CN111233347A - Method for modifying basalt fiber carrier through ultraviolet light grafting - Google Patents
Method for modifying basalt fiber carrier through ultraviolet light grafting Download PDFInfo
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- CN111233347A CN111233347A CN202010134275.XA CN202010134275A CN111233347A CN 111233347 A CN111233347 A CN 111233347A CN 202010134275 A CN202010134275 A CN 202010134275A CN 111233347 A CN111233347 A CN 111233347A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
- C03C13/06—Mineral fibres, e.g. slag wool, mineral wool, rock wool
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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
- C02F2203/00—Apparatus and plants for the biological treatment of water, waste water or sewage
- C02F2203/006—Apparatus and plants for the biological treatment of water, waste water or sewage details of construction, e.g. specially adapted seals, modules, connections
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Abstract
The invention relates to a method for modifying a basalt fiber carrier by ultraviolet light grafting. Immersing the basalt fiber pretreated by acetone into an ethanol water solution of a silane coupling agent KH550, performing ultrasonic coating for a certain time, and taking out and drying; dissolving an initiator and a monomer in a solvent according to a certain proportion to prepare a reaction solution; the basalt fiber with the coated surface is subjected to ultraviolet pre-radiation, then is immersed in a quartz beaker filled with reaction solution, is subjected to ultraviolet secondary radiation for a certain time under the condition of introducing nitrogen, is taken out, is washed by deionized water and is dried, and the modified basalt fiber carrier can be obtained. According to the method, the surface of the basalt fiber is treated by utilizing ultraviolet pre-radiation firstly, surface chemical bonds of the basalt fiber are damaged, active sites are increased, and then graft polymerization is initiated by ultraviolet secondary radiation induction, so that the hydrophilicity and the biocompatibility of the basalt fiber are enhanced, the load capacity of microorganisms is increased, and the effect of the basalt fiber carrier for purifying sewage and wastewater is improved.
Description
Technical Field
The invention belongs to the field of sewage and wastewater and the field of microbial carrier materials, relates to a surface modification method of a basalt fiber carrier, and particularly relates to a method for initiating polymerization and grafting a polymer chain on the surface of basalt fiber through ultraviolet induction.
Background
The basalt fiber is a green and environment-friendly high-performance inorganic fiber, is one of four major fibers which are mainly developed by China, is widely applied to the fields of aerospace, war industry, automobile and ship manufacturing, engineering plastics, buildings and the like, and has great advantages and potential markets in the field of environmental protection at present. Application of Jiangxian and the like (Jiangxian, Wuchuu, Wu Chi ren, et al. basalt fiber filler in wastewater treatment [ J]Carrying out a film formation comparison experiment on basalt fiber filler, elastic filler and combined filler by an inoculation sludge method, wherein the result shows that the film formation speed of the basalt fiber is fastest, and the total biomass of the biological film is 90-150 kg/m after short-term culture for 7d3The removal rate of COD can reach 85.3 percent, which is superior to that of elastic filler and combined filler. Chinese patent 'a basalt fiber carrier for water treatment' (CN202953860U) also mentions that the basalt fiber carrier can effectively improve the surface area of the carrier required by attachment of a microbial biofilm in unit volume, and greatly improve the effect of sewage treatment. Therefore, the basalt fiber has been developed into a novel microorganism carrier to be applied to sewage and wastewater treatment. However, the basalt fiber is an inorganic fiber, has no hydrophilic functional group on the surface, and belongs to a hydrophobic material, so that the surface of the basalt fiber needs to be modified before being put into application.
A method for improving the surface performance of fibers by introducing various functional groups on the surfaces of the fibers through graft polymerization is a common method at home and abroad. The ultraviolet light initiated surface grafting is simple and efficient, and compared with other irradiation grafting methods, the method has the following advantages: 1) because of the poor penetration of ultraviolet light to the substrate, grafting can be strictly limited to the substrate surface or subsurface; 2) the controllability of the reaction degree is strong; 3) the ultraviolet generating device has low cost, simple and convenient operation and easy continuous production.
According to the invention, firstly, a silane coupling agent is coated on the surface of the basalt fiber, a photosensitive gene is introduced, then, the ultraviolet irradiation is used for inducing the graft polymerization of acrylamide on the surface of the basalt fiber, and a hydrophilic functional group is introduced, so that the hydrophilicity of the basalt fiber is improved.
Disclosure of Invention
The technical problem is as follows: aiming at the defects of the prior art, the invention aims to provide a preparation method of an ultraviolet grafting modified basalt fiber carrier, which obtains the basalt fiber with high performance through simple processes of pretreatment, surface coating, reaction solution preparation, ultraviolet grafting and the like, loads more biomass and improves the sewage purification effect.
The technical scheme is as follows: in order to solve the technical problem, the method for grafting and modifying the basalt fiber carrier by using the ultraviolet light comprises the following steps:
step 1, pretreatment: immersing basalt fibers into acetone, cleaning for 1-3 h under the action of ultrasonic waves to remove impurities added on the surface in the production process, repeatedly washing the basalt fibers with distilled water for many times after taking out, and drying the basalt fibers at 105-120 ℃ for later use;
step 2, surface coating: firstly, preparing a surface coating solution, preparing a 5-10% ethanol water solution, adding acetic acid to adjust the pH to 4.5-5.5, stirring, and adding into a silane coupling agent KH550 solution to prepare the surface coating solution; immersing the basalt fibers treated in the step 1 in the surface coating solution, putting the basalt fibers into ultrasonic waves for coating for 1 hour, taking out the basalt fibers, and drying the basalt fibers at 105-120 ℃ for later use;
step 3, reaction solution preparation: dissolving an initiator and a monomer in a solvent to prepare a reaction solution; the initiator is benzophenone, the monomer is acrylamide, and the solvent is a mixed solution of acetone and ethanol;
step 4, ultraviolet grafting: carrying out ultraviolet pre-radiation on the basalt fibers obtained in the step 2, wherein the radiation time is 30-40 min; then placing the pre-radiated basalt fibers into a quartz beaker filled with the reaction solution prepared in the step (3), introducing nitrogen for 10-20 min to fully remove oxygen in the system, and then placing under an ultraviolet lamp for secondary ultraviolet radiation, wherein the radiation time is 25-35 min; finally, taking out the basalt fiber, cleaning the basalt fiber with deionized water, and drying the basalt fiber at the temperature of 40-50 ℃ for later use.
Wherein:
the concentration mass fraction of the silane coupling agent KH550 solution in the step 2 is 20%.
In the step 3, the solvent is a mixed solution of acetone and ethanol, and the volume ratio of the acetone to the ethanol is 3: 2.
In the step 3, the mass ratio of the benzophenone to the solvent is 1: 100-1: 200, wherein the mass ratio of acrylamide to a solvent is 1: 5-1: 10.
The ultraviolet pre-radiation time in the step 4 is preferably 35 min; the ultraviolet secondary radiation time is preferably 30 min.
Has the advantages that: according to the modification method of the basalt fiber carrier disclosed by the invention, ultraviolet irradiation is utilized to induce and initiate the graft polymerization of acrylamide on the surface of the basalt fiber, and a hydrophilic functional group is introduced, so that the hydrophilicity of the basalt fiber is improved, more microorganisms are loaded, and the effect of applying the basalt fiber as the carrier to sewage and wastewater purification is enhanced. In addition, the ultraviolet light grafting has simple operation, short reaction time, small environmental pollution and mature free radical polymerization grafting reaction mechanism, and the method has wide industrial application prospect.
Drawings
FIG. 1 is electron microscope scanning images of basalt fiber carriers before and after modification, wherein (a) is before modification and (b) is after modification.
FIG. 2 is a diagram showing the filming effect of the modified basalt fiber carrier, wherein (a) is before modification and (b) is after modification.
Detailed Description
The invention is further described below with reference to specific examples:
example 1
(1) Weighing 40g of basalt fiber, immersing the basalt fiber into 500ml of acetone solution, putting the basalt fiber into an ultrasonic cleaning instrument for cleaning for 2 hours, taking out the basalt fiber, repeatedly cleaning the basalt fiber with deionized water, and putting the basalt fiber into a 105 ℃ drying oven for drying;
(2) preparing a surface coating solution, preparing a 5% ethanol water solution, adding acetic acid to adjust the pH value to 4.5-5.5, stirring, and adding the mixture into a 20% silane coupling agent KH550 solution. Immersing the basalt fibers obtained in the step (1) in a surface coating solution, putting the basalt fibers into ultrasonic waves for coating for 1h, taking out the basalt fibers, and drying the basalt fibers at 105 ℃ for later use;
(3) preparing a reaction solution, dissolving benzophenone and acrylamide in a solvent, wherein the solvent is a mixed solution of acetone and ethanol (3:2), the mass ratio of the benzophenone to the solvent is 1:200, and the mass ratio of the acrylamide to the solvent is 1: 10;
(4) and (3) carrying out ultraviolet pre-radiation on the basalt fibers obtained in the step (2), wherein the radiation time is 30-40 min. (ii) a
(5) And (3) putting the basalt fibers pre-radiated in the step (4) into a quartz beaker filled with the reaction solution prepared in the step (3), introducing nitrogen for 10min to fully remove oxygen in the system, and then putting the quartz beaker under an ultraviolet lamp for secondary ultraviolet radiation, wherein the radiation time is 25-35 min. And finally, taking out the basalt fiber, cleaning the basalt fiber with deionized water, and drying the basalt fiber at the temperature of 40-50 ℃ for later use to prepare the maleic anhydride liquid-phase grafted basalt fiber carrier (MBF-1).
Example 2
(1) Weighing 40g of basalt fiber, immersing the basalt fiber into 500ml of acetone solution, putting the basalt fiber into an ultrasonic cleaning instrument for cleaning for 2 hours, taking out the basalt fiber, repeatedly cleaning the basalt fiber with deionized water, and putting the basalt fiber into a 105 ℃ drying oven for drying;
(2) preparing a reaction solution, dissolving benzophenone and acrylamide in a solvent, wherein the solvent is a mixed solution of acetone and ethanol (3:2), the mass ratio of the benzophenone to the solvent is 1:200, and the mass ratio of the acrylamide to the solvent is 1: 10;
(3) and (2) carrying out ultraviolet pre-radiation on the basalt fibers obtained in the step (1), wherein the radiation time is 30-40 min. (ii) a
(4) Putting the basalt fiber pre-radiated in the step (3) into a quartz beaker filled with the reaction solution prepared in the step (2), introducing nitrogen for 10min to fully remove oxygen in the system, and then putting the quartz beaker under an ultraviolet lamp for secondary ultraviolet radiation, wherein the radiation time is 25-35 min. And finally, taking out the basalt fiber, cleaning the basalt fiber with deionized water, and drying the basalt fiber at the temperature of 40-50 ℃ for later use to prepare the maleic anhydride liquid-phase grafted basalt fiber carrier (MBF-2).
The experimental results are as follows:
1. scanning Electron Microscopy (SEM) analysis:
as shown in figure 1, the surface of the basalt fiber carrier before modification is smooth and almost contains no impurities, and the basalt fiber carrier after ultraviolet grafting can clearly see polymers attached to the surface of the basalt fiber, so that the surface roughness of the basalt fiber is increased, the attachment of microorganisms is facilitated, and the load of microorganisms is increased.
2. And (3) analyzing the film forming performance:
TABLE 1 comparison of the biofilm formation effects of basalt fiber carriers before and after modification
As can be seen from the table 1, the attachment performance of microorganisms on the surface of the basalt fiber carrier after ultraviolet grafting is improved to a certain extent, and the film forming rate is remarkably improved compared with that of unmodified basalt fiber, and especially MBF-1 in the market indicates that the attachment amount of the microorganisms on the surface of the basalt fiber carrier modified by the method is increased, the sewage/wastewater purification effect can be improved to a certain extent, while the residual film forming rate of MBF-2 is higher than that of MBF-1, which indicates that the microorganisms of MBF-2 can be attached for a longer time.
Evaluation of amount of microorganism attached:
modified and unmodified basalt fibers are made into fiber bundles, and the fiber bundles are put into a contact oxidation reaction device (5L) for a biofilm culturing experiment. The water is artificially synthesized sewage, sodium acetate is used as a carbon source, ammonium sulfate is used as a nitrogen source, and dipotassium hydrogen phosphate is used as a phosphorus source, wherein the COD (chemical oxygen demand) N and P are 100:5: 1. Inoculating sludge is taken from a sewage treatment plant (MLSS is 8000mg/L) in Jiangning development area, continuously aerating for 72h, taking out, recording a macroscopic topography of microorganisms fixed on the surface of the basalt fiber carrier, and measuring the biofilm formation rate and the residual biofilm formation rate.
1) Film forming rate: and taking out the basalt fiber carrier, and drying to constant weight.
Wherein: w0: the original weight (g) of basalt fiber; w1: the sum (g) of the mass of basalt fibers and microorganisms after a certain period of time of fixing the microorganisms.
2) Residual film forming rate: and taking out the basalt fiber carrier, immersing the basalt fiber carrier into a standard PBS buffer solution, putting the basalt fiber carrier and the standard PBS buffer solution into an ultrasonic oscillator at room temperature, oscillating the basalt fiber carrier and the standard PBS buffer solution for 20min at the power of 30w, slowly washing the basalt fiber carrier by using distilled water, and drying the basalt fiber carrier to constant weight.
Wherein: w2: (g) mass sum of basalt fiber and microorganism after ultrasonic oscillation.
Further, the standard PBS buffer described in 2) was 8.5g/L sodium chloride, 2.28.5g/L disodium hydrogenphosphate, 0.48.5g/L sodium dihydrogenphosphate, and pH 7.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (5)
1. A method for modifying a basalt fiber carrier by ultraviolet light grafting is characterized by comprising the following steps:
step 1, pretreatment: immersing basalt fibers into acetone, cleaning for 1-3 h under the action of ultrasonic waves to remove impurities added on the surface in the production process, repeatedly washing the basalt fibers with distilled water for many times after taking out, and drying the basalt fibers at 105-120 ℃ for later use;
step 2, surface coating: firstly, preparing a surface coating solution, preparing a 5-10% ethanol water solution, adding acetic acid to adjust the pH to 4.5-5.5, stirring, and adding into a silane coupling agent KH550 solution to prepare the surface coating solution; immersing the basalt fibers treated in the step 1 in the surface coating solution, putting the basalt fibers into ultrasonic waves for coating for 1 hour, taking out the basalt fibers, and drying the basalt fibers at 105-120 ℃ for later use;
step 3, reaction solution preparation: dissolving an initiator and a monomer in a solvent to prepare a reaction solution; the initiator is benzophenone, the monomer is acrylamide, and the solvent is a mixed solution of acetone and ethanol;
step 4, ultraviolet grafting: carrying out ultraviolet pre-radiation on the basalt fibers obtained in the step 2, wherein the radiation time is 30-40 min; then placing the pre-radiated basalt fibers into a quartz beaker filled with the reaction solution prepared in the step (3), introducing nitrogen for 10-20 min to fully remove oxygen in the system, and then placing under an ultraviolet lamp for secondary ultraviolet radiation, wherein the radiation time is 25-35 min; finally, taking out the basalt fiber, cleaning the basalt fiber with deionized water, and drying the basalt fiber at the temperature of 40-50 ℃ for later use.
2. The method for grafting and modifying the basalt fiber carrier by using the ultraviolet light as claimed in claim 1, wherein the method comprises the following steps: the concentration mass fraction of the silane coupling agent KH550 solution in the step 2 is 20%.
3. The method for grafting and modifying the basalt fiber carrier by using the ultraviolet light as claimed in claim 1, wherein the method comprises the following steps: in the step 3, the solvent is a mixed solution of acetone and ethanol, and the volume ratio of the acetone to the ethanol is 3: 2.
4. The method for grafting and modifying the basalt fiber carrier by using the ultraviolet light as claimed in claim 1, wherein the method comprises the following steps: in the step 3, the mass ratio of the benzophenone to the solvent is 1: 100-1: 200, wherein the mass ratio of acrylamide to a solvent is 1: 5-1: 10.
5. The method for grafting and modifying the basalt fiber carrier by using the ultraviolet light as claimed in claim 1, wherein the method comprises the following steps: the ultraviolet pre-radiation time in the step 4 is preferably 35 min; the ultraviolet secondary radiation time is preferably 30 min.
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| CN107200867A (en) * | 2017-06-15 | 2017-09-26 | 中北大学 | Basalt fibre nano surface coats the preparation method and application of multi-scale reinforcing body |
| CN109053040A (en) * | 2018-07-17 | 2018-12-21 | 枞阳县天筑新型建筑材料有限公司 | A kind of preparation process of the conductive epoxy bituminous concrete of basalt fiber and carbon fiber enhancing |
| CN110818958A (en) * | 2019-10-16 | 2020-02-21 | 安徽华烨特种材料有限公司 | Basalt fiber rubber composite material and preparation method thereof |
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- 2020-03-02 CN CN202010134275.XA patent/CN111233347B/en active Active
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| CN102701602A (en) * | 2012-06-12 | 2012-10-03 | 常州大学 | Method for initiating graft polymer through ultraviolet induction on surface of glass |
| CN104830057A (en) * | 2015-05-12 | 2015-08-12 | 浙江镜湖建设集团有限公司 | Preparation method of heat-resistant polyamide-base composite material |
| CN107200867A (en) * | 2017-06-15 | 2017-09-26 | 中北大学 | Basalt fibre nano surface coats the preparation method and application of multi-scale reinforcing body |
| CN109053040A (en) * | 2018-07-17 | 2018-12-21 | 枞阳县天筑新型建筑材料有限公司 | A kind of preparation process of the conductive epoxy bituminous concrete of basalt fiber and carbon fiber enhancing |
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