CN106634856A - Two-gradient phase-change thermal storage material and preparation method thereof - Google Patents
Two-gradient phase-change thermal storage material and preparation method thereof Download PDFInfo
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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 invention relates to a two-gradient phase-change thermal storage material and a preparation method thereof. The phase-change thermal storage material is prepared from the following material components in percentage by weight: 38 to 42% of p-methoxyphenol, 45 to 48% of pyrogallol, 4 to 6% of nanometer silica, 3 to 5% of nanometer graphite powder, 2% of polyoxyethylene fatty acid nonionic surfactant and 2% of hydroquinone. The preparation method of the two-gradient phase-change thermal storage material comprises the steps of adding p-methoxyphenol into a mixing kettle; heating to 60 to 70 DEG C; stirring for 1 hour; then sequentially adding the polyoxyethylene fatty acid and the hydroquinone; continuing to stir and heat to 150 to 160 DEG C; adding the pyrogallol into the mixing kettle; after stirring for 2 hours, sequentially adding the nanometer silica and the nanometer graphite powder; carrying out melting adsorption for 3 hours at a temperature of 150 to 160 DEG C; carrying out cooling pelletizing forming to obtain the phase-change thermal storage material. Gradient utilization of industrial waste heat can be implemented, and requirements of users for steam and hot water are met.
Description
Technical field
The invention belongs to heat-storing material technical field, more particularly to a kind of gradient phase change heat storage material of middle low temperature two and its system
Preparation Method.
Background technology
China's industrial waste heat resource enriches, mainly include high-temp waste gas waste heat, cooling medium waste heat, waste vapour waste water residual heat,
High-temperature product and afterheat of slags, chemical reaction waste heat etc., residual heat resources account for the 17%～67% of its fuel consumption total amount, wherein
, up to 60%, utilization rate of waste heat room for promotion is big, and energy-saving potential is huge for recovery rate.But, heat energy all existence time in utilization
Discontinuity, the otherness in space and intensity unstability the shortcomings of, this significantly limit its large-scale application.Accumulation of heat
Technology can be collected to heat energy, be stored and release using the conversion of phase change heat storage material internal energy, and then be realized to heat energy
The Reasonable Regulation And Control of supply-demand relationship, reaches the purpose that energy efficient is rationally utilized.
Phase change heat storage material typically have good reversibility, energy storage density it is high, it is workable the features such as.Phase change heat storage material
Using material absorb heat in phase transition process heat release carry out storage release latent heat, being divided into high temperature using phase transition temperature by it (is higher than
450 DEG C), middle temperature (100～450 DEG C), four classes such as low temperature (0～100 DEG C) and ultralow temperature (being less than 0 DEG C), by its chemical composition master
It is divided into organic phase-change heat-storing material and inorganic-phase variable heat-storing material.Organic phase-change heat-storing material mainly have paraffin, acetic acid, oneself two
The organic matters such as acid, organic phase-change heat-storing material performance is more stable, and almost without supercooling and problem of phase separation, major defect is that phase transformation is dived
Heat is low, and material density is less, and it is less to have thereby resulted in organic phase-change heat-storing material unit volume amount of stored heat, and in addition organic phase-change stores
Hot material thermal conductivity factor is low.Inorganic-phase variable heat-storing material mainly has crystalline hydrate salt, molten salts, metal or alloy class etc.,
Inorganic-phase variable heat-storing material has higher unit volume amount of stored heat and good thermal conductivity, and it has the disadvantage to be also easy to produce supercooling and phase
Separate.
At present many researchers are based on the hot property of organic phase-change heat-storing material and supercooling, the phase of inorganic-phase variable heat-storing material
Separation problem has carried out a series of research.Research shows, cryogenic applications field (being less than 100 DEG C), holds with higher sensible heat
It is optimum heat storage medium with the water of low price, and in high temperature field, the heat-storing material of particularly middle temperature (80～250 DEG C)
Research it is relatively fewer, heat utilization technology is relatively weak, lack systematic research.Chinese patent CN103834366A discloses one
Industrial medium temperature phase change heat storage material and preparation method thereof is planted, heat-storing material is by adipic acid, copper facing CNT and binding agent group
Into CNT needs the treatment measures through some row such as 400 DEG C of high-temperature process, ultrasonication, copper coating process, work
Skill process is complicated.Chinese patent CN104559936A discloses a kind of middle temperature phase change heat storage material and preparation method thereof, accumulation of heat
Material is made up of adipic acid, rare earth oxide, Graphene and binding agent, the adipic acid heat-storing material production cost of preparation compared with
It is high.Therefore, necessary exploitation a kind of amount of stored heat height, low degree of supercooling, good heat conductivity, the heat of entirely appropriate industrial exhaust heat demand
Good stability, process is simple, gradient phase change heat storage material of middle low temperature two of low cost and preparation method thereof, with important practicality
Value.
The content of the invention
Present invention aim at not enough present on prior art, there is provided a kind of amount of stored heat is high, degree of supercooling is low, heat conduction
Performance is good, heat endurance is good, process is simple, the gradient phase change heat storage material of middle low temperature two and preparation method thereof of low cost.
For achieving the above object, the present invention takes technical scheme below：
A kind of two gradient phase change heat storage materials, are made up of the material component of following mass content：P methoxy phenol 38～
42%, pyrogallol 45～48%, nanometer grade silica 4～6%, nanoscale graphite powder 3～5%, aliphatic acid polyethenoxy
Ester 2%, hydroquinones 2%.
A kind of preparation method of two gradients phase change heat storage material, its step is as follows：
(1) raw material for preparing two gradient phase change heat storage materials are weighed according to mass ratio, the quality of raw material each component
Proportioning is：P methoxy phenol 38～42%, pyrogallol 45～48%, nanometer grade silica 4～6%, nanoscale graphite
Powder 3～5%, polyoxyethylene carboxylate 2%, hydroquinones 2%, wherein, p methoxy phenol, the mesh of pyrogallol 100 sieve
It is standby.
(2) p methoxy phenol is put into mixing kettle by proportioning, mixing kettle is warming up to 60～70 DEG C, is stirred 1 hour, made
P methoxy phenol is in complete molten condition.
(3) polyoxyethylene carboxylate and hydroquinones, warming while stirring are sequentially added in mixing kettle by proportioning.
(4) when kettle is warming up to 150～160 DEG C, pyrogallol is added in mixing kettle by proportioning, is stirred 2 hours, make adjacent benzene
Triphenol is well mixed in complete molten condition and p methoxy phenol, pyrogallol.
(5) under stirring, nanometer grade silica, nanoscale graphite powder are sequentially added in mixing kettle by proportioning,
Melting absorption 3 hours at a temperature of 150～160 DEG C.
(6) cooling granulation shaping, that is, obtain the two gradients phase change heat storage material.
The present invention principle be：Phase-change material p methoxy phenol and pyrogallol are respectively low-temperature phase-change material with
Warm phase-change material, the two latent heat of phase change is high, hot property is excellent, and the two is applied in combination, and on the one hand can realize the ladder of industrial exhaust heat
Level is utilized, and reduces requirement to thermal source, is met the needs of different users, and on the other hand, middle temperature phase-change material pyrogallol accumulation of heat, is put
When hot, low-temperature phase-change material p methoxy phenol is molten condition, can improve the capacity of heat transmission of middle temperature phase-change material pyrogallol,
Greatly shorten accumulation of heat, the Exotherm Time of middle temperature phase-change material pyrogallol.Nanometer grade silica have stronger heat storage capacity,
Heat conductivility and absorption property, nanoscale graphite powder have stronger heat conductivility and absorption property, nanometer grade silica and
Nanoscale graphite powder enhances phase-change material while phase-change material p methoxy phenol and pyrogallol heat storage capacity is improved
The heat conductivility and heat endurance of p methoxy phenol and pyrogallol, improves the service life of phase-change material.Fatty acid polyglycol
Oxygen vinyl acetate nonionic surfactant can make phase-change material p methoxy phenol, pyrogallol and nanometer grade silica, receive
Meter level graphite powder is sufficiently mixed, it is to avoid the generation of phenomenon of phase separation, while hydroquinones improves system stability.
The positive effect of the present invention is：
(1) present invention is with p methoxy phenol, pyrogallol, nanometer grade silica, nanoscale graphite powder, fatty acid polyglycol
Oxygen vinyl acetate nonionic surfactant, hydroquinones are raw material, and by simple process two gradient phase change heat storage materials are prepared,
It is with short production cycle.
(2) two gradient phase change heat storage materials prepared by the present invention are two-stage phase-change material, are capable of achieving the step of industrial exhaust heat
Utilize.The simultaneously heat-storing material, the requirement to thermal source is low, can meet user to steam and the demand of hot water.Middle temperature phase-change material
When pyrogallol accumulation of heat, heat release, low-temperature phase-change material p methoxy phenol is molten condition, can improve middle temperature phase-change material neighbour benzene
The capacity of heat transmission of triphenol, greatly shortens accumulation of heat, the Exotherm Time of middle temperature phase-change material pyrogallol.
(3) nanometer grade silica and nanoscale graphite powder are mixed in two gradient phase change heat storage materials prepared by the present invention,
Heat storage capacity, heat conductivility and the absorption property of phase-change material can be strengthened, the service life of phase-change material is improved.
(4) polyoxyethylene carboxylate nonionic surfactant and hydroquinones are mixed, phase-change material can be made to methoxy
Base phenol, pyrogallol and nanometer grade silica, nanoscale graphite powder are sufficiently mixed, it is to avoid the generation of phenomenon of phase separation, increase
Strong system stability.
In a word, the present invention prepare two gradient phase change heat storage materials have amount of stored heat height, low degree of supercooling, good heat conductivity,
Heat endurance is good, process is simple, low cost the advantages of, be capable of achieving industrial exhaust heat cascade utilization, meet user to steam and heat
The demand of water.
Description of the drawings
Fig. 1 is a kind of flow chart of two gradients phase change heat storage material preparation method of the present invention.
Fig. 2 is a kind of two gradients phase change heat storage material thermal storage time of the present invention and system temperature variation diagram.
Specific embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is done below in conjunction with the accompanying drawings into
One step is described in detail.
Embodiment 1
The starting components and mass ratio of two gradient phase change heat storage materials are：P methoxy phenol 38%, pyrogallol
48%, nanometer grade silica 6%, nanoscale graphite powder 4%, polyoxyethylene carboxylate nonionic surfactant 2% is right
Benzenediol 2%.
During preparation as shown in Figure 1, the p methoxy phenol for first 100 mesh sieving adds mixing kettle, is heated to 60～70 DEG C,
Stirring 1 hour, makes p methoxy phenol melt completely, then sequentially adds polyoxyethylene carboxylate, hydroquinones.Continue to stir
Mix and be warming up to 150～160 DEG C, the pyrogallol that 100 mesh are sieved adds mixing kettle, stir 2 hours, pyrogallol is melted completely
Melt and be well mixed with p methoxy phenol, nanometer grade silica, nanoscale graphite powder are then sequentially added, 150～160
Melting absorption 3 hours at a temperature of DEG C.The phase-change material of generation sends into comminutor, that is, obtain the gradient phase-transition heat-storage of the middle low temperature two
Material.
Jing is tested, and the temperature of the gradient phase change heat storage material phase transformation twice of middle low temperature two prepared by the present embodiment is respectively
54.3 DEG C, 133.5 DEG C, thermal conductivity is 2.46W/ (mK), and degree of supercooling is 0.8 DEG C.With certain heating rate from room temperature
To 180 degrees Celsius, 5min is incubated, is subsequently cooled to room temperature, after such 500 accumulation of heats, heat release circulation, mass loss rate
Less than 1%.
Embodiment 2
The starting components and mass ratio of two gradient phase change heat storage materials are：P methoxy phenol 40%, pyrogallol
46%, nanometer grade silica 5%, nanoscale graphite powder 5%, polyoxyethylene carboxylate nonionic surfactant 2% is right
Benzenediol 2%.
During preparation as shown in Figure 1, the p methoxy phenol for first 100 mesh sieving adds mixing kettle, is heated to 60～70 DEG C,
Stirring 1 hour, makes p methoxy phenol melt completely, then sequentially adds polyoxyethylene carboxylate, hydroquinones.Continue to stir
Mix and be warming up to 150～160 DEG C, the pyrogallol that 100 mesh are sieved adds mixing kettle, stir 2 hours, pyrogallol is melted completely
Melt and be well mixed with p methoxy phenol, nanometer grade silica, nanoscale graphite powder are then sequentially added, 150～160
Melting absorption 3 hours at a temperature of DEG C.The phase-change material of generation sends into comminutor, that is, obtain the gradient phase-transition heat-storage of the middle low temperature two
Material.
Jing is tested, the temperature of two gradient phase change heat storage material phase transformations twice prepared by the present embodiment be respectively 54.2 DEG C,
133.4 DEG C, thermal conductivity is 2.38W/ (mK), and degree of supercooling is 0.8 DEG C.Taken the photograph to 180 from room temperature with certain heating rate
Family name's degree, is incubated 5min, is subsequently cooled to room temperature, and after such 500 accumulation of heats, heat release circulation, mass loss rate is less than
1%.
Embodiment 3
The starting components and mass ratio of two gradient phase change heat storage materials are：P methoxy phenol 42%, pyrogallol
45%, nanometer grade silica 4%, nanoscale graphite powder 5%, polyoxyethylene carboxylate nonionic surfactant 2% is right
Benzenediol 2%.
During preparation as shown in Figure 1, the p methoxy phenol for first 100 mesh sieving adds mixing kettle, is heated to 60～70 DEG C,
Stirring 1 hour, makes p methoxy phenol melt completely, then sequentially adds polyoxyethylene carboxylate, hydroquinones.Continue to stir
Mix and be warming up to 150～160 DEG C, the pyrogallol that 100 mesh are sieved adds mixing kettle, stir 2 hours, pyrogallol is melted completely
Melt and be well mixed with p methoxy phenol, nanometer grade silica, nanoscale graphite powder are then sequentially added, 150～160
Melting absorption 3 hours at a temperature of DEG C.The phase-change material of generation sends into comminutor, that is, obtain the gradient phase-transition heat-storage of the middle low temperature two
Material.
Jing is tested, the temperature of two gradient phase change heat storage material phase transformations twice prepared by the present embodiment be respectively 54 DEG C,
133.4 DEG C, thermal conductivity is 2.35W/ (mK), and degree of supercooling is 0.7 DEG C.Taken the photograph to 180 from room temperature with certain heating rate
Family name's degree, is incubated 5min, is subsequently cooled to room temperature, and after such 500 accumulation of heats, heat release circulation, mass loss rate is less than
1%.
Claims (2)
1. a kind of two gradients phase change heat storage material, it is characterised in that phase change heat storage material by following mass content material component group
Into：P methoxy phenol 38～42%, pyrogallol 45～48%, nanometer grade silica 4～6%, nanoscale graphite powder 3～
5%, polyoxyethylene carboxylate nonionic surfactant 2%, hydroquinones 2%.
2. a kind of preparation method of two gradients phase change heat storage material, it is characterised in that add the p methoxy phenol that 100 mesh sieve
Enter mixing kettle, be heated to 60～70 DEG C, stir 1 hour, after sequentially add polyoxyethylene carboxylate, hydroquinones, continuously stir
Mix and be warming up to 150～160 DEG C, the pyrogallol for adding 100 mesh to sieve is stirred 2 hours, after sequentially add nanoscale titanium dioxide
Silicon, nanoscale graphite powder, continuously stir down and adsorb 3 hours in 150～160 DEG C of temperature meltings.
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Cited By (1)
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| CN109631649A (en) * | 2018-11-28 | 2019-04-16 | 东北电力大学 | A kind of preparation method of stairs combined type mixed type phase transition heat accumulation unit and its phase change heat storage material and phase-transition heat-storage stick |
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Application publication date: 20170510 |