CN102493187A - Method for producing polypropylene-based ion-chelating fibers capable of absorbing heavy metal ions - Google Patents
Method for producing polypropylene-based ion-chelating fibers capable of absorbing heavy metal ions Download PDFInfo
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Abstract
A method for producing polypropylene-based ion-chelating fibers capable of absorbing heavy metal ions includes: using a polypropylene fiber as a framework; grafting and polymerizing acrylic acid functional monomers and N, N-methylene-bis-acrylamide crosslinking agent to the surface of the polypropylene fiber under irradiation of ultraviolet; and obtaining the polypropylene-based ion-chelating fiber capable of absorbing heavy metal ions. The crosslinking agent is used for reaction in the method, so that the functional monomers are crosslinked and polymerized on the surface of the fiber to form a three-dimensional polymer network, surface grafting and polymerizing rates of ultraviolet are evidently improved, and content of ion-chelating groups on the surface of the fiber is increased. The method is simple in reaction and operation, short in reaction time, and free of organic solvents in production. The polypropylene-based ion-chelating fibers made by the method have good mechanical properties and chemical stability, are capable of well chelating and absorbing a plurality of types of heavy metal ions, and can be used for absorption separation and purification of trace heavy metal ions in water.
Description
Technical field
The present invention relates to a kind of branch dried up in the ion chelating fiber preparation method of micro-harmful heavy metal ion, relate to particularly and a kind ofly adopt the ultraviolet radiation graft legal system to be equipped with the surface to have the method for the polypropylene-base ion chelating fiber of high-load ion chelating group.
Technical background
Water is the material base that the mankind depend on for existence and development, and the harmful heavy metal ionic contamination that dissolves in the water has potential threat to health.Can cause serious injury to kidney after for example cadmium is absorbed by the body, and make skeleton become soft, cause " Itai-itai diseases ".Lead poisoning causes illnesss such as intestinal colic, anaemia and muscle paralysis usually, encephalopathic can take place even cause death when serious.China has stipulated the limit value of some content of beary metal in " drinking water sanitary standard ", like cadmium 0.005 mg/L, plumbous 0.01 mg/L, copper 1.0 mg/L etc.But the heavy metal ion of these traces still can be in human body long-term accumulated and health is had potential threat.Therefore, remove effectively that heavy metal ion becomes a challenging job in the water, included in China " 12 " planning.
Mostly traditional solid-phase adsorbent such as active carbon and ion exchange resin etc. are particle shape adsorbent, and the adsorption equilibrium time is long, and selectivity and reproducibility are poor, emboliform adsorbent dense arrangement of while, easy blocking packed column.In recent years; High-molecule chelated fiber has higher selectivity to adsorbing metal ions; Adsorption rate is fast; Adsorption capacity is big, is convenient to again be filled in the splitter with fibre bundle, form such as netted, make that it reclaims in heavy metal ion, concentrates, enrichment with the field such as separate and demonstrate good application prospects.
Polypropylene fibre has mechanical performance and chemical stability preferably, and with low cost, nontoxic, can cause method, high-energy radiation initiation method and ultraviolet light initiation method etc. through chemistry its surface modification is prepared high-molecule chelated fiber.But in above-mentioned surface grafting method, function monomer such as acrylic acid, acrylonitrile and methacrylic acid etc. are all lower at the percent grafting on polypropylene fibre surface at present, thereby the chelating function group content of fiber surface is less, and are limited to the adsorption capacity of heavy metal ion.
Summary of the invention
The purpose of this invention is to provide the polypropylene-base ion chelating fiber that a kind of surface has high-load ion chelating group.Adopting uv irradiation method, is skeleton with the polypropylene fibre, and with acrylate functional monomer and N, the graft copolymerization of N-methylene-bisacrylamide crosslinking agent is on the polypropylene fibre surface.Owing to the introducing of crosslinking agent, obtained to have the polypropylene-base ion chelating fiber of high-load ion chelating group, its graft copolymerization rate can reach 230 %.Development proposition new way for micro-harmful heavy metal ion isolation technology in the following water.
The objective of the invention is to realize through following technical scheme.
A kind of polypropylene-base ion chelating fiber preparation method of Adsorption of Heavy Metal Ions, its preparation method is the ultraviolet surface graft method, this method may further comprise the steps:
(1) polypropylene fibre successively water and acetone are embathed, the impurity such as sand and dust, dirt and oil stain to remove fiber surface are dried to constant weight;
(2) preparation of ultraviolet surface graft reactant liquor: in conical flask, add function monomer, crosslinking agent; Its weight percent concentration is 0.5 % ~ 10 % of monomer; Add light trigger, its weight percent concentration is 0.1 % ~ 1.0 % of monomer, adopts ultrasonic oscillation to dissolving;
(3) UV-irradiation graft reaction: in proportion above-mentioned reactant liquor is evenly dripped on the polypropylene fibre surface, be positioned in the UV-irradiation reactor, the sealing back feeds nitrogen 30 min to get rid of oxygen; Open high voltage mercury lamp radiation 5～25 min, the power of light source is 500 W, and the ultraviolet light source wavelength is 365 nm; Fluorescent tube is 5～25 cm apart from the sample distance; Nitrogen flow is 10～30 mL/min, after the irradiation, product is neutral with rinsed with deionized water to pH value; Through the washing of deionization boiling water, drying; Be solvent Suo Shi extracting 24 h again with acetone, be dried to constant weight, obtain the polypropylene-base ion chelating fiber that the surface has high-load ion chelating group.
The polypropylene-base ion chelating fiber preparation method of described a kind of Adsorption of Heavy Metal Ions, its macromolecule matrix material are that the polypropylene fibre of processing is sprayed in fusion.
The polypropylene-base ion chelating fiber preparation method of described a kind of Adsorption of Heavy Metal Ions, its function monomer is an acrylic acid, its weight percent concentration is 10 % ~ 500 % of polypropylene fibre matrix.
The polypropylene-base ion chelating fiber preparation method of described a kind of Adsorption of Heavy Metal Ions, its light trigger is a benzophenone, its weight percent concentration is 0.1 % ~ 1.0 % of monomer.
The polypropylene-base ion chelating fiber preparation method of described a kind of Adsorption of Heavy Metal Ions; In the UV-irradiation graft reaction, add the crosslinking agent that improves product graft copolymerization rate; Crosslinking agent is N, the N-methylene-bisacrylamide, and its weight percent concentration is 0.5 % ~ 10 % of monomer.The step and the condition of the polypropylene-base ion chelating fiber production method of a kind of Adsorption of Heavy Metal Ions that the present invention relates to are following:
Main feature of the present invention is following:
Adopt the ultraviolet surface graft method, with acrylic monomers and N, the copolymerization of N-methylene-bisacrylamide crosslinking agent graft crosslinking is on the polypropylene fibre surface.This method has added crosslinking agent in reactant liquor; (its graft copolymerization rate can reach 230 % to have significantly improved ultraviolet surface graft copolymerization rate; And the percent grafting that does not add the Polypropylene Fibers Grafted with Acrylic Acid of crosslinking agent preparation is merely 76 %); And the amino of crosslinking agent can and metal ion-chelant, increased the content of the ion chelating group on polypropylene fibre surface.Through the consumption of adjusting UV-irradiation time, light trigger consumption, function monomer consumption and crosslinking agent, the ion chelating group content on flexibly changing polypropylene fibre surface.This method operation is easy, and the reaction time is short, in the preparation process not with an organic solvent.The polypropylene-base ion chelating fiber that adopts the inventive method to prepare has mechanical performance and chemical stability preferably; Contents of many kinds of heavy metal ion is had good chelating absorption property, can be used for the adsorbing separation and the purified treatment of micro heavy ion in the water.
Description of drawings
Fig. 1 is the infrared spectrogram of virgin pp fiber (a), Polypropylene Fibers Grafted with Acrylic Acid (b) and polypropylene-base ion chelating fiber (c).
Annotate: Fig. 1 of the present invention is the analysis sketch map of product state, the unintelligible understanding that does not influence technical scheme of the present invention of figure Chinese words.
The specific embodiment
As shown in the figure, the infrared spectrum of comparison virgin pp fiber, Polypropylene Fibers Grafted with Acrylic Acid is at 2500 cm
-1～3500 cm
-1The stretching vibration absworption peak of O-H among the appearance-COOH of place is at 1715 cm
-1The stretching vibration absworption peak of very wide carbonyl C=O has appearred in the place, shows acrylic acid-grafted on the polypropylene fibre surface.And polypropylene-base ion chelating fiber is when having above-mentioned characteristic peak, at 1541 cm
-1The N-H flexural vibrations absworption peak of acid amides II bands of a spectrum appears in the place, shows acrylic acid and N, and N-methylene-bisacrylamide copolymerzation with cross-linking is on the polypropylene fibre surface, and prepared product is a polypropylene-base ion chelating fiber.
The prepared polypropylene-base ion chelating of the present invention fiber is to the adsorption effect of micro heavy ion in the water.
Below with Cu
2+Ion is the adsorption effect of example explanation polypropylene-base ion chelating fiber.
The Cu that in 100 mL conical flasks, adds various gradient concentrations (50 ~ 300 mg/L)
2+Metal ion solution 50 mL add 0.5 g polypropylene-base ion chelating of the present invention fiber respectively, and intermittent oscillation is adsorbed 48 h under room temperature, to guarantee to reach adsorption equilibrium.Adopt U-3310 type ultraviolet-uisible spectrophotometer to measure Cu in the solution of absorption front and back
2+Ion concentration detects wavelength 800 nm.
The adsorption rate of polypropylene-base ion chelating fiber and adsorbance adopt formula to calculate:
A?=?(
C 0 -?
C)?/?
C 0 ?×?100?%
Q?=?(
C 0 -?
C)?
V?/?
M
In the formula,
ABe adsorption rate (%),
QBe adsorbance (mg/g),
C 0 Be absorption initial concentration (mg/L),
CBe adsorption equilibrium concentration (mg/L),
MBe the quality (g) of adsorbing fiber,
VVolume (L) for solution.
Polypropylene-base ion chelating fiber of the present invention is the Cu of 50 mg/L to initial mass concentration
2+The adsorption rate of ion is as shown in table 1.Simultaneously table 1 listed different graft copolymerization rates polypropylene-base ion chelating fiber to Cu
2+The maximal absorptive capacity of ion.
Table 1 polypropylene-base ion chelating fiber is to Cu
2+The adsorption rate of ion and maximal absorptive capacity
| Graft copolymerization rate (%) | 76 a | 140 | 190 | 230 |
| Adsorption rate b（%） | 80.5 | 93.5 | 94.2 | 96.4 |
| Maximal absorptive capacity (mg/g) | 7.5 | 10.5 | 12.6 | 24.8 |
A: the Polypropylene Fibers Grafted with Acrylic Acid that does not add crosslinking agent
B: Cu
2+Ion initial mass concentration is 50 mg/L
Experimental result shows that the percent grafting that does not add the Polypropylene Fibers Grafted with Acrylic Acid of crosslinking agent preparation is merely 76 %, introduces its graft copolymerization rate of crosslinking agent and significantly improves, and can reach 230 %.Polypropylene-base ion chelating fiber of the present invention is to Cu in the water
2+The adsorption capacity of ion is significantly higher than the Polypropylene Fibers Grafted with Acrylic Acid that does not add crosslinking agent, and along with the increase adsorption capacity of graft copolymerization rate increases.When the graft copolymerization rate was 230 %, polypropylene-base ion chelating fiber was to Cu in the water
2+The adsorption rate of ion is 96.4 %, and maximal absorptive capacity can reach 24.8 mg/g.
The regeneration of the prepared polypropylene-base ion chelating of the present invention fiber.
Using concentration is that the hydrochloric acid solution of 0.1 mol/L is to Adsorption of Cu
2+Polypropylene-base ion chelating fiber behind the ion carries out wash-out, blue Cu
2+Ion is easy to desorption from the polypropylene-base ion chelating fiber, uses rinsed with deionized water to pH value to be neutrality again, after drying, can reuse.
Embodiment 1:
Polypropylene fibre successively water and acetone are embathed, and the impurity such as sand and dust, dirt and oil stain to remove fiber surface are dried to constant weight.In conical flask, add 10 g acrylic acid, 0.05 g benzophenone (its weight percent concentration is 0.5 % of monomer), adopt ultrasonic oscillation to dissolving.Get above-mentioned reactant liquor 5.0 g and evenly drip on the polypropylene fibre surface after 1.0 g handle, be positioned in the UV-irradiation reactor, the sealing back feeds nitrogen 30 min to get rid of oxygen.Open high voltage mercury lamp radiation 25 min, the power of light source is 500 W, and the ultraviolet light source wavelength is 365 nm, and fluorescent tube is 15 cm apart from the sample distance, and nitrogen flow is 10 mL/min.After the irradiation, product being neutral with rinsed with deionized water to pH value, through repeatedly deionization boiling water washing, drying, is solvent Suo Shi extracting 24 h with acetone again, is dried to constant weight, obtains the Polypropylene Fibers Grafted with Acrylic Acid that percent grafting is 76 %.
Embodiment 2:
Polypropylene fibre successively water and acetone are embathed, and the impurity such as sand and dust, dirt and oil stain to remove fiber surface are dried to constant weight.In conical flask, add 10 g acrylic acid, 0.5 g N, N-methylene-bisacrylamide (its weight percent concentration is 5.0 % of monomer) and 0.05 g benzophenone (its weight percent concentration is 0.5 % of monomer) adopt ultrasonic oscillation to dissolving.Get above-mentioned reactant liquor 3.0 g and evenly drip on the polypropylene fibre surface after 1.0 g handle, be positioned in the UV-irradiation reactor, the sealing back feeds nitrogen 30 min to get rid of oxygen.Open high voltage mercury lamp radiation 25 min, the power of light source is 500 W, and the ultraviolet light source wavelength is 365 nm, and fluorescent tube is 15 cm apart from the sample distance, and nitrogen flow is 10 mL/min.After the irradiation, product being neutral with rinsed with deionized water to pH value, through repeatedly deionization boiling water washing, drying, is solvent Suo Shi extracting 24 h with acetone again, is dried to constant weight, and obtaining the graft copolymerization rate is the polypropylene-base ion chelating fiber of 130 %.
Embodiment 3:
Polypropylene fibre successively water and acetone are embathed, and the impurity such as sand and dust, dirt and oil stain to remove fiber surface are dried to constant weight.In conical flask, add 10 g acrylic acid, 0.5 g N, N-methylene-bisacrylamide (its weight percent concentration is 5.0 % of monomer) and 0.05 g benzophenone (its weight percent concentration is 0.5 % of monomer) adopt ultrasonic oscillation to dissolving.Get above-mentioned reactant liquor 4.0 g and evenly drip on the polypropylene fibre surface after 1.0 g handle, be positioned in the UV-irradiation reactor, the sealing back feeds nitrogen 30 min to get rid of oxygen.Open high voltage mercury lamp radiation 25 min, the power of light source is 500 W, and the ultraviolet light source wavelength is 365 nm, and fluorescent tube is 15 cm apart from the sample distance, and nitrogen flow is 10 mL/min.After the irradiation, product being neutral with rinsed with deionized water to pH value, through repeatedly deionization boiling water washing, drying, is solvent Suo Shi extracting 24 h with acetone again, is dried to constant weight, and obtaining the graft copolymerization rate is the polypropylene-base ion chelating fiber of 140 %.
Embodiment 4:
Polypropylene fibre successively water and acetone are embathed, and the impurity such as sand and dust, dirt and oil stain to remove fiber surface are dried to constant weight.In conical flask, add 10 g acrylic acid, 0.1 g N, N-methylene-bisacrylamide (its weight percent concentration is 1.0 % of monomer) and 0.05 g benzophenone (its weight percent concentration is 0.5 % of monomer) adopt ultrasonic oscillation to dissolving.Get above-mentioned reactant liquor 5.0 g and evenly drip on the polypropylene fibre surface after 1.0 g handle, be positioned in the UV-irradiation reactor, the sealing back feeds nitrogen 30 min to get rid of oxygen.Open high voltage mercury lamp radiation 25 min, the power of light source is 500 W, and the ultraviolet light source wavelength is 365 nm, and fluorescent tube is 15 cm apart from the sample distance, and nitrogen flow is 10 mL/min.After the irradiation, product being neutral with rinsed with deionized water to pH value, through repeatedly deionization boiling water washing, drying, is solvent Suo Shi extracting 24 h with acetone again, is dried to constant weight, and obtaining the graft copolymerization rate is the polypropylene-base ion chelating fiber of 150 %.
Embodiment 5:
Polypropylene fibre successively water and acetone are embathed, and the impurity such as sand and dust, dirt and oil stain to remove fiber surface are dried to constant weight.In conical flask, add 10 g acrylic acid, 0.3 g N, N-methylene-bisacrylamide (its weight percent concentration is 3.0 % of monomer) and 0.05 g benzophenone (its weight percent concentration is 0.5 % of monomer) adopt ultrasonic oscillation to dissolving.Get above-mentioned reactant liquor 5.0 g and evenly drip on the polypropylene fibre surface after 1.0 g handle, be positioned in the UV-irradiation reactor, the sealing back feeds nitrogen 30 min to get rid of oxygen.Open high voltage mercury lamp radiation 25 min, the power of light source is 500 W, and the ultraviolet light source wavelength is 365 nm, and fluorescent tube is 15 cm apart from the sample distance, and nitrogen flow is 10 mL/min.After the irradiation, product being neutral with rinsed with deionized water to pH value, through repeatedly deionization boiling water washing, drying, is solvent Suo Shi extracting 24 h with acetone again, is dried to constant weight, and obtaining the graft copolymerization rate is the polypropylene-base ion chelating fiber of 190 %.
Embodiment 6:
Polypropylene fibre successively water and acetone are embathed, and the impurity such as sand and dust, dirt and oil stain to remove fiber surface are dried to constant weight.In conical flask, add 10 g acrylic acid, 0.5 g N, N-methylene-bisacrylamide (its weight percent concentration is 5.0 % of monomer) and 0.05 g benzophenone (its weight percent concentration is 0.5 % of monomer) adopt ultrasonic oscillation to dissolving.Get above-mentioned reactant liquor 5.0 g and evenly drip on the polypropylene fibre surface after 1.0 g handle, be positioned in the UV-irradiation reactor, the sealing back feeds nitrogen 30 min to get rid of oxygen.Open high voltage mercury lamp radiation 25 min, the power of light source is 500 W, and the ultraviolet light source wavelength is 365 nm, and fluorescent tube is 15 cm apart from the sample distance, and nitrogen flow is 10 mL/min.After the irradiation, product being neutral with rinsed with deionized water to pH value, through repeatedly deionization boiling water washing, drying, is solvent Suo Shi extracting 24 h with acetone again, is dried to constant weight, and obtaining the graft copolymerization rate is the polypropylene-base ion chelating fiber of 230 %.
Embodiment 7:
Polypropylene fibre successively water and acetone are embathed, and the impurity such as sand and dust, dirt and oil stain to remove fiber surface are dried to constant weight.In conical flask, add 10 g acrylic acid, 0.5 g N, N-methylene-bisacrylamide (its weight percent concentration is 5.0 % of monomer) and 0.05 g benzophenone (its weight percent concentration is 0.5 % of monomer) adopt ultrasonic oscillation to dissolving.Get above-mentioned reactant liquor 5.0 g and evenly drip on the polypropylene fibre surface after 1.0 g handle, be positioned in the UV-irradiation reactor, the sealing back feeds nitrogen 30 min to get rid of oxygen.Open high voltage mercury lamp radiation 20 min, the power of light source is 500 W, and the ultraviolet light source wavelength is 365 nm, and fluorescent tube is 15 cm apart from the sample distance, and nitrogen flow is 10 mL/min.After the irradiation, product being neutral with rinsed with deionized water to pH value, through repeatedly deionization boiling water washing, drying, is solvent Suo Shi extracting 24 h with acetone again, is dried to constant weight, and obtaining the graft copolymerization rate is the polypropylene-base ion chelating fiber of 200 %.
Claims (5)
1. the polypropylene-base ion chelating fiber preparation method of an Adsorption of Heavy Metal Ions, its preparation method is the ultraviolet surface graft method, it is characterized in that, this method may further comprise the steps:
(1) polypropylene fibre successively water and acetone are embathed, the impurity such as sand and dust, dirt and oil stain to remove fiber surface are dried to constant weight;
(2) preparation of ultraviolet surface graft reactant liquor: in conical flask, add function monomer, crosslinking agent; Its weight percent concentration is 0.5 % ~ 10 % of monomer; Add light trigger, its weight percent concentration is 0.1 % ~ 1.0 % of monomer, adopts ultrasonic oscillation to dissolving;
(3) UV-irradiation graft reaction: in proportion above-mentioned reactant liquor is evenly dripped on the polypropylene fibre surface, be positioned in the UV-irradiation reactor, the sealing back feeds nitrogen 30 min to get rid of oxygen; Open high voltage mercury lamp radiation 5～25 min, the power of light source is 500 W, and the ultraviolet light source wavelength is 365 nm; Fluorescent tube is 5～25 cm apart from the sample distance; Nitrogen flow is 10～30 mL/min, after the irradiation, product is neutral with rinsed with deionized water to pH value; Through the washing of deionization boiling water, drying; Be solvent Suo Shi extracting 24 h again with acetone, be dried to constant weight, obtain the polypropylene-base ion chelating fiber that the surface has high-load ion chelating group.
2. the polypropylene-base ion chelating fiber preparation method of a kind of Adsorption of Heavy Metal Ions according to claim 1 is characterized in that, the macromolecule matrix material is that the polypropylene fibre of processing is sprayed in fusion.
3. the polypropylene-base ion chelating fiber preparation method of a kind of Adsorption of Heavy Metal Ions according to claim 1 is characterized in that function monomer is an acrylic acid, and its weight percent concentration is 10 % ~ 500 % of polypropylene fibre matrix.
4. the polypropylene-base ion chelating fiber preparation method of a kind of Adsorption of Heavy Metal Ions according to claim 1 is characterized in that, light trigger is a benzophenone, and its weight percent concentration is 0.1 % ~ 1.0 % of monomer.
5. the polypropylene-base ion chelating fiber preparation method of a kind of Adsorption of Heavy Metal Ions according to claim 1; It is characterized in that; In the UV-irradiation graft reaction, add the crosslinking agent that improves product graft copolymerization rate; Crosslinking agent is N, the N-methylene-bisacrylamide, and its weight percent concentration is 0.5 % ~ 10 % of monomer.
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| CN104611926A (en) * | 2014-12-30 | 2015-05-13 | 中国地质大学（武汉） | Method for preparing ion exchange fiber by ultraviolet grafting |
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| CN104611926A (en) * | 2014-12-30 | 2015-05-13 | 中国地质大学（武汉） | Method for preparing ion exchange fiber by ultraviolet grafting |
| CN104594037A (en) * | 2014-12-30 | 2015-05-06 | 中国地质大学（武汉） | Method for preparing graft polypropylene non-woven fabric-based ion-exchange material |
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| CN106215910A (en) * | 2016-05-25 | 2016-12-14 | 马鞍山中创环保科技有限公司 | A kind of preparation method of acid cation exchange fiber |
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| CN113263805B (en) * | 2021-01-07 | 2023-08-11 | 湖南盛业土工材料制造有限公司 | Heavy metal-blocking fiber net/high polymer composite waterproof coiled material and preparation method thereof |
| CN113171762A (en) * | 2021-04-27 | 2021-07-27 | 重庆科技学院 | Fiber-based adsorption material, preparation method thereof and application of recovered palladium |
| CN113171762B (en) * | 2021-04-27 | 2023-02-24 | 重庆科技学院 | Fiber-based adsorption material, preparation method thereof and application of recovered palladium |
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