发剂过硫酸钾配制为的浓度为10mg/ml的溶液、交联剂N,N'-亚甲基双丙烯酰胺配制为浓度为2.5mg/ml的溶液。
最佳条件下的产品在1000mlCo2+浓度为10ppm的溶液中对Co2+的吸附量为49.84mg/g,在1000mlCo2+浓度为350ppm的溶液中Co2+的吸附量为1012.13mg/g,去除率为95.70%。
本发明的优点:
(1)羧甲基马铃薯淀粉易溶于水,在吸附Co2+树脂制备的过程中不需要传统的淀粉糊化工艺,工艺流程简单易行;
(2)聚合反应温度低,可减少能量消耗,实用性强;
(3)产品对Co2+的吸附效果好。
附图说明
图1是羧甲基马铃薯淀粉与丙烯酰胺合成吸附Co2+树脂的工艺流程图
图2是引发剂用量对初始浓度为10ppm的Co2+树脂的影响曲线
图3是交联剂用量对初始浓度为10ppm的Co2+树脂的影响曲线
图4是丙烯酰胺水解度对初始浓度为10ppm的Co2+树脂的影响曲线
图5是溶解羧甲基马铃薯淀粉的用水量对初始浓度为10ppm的Co2+树脂的影响曲线
图6是羧甲基马铃薯淀粉与丙烯酰胺质量比对初始浓度为10ppm的Co2+树脂的影响曲线
图7是Co2+的初始浓度对初始浓度为10ppm的Co2+树脂的影响曲线。
具体实施方式
实施例1:称取15g丙烯酰胺,溶解于25ml去离子水中,称取7.04g氢氧化钠,溶解于15ml去离子水中,将该氢氧化钠溶液滴加到上述丙烯酰胺溶液中,室温下搅拌使丙烯酰胺水解;称取2.5g羧甲基马铃薯淀粉与30ml去离子水混合均匀,将丙烯酰胺的水解液与羧甲基马铃薯淀粉混合液混合均匀,加入5ml浓度为10mg/ml的过硫酸钾溶液、6ml浓度为2.5mg/ml的N,N'-亚甲基双丙烯酰胺溶液,通入氮气,缓慢加热使反应体系温度逐步升高,聚合反应发生在35℃,待温度上升到80℃时保温1.5h,然后取出产物,经烘干、粉碎得到吸附Co2+树脂,本实施例所制得的吸附Co2+树脂在1000mlCo2+浓度为10ppm的溶液中对Co2+的吸附量为44.76mg/g,去除率为94.52%。
实施例2:称取25g丙烯酰胺,溶解于25ml去离子水中,称取7.04g氢氧化钠,溶解于15ml去离子水中,将该氢氧化钠溶液滴加到上述丙烯酰胺溶液中,室温下搅拌使丙烯酰胺水解;称取2.5g羧甲基马铃薯淀粉与30ml去离子水混合均匀,将丙烯酰胺的水解液与羧甲基马铃薯淀粉混合液混合均匀,加入5ml浓度为10mg/ml的过硫酸钾溶液、10ml浓度为2.5mg/ml的N,N'-亚甲基双丙烯酰胺溶液,通入氮气,缓慢加热使反应体系温度逐步升高,聚合反应发生在39℃,待温度上升到80℃时保温1.5h,然后取出产物,经烘干、粉碎得到吸附Co2+树脂,本实施例所制得的吸附Co2+树脂在1000mlCo2+浓度为10ppm的溶液中对Co2+的吸附量为45.51mg/g,去除率为96.28%。
实施例3:称取25g丙烯酰胺,溶解于25ml去离子水中,称取7.04g氢氧化钠,溶解于15ml去离子水中,将该氢氧化钠溶液滴加到上述丙烯酰胺溶液中,室温下搅拌使丙烯酰胺水解;称取2.5g羧甲基马铃薯淀粉与45ml去离子水混合均匀,将丙烯酰胺的水解液与羧甲基马铃薯淀粉混合液混合均匀,加入5ml浓度为10mg/ml的过硫酸钾溶液、6ml浓度为2.5mg/ml的N,N'-亚甲基双丙烯酰胺溶液,通入氮气,缓慢加热使反应体系温度逐步升高,聚合反应发生在28℃,待温度上升到80℃时保温1.5h,然后取出产物,经烘干、粉碎得到吸附Co2+树脂。本实施例所制得的吸附Co2+树脂在1000mlCo2+浓度为10ppm的溶液中对Co2+的吸附量为49.84mg/g,去除率为99.85%,在1000mlCo2+浓度为350ppm的溶液中Co2+的吸附量为1012.13mg/g,去除率为95.70%。
实施例4:称取25g丙烯酰胺,溶解于25ml去离子水中,称取7.04g氢氧化钠,溶解于15ml去离子水中,将该氢氧化钠溶液滴加到上述丙烯酰胺溶液中,室温下搅拌使丙烯酰胺水解;称取2.5g羧甲基马铃薯淀粉与30ml去离子水混合均匀,将丙烯酰胺的水解液与羧甲基马铃薯淀粉混合液混合均匀,加入5ml浓度为10mg/ml的过硫酸钾溶液、6ml浓度为2.5mg/ml的N,N'-亚甲基双丙烯酰胺溶液,通入氮气,缓慢加热使反应体系温度逐步升高,聚合反应发生在29℃,待温度上升到80℃时保温1.5h,然后取出产物,经烘干、粉碎得到吸附Co2+树脂,本实施例所制得的吸附Co2+树脂在1000mlCo2+浓度为10ppm的溶液中对Co2+的吸附量为43.64mg/g,去除率为93.87%。
实施例5:称取25g丙烯酰胺,溶解于25ml去离子水中,称取7.04g氢氧化钠,溶解于15ml去离子水中,将该氢氧化钠溶液滴加到上述丙烯酰胺溶液中,室温下搅拌使丙烯酰胺水解;称取2.5g羧甲基马铃薯淀粉与30ml去离子水混合均匀,将丙烯酰胺的水解液与羧甲基马铃薯淀粉混合液混合均匀,加入6ml浓度为10mg/ml的过硫酸钾溶液、6ml浓度为2.5mg/ml的N,N'-亚甲基双丙烯酰胺溶液,通入氮气,缓慢加热使反应体系温度逐步升高,聚合反应发生在31℃,待温度上升到80℃时保温1.5h,然后取出产物,经烘干、粉碎得到吸附Co2+树脂,本实施例所制得的吸附Co2+树脂在1000mlCo2+浓度为10ppm的溶液中对Co2+的吸附量为47.09mg/g,去除率为96.52%。
Claims (3)
1.本发明提供了一种操作工艺简单、吸附Co2+能力强、吸附量及去除率高的树脂产品及其制备方法,其方法及步骤如下:
将羧甲基马铃薯淀粉与一定量的去离子水混合;称取一定量的丙烯酰胺,配制氢氧化钠溶液,按一定水解度将其与一定量的丙烯酰胺反应;将上述羧甲基马铃薯淀粉与去离子水的混合液与用氢氧化钠部分水解的丙烯酰胺溶液在反应瓶中混合均匀,加入一定量的引发剂过硫酸钾与一定量的交联剂N,N'-亚甲基双丙烯酰胺,搅拌使之均匀,通入氮气,缓慢加热,使反应体系温度逐步升高,聚合反应发生在30-60℃之间,温度继续升高达到80℃时保温1.5h,然后取出产物,经烘干、粉碎即得吸附Co2+树脂;上述使用的引发剂过硫酸钾配制成浓度为10mg/ml的溶液、交联剂N,N'-亚甲基双丙烯酰胺配制成浓度为2.5mg/ml的溶液。
2.上述以羧甲基马铃薯淀粉与丙烯酰胺为原料合成吸附Co2+树脂的方法制得的吸附Co2+树脂,最佳条件下的产品在1000mlCo2+浓度为10ppm的溶液中对Co2+的吸附量为49.84mg/g,去除率为99.85%,在1000mlCo2+浓度为350ppm的溶液中对Co2+的吸附量为1012.13mg/g,去除率为95.70%。
3. 按权利要求1所述过程最佳条件下合成的吸附Co2+树脂,其中羧甲基马铃薯淀粉:溶解羧甲基马铃薯淀粉用水量:丙烯酰胺:溶解丙烯酰胺的水量:氢氧化钠:溶解氢氧化钠的水量:过硫酸钾:溶解过硫酸钾的水量:N,N'-亚甲基双丙烯酰胺:溶解N,N'-亚甲基双丙烯酰胺的水量=1:18:10:10:2.816:6:0.02:2:0.006:2.4。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610480146.XA CN105968263A (zh) | 2016-06-28 | 2016-06-28 | 以羧甲基马铃薯淀粉与丙烯酰胺为原料合成吸附Co2+树脂的方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610480146.XA CN105968263A (zh) | 2016-06-28 | 2016-06-28 | 以羧甲基马铃薯淀粉与丙烯酰胺为原料合成吸附Co2+树脂的方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN105968263A true CN105968263A (zh) | 2016-09-28 |
Family
ID=57020059
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610480146.XA Pending CN105968263A (zh) | 2016-06-28 | 2016-06-28 | 以羧甲基马铃薯淀粉与丙烯酰胺为原料合成吸附Co2+树脂的方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN105968263A (zh) |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101638460A (zh) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | 羧甲基马铃薯淀粉与丙烯酰胺、丙烯酸及其钠盐接枝共聚制备高吸水树脂的方法 |
-
2016
- 2016-06-28 CN CN201610480146.XA patent/CN105968263A/zh active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101638460A (zh) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | 羧甲基马铃薯淀粉与丙烯酰胺、丙烯酸及其钠盐接枝共聚制备高吸水树脂的方法 |
Non-Patent Citations (6)
Title |
---|
GHANSHYAM S. CHAUHAN等: "Synthesis and Characterization of Starch and Acrylamides Based Hydrogels", 《POLYMERS AND POLYMER COMPOSITES》 * |
GHANSHYAM S. CHAUHAN等: "Use of biopolymers and acrylamide-based hydrogels for sorption of Cu2+, Fe2+ and Cr 6+ ions from their aqueous solutions", 《DESALINATION》 * |
冯玉杰等: "《环境工程中的功能材料》", 31 August 2003, 化学工业出版社 * |
吴季怀等: "《高吸水保水材料》", 31 March 2005, 化学工业出版社 * |
张媛等: "羧甲基淀粉基含钾和氮高吸水树脂吸附Fe3+性能研究", 《功能材料与器件学报》 * |
祝志峰: "《纺织工程化学》", 30 June 2010, 东华大学出版社 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Janker-Obermeier et al. | Solubilization of hemicellulose and lignin from wheat straw through microwave-assisted alkali treatment | |
Dai et al. | Enhanced swelling and responsive properties of pineapple peel carboxymethyl cellulose-g-poly (acrylic acid-co-acrylamide) superabsorbent hydrogel by the introduction of carclazyte | |
Xu et al. | Preparation and utilization of wheat straw bearing amine groups for the sorption of acid and reactive dyes from aqueous solutions | |
Vieira et al. | Copper sorption from aqueous solutions and sugar cane spirits by chemically modified babassu coconut (Orbignya speciosa) mesocarp | |
Khalilzadeh et al. | Natural clinoptilolite/KOH: an efficient heterogeneous catalyst for carboxymethylation of hemicellulose | |
JP2006129735A (ja) | 触媒を用いたセルロースの加水分解方法および触媒を用いたグルコースの生産方法 | |
CN105713049A (zh) | 一种腐植酸及其钠盐的生产方法 | |
Liu et al. | Removal of copper and lead from aqueous solution by carboxylic acid functionalized deacetylated konjac glucomannan | |
Pragya et al. | Dynamic cross-linking of an alginate–acrylamide tough hydrogel system: time-resolved in situ mapping of gel self-assembly | |
Kolya et al. | Starch-g-Poly-(N, N-dimethyl acrylamide-co-acrylic acid): An efficient Cr (VI) ion binder | |
CN102060942B (zh) | 一种6-氨基-6-脱氧菊糖及其制备和应用 | |
CN110624514B (zh) | 一种提高腐植酸对金属离子吸附量的方法 | |
Mishra et al. | Treatment of gray wastewater and heavy metal removal from aqueous medium using hydrogels based on novel crosslinkers | |
CN103613709A (zh) | 以马铃薯淀粉黄原酸酯为原料合成吸附重金属离子专用树脂的方法 | |
Krishnan et al. | Proton play in the formation of low molecular weight chitosan (LWCS) by hydrolyzing chitosan with a carbon based solid acid | |
Feng et al. | Synthesis and characterization of porous hydrogel based on lignin and polyacrylamide | |
Sun et al. | A new approach to chemically modified carboxymethyl chitosan and study of its moisture‐absorption and moisture‐retention abilities | |
Hao et al. | Sweet potato starch residue as starting material to prepare polyacrylonitrile adsorbent via SI-SET-LRP | |
Zhang et al. | Facile synthesis of phenolic hydroxyl-rich modified lignin: Evaluation of their applications as an antioxidant and for Cr (VI) removal | |
CN105968263A (zh) | 以羧甲基马铃薯淀粉与丙烯酰胺为原料合成吸附Co2+树脂的方法 | |
Najaf Iqbal et al. | Microwave-assisted green synthesis of guar gum esters with enhanced physicochemical properties | |
CN107619483A (zh) | 一种硒化海藻酸钠水凝胶的制备方法 | |
CN106008837B (zh) | 以羧甲基马铃薯淀粉与丙烯酰胺为原料合成吸附Fe3+树脂的方法 | |
Sympson et al. | Recirculating calcium hydroxide solution: a practical choice for on-farm high solids lignocellulose pretreatment | |
CN105936661A (zh) | 以羧甲基马铃薯淀粉与丙烯酰胺为原料合成吸附Ni2+树脂的方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160928 |