CN107502301A - A kind of fly ash base composite phase-change heat-storage material and preparation method thereof - Google Patents
A kind of fly ash base composite phase-change heat-storage material and preparation method thereof Download PDFInfo
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- CN107502301A CN107502301A CN201710933608.3A CN201710933608A CN107502301A CN 107502301 A CN107502301 A CN 107502301A CN 201710933608 A CN201710933608 A CN 201710933608A CN 107502301 A CN107502301 A CN 107502301A
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- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
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Abstract
The present invention relates to a kind of fly ash base composite phase-change heat-storage material and preparation method thereof, belong to energy storage material technical field.The present invention is by handling expansible graphite, expand its interlamellar spacing and specific surface area, and peeled off using ultrasonic stripping method into nanometer thin skin, again by being modified again with diluted acid after the processing of flyash high-temperature expansion, increase flyash specific surface area, improve Powder ash adsorption and dispersiveness, using Expandable graphite sheet heat conduction network is formed in the high hole of modified coal ash, the energy that phase-change material stores can quickly be transmitted, augmentation of heat transfer effect, and myristic acid, stearic acid, polyethylene glycol is as ternary phase transformation base material, in the loose structure of uniform embedded modified coal ash, heat endurance is good, thermal storage performance is excellent, flyash used in composite phase-change energy storage material prepared by the present invention can twice laid, reduce the pollution to environment, and it is expected to obtain practical application in the field such as building thermal insulation material and Solar use.
Description
Technical field
The present invention relates to a kind of fly ash base composite phase-change heat-storage material and preparation method thereof, belongs to energy storage material technology neck
Domain.
Background technology
The energy is the basis of human survival and development.The energy crisis that energy resource supply system based on fossil fuel is brought
And the problems such as environmental degradation, is paid close attention to by people, utilization regenerative resource, energy-saving and emission-reduction and raising energy utilization rate
Turn into countries in the world to alleviate energy supply and demand contradiction, mitigate environmental pollution, readjust the energy structure and transform mode of economic growth
Important channel.In the regenerative resources such as solar energy, wind energy, biomass, tide energy, solar energy because its reserves unlimitedness, deposit
Generality, the spatter property that utilizes and the economy of exploitation turn into most important regenerative resource.
Because solar radiant energy metric density is low, radiation intensity constantly changes, causes it in exploitation, conversion, transport and utilize
During, between supply and demand there is in quantity, in form and temporal difference, have significant unstability, seasonality and
It is intermittent.Therefore, stable, reliable, efficient energy storage technology is not only the key and core of Solar Energy Heat Utilization System, and solution
The certainly key of energy supply and demand mismatch over time and space.While regenerative resource is developed, existing energy is improved
The utilization rate in source is another important channel of alleviating energy crisis.In whole energy expenditure structure, most energy is
It is converted into what is be used again after the energy of other forms by the form of heat energy or by heat energy.Therefore, the profit of heat energy is improved
With efficiency, realize heat energy recycle be improve energy utilization rate inevitable approach.The protrusion waste of current heat energy utilization is
" degrade and use ", i.e., it is used to produce and live after directly producing heat energy using fossil fuel, the Land use systems have a large amount of low temperature
The waste of waste heat.Therefore, seek low Cheng Mu, efficient low temperature heat energy storage method, can not only improve energy utilization rate, solve energy
The contradiction between supply and demand is measured, and the purpose of energy-saving and emission-reduction can be realized.It can be seen that heat-storage technology is to improve energy utilization rate and protection ring
The effective means in border.
Therefore, in terms of the demand of national economy and social development, the research about heat energy utilization and memory technology is advantageous to
Heat energy wider scope, higher level comprehensive utilization are promoted, is advantageously implemented the target of energy-saving and emission-reduction and low-carbon economy.With heat
It can store and the material of temperature adjusting function is referred to as phase-change material.In theory, any material can serve as phase-changing energy storage material,
Therefore phase-change material substantial amounts, species are various.But presently commercially available phase-changing energy storage material heat endurance is poor, and thermal storage performance is weak,
Also need to its further research.
The content of the invention
The technical problems to be solved by the invention：It is poor for heat endurance, a kind of the problem of thermal storage performance is weak, there is provided powder
Coal ash base composite phase-change heat accumulating and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of fly ash base composite phase-change heat-storage material, it is characterised in that the phase-change heat-storage material is with Expandable graphite sheet and changes
Property flyash is backing material, and ternary phase transformation base material is used as using myristic acid, stearic acid, polyethylene glycol.
The parts by weight of each raw material are 1~2 part of Expandable graphite sheet, 12~24 parts of modified coal ash, 20~25 portions of Pork and beans
Cool acid, 20~25 parts of stearic acid, 20~25 parts of polyethylene glycol.
The Expandable graphite sheet be expansible graphite grinding sieving dry after be heated to 850~950 DEG C of insulation reactions 30~
40s, then ultrasonic disperse 5~8h in ethanol solution, filtering alcohol wash drying, obtain Expandable graphite sheet.
The modified coal ash be through 600~650 DEG C be calcined 2~3h flyash citric acid immersion treatment after filtering,
Washing, drying, grinding, 400 mesh sieves excessively are made.
The citric acid mass fraction is 1%, and the immersion treatment is stirred to be immersed in citric acid solution at 50~60 DEG C
Mix 2~3h.
Concretely comprise the following steps：
S1. expansible graphite is ground after sieving is dried and is heated to 850~950 DEG C of 30~40s of insulation reaction, then ultrasonic disperse exists
5~8h in ethanol solution, filtering alcohol wash drying, obtain Expandable graphite sheet；
S2. it is immersed in citric acid solution after flyash being heated into 600~650 DEG C of 2~3h of roasting, is stirred at 50~60 DEG C
Filtered after 2~3h, wash, dry, grind, cross 400 mesh sieves, obtain modified coal ash；
S3. Expandable graphite sheet, modified coal ash, myristic acid, stearic acid, polyethylene glycol are taken, 60~70 are heated to 5 DEG C/min
DEG C, and in the case where vacuum is 60~80kPa, with 150W ultrasonic powers, 40kHz frequency 20~30min of synergistic sorption, continue with 5
DEG C/min is heated to 80~90 DEG C, continues 20~30min of absorption, it is cooled to after room temperature to obtain fly ash base composite phase-change heat-storage material
Material.
Compared with other method, advantageous effects are the present invention：
（1）The present invention expands its interlamellar spacing and specific surface area, and utilize ultrasonic stripping method by handling expansible graphite
Nanometer thin skin is peeled off into, then by being modified again with diluted acid after the processing of flyash high-temperature expansion, increasing flyash specific surface area, carrying
High fly-ash adsorptivity and dispersiveness, heat conduction network is formed in the high hole of modified coal ash using Expandable graphite sheet, can
The energy that phase-change material stores quickly is transmitted, augmentation of heat transfer effect, and myristic acid, stearic acid, polyethylene glycol are as three
First phase transformation base material, uniformly in the loose structure of embedded modified coal ash, heat endurance is good, and thermal storage performance is excellent；
（2）Flyash used in composite phase-change energy storage material prepared by the present invention gives up from solid caused by the generating of city
Gurry, can twice laid, reduce the pollution to environment, and be expected to obtain reality in the field such as building thermal insulation material and Solar use
Apply on border.
Embodiment
Take 2~3g expansible graphites to be fitted into mortar to grind, cross 60 mesh sieves, the expansible graphite powder after sieving is placed in
In drying box, dry to constant weight, then be transferred in Muffle furnace at 105~110 DEG C, be heated to 850~950 DEG C, insulation reaction 30
~40s, mass fraction is added as in 75% ethanol solution, 20~30min is stirred with 180~240r/min after being cooled to room temperature, then
It is transferred to after being ultrasonically treated 5~8h in ultrasonic disperse instrument, filters to obtain filter residue, vacuum is placed in after washing filter residue 2~3 times with absolute ethyl alcohol
In drying box, to constant weight at 105~110 DEG C, Expandable graphite sheet is obtained, 100~200g flyash is taken, is fitted into Muffle furnace, add
Heat is cooled to after room temperature and adds 500~1000g mass fractions and be in 1% citric acid solution to 600~650 DEG C of 2~3h of roasting,
2~3h is stirred at 50~60 DEG C, filters to obtain filter cake, filter cake is washed with deionized and is transferred to vacuum drying in after neutral to cleaning solution
In case, dried at 105~110 DEG C to constant weight, then be transferred in mortar and grind, crossed 400 mesh sieves, obtain modified coal ash, take 1~2g
Expandable graphite sheet, 12~24g modified coal ash, 20~25g myristic acids, 20~25g stearic acid, 20~25g polyethylene glycol, with
5 DEG C/min is heated to 60~70 DEG C, and in the case where vacuum is 60~80kPa, with 150W ultrasonic powers, the collaboration of 40kHz frequencies is inhaled
Attached 20~30min, continue to be heated to 80~90 DEG C with 5 DEG C/min, continue 20~30min of absorption, fine coal is obtained after being cooled to room temperature
Grey base composite phase-change heat accumulating.
Example 1
Take 2g expansible graphites to be fitted into mortar to grind, cross 60 mesh sieves, the expansible graphite powder after sieving is placed in drying box
In, dried at 105 DEG C to constant weight, then be transferred in Muffle furnace, 850 DEG C, insulation reaction 30s are heated to, is added after being cooled to room temperature
Enter mass fraction in 75% ethanol solution, 20min is stirred with 180r/min, then be transferred in ultrasonic disperse instrument after supersound process 5h,
Filter residue is filtered to obtain, is placed in after washing filter residue 2 times with absolute ethyl alcohol in vacuum drying chamber, to constant weight at 105 DEG C, obtains expanded graphite
Piece, 100g flyash is taken, is fitted into Muffle furnace, be heated to 600 DEG C of roasting 2h, addition 500g mass fractions are after being cooled to room temperature
In 1% citric acid solution, 2h is stirred at 50 DEG C, filters to obtain filter cake, filter cake is washed with deionized to cleaning solution in after neutrality turns
Enter in vacuum drying chamber, dried at 105 DEG C to constant weight, then be transferred in mortar and grind, cross 400 mesh sieves, obtain modified coal ash, take
1g Expandable graphite sheets, 12g modified coal ash, 20g myristic acids, 20g stearic acid, 20g polyethylene glycol, it is heated to 5 DEG C/min
60 DEG C, and in the case where vacuum is 60kPa, with 150W ultrasonic powers, 40kHz frequency synergistic sorption 20min, continue with 5 DEG C/min
80 DEG C are heated to, continues to adsorb 20min, fly ash base composite phase-change heat-storage material is obtained after being cooled to room temperature.
Example 2
Take 2.5g expansible graphites to be fitted into mortar to grind, cross 60 mesh sieves, the expansible graphite powder after sieving is placed in drying
In case, dry to constant weight, then be transferred in Muffle furnace at 107 DEG C, be heated to 900 DEG C, insulation reaction 35s, after being cooled to room temperature
It is in 75% ethanol solution to add mass fraction, stirs 25min with 210r/min, then be transferred in ultrasonic disperse instrument and be ultrasonically treated 6h
Afterwards, filter residue is filtered to obtain, is placed in vacuum drying chamber after washing filter residue 2 times with absolute ethyl alcohol, to constant weight at 107 DEG C, must expand
Graphite flake, 150g flyash is taken, is fitted into Muffle furnace, be heated to 625 DEG C of roasting 2h, 750g mass point is added after being cooled to room temperature
Number is in 1% citric acid solution, stirs 2h at 55 DEG C, filters to obtain filter cake, and filter cake is washed with deionized to cleaning solution in neutrality
After be transferred in vacuum drying chamber, dried at 107 DEG C to constant weight, then be transferred in mortar and grind, crossed 400 mesh sieves, obtain modified fine coal
Ash, 1g Expandable graphite sheets are taken, 18g modified coal ash, 22g myristic acids, 22g stearic acid, 22g polyethylene glycol, are added with 5 DEG C/min
Heat is to 65 DEG C, and in the case where vacuum is 70kPa, with 150W ultrasonic powers, 40kHz frequency synergistic sorption 25min, continue with 5 DEG C/
Min is heated to 85 DEG C, continues to adsorb 25min, and fly ash base composite phase-change heat-storage material is obtained after being cooled to room temperature.
Example 3
Take 3g expansible graphites to be fitted into mortar to grind, cross 60 mesh sieves, the expansible graphite powder after sieving is placed in drying box
In, dried at 110 DEG C to constant weight, then be transferred in Muffle furnace, 950 DEG C, insulation reaction 40s are heated to, is added after being cooled to room temperature
Enter mass fraction in 75% ethanol solution, 30min is stirred with 240r/min, then be transferred in ultrasonic disperse instrument after supersound process 8h,
Filter residue is filtered to obtain, is placed in after washing filter residue 3 times with absolute ethyl alcohol in vacuum drying chamber, to constant weight at 110 DEG C, obtains expanded graphite
Piece, 200g flyash is taken, is fitted into Muffle furnace, be heated to 650 DEG C of roasting 3h, 1000g mass fractions are added after being cooled to room temperature
For in 1% citric acid solution, 3h is stirred at 60 DEG C, filter cake is filtered to obtain, filter cake is washed with deionized to cleaning solution in after neutral
It is transferred in vacuum drying chamber, is dried at 110 DEG C to constant weight, then be transferred in mortar and grind, crosses 400 mesh sieves, obtain modified coal ash,
2g Expandable graphite sheets are taken, 24g modified coal ash, 25g myristic acids, 25g stearic acid, 25g polyethylene glycol, are added with 5 DEG C/min
Heat is to 70 DEG C, and in the case where vacuum is 80kPa, with 150W ultrasonic powers, 40kHz frequency synergistic sorption 30min, continue with 5 DEG C/
Min is heated to 90 DEG C, continues to adsorb 30min, and fly ash base composite phase-change heat-storage material is obtained after being cooled to room temperature.
The heat accumulating that the fly ash base composite phase-change heat-storage material being prepared into and Heilungkiang company produce is examined
Survey, specific detection is as follows：
（1）Thermal storage performance is tested
The heat accumulation of phase-change material/exothermicity curve, the melting time obtained by tangential method and setting time.Melting time point
Not Wei 580s and 600s, setting time is respectively 940s and 620s, and this shows SA/PMMA heat storage capacity entirely from its core
Material SA, there is excellent heat storage capacity.In thermal process is stored, SA and SA/PMMA thawing time master short compared with setting time
It is that heat, sink temperature are different and cause temperature difference between phase-change material and cold and hot medium to have differences in storage, exothermic process to want reason
Caused by.
（2）Stability test
The phase-change material of function admirable should not only have good heat storage capacity, but also should have good heat endurance and chemistry
Structural stability, i.e., after experience cold cycling (heat accumulation-heat release) circulation several times, its hot property (latent heat of phase change, phase alternating temperature
Degree) do not occur or occur small change, degraded or other reactions should not occur for its chemical constitution.Table 1 is that SA/PMMA is undergoing
The forward and backward DSC curve of 500 acceleration cold cyclings, the relevant parameter of DSC curve reflection.
Specific test result such as table 1.
The fly ash base composite phase-change heat-storage material performance characterization of table 1
As shown in Table 1, a kind of fly ash base composite phase-change heat-storage material produced by the present invention, heat endurance is good, and thermal storage performance is excellent
It is different.Flyash used in composite phase-change energy storage material prepared by the present invention is from solid waste caused by the generating of city
Thing, can twice laid, reduce the pollution to environment, and be expected to obtain reality in the field such as building thermal insulation material and Solar use
Using.
Claims (6)
- A kind of 1. fly ash base composite phase-change heat-storage material, it is characterised in that the phase-change heat-storage material with Expandable graphite sheet and Modified coal ash is backing material, and ternary phase transformation base material is used as using myristic acid, stearic acid, polyethylene glycol.
- A kind of 2. fly ash base composite phase-change heat-storage material as claimed in claim 1, it is characterised in that the weight of each raw material Amount part is 1~2 part of Expandable graphite sheet, 12~24 parts of modified coal ash, 20~25 parts of myristic acids, 20~25 parts of stearic acid, 20 ~25 parts of polyethylene glycol.
- A kind of 3. fly ash base composite phase-change heat-storage material as claimed in claim 1, it is characterised in that the Expandable graphite sheet Ground for expansible graphite and 850~950 DEG C of 30~40s of insulation reaction are heated to after sieving is dried, then ultrasonic disperse is molten in ethanol 5~8h in liquid, filtering alcohol wash drying, obtain Expandable graphite sheet.
- A kind of 4. fly ash base composite phase-change heat-storage material as claimed in claim 1, it is characterised in that the modified coal ash For through 600~650 DEG C be calcined 2~3h flyash citric acid immersion treatment after filtering, washing, dry, grinding, cross 400 mesh Sieve series obtains.
- A kind of 5. fly ash base composite phase-change heat-storage material as claimed in claim 4, it is characterised in that the citric acid quality Fraction is 1%, and the immersion treatment stirs 2~3h to be immersed in citric acid solution at 50~60 DEG C.
- 6. a kind of preparation method of fly ash base composite phase-change heat-storage material as claimed in any one of claims 1 to 5, wherein, it is special Sign is, concretely comprises the following steps：S1. expansible graphite is ground after sieving is dried and is heated to 850~950 DEG C of 30~40s of insulation reaction, then ultrasonic disperse exists 5~8h in ethanol solution, filtering alcohol wash drying, obtain Expandable graphite sheet；S2. it is immersed in citric acid solution after flyash being heated into 600~650 DEG C of 2~3h of roasting, is stirred at 50~60 DEG C Filtered after 2~3h, wash, dry, grind, cross 400 mesh sieves, obtain modified coal ash；S3. Expandable graphite sheet, modified coal ash, myristic acid, stearic acid, polyethylene glycol are taken, 60~70 are heated to 5 DEG C/min DEG C, and in the case where vacuum is 60~80kPa, with 150W ultrasonic powers, 40kHz frequency 20~30min of synergistic sorption, continue with 5 DEG C/min is heated to 80~90 DEG C, continues 20~30min of absorption, it is cooled to after room temperature to obtain fly ash base composite phase-change heat-storage material Material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109053064A (en) * | 2018-11-01 | 2018-12-21 | 肥西县创玺建材科技有限公司 | A kind of high-quality mortar for exterior walls of buildings |
| CN109305771A (en) * | 2018-11-01 | 2019-02-05 | 肥西县创玺建材科技有限公司 | A kind of high-quality flyash and preparation method thereof for concrete additive |
| CN109336487A (en) * | 2018-11-15 | 2019-02-15 | 肥西县创玺建材科技有限公司 | A kind of novel architecture thermal insulation mortar |
| CN109796938A (en) * | 2019-01-23 | 2019-05-24 | 北华大学 | A kind of phase-variable energy-storage economical material and preparation method thereof |
| CN110643329A (en) * | 2019-08-30 | 2020-01-03 | 上海大学 | Fatty acid/modified fly ash composite phase change energy storage material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109053064A (en) * | 2018-11-01 | 2018-12-21 | 肥西县创玺建材科技有限公司 | A kind of high-quality mortar for exterior walls of buildings |
| CN109305771A (en) * | 2018-11-01 | 2019-02-05 | 肥西县创玺建材科技有限公司 | A kind of high-quality flyash and preparation method thereof for concrete additive |
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| CN109796938A (en) * | 2019-01-23 | 2019-05-24 | 北华大学 | A kind of phase-variable energy-storage economical material and preparation method thereof |
| CN110643329A (en) * | 2019-08-30 | 2020-01-03 | 上海大学 | Fatty acid/modified fly ash composite phase change energy storage material and preparation method thereof |
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