CN106049047B - A kind of preparation method of sodium alginate-polypropylene functionalization heavy metal adsorption fiber - Google Patents
A kind of preparation method of sodium alginate-polypropylene functionalization heavy metal adsorption fiber Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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
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- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
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- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
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- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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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
- C02F2101/00—Nature of the contaminant
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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Abstract
The present invention discloses a kind of preparation method of sodium alginate-polypropylene functionalization heavy metal adsorption fiber comprising the steps of: by matrix material, ultrasound blending forms polymer solution in a suitable solvent；A nanometer heavy metal fiber adsorbing material is made in the polymer solution prepared by method of electrostatic spinning；This nanometer of heavy metal fiber adsorbing material is subjected to functionalization, functionalization operation step are as follows: in round-bottomed flask, NaOH solution is added, dissolves sodium hydroxide under stirring, is cooled to room temperature；With ice-water bath control system temperature, the nanometer heavy metal fiber adsorbing material prepared is added, carbon disulfide is added dropwise under stiring；It is gradually warmed up after completion of dropwise addition, washs fibrous material repeatedly with distilled water later.Operation of the present invention is easy, safety, and prepared fibrous material has diameter small, and porosity and large specific surface area, the advantage strong to heavy metal ion adsorbed ability have a good application prospect in terms of environmental improvement, purification of water quality.
Description
Technical field
The present invention relates to a kind of preparation method of fibrous material, in particular to a kind of adsorbing heavy metal in water functional fiber
Preparation method, specifically a kind of sodium alginate-polypropylene functionalization heavy metal adsorption fiber preparation method.
Background technique
Environmental pollution mainly includes atmosphere pollution, water pollution, noxious waste pollution, noise pollution.And heavy metal both may be used
To be directly entered atmosphere, water body and soil, the direct pollution of all kinds of environmental elements is caused；It can also be in atmosphere, water body and soil
In mutually migrate, cause the indirect pollution of all kinds of environmental elements.Since heavy metal cannot be degraded by microorganisms, in the environment can only
Mutually converting between various forms occurs, so, the elimination of heavy metal pollution is frequently more difficult, influences on caused by biology
It is also the problem of people more pay close attention to harm.With the continuous development of China's process of industrialization, the environment negative effect of generation
It can not be ignored.
Currently, heavy metal processing is handled mainly by adsorption method, traditional adsorbent material is in processing capacity, desorption etc.
Aspect has very big deficiency.Ion-exchange fibre is a kind of fibrous ion exchange material, itself containing fixed ion and and
The opposite movable ion of fixed ion symbol, when being in contact with the solution that can dissociate compound, movable ion can be with solution
The ion of middle the same symbol swaps, and generally using various chemical synthetic materials as matrix, converts or is grafted through macromolecular chemistry
The novel functional fiber material of one kind obtained from reaction.Ion-exchange fibre is opened on the basis of amberlite fat prod
The function new material with certain characteristics of hair.The mechanism of action of the two is the same, is all that the zwitterion on group rises
Exchange interaction, resin be usually it is spherical, generally between 0.3~1.5mm, fiber is amorphous more the partial size of resin of industry
It is smaller, it may be said that the adaptable field of ion exchange resin, ion-exchange fibre can preferably substitutional ion exchanges
Resin.
The large specific surface area that has due to ion-exchange fibre and can also in different forms (such as non-woven fabrics, film etc.)
It applies in practice, in certain ion exchange resin using difficult field, ion-exchange fibre has unique advantage.Cause
This, develops novel functionalization ion-exchange fibre for having a very important significance in terms of environmental improvement.
Summary of the invention
The present invention is directed to the problem of existing heavy metal processing technique and deficiency, provides a kind of sodium alginate-poly- third
The preparation method of olefinic functionality heavy metal adsorption fiber, the sodium alginate that the present invention prepares-polypropylene fiber material diameter exist
10~800ppm, specific surface area reach 2000m2Then/g carries out activation and graft reaction on the surface layer of fibrous material, is not related to
The inside of fibrous material；The preparation method is simple to operation, and obtained functionalization adsorbing fiber holds the exchange of heavy metal ion
Amount is big.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of sodium alginate-polypropylene functionalization heavy metal adsorption fiber, the preparation method include following
Step:
(1) by matrix material, ultrasound blending forms polymer solution in a solvent；
(2) polymer solution prepared is made by a nanometer heavy metal fiber adsorbing material by method of electrostatic spinning；
(3) this nanometer of heavy metal fiber adsorbing material is subjected to functionalization.
Matrix material described in step (1) is sodium alginate, polypropylene, polyvinylpyrrolidone.
Solvent described in step (1) in methanol, formic acid, ethyl alcohol, acetic acid, tetrahydrofuran, propyl alcohol, isopropanol one
The mixed solvent of kind or above-mentioned solution.
Sodium alginate quality described in step (1) is the 15.21%~28.50% of polymer blend solution quality, is gathered
Vinylpyrrolidone quality is the 5.16%~15.35% of polymer blend solution quality, and polypropylene is polymer blend solution
The 20.65%~35.25% of quality.
Nanometer heavy metal fiber adsorbing material described in step (3) carries out functionalization operation, and steps are as follows:
(1) in round-bottomed flask, NaOH solution is added, dissolves sodium hydroxide under stirring, is cooled to room temperature；
(2) use ice-water bath control system temperature, the nanometer heavy metal fiber adsorbing material prepared is added, under stiring by
It is added dropwise to carbon disulfide；
(3) it is gradually warmed up after completion of dropwise addition, insulation reaction 2h, washing fibrous material repeatedly with distilled water later can be obtained
Functionalization heavy metal adsorption fibrous material.
The mass fraction of above-mentioned NaOH solution is 5.0%~16.5%；Nanometer heavy metal fiber adsorbing material quality be
The 0.2%~1.0% of NaOH solution quality, the carbon disulfide quality of dropwise addition are the 8%~16% of NaOH solution quality；Heat preservation temperature
Degree is 30~45 DEG C.
Above-mentioned functionalization heavy metal adsorption fibrous material diameter is small, and porosity and specific surface area are larger, and fibre diameter 10~
800ppm；Functionalization heavy metal adsorption fibrous material has good absorption property for heavy metal ion.
Beneficial effects of the present invention: the present invention, which prepares sodium alginate and polypropylene mixed solution by method of electrostatic spinning, to be had
There is sodium alginate-polypropylene composite materials fiber of heavy metal ion adsorbed function, functional modification then carried out to the composite fibre,
The fiber has good adsorption effect for heavy metal ion in water.
Specific embodiment
Illustrate the present invention below by way of specific embodiment, but the present invention is not only limited to these embodiments, it is all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on should be included in protection scope of the present invention it
It is interior.
Embodiment 1
Sodium alginate 4.0g, polypropylene 3.0g, polyvinylpyrrolidone 0.5g are taken, the acetic acid water of 100ml 30% is added to
In solution, it is ultrasonically formed blending and forms uniform polymer solution, as electrostatic spinning solution；
Above-mentioned sodium alginate-Polypropylene copolymer solution (i.e. polymer solution, similarly hereinafter) is made using electrostatic spinning apparatus
Nanofiber (i.e. nanometer heavy metal fiber adsorbing material, similarly hereinafter)；
Method of electrostatic spinning specific steps and parameter are as follows: in electrostatic spinning, the polymer solution of above-mentioned preparation is placed in note
In emitter, the positive connecting needle of HV generator, cathode is connected on clean bare electrode, voltage 15V, syringe needle with
Electrode distance 15cm is applied directly to injection by the high-pressure electrostatic that HV generator generates using micro-injection pump feed flow
On device syringe needle, collecting nanofibers are on bare electrode；Environment temperature is 20~25 DEG C, and humid control is in 30~40% (Static Spinnings
Knit step and parameter similarly hereinafter)；
This nanometer of heavy metal fiber adsorbing material is subjected to functionalization: first in 100mL round-bottomed flask, 2.4g is added
NaOH and 20mL distilled water dissolves sodium hydroxide under stirring, is cooled to room temperature, and with ice-water bath control system temperature at 0 DEG C, adds
Enter 0.1g cross filament film (i.e. nanometer heavy metal fiber adsorbing material, similarly hereinafter), then 2.4mL carbon disulfide is added dropwise, is added dropwise
After be gradually heated to 35 DEG C, insulation reaction 2h washs tunica fibrosa with distilled water repeatedly, be dried under vacuum to constant weight at 45 DEG C,
Obtain sodium alginate-polypropylene functionalization heavy metal adsorption fiber.
Embodiment 2
Sodium alginate 4.0g, polypropylene 2.0g, polyvinylpyrrolidone 0.5g are taken, the acetic acid water of 100ml 30% is added to
In solution, it is ultrasonically formed blending and forms uniform polymer solution, as electrostatic spinning solution；Using electrostatic spinning apparatus by seaweed
Nanofiber is made in sour sodium-Polypropylene copolymer solution；In 100mL round-bottomed flask, 2.4g NaOH and 20mL distilled water is added,
Sodium hydroxide is dissolved under stirring, is cooled to room temperature, with ice-water bath control system temperature, is added 0.1g cross filament film, then by
It is added dropwise to 2.4mL carbon disulfide, 35 DEG C are gradually heated to after completion of dropwise addition, insulation reaction 2h washs fiber with distilled water repeatedly
Film is dried under vacuum to constant weight at 45 DEG C to get sodium alginate-polypropylene functionalization heavy metal adsorption fiber is arrived.
Embodiment 3
Sodium alginate 4.0g, polypropylene 3.0g, polyvinylpyrrolidone 0.6g are taken, the acetic acid water of 100ml 30% is added to
In solution, it is ultrasonically formed blending and forms uniform polymer solution, as electrostatic spinning solution；Using electrostatic spinning apparatus by seaweed
Nanofiber is made in sour sodium-Polypropylene copolymer solution；In 100mL round-bottomed flask, 2.0g NaOH and 20mL distilled water is added,
Sodium hydroxide is dissolved under stirring, is cooled to room temperature, with ice-water bath control system temperature, is added 0.1g cross filament film, then by
It is added dropwise to 2.4mL carbon disulfide, 35 DEG C are gradually heated to after completion of dropwise addition, insulation reaction 2h washs fiber with distilled water repeatedly
Film is dried under vacuum to constant weight at 45 DEG C to get sodium alginate-polypropylene functionalization heavy metal adsorption fiber is arrived.
Embodiment 4
Sodium alginate 4.0g, polypropylene 3.0g, polyvinylpyrrolidone 0.5g are taken, the acetic acid water of 100ml 30% is added to
In solution, it is ultrasonically formed blending and forms uniform polymer solution, as electrostatic spinning solution；Using electrostatic spinning apparatus by seaweed
Nanofiber is made in sour sodium-Polypropylene copolymer solution；In 100mL round-bottomed flask, 2.4g NaOH and 20mL distilled water is added,
Sodium hydroxide is dissolved under stirring, is cooled to room temperature, with ice-water bath control system temperature, is added 0.1g cross filament film, then by
It is added dropwise to 2.4mL carbon disulfide, 30 DEG C are gradually heated to after completion of dropwise addition, insulation reaction 2h washs fiber with distilled water repeatedly
Film is dried under vacuum to constant weight at 45 DEG C to get sodium alginate-polypropylene functionalization heavy metal adsorption fiber is arrived.
Embodiment 5
Sodium alginate 4.0g, polypropylene 3.0g, polyvinylpyrrolidone 0.5g are taken, the acetic acid water of 100ml 30% is added to
In solution, it is ultrasonically formed blending and forms uniform polymer solution, as electrostatic spinning solution；Using electrostatic spinning apparatus by seaweed
Nanofiber is made in sour sodium-Polypropylene copolymer solution；In 100mL round-bottomed flask, 2.4g NaOH and 20mL distilled water is added,
Sodium hydroxide is dissolved under stirring, is cooled to room temperature, with ice-water bath control system temperature, is added 0.1g cross filament film, then by
It is added dropwise to 3.0mL carbon disulfide, 40 DEG C are gradually heated to after completion of dropwise addition, insulation reaction 2h washs fiber with distilled water repeatedly
Film is dried under vacuum to constant weight at 45 DEG C to get sodium alginate-polypropylene functionalization heavy metal adsorption fiber is arrived.
Embodiment 6
Sodium alginate 4.0g, polypropylene 3.0g are taken, polyvinylpyrrolidone 0.8g is added to the ethanol water of 100ml 30%
In solution, it is ultrasonically formed blending and forms uniform polymer solution, as electrostatic spinning solution；Using electrostatic spinning apparatus by seaweed
Nanofiber is made in sour sodium-Polypropylene copolymer solution；In 100mL round-bottomed flask, 2.4g NaOH and 20mL distilled water is added,
Sodium hydroxide is dissolved under stirring, is cooled to room temperature, with ice-water bath control system temperature, is added 0.1g cross filament film, then by
It is added dropwise to 2.4mL carbon disulfide, 35 DEG C are gradually heated to after completion of dropwise addition, insulation reaction 2h washs fiber with distilled water repeatedly
Film is dried under vacuum to constant weight at 45 DEG C to get sodium alginate-polypropylene functionalization heavy metal adsorption fiber is arrived.
Operation of the present invention is easy, safety, and prepared fibrous material has diameter small, porosity and specific surface area
Greatly, the advantage strong to heavy metal ion adsorbed ability, has a good application prospect in terms of environmental improvement, purification of water quality.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to being retouched
The specific embodiment stated does various modifications or additions or is substituted in a similar manner, and without departing from invention or surpasses
More range defined in the claims, is within the scope of protection of the invention.
Claims (5)
1. a kind of sodium alginate-polypropylene functionalization heavy metal adsorption fiber preparation method, which is characterized in that the preparation method
It comprises the steps of:
(1) by matrix material, ultrasound blending forms polymer solution in a solvent；
(2) polymer solution prepared is made by a nanometer heavy metal fiber adsorbing material by method of electrostatic spinning；
(3) this nanometer of heavy metal fiber adsorbing material is subjected to functionalization；
Matrix material described in step (1) is sodium alginate, polypropylene, polyvinylpyrrolidone, the seaweed
Sour sodium quality is the 15.21%~28.50% of polymer blend solution quality, and polyvinylpyrrolidone quality is polymer blend
The 5.16%~15.35% of solution quality, polypropylene are the 20.65%~35.25% of polymer blend solution quality；
Nanometer heavy metal fiber adsorbing material described in step (3) carries out functionalization operation, and steps are as follows:
(1) in round-bottomed flask, NaOH solution is added, dissolves sodium hydroxide under stirring, is cooled to room temperature；
(2) ice-water bath control system temperature is used, the nanometer heavy metal fiber adsorbing material prepared is added, is added dropwise under stiring
Enter carbon disulfide；
(3) it is gradually warmed up after completion of dropwise addition, insulation reaction 2h, washing fibrous material repeatedly with distilled water later can be obtained function
Change heavy metal adsorption fibrous material.
2. a kind of sodium alginate according to claim 1-polypropylene functionalization heavy metal adsorption fiber preparation method,
It is characterized in that, solvent described in step (1) is in methanol, formic acid, ethyl alcohol, acetic acid, tetrahydrofuran, propyl alcohol, isopropanol
A kind of mixed solvent of or above-mentioned solution.
3. a kind of sodium alginate according to claim 1-polypropylene functionalization heavy metal adsorption fiber preparation method,
It is characterized in that, the mass fraction of the NaOH solution is 5.0%~16.5%.
4. a kind of sodium alginate according to claim 1-polypropylene functionalization heavy metal adsorption fiber preparation method,
It is characterized in that, the quality of the nanometer heavy metal fiber adsorbing material is the 0.2%~1.0% of NaOH solution quality, is added dropwise
Carbon disulfide quality be the 8%~16% of NaOH solution quality.
5. a kind of sodium alginate according to claim 1-polypropylene functionalization heavy metal adsorption fiber preparation method,
It is characterized in that, the holding temperature is 30~45 DEG C.
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| CN109351350A (en) * | 2018-12-27 | 2019-02-19 | 安徽工业大学 | A kind of method that emulsion polymerization prepares sodium alginate micro ball adsorbent |
| CN110124636B (en) * | 2019-05-29 | 2022-07-26 | 太仓市洪宇新材料科技有限公司 | Magnetic nanofiber material for textile industry wastewater treatment |
| CN110592808B (en) * | 2019-09-02 | 2020-11-24 | 中科纺织研究院（青岛）有限公司 | Alga modified PP spunbonded non-woven fabric |
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