CN104607157A - Method for preparing heavy metal complexing fiber by quickly modified jute through microwaves and application of fiber - Google Patents
Method for preparing heavy metal complexing fiber by quickly modified jute through microwaves and application of fiber Download PDFInfo
- Publication number
- CN104607157A CN104607157A CN201510013522.XA CN201510013522A CN104607157A CN 104607157 A CN104607157 A CN 104607157A CN 201510013522 A CN201510013522 A CN 201510013522A CN 104607157 A CN104607157 A CN 104607157A
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- jute
- heavy metal
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- metal complexing
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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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- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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
Abstract
The invention discloses a method for a preparing heavy metal complexing fiber by quickly modified jute through microwaves and the application of the fiber. The method comprises the following steps: (1) firstly, cooking jute fibers with boiling water, then soaking the cooked jute fibers with a sodium hydroxide solution, and baking the soaked jute fibers for preservation; (2) adding the preprocessed jute fiber and epoxy chloropropane into a solution, performing early stage etherification in a microwave oven, then adding activated monomers of complexing groups for ammoniation and heating in a water bath, taking out materials after reaction, cleaning the materials to obtain products, and placing the products in an oven, baking the products in the oven to constant weight so as to obtain a jute-based modified adsorbing material which can be used for processing unexpected heavy metal pollution and conventional heavy metal wastewater. In the preparation process, a microwave irradiation technology is used for quickly grafting and modifying basal bodies to prepare the fiber with a complexing function, the non-heat effect of the microwaves and the advantage of high grafting and penetrating power of the microwaves are fully utilized, a chemical grafting reaction can be quickly and efficiently completed, the preparation time is greatly shortened, and the method is simple to operate and is convenient and feasible.
Description
Technical field
The invention belongs to water-treatment technology field, relate to method and application that the quick modification jute of a kind of microwave prepares heavy metal complexing fiber.
Background technology
In recent years, develop rapidly along with socioeconomic, the sudden heavy metal pollution event of China's water body takes place frequently, and this environment of not only depending on for existence to us damages and pollutes, and the safety and Health of the mankind in serious threat.The emergence treating method of current energy practical application is also very limited, main employing coagulation sedimentation method, though the method can make the solubilised state content of beary metal in water body up to standard, but the total amount of Heavy Metals in Waters does not decline, but also existence investment is high, disposal efficiency is low, on-the-spot applicability is poor and very easily cause secondary pollution problems.Adopt absorption method to remove water pollutant not need to add other medicaments, reaction speed is fast, and treatment effeciency is high, is easy to operation and applicability is wide, than coagulant sedimentation advantageously.
At present in the emergent absorption of burst heavy metal pollution is disposed, use that the form free degree is large, applying flexible and the good fibrous sorbing material of mechanical strength become a kind of trend, but there is the long and more difficult acquisition of material of preparation method's time or the realistic problem such as expensive, therefore, the emergency disposal of fibrous sorbing material to burst heavy metal pollution of research and development Cheap highly effective seems particularly important fast.
Tossa is that a class quantity is enriched, wide material sources, absorption raw material cheap and easy to get, and containing abundant cellulose, mechanical strength is high.We can introduce by chemical graft means the complexing group (as carboxyl and amino etc.) that one or more heavy metal ions (as copper ion etc.) have very strong adsorption capacity on tossa, reach the object of rapidly and efficiently removal heavy metal.But before for the research multiselect commercial fiber (modification-Chinese Patent Application No. as polyacrylonitrile fibre: 201410120143.6) costly of heavy metal ion fiber adsorbing material, even if or select agriculture and forestry organic waste material cheap and easy to get, but its modification cycle relatively grows the (modification-Chinese Patent Application No. as agricultural crop straw: 201410160822.6; Preparation method-the Chinese Patent Application No. of modified cellulose: 201310483542.4), these materials are all difficult to carry out in actual emergency work.
Summary of the invention
In order to solve at present, burst heavy metal water pollutions emergency disposal technology is deficient, disposal material is difficult to recovery or flow resistance is difficult to realistic problems such as using greatly, the invention provides method and application that the quick modification jute of a kind of microwave prepares heavy metal complexing fiber.The method can prepare strong, the environmentally friendly fibrous sorbing material of the on-the-spot applicability of emergency disposal fast, and raw material sources are extensive, cheap and easy to get, and preparation method fast simple, be easy to realize industrialization.
The object of the invention is to be achieved through the following technical solutions:
The quick modification jute of microwave prepares a method for heavy metal complexing fiber, and carry out indirect graft reaction by microwave irradiation complexing group activated monomer to tossa surface after pretreatment, detailed description of the invention step is as follows:
One, fibriilar pretreatment
First use boiling water boiling tossa 10 ~ 60min, then soak above-mentioned tossa 5 ~ 30min with sodium hydroxide solution, preserve after drying.
In this step, the mass concentration of described sodium hydroxide solution is 1 ~ 30%.
Two, the quick modification of the microwave of pretreatment of fiber
Pretreated for step one tossa, epoxychloropropane are joined in solution, etherificate in early stage is carried out in micro-wave oven, control temperature is at 50 ~ 120 DEG C, add complexing group activated monomer after reaction 5 ~ 15min and carry out ammonification heating water bath, control jute, the mass ratio of epoxychloropropane and multiamino compound is 1:4 ~ 10:4 ~ 10, bath temperature be at 50 ~ 120 DEG C, takes out material after reacting 1 ~ 5h, after cleaning, product is placed in drying in oven to constant weight, obtains jute base modified absorbing material.
In this step, described complexing group activated monomer is multiamino compound (as triethylene tetramine, ethylenediamine or diethylenetriamine etc.).When complexing group activated monomer is multiamino compound, itself and the indirect grafting of the pretreated tossa of step one, first carry out etherificate with epoxychloropropane, then grafting multiamino compound.
In this step, described solution can be selected in water, DMF and pyridine etc. a kind of.
In this step, the mass ratio of described jute, epoxychloropropane and multiamino compound is preferably 1:5 ~ 10:5.
In this step, described bake out temperature is 70 ~ 100 DEG C.
Jute base modified absorbing material prepared by said method can be used in burst heavy metal pollution and conventional heavy metal containing wastewater treatment, and concrete steps are as follows:
Under the condition not changing initial copper ion solution pH, carry out Static Adsorption under room temperature to the copper ion of 20 ~ 500mg/L, can reach adsorption equilibrium in 20min, its adsorption capacity is 30 ~ 110mg/g.
The present invention is compared to prior art, and tool has the following advantages:
1, the present invention adopts Microwave Radiation in Manufacturing to carry out quick graft modification to matrix to prepare complexing functional fibre in preparation process, take full advantage of the non-thermal effect of microwave and the strong advantage of grafting penetration power, when adsorption capacity is 30 ~ 110mg/g, adsorption equilibrium can be reached in 20min, complete chemical graft reaction more quickly and efficiently, preparation time shortens greatly, and simple, convenient easy.
2, the raw material tossa wide material sources selected of the present invention, cheap and easy to get, is easy to industrialization.
3, the present invention select complexing group activated monomer be multiamino compound as triethylene tetramine, ethylenediamine and diethylenetriamine etc., make fibrous matrix has amino, the two has synergy, easily and heavy metal ion form complex compound.
4, the jute base modified absorbing material mechanical strength of rapid development of the present invention is high and keep fiber shape, and use flexibly, be convenient to recycle, on-the-spot applicability is stronger.
5, in order can prepare fast when happening suddenly heavy metal water pollutions, throwing in fast, to reclaim fast, replacings, flow resistance are little, mass transfer advantages of good adsorption effect contour effect urgency handle demand provides technical support in the present invention.
6, cellulose base modified adsorbent of the present invention both can be applicable to the adsorption treatment of actual burst heavy metal pollution, also can be applicable to the process of conventional heavy metal wastewater thereby, its achievement solves the bottleneck problem of disposal efficiency and the response speed raising affecting heavy metal water pollutions, has important environment, economic implications.
Detailed description of the invention
Below technical scheme of the present invention is further described, but is not limited thereto, everyly technical solution of the present invention is modified or equivalent to replace, and do not depart from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
embodiment 1:
The present embodiment take tossa as absorption raw material, and select copper ion as target contaminant, concrete technical scheme is as follows:
One, first use boiling water boiling ortho states jute 30min, then use 20% soaking with sodium hydroxide, spend after 30min under deionized water to neutrality is placed on baking oven and dry.
Two, pretreated for step one tossa, epoxychloropropane are joined N, in dinethylformamide solution, 90 DEG C are adjusted the temperature in micro-wave oven, add triethylene tetramine after reaction 5min and carry out water-bath, the mass ratio of jute, epoxychloropropane and multiamino compound is 1:10:5, take out material after heating water bath 1h, dry at product being placed in 80 DEG C after cleaning to constant weight, obtain jute base modified absorbing material prepared by microwave method.
Etherification reaction equation is as follows:
；
Aminating reaction equation is as follows:
。
Get modification jute 0.1g that said method obtains in the screw socket bottle of 250mL, add Cu (II) solution of a series of concentration of 100mL, room temperature, do not change pH value of solution condition under carry out Static Adsorption, its adsorption capacity is about 85.52mg/g, and 20min can reach adsorption equilibrium.
embodiment 2:
The present embodiment take tossa as absorption raw material, and select copper ion as target contaminant, concrete technical scheme is as follows:
One, first use boiling water boiling ortho states jute 30min, then use 20% soaking with sodium hydroxide, spend after 30min under deionized water to neutrality is placed on baking oven and dry.
Two, pretreated for step one tossa, epoxychloropropane are joined N, in dinethylformamide solution, 90 DEG C are adjusted the temperature in micro-wave oven, add triethylene tetramine after reaction 5min and carry out water-bath, the mass ratio of jute, epoxychloropropane and triethylene tetramine is 1:5:10, take out material after heating water bath 1h, dry at product being placed in 80 DEG C after cleaning to constant weight, obtain jute base modified absorbing material prepared by microwave method.
Get modification jute 0.1g that said method obtains in the screw socket bottle of 250mL, add Cu (II) solution of a series of concentration of 100mL, room temperature, do not change pH value of solution condition under carry out Static Adsorption, its adsorption capacity is about 72.59mg/g, and 20min can reach adsorption equilibrium.
embodiment 3:
The present embodiment take tossa as absorption raw material, and select copper ion as target contaminant, concrete technical scheme is as follows:
One, first use boiling water boiling ortho states jute 30min, then use 20% soaking with sodium hydroxide, spend after 30min under deionized water to neutrality is placed on baking oven and dry.
Two, pretreated for step one tossa, epoxychloropropane are joined N, in dinethylformamide solution, 90 DEG C are adjusted the temperature in micro-wave oven, add diethylenetriamine after reaction 5min and carry out water-bath, the mass ratio of jute, epoxychloropropane and diethylenetriamine is 1:10:5, take out material after heating water bath 1h, dry at product being placed in 80 DEG C after cleaning to constant weight, obtain jute base modified absorbing material prepared by microwave method.
Get modification jute 0.1g that said method obtains in the screw socket bottle of 250mL, add Cu (II) solution of a series of concentration of 100mL, room temperature, do not change pH value of solution condition under carry out Static Adsorption, its adsorption capacity is about 28.85mg/g, and 20min can reach adsorption equilibrium.
Claims (8)
1. the quick modification jute of microwave prepares a method for heavy metal complexing fiber, it is characterized in that described method step is as follows:
One, fibriilar pretreatment
First use boiling water boiling tossa 10 ~ 60min, then soak above-mentioned tossa 5 ~ 30min with sodium hydroxide solution, preserve after drying;
Two, the quick modification of the microwave of pretreatment of fiber
Pretreated for step one tossa, epoxychloropropane are joined in solution, etherificate in early stage is carried out in micro-wave oven, control temperature is at 50 ~ 120 DEG C, add complexing group activated monomer after reaction 5 ~ 15min and carry out ammonification heating water bath, control jute, the mass ratio of epoxychloropropane and multiamino compound is 1:4 ~ 10:4 ~ 10, bath temperature be at 50 ~ 120 DEG C, takes out material after reacting 1 ~ 5h, after cleaning, product is placed in drying in oven to constant weight, obtains jute base modified absorbing material.
2. the quick modification jute of microwave according to claim 1 prepares the method for heavy metal complexing fiber, it is characterized in that in described step one, and the mass concentration of sodium hydroxide solution is 1 ~ 30%.
3. the quick modification jute of microwave according to claim 1 prepares the method for heavy metal complexing fiber, it is characterized in that in described step 2, and complexing group activated monomer is multiamino compound.
4. the quick modification jute of microwave according to claim 3 prepares the method for heavy metal complexing fiber, it is characterized in that described multiamino compound is triethylene tetramine, ethylenediamine or diethylenetriamine.
5. the quick modification jute of microwave according to claim 1 prepares the method for heavy metal complexing fiber, it is characterized in that in described step 2, and solution is a kind of in water, DMF and pyridine.
6. the quick modification jute of the microwave according to claim 1,3 or 4 prepares the method for heavy metal complexing fiber, it is characterized in that in described step 2, and the mass ratio of jute, epoxychloropropane and multiamino compound is preferably 1:5 ~ 10:5.
7. the quick modification jute of microwave according to claim 1 prepares the method for heavy metal complexing fiber, it is characterized in that in described step 2, and bake out temperature is 70 ~ 100 DEG C.
8. the heavy metal complexing fiber that prepared by method described in a claim 1 can be used in burst heavy metal pollution and conventional heavy metal containing wastewater treatment.
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Cited By (12)
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| CN105478085A (en) * | 2015-12-16 | 2016-04-13 | 湖南广播电视大学 | Preparation and application of adsorbent with jute as raw material |
| CN105498708A (en) * | 2015-12-16 | 2016-04-20 | 湖南广播电视大学 | Supercritical extraction method for jute polysaccharide and application of jute polysaccharide |
| CN105536712A (en) * | 2015-12-16 | 2016-05-04 | 湖南广播电视大学 | Ephedran prepared through steam explosion method and use thereof |
| CN105536713A (en) * | 2015-12-16 | 2016-05-04 | 湖南广播电视大学 | Modified Corchorus capsularis polysaccharide, preparation and application thereof |
| CN106064077A (en) * | 2016-07-19 | 2016-11-02 | 哈尔滨工业大学 | The method of the quick modified cellulose fibre of a kind of microwave and application |
| CN106076290A (en) * | 2016-06-21 | 2016-11-09 | 哈尔滨工业大学 | The method of the quick modified acrylic fibre of a kind of microwave and application |
| CN106215882A (en) * | 2016-09-08 | 2016-12-14 | 河海大学 | A kind of preparation method of the Exocarpium Citrulli adsorbent for processing waste water from dyestuff |
| CN108043364A (en) * | 2017-12-19 | 2018-05-18 | 湖南广播电视大学 | A kind of preparation and application of novel porous flaxen fiber heavy metal absorbent |
| CN108854989A (en) * | 2018-07-12 | 2018-11-23 | 中国农业科学院麻类研究所 | A kind of modified jute, preparation method and application |
| CN110681369A (en) * | 2019-10-08 | 2020-01-14 | 华南师范大学 | Preparation method and application of polyamino-carboxyl cross-linked straw fiber adsorbing material |
| CN111729653A (en) * | 2020-07-01 | 2020-10-02 | 北京理工大学珠海学院 | Polyamine vegetable fiber-based adsorption material and preparation method and application thereof |
| CN114985431A (en) * | 2022-05-12 | 2022-09-02 | 南华大学 | Modified fiber composite material based on microorganism reinforcement process and preparation method thereof |
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Cited By (18)
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| CN105478085B (en) * | 2015-12-16 | 2018-06-29 | 湖南广播电视大学 | Using jute as the preparation and application of the adsorbent of raw material |
| CN105498708A (en) * | 2015-12-16 | 2016-04-20 | 湖南广播电视大学 | Supercritical extraction method for jute polysaccharide and application of jute polysaccharide |
| CN105536712A (en) * | 2015-12-16 | 2016-05-04 | 湖南广播电视大学 | Ephedran prepared through steam explosion method and use thereof |
| CN105536713A (en) * | 2015-12-16 | 2016-05-04 | 湖南广播电视大学 | Modified Corchorus capsularis polysaccharide, preparation and application thereof |
| CN105478085A (en) * | 2015-12-16 | 2016-04-13 | 湖南广播电视大学 | Preparation and application of adsorbent with jute as raw material |
| CN105536712B (en) * | 2015-12-16 | 2018-03-06 | 湖南广播电视大学 | Jute polysaccharide and its application made from steam explosion method |
| CN105498708B (en) * | 2015-12-16 | 2018-03-06 | 湖南广播电视大学 | The means of supercritical extraction of jute polysaccharide and its application |
| CN105536713B (en) * | 2015-12-16 | 2018-06-29 | 湖南广播电视大学 | The extraction of jute polysaccharide and its application in hexavalent chromium is removed |
| CN106076290A (en) * | 2016-06-21 | 2016-11-09 | 哈尔滨工业大学 | The method of the quick modified acrylic fibre of a kind of microwave and application |
| CN106076290B (en) * | 2016-06-21 | 2019-01-18 | 哈尔滨工业大学 | A kind of method and application of the quick modified acrylic fibre of microwave |
| CN106064077A (en) * | 2016-07-19 | 2016-11-02 | 哈尔滨工业大学 | The method of the quick modified cellulose fibre of a kind of microwave and application |
| CN106215882B (en) * | 2016-09-08 | 2018-12-14 | 河海大学 | It is a kind of for handling the preparation method of the watermelon peel adsorbent of waste water from dyestuff |
| CN106215882A (en) * | 2016-09-08 | 2016-12-14 | 河海大学 | A kind of preparation method of the Exocarpium Citrulli adsorbent for processing waste water from dyestuff |
| CN108043364A (en) * | 2017-12-19 | 2018-05-18 | 湖南广播电视大学 | A kind of preparation and application of novel porous flaxen fiber heavy metal absorbent |
| CN108854989A (en) * | 2018-07-12 | 2018-11-23 | 中国农业科学院麻类研究所 | A kind of modified jute, preparation method and application |
| CN110681369A (en) * | 2019-10-08 | 2020-01-14 | 华南师范大学 | Preparation method and application of polyamino-carboxyl cross-linked straw fiber adsorbing material |
| CN111729653A (en) * | 2020-07-01 | 2020-10-02 | 北京理工大学珠海学院 | Polyamine vegetable fiber-based adsorption material and preparation method and application thereof |
| CN114985431A (en) * | 2022-05-12 | 2022-09-02 | 南华大学 | Modified fiber composite material based on microorganism reinforcement process and preparation method thereof |
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Application publication date: 20150513 |