CN109336249B - Phase-change modified porous polyvinyl alcohol particle filler, preparation method thereof and application thereof in low-temperature environment sewage denitrification - Google Patents
Phase-change modified porous polyvinyl alcohol particle filler, preparation method thereof and application thereof in low-temperature environment sewage denitrification Download PDFInfo
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- CN109336249B CN109336249B CN201811282296.5A CN201811282296A CN109336249B CN 109336249 B CN109336249 B CN 109336249B CN 201811282296 A CN201811282296 A CN 201811282296A CN 109336249 B CN109336249 B CN 109336249B
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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
- C02F3/02—Aerobic processes
- C02F3/10—Packings; Fillings; Grids
- C02F3/105—Characterized by the chemical composition
- C02F3/108—Immobilising gels, polymers or the like
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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
- C02F3/02—Aerobic processes
- C02F3/10—Packings; Fillings; Grids
- C02F3/104—Granular carriers
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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
- C02F3/02—Aerobic processes
- C02F3/12—Activated sludge processes
- C02F3/1236—Particular type of activated sludge installations
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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
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
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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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/163—Nitrates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
Abstract
The invention provides a phase-change modified porous polyvinyl alcohol particle filler, a preparation method thereof and application thereof in sewage denitrification in a low-temperature environment, comprising the following steps: mixing expanded graphite and a phase-change material, heating until the mixture is completely melted, and then carrying out spray cooling to obtain a paraffin-loaded expanded graphite particle core material; heating and stirring melamine and formaldehyde, adding a core material and sodium chloride, adjusting the pH value of the system to acidity, heating and stirring to obtain a phase-change microcapsule; adding water-soluble polyvinyl alcohol, phase-change microcapsules and a surfactant into water, mechanically mixing, performing strong ultrasonic dispersion to obtain a phase-change modified polyvinyl alcohol emulsion, dripping the phase-change modified polyvinyl alcohol emulsion into a refrigerating fluid for quick freezing, and performing freeze drying to obtain the phase-change modified porous polyvinyl alcohol particle filler. The phase change modified porous polyvinyl alcohol particle filler prepared by the invention has good temperature control performance, is beneficial to maintaining the reaction temperature at 25 ℃, is more beneficial to maintaining the activity of nitrobacteria, and improves the denitrification efficiency of the biofilm reactor in a low-temperature environment.
Description
Technical Field
The invention belongs to the technical field of low-temperature-resistant sewage treatment, and particularly relates to a phase-change modified porous polyvinyl alcohol particle filler, a preparation method thereof and application thereof in sewage denitrification in a low-temperature environment.
Background
With the continuous development of science and technology, a large amount of pollutants are discharged into a water body, nitrate in the pollutants is generally existed as a main pollutant and tends to be aggravated year by year, the self-cleaning capability of the pollutants simply depending on a water body pair is far from meeting the requirement of society on water quality, and if a sewage treatment process is not carried out, pollutants such as over-standard nitrate in sewage can seriously affect human health, so that how to remove the nitrate in the water becomes the key point of sewage treatment. And the nitrification of ammonia nitrogen is an important prerequisite for the denitrification of sewage treatment.
The biomembrane technology is a sewage treatment technology combining the membrane technology with the traditional activated sludge treatment technology, and has the advantages of better organic matter removal rate, effective removal of ammonia nitrogen and other refractory substances, and reduced nitrification capacity under the low-temperature condition in winter, so that the treated water quality can hardly meet the requirements of people. At present, various enhanced nitrification technologies, such as operation optimization and enhancement, biomembrane enhancement, nitrobacteria inoculation and materialization enhancement technologies, are researched, wherein the biomembrane enhancement technology can keep the structure of the original process and the structure of the main structure of the process unchanged, and only the modification treatment is needed to be carried out on the carrier filler for growth of nitrobacteria, so that the ideal nitrification efficiency can be obtained, but the traditional nitrobacteria, such as nitrite and nitrobacteria, have the maximum activity in weak alkaline water at the temperature of 25 ℃, and when the temperature is lower than 23 ℃, the growth of the nitrobacteria can be gradually stopped, so that the nitrification of ammonia nitrogen is directly influenced.
The culture method uses industrial ammonia-containing wastewater as a culture solution, adopts a mode of alternately culturing at a normal temperature of 18-40 ℃ and a low temperature of 8-18 ℃, adds a nitrobacteria growth promoter consisting of calcium salt, copper salt, magnesium salt and/or ferrous salt metal salt and spermine, spermidine, hydroxylamine hydrochloride, hydroxylamine sulfate or hydroxylamine phosphate polyamine substances into activated sludge rich in nitrobacteria, and carries out enrichment culture, wherein in the enrichment culture method, the nitrobacteria growth promoter is supplemented while the culture solution is replaced in each batch, so that the low-temperature resistant nitrobacteria is obtained. The low-temperature-resistant thalli prepared by the method can realize high-efficiency deamination and denitrification under the low-temperature condition, and can solve the problems of unstable low-temperature operation in winter, substandard sewage treatment and the like. Chinese patent CN103342417B discloses enrichment of a low temperature resistant heterotrophic synchronous nitrification and denitrification bacterial agent and an anoxic denitrification application of sewage, wherein mixed sewage of ammonia nitrogen and nitrate nitrogen containing an organic carbon source is used as a raw material, the mixed sewage comprises sodium acetate, NH4Cl, KNO3, KH2PO4, MgSO 4.7H2O, CaCl 2.2H 2O, FeSO4.7H2O and NaHCO3, and the balance of water, the mixed sewage of the ammonia nitrogen and the nitrate nitrogen containing the organic carbon is cultured and enriched under aerobic conditions in a low-temperature room at 10 ℃, and then the mixed sewage of the ammonia nitrogen and the nitrate nitrogen containing the organic carbon is further enriched and domesticated in SBR under anoxic conditions to obtain the heterotrophic nitrification aerobic/anoxic denitrification bacterial agent with low temperature resistance. The microbial inoculum can realize synchronous nitrification and denitrification in an aerobic or anoxic environment by taking sodium acetate as a unique organic carbon source under the low-temperature condition of 10 ℃ and in the environment with ammonia nitrogen and nitrate nitrogen coexisting, has a stable model, and also has a high total nitrogen removal rate under the anoxic condition. As is apparent from the above-mentioned prior art, in order to improve the efficiency of the nitration reaction at low temperatures, the low temperature resistance of nitrifying bacteria has been often modified, and the heat retaining property of fillers attached to the nitrifying bacteria has not been common. The invention introduces phase-change materials into the filler of the biofilm reactor to improve the nitration reaction efficiency of the biofilm reactor in low-temperature environment.
Disclosure of Invention
The invention aims to solve the technical problem of providing a phase change modified porous polyvinyl alcohol particle filler, a preparation method thereof and application thereof in sewage denitrification in a low-temperature environment.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the phase change modified porous polyvinyl alcohol particle filler is characterized by comprising a phase change microcapsule, wherein the phase change microcapsule comprises a resin wall material, a phase change material core material and an adsorption support material.
Preferably, in the above technical solution, the resin wall material is melamine resin, and the adsorption support material is expanded graphite.
The invention also provides a preparation method of the phase change modified porous polyvinyl alcohol particle filler, which is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing expanded graphite and a phase-change material, heating until the mixture is completely melted, and then carrying out spray cooling to obtain a paraffin-loaded expanded graphite particle core material;
(2) heating and stirring melamine and formaldehyde, adding the paraffin-loaded expanded graphite particle core material prepared in the step (1) and sodium chloride, adjusting the pH value of the system to acidity, and heating and stirring uniformly to obtain a phase-change microcapsule;
(3) adding water-soluble polyvinyl alcohol, the phase-change microcapsule prepared in the step (2) and a surfactant into water, mechanically mixing, and performing strong ultrasonic dispersion to obtain a phase-change modified polyvinyl alcohol emulsion;
(4) and dripping the phase-change modified polyvinyl alcohol emulsion into a refrigerating fluid for quick freezing, and then carrying out freeze drying to obtain the phase-change modified porous polyvinyl alcohol particle filler.
Preferably, in the step (1), the phase-change material is paraffin wax, and the mass ratio of the expanded graphite to the phase-change material is 1: 0.3-0.6.
Preferably, in the step (1), the particle diameter of the wax-supporting expanded graphite particle core material is in the order of micrometers.
Preferably, in the step (2), the content of the core material of the expanded graphite particles loaded with paraffin in the phase-change microcapsule is 15 to 25%.
Preferably, in the step (3), the water-soluble polyvinyl alcohol includes polyvinyl alcohol with a molecular weight of 2.5-3.5W and polyvinyl alcohol with a molecular weight of 17-22W in a mass ratio of 1: 1.5-2.3.
Preferably, in the step (3), the process of the intensive ultrasonic dispersion comprises: ultrasonic treatment is carried out for 3-5min at the frequency of 15-20kHz with the power of 1000-.
Preferably, in the step (4), the freezing fluid is liquid nitrogen or frozen ethanol, the freezing time is 5-10s, and the dropping speed is 0.5-1 mL/min.
The invention also provides application of any one of the phase change modified porous polyvinyl alcohol particle fillers in sewage denitrification in a low-temperature environment.
Compared with the prior art, the invention has the following beneficial effects:
(1) the phase change modified porous polyvinyl alcohol particle filler comprises phase change microcapsules, wherein the phase change microcapsules are mixed with water-soluble polyvinyl alcohol, and the porous polyvinyl alcohol is prepared through a freeze drying process.
(2) The phase-change microcapsule in the phase-change modified porous polyvinyl alcohol particle filler prepared by the invention is firmly coated by polyvinyl alcohol, so that the problem of permeation of the phase-change material in the use process is solved, the particle size of the phase-change material is small, and the phase-change material is uniformly dispersed in porous polyvinyl alcohol particles, so that the prepared phase-change modified porous polyvinyl alcohol particle filler has excellent temperature control performance, and the biomembrane reactor still has good heat storage and heat preservation performance in a low-temperature environment.
(3) In addition, in order to further improve the heat storage and insulation performance of the phase-change microcapsule, expanded graphite is selected as a supporting material, the expanded graphite is large in specific surface area and complete in pore structure, paraffin phase-change materials are favorably and firmly adsorbed in the expanded graphite, and then the expanded graphite is coated by a wall material, so that the leakage possibility of the phase-change microcapsule is reduced.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1:
(1) mixing the components in a mass ratio of 1: and mixing 0.3 of expanded graphite with the paraffin wax, heating to completely melt, and then carrying out spray cooling to obtain the micron-sized paraffin-loaded expanded graphite particle core material.
(2) Heating and stirring melamine and formaldehyde with the dosage ratio of 3g:6mL at 70 ℃, adding the expanded graphite particle core material loaded with paraffin and sodium chloride, adjusting the pH value of the system to 2, and heating and stirring uniformly at 80 ℃ to obtain the phase-change microcapsule, wherein the content of the expanded graphite particle core material loaded with paraffin in the phase-change microcapsule is 15%.
(3) Adding polyvinyl alcohol with molecular weight of 2.5-3.5W and polyvinyl alcohol with molecular weight of 17-22W in a mass ratio of 1:1.5, phase-change microcapsules and a sodium dodecyl benzene sulfonate surfactant into water, mechanically mixing, performing ultrasonic treatment for 3min at the frequency of 15kHz and the power of 1600W for 30min to obtain the phase-change modified polyvinyl alcohol emulsion.
(4) Dripping the phase change modified polyvinyl alcohol emulsion into liquid nitrogen refrigerating fluid at the speed of 0.5mL/min for quick freezing treatment for 5s, and then carrying out freeze drying to obtain the phase change modified porous polyvinyl alcohol particle filler.
Example 2:
(1) mixing the components in a mass ratio of 1: and mixing 0.6 of expanded graphite with the paraffin wax, heating to completely melt, and then carrying out spray cooling to obtain the micron-sized paraffin-loaded expanded graphite particle core material.
(2) Heating and stirring melamine and formaldehyde with the dosage ratio of 3g:6mL at 75 ℃, adding the expanded graphite particle core material loaded with paraffin and sodium chloride, adjusting the pH value of the system to 3, and heating and stirring uniformly at 90 ℃ to obtain the phase-change microcapsule, wherein the content of the expanded graphite particle core material loaded with paraffin in the phase-change microcapsule is 25%.
(3) Adding polyvinyl alcohol with molecular weight of 2.5-3.5W and polyvinyl alcohol with molecular weight of 17-22W in a mass ratio of 1:2.3, phase-change microcapsules and a sodium dodecyl sulfate surfactant into water, mechanically mixing, performing ultrasonic treatment for 5min at the frequency of 20kHz and the power of 2000W, and performing ultrasonic treatment for 90min at the frequency of 25kHz to obtain the phase-change modified polyvinyl alcohol emulsion.
(4) Dripping the phase-change modified polyvinyl alcohol emulsion into frozen ethanol refrigerating fluid at the speed of 1mL/min for quick freezing treatment for 10s, and then carrying out freeze drying to obtain the phase-change modified porous polyvinyl alcohol particle filler.
Example 3:
(1) mixing the components in a mass ratio of 1: and mixing 0.5 of expanded graphite with the paraffin wax, heating to completely melt, and then carrying out spray cooling to obtain the micron-sized paraffin-loaded expanded graphite particle core material.
(2) Heating and stirring melamine and formaldehyde with the dosage ratio of 3g:6mL at 73 ℃, adding the expanded graphite particle core material loaded with paraffin and sodium chloride, adjusting the pH value of the system to 2.5, heating and stirring uniformly at 83 ℃, and obtaining the phase-change microcapsule, wherein the content of the expanded graphite particle core material loaded with paraffin in the phase-change microcapsule is 18%.
(3) Adding polyvinyl alcohol with molecular weight of 2.5-3.5W and polyvinyl alcohol with molecular weight of 17-22W in a mass ratio of 1:1.9, phase-change microcapsules and cetyl trimethyl ammonium bromide surfactant into water, mechanically mixing, performing ultrasonic treatment for 4min at the frequency of 18kHz and the power of 1800W for 60min to obtain the phase-change modified polyvinyl alcohol emulsion.
(4) Dripping the phase-change modified polyvinyl alcohol emulsion into frozen ethanol refrigerating fluid at the speed of 0.6mL/min for quick freezing treatment for 8s, and then carrying out freeze drying to obtain the phase-change modified porous polyvinyl alcohol particle filler.
Example 4:
(1) mixing the components in a mass ratio of 1: and mixing 0.4 of expanded graphite with the section paraffin, heating to completely melt, and then carrying out spray cooling to obtain the micron-sized paraffin-loaded expanded graphite particle core material.
(2) Heating and stirring melamine and formaldehyde with the dosage ratio of 3g:6mL at 74 ℃, adding the expanded graphite particle core material loaded with paraffin and sodium chloride, adjusting the pH value of the system to 2.8, heating and stirring uniformly at 88 ℃ to obtain the phase-change microcapsule, wherein the content of the expanded graphite particle core material loaded with paraffin in the phase-change microcapsule is 23%.
(3) Adding polyvinyl alcohol with molecular weight of 2.5-3.5W and polyvinyl alcohol with molecular weight of 17-22W in a mass ratio of 1:2, adding the polyvinyl alcohol, the phase-change microcapsule and the nonylphenol polyoxyethylene ether surfactant into water, mechanically mixing, performing ultrasonic treatment for 3.5min at the frequency of 18kHz and the power of 1900W, and performing ultrasonic treatment for 45min at the frequency of 24kHz to obtain the phase-change modified polyvinyl alcohol emulsion.
(4) Dripping the phase change modified polyvinyl alcohol emulsion into liquid nitrogen refrigerating fluid at the speed of 0.6mL/min for quick freezing treatment for 8s, and then carrying out freeze drying to obtain the phase change modified porous polyvinyl alcohol particle filler.
Example 5:
(1) mixing the components in a mass ratio of 1: and mixing 0.4 of expanded graphite with the section paraffin, heating to completely melt, and then carrying out spray cooling to obtain the micron-sized paraffin-loaded expanded graphite particle core material.
(2) Heating and stirring melamine and formaldehyde with the dosage ratio of 3g:6mL at 75 ℃, adding the expanded graphite particle core material loaded with paraffin and sodium chloride, adjusting the pH value of the system to 2.1, heating and stirring uniformly at 83 ℃, and obtaining the phase-change microcapsule, wherein the content of the expanded graphite particle core material loaded with paraffin in the phase-change microcapsule is 19%.
(3) Adding polyvinyl alcohol with molecular weight of 2.5-3.5W and polyvinyl alcohol with molecular weight of 17-22W in a mass ratio of 1:2.1, phase-change microcapsules and a sodium dodecyl sulfate surfactant into water, mechanically mixing, performing ultrasonic treatment for 4.5min at 16kHz power of 1450W, and performing ultrasonic treatment for 60min at 23kHz power of 1900W to obtain the phase-change modified polyvinyl alcohol emulsion.
(4) Dripping the phase-change modified polyvinyl alcohol emulsion into frozen ethanol refrigerating fluid at the speed of 0.7mL/min for quick freezing treatment for 9s, and then carrying out freeze drying to obtain the phase-change modified porous polyvinyl alcohol particle filler.
Example 6:
(1) mixing the components in a mass ratio of 1: and mixing 0.3 of expanded graphite with the paraffin wax, heating to completely melt, and then carrying out spray cooling to obtain the micron-sized paraffin-loaded expanded graphite particle core material.
(2) Heating and stirring melamine and formaldehyde with the dosage ratio of 3g:6mL at 75 ℃, adding the expanded graphite particle core material loaded with paraffin and sodium chloride, adjusting the pH value of the system to 2, and heating and stirring uniformly at 90 ℃ to obtain the phase-change microcapsule, wherein the content of the expanded graphite particle core material loaded with paraffin in the phase-change microcapsule is 15%.
(3) Adding polyvinyl alcohol with molecular weight of 2.5-3.5W and polyvinyl alcohol with molecular weight of 17-22W in a mass ratio of 1:2.3, phase-change microcapsules and a nonylphenol polyoxyethylene ether surfactant into water, mechanically mixing, performing ultrasonic treatment for 3min at the frequency of 20kHz and the power of 1000W, and performing ultrasonic treatment for 90min at the frequency of 20kHz and dispersing at the power of 2000W to obtain the phase-change modified polyvinyl alcohol emulsion.
(4) Dripping the phase-change modified polyvinyl alcohol emulsion into frozen ethanol refrigerating fluid at the speed of 0.5mL/min for quick freezing treatment for 10s, and then carrying out freeze drying to obtain the phase-change modified porous polyvinyl alcohol particle filler.
Example 7:
(1) mixing the components in a mass ratio of 1: and mixing 0.6 of expanded graphite with the paraffin wax, heating to completely melt, and then carrying out spray cooling to obtain the micron-sized paraffin-loaded expanded graphite particle core material.
(2) Heating and stirring melamine and formaldehyde with the dosage ratio of 3g:6mL at 70 ℃, adding the expanded graphite particle core material loaded with paraffin and sodium chloride, adjusting the pH value of the system to 3, and heating and stirring uniformly at 80 ℃ to obtain the phase-change microcapsule, wherein the content of the expanded graphite particle core material loaded with paraffin in the phase-change microcapsule is 25%.
(3) Adding polyvinyl alcohol with molecular weight of 2.5-3.5W and polyvinyl alcohol with molecular weight of 17-22W in a mass ratio of 1:1.5, phase-change microcapsules and cetyl trimethyl ammonium bromide surfactant into water, mechanically mixing, performing ultrasonic treatment for 5min at the frequency of 15kHz and the power of 1500W, and performing ultrasonic treatment for 30min at the frequency of 25kHz and dispersing to obtain the phase-change modified polyvinyl alcohol emulsion.
(4) Dropping the phase change modified polyvinyl alcohol emulsion into liquid nitrogen or frozen ethanol refrigerating fluid at the speed of 1mL/min for quick freezing treatment for 5s, and then carrying out freeze drying to obtain the phase change modified porous polyvinyl alcohol particle filler.
The results of the measurements of the diameter, specific surface area and pore volume of the phase change modified porous polyvinyl alcohol particulate fillers prepared in examples 1-7 and the porous polyvinyl alcohol particulate fillers of the prior art are shown below:
as can be seen from the table above, the phase change modified porous polyvinyl alcohol particle filler prepared by the invention has similar diameter, specific surface area and pore volume with the traditional porous polyvinyl alcohol particle filler, and can be completely suitable for the use requirements of the biofilm reactor.
The results of measuring the biofilm amount, biofilm formation time and COD and ammonia nitrogen removal effect in a biofilm reactor operated at 10 ℃ in the same moving bed biofilm reactor with the porous polyvinyl alcohol particulate filler of the prior art as the filler in which the phase change modified porous polyvinyl alcohol particulate fillers prepared in examples 1 to 7 were placed in the biofilm reactor are shown in the following table:
as can be seen from the above table, the phase change modified porous polyvinyl alcohol particle filler prepared by the invention is used in the biofilm reactor in the low-temperature environment, the biofilm formation efficiency is obviously improved, the total amount and activity of the biofilm are improved, the ammonia nitrogen removal effect is ensured, the problem that sewage treatment does not reach the standard in the low-temperature environment is solved, and the production energy consumption and the production cost are reduced.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. The phase change modified porous polyvinyl alcohol particle filler is characterized by comprising phase change microcapsules, wherein the phase change microcapsules comprise a resin wall material, a phase change material core material and an adsorption support material; the resin wall material is melamine resin, and the adsorption support material is expanded graphite;
the preparation method comprises the following steps:
(1) mixing expanded graphite and a phase-change material, heating until the mixture is completely melted, and then carrying out spray cooling to obtain a paraffin-loaded expanded graphite particle core material;
(2) heating and stirring melamine and formaldehyde, adding the paraffin-loaded expanded graphite particle core material prepared in the step (1) and sodium chloride, adjusting the pH value of the system to acidity, and heating and stirring uniformly to obtain a phase-change microcapsule;
(3) adding water-soluble polyvinyl alcohol, the phase-change microcapsule prepared in the step (2) and a surfactant into water, mechanically mixing, and performing strong ultrasonic dispersion to obtain a phase-change modified polyvinyl alcohol emulsion;
(4) and dripping the phase-change modified polyvinyl alcohol emulsion into a refrigerating fluid for quick freezing, and then carrying out freeze drying to obtain the phase-change modified porous polyvinyl alcohol particle filler.
2. The phase change modified cellular polyvinyl alcohol particulate filler of claim 1, wherein: in the step (1), the phase-change material is paraffin wax, and the mass ratio of the expanded graphite to the phase-change material is 1: 0.3-0.6.
3. The phase change modified cellular polyvinyl alcohol particulate filler of claim 1, wherein: in the step (1), the particle size of the expanded graphite particle core material loaded with paraffin is micron-sized.
4. The phase change modified cellular polyvinyl alcohol particulate filler of claim 1, wherein: in the step (2), the content of the expanded graphite particle core material loaded with paraffin in the phase-change microcapsule is 15-25%.
5. The phase change modified cellular polyvinyl alcohol particulate filler of claim 1, wherein: in the step (3), the water-soluble polyvinyl alcohol comprises polyvinyl alcohol with molecular weight of 2.5-3.5W and polyvinyl alcohol with molecular weight of 17-22W in a mass ratio of 1: 1.5-2.3.
6. The phase change modified cellular polyvinyl alcohol particulate filler of claim 1, wherein: in the step (3), the process of the powerful ultrasonic dispersion comprises the following steps: ultrasonic treatment is carried out for 3-5min at the frequency of 15-20kHz with the power of 1000-.
7. The phase change modified cellular polyvinyl alcohol particulate filler of claim 1, wherein: in the step (4), the refrigerating fluid is liquid nitrogen or frozen ethanol, the freezing time is 5-10s, and the dropping speed is 0.5-1 mL/min.
8. Use of the phase change modified porous polyvinyl alcohol particulate filler according to any one of claims 1 to 7 for denitrification of sewage in low temperature environment.
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| KR20180057440A (en) * | 2016-11-22 | 2018-05-30 | 전남대학교산학협력단 | Capsulated latent heat storage microcapsule and preparation method thereof |
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