CN105925249A - Preparation method of phase change material with palm oil as raw material - Google Patents
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/0068—Ingredients with a function or property not provided for elsewhere in C04B2103/00
- C04B2103/0071—Phase-change materials, e.g. latent heat storage materials used in concrete compositions
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Abstract
The invention discloses a preparation method of a phase change material with palm oil as a raw material. According to the invention, palm oil is adopted as a raw material, and methanol is added; after two transesterification reactions, refined methyl ester is obtained; the refined methyl ester is separated, such that saturated fatty acid methyl ester is obtained; the saturated fatty acid methyl ester is mixed with hexadecanol according to a mass ratio of 10:1-2.5:1, such that a binary composite phase change material with phase change temperature of 22-27 DEG C and phase change latent heat of 160-190J/g is obtained. According to the invention, the prepared binary phase change material is subjected to morphological curing either by encapsulating the material with microcapsules or by compounding the material with a porous medium substrate. The material can be combined with a building material to form a composite building envelop structure with an energy-saving property. Therefore, indoor temperature difference between day and night can be effectively reduced, thermal comfort can be improved, and energy consumption can be reduced.
Description
Technical field
The present invention relates to phase-change material field, be specifically related to the preparation method of a kind of phase-change material with Petiolus Trachycarpi oil as raw material.
Background technology
Phase-change material makes it have more advantage than common heat preserving and insulating material due to the energy storage characteristic of self, uses phase-change material
Can be greatly improved the thermal inertia of body of wall, and its occupation mode is flexible and changeable, energy-saving effect is not affected by the heat bridge effect of body of wall.
Correlational study currently for phase-change material complex building building enclosure has a lot, and either on climatic province or in phase
Become and all achieve certain achievement in research in the selection of material, but in the actual application of phase-change material Composite Enclosure Structure and popularization
On, or suitable scarcity.The phase-change material Composite Enclosure Structure that exploitation is the most available, will widen the building of hot summer and warm winter region
Body of wall energy-conserving product.
Most important for the selection of the phase-change material of architectural exterior-protecting construction, it should have a following feature: (1) latent heat of fusion
High so that it is to preserve in phase transformation or release more heat；(2) there is suitable phase transition temperature, the spy that needs control can be met
Fixed temperature；(3) phase transition process good reversibility, expansibility and contractibility is little, supercool or superheating phenomenon is few；(4) heat conductivity is big, close
Degree is big, and specific heat capacity is big；(5) phase-change material is nontoxic, non-corrosiveness, and low cost is easily manufactured.
The research to organic phase change material abroad starts to walk to compare early, just considers to store up the heat accumulation of phase-change material at the beginning of the eighties in last century
Cold function is applied in building, and phase-change material is attached to concrete wall, gypsum wallboard, roof, shutter, ceiling
With in floor heating system, can effectively reduce indoor day and night temperature, improve hot comfort, transfer building power peak value is born
Lotus and reduction energy consumption.The research of domestic phase-changing energy storage material is the most still partial to the material of laboratory stage and is prepared, form
On solidifying and being heat conduction reinforced, the phase-change material actual application in architectural exterior-protecting construction is the most less.
Summary of the invention
For solving the problems referred to above, the invention provides the preparation method of a kind of phase-change material with Petiolus Trachycarpi oil as raw material, by preparation
The method that binary phase-change material uses microcapsule encapsulation or porous media matrix to be combined carries out form solidification, is combined into construction material
There is the complex building building enclosure of energy-conservation character, it is adaptable to hot summer and warm winter region.
The present invention is with Petiolus Trachycarpi oil as raw material, and Petiolus Trachycarpi oil is the oils and fats extracted by oil palm fruit mesocarp, is that yield is maximum the most in the world
Tropical xylophyta oil, the present invention effectively utilizes biomass resource, can not only realize low-carbon emission reduction, preserve the ecological environment, also
Can be that society produces multi value.
The present invention is achieved by the following technical programs:
It is an object of the invention to provide the preparation method of a kind of phase-change material with Petiolus Trachycarpi oil as raw material, comprise the steps:
(1) preparation of essence methyl ester: add Petiolus Trachycarpi oil and methanol that mol ratio is 1:2～1:5 in reaction vessel, be heated with stirring to
Add catalyst sodium methoxide when 50～75 DEG C to final concentration of mass percent 0.6%, take methyl ester after reaction 5～15min and carry out the mutually
Secondary ester exchange reaction, adds Petiolus Trachycarpi oil and methanol that mol ratio is 1:1～1:5, adds catalyst sodium methoxide to end at 50～75 DEG C
Concentration is mass percent 0.2～0.4%, adds phosphoric acid solution and be neutralized to neutrality after reaction 15～30min, and stirring takes methyl ester phase,
Washed, be dried, obtained essence methyl ester；
(2) preparation of saturated fatty acid methyl ester: add carbamide in reaction vessel and mass percent is the ethanol solution of 95%,
The mass ratio of carbamide and ethanol is 1:2～1:3.5, heated and stirred, condensing reflux, and carbamide adds the step (1) of 45～55 DEG C after dissolving
The smart methyl ester of preparation, the mass ratio of essence methyl ester and carbamide is 1:1～1:2.5,70～90 DEG C of backflows, pours in container and seals, at 5 DEG C
Placing 16～24h and carry out inclusion, vacuum filtration, isolated solid phase and liquid phase, solid phase adds water heating makes urine bag thing decompose, and uses
Acid adjusts pH value to 5～6, extracts and is dried, obtains saturated fatty acid methyl ester；
(3) preparation of phase-change material: saturated fatty acid methyl ester prepared by step (2) and hexadecanol 2.5:1～10:1 in mass ratio
Mix at room temperature, be combined into binary phase-change material.
Compound binary phase-change material is combined with construction substrate, can choose following technique: 1) is encapsulated by binary phase transformation material seal and is placed in
In construction material；2) by soaking the building material substrate that binary phase-change material is penetrated into porous (as gypsum wallboard, cement concrete try
Block etc.)；3) binary phase-change material is directly mixed with construction material.
The urea adduct method that step of the present invention (2) proposes is a kind of more common urea clathration method, and its principle is
Urea molecule easily forms more stable crystal inclusion compound, under freezing conditions with saturated or monounsaturated fatty acid in crystallization process
Crystallization, and polyunsaturated fatty acid is more due to double bond, carbochain bends, and has certain space structure, is difficult to by carbamide
Inclusion.Filter method is used to remove the clathrate that satisfied fatty acid and monounsaturated fatty acid are formed with carbamide, i.e. available higher
The polyunsaturated fatty acid of purity.The separating effect of urea adduct method is affected by crystallization temperature and amount of urea, and crystallization temperature is more
Low, amount of urea is the most, and products obtained therefrom purity is the highest, but product yield is the lowest.In order to improve product purity, can use repeatedly
Urea adduct method.Urea adduct method cost is relatively low, and application is relatively universal, but is difficult to by fatty acid close for double key number separately.
Preferably, the mass ratio of described saturated fatty acid methyl ester and hexadecanol is 7:1.
Preferably, the phase transition temperature of described phase-change material is 22～27 DEG C, and latent heat of phase change is 160～190J/g.
The invention has the beneficial effects as follows: the present invention selects Petiolus Trachycarpi oil to be that phase-change material prepared by raw material, this melt material latent heat is high, phase
Becoming reversibility of heat conduction process good, expansibility and contractibility is little, supercool few with superheating phenomenon, and low cost is easily manufactured, compatible with construction material
Property is good.Phase-change material is attached in concrete wall, gypsum wallboard, roof, shutter, ceiling, it is achieved biomass material
Material application in architectural exterior-protecting construction, can effectively reduce indoor day and night temperature, improves hot comfort, transfer building electricity
Power peak load and reduction energy consumption.
Accompanying drawing explanation
When Fig. 1 is saturated fatty acid methyl ester and hexadecanol mass ratio 7:1, saturated fatty acid methyl ester and hexadecanol binary phase-change material
DSC tests figure.
Detailed description of the invention
Below in conjunction with instantiation, it is further elucidated with the present invention.It should be understood that these embodiments are merely to illustrate the present invention, and
It is not intended to limit the scope of the invention.Technical staff makes according to the present invention in actual applications improvement and adjustment, still belong to
In protection scope of the present invention.
Except special instruction, equipment and raw material that the present invention uses are the art routine commercial products.
The preparation method of a kind of phase-change material with Petiolus Trachycarpi oil as raw material, comprises the steps:
(1) preparation of essence methyl ester: add Petiolus Trachycarpi oil and methanol that mol ratio is 1:2～1:5 in reaction vessel, be heated with stirring to
Add catalyst sodium methoxide when 50～75 DEG C to final concentration of mass percent 0.6%, take methyl ester after reaction 5～15min and carry out the mutually
Secondary ester exchange reaction, adds Petiolus Trachycarpi oil and methanol that mol ratio is 1:1～1:5, adds catalyst sodium methoxide to end at 50～75 DEG C
Concentration is mass percent 0.2～0.4%, adds phosphoric acid solution and be neutralized to neutrality after reaction 15～30min, and stirring takes methyl ester phase,
Washed, be dried, obtained essence methyl ester；
(2) preparation of saturated fatty acid methyl ester: add carbamide in reaction vessel and mass percent is the ethanol of 95%, carbamide
Being 1:2～1:3.5 with the mass ratio of ethanol, heated and stirred, condensing reflux, carbamide adds step (1) system of 45～55 DEG C after dissolving
Standby smart methyl ester, the mass ratio of essence methyl ester and carbamide is 1:1～1:2.5,70～90 DEG C of backflows, pours in container and seals, transfers for 5 DEG C
Putting 16～24h and carry out inclusion, vacuum filtration, isolated solid phase and liquid phase, solid phase adds water heating makes urine bag thing decompose, with acid
Adjust pH value to 5～6, extract and be dried, obtain saturated fatty acid methyl ester；
(3) preparation of phase-change material: saturated fatty acid methyl ester prepared by step (2) and hexadecanol 2.5:1～10:1 in mass ratio
Mixing, is combined into binary phase-change material.
The urea adduct method that the present invention proposes is a kind of more common urea clathration method, and its principle is urea molecule
Easily form more stable crystal inclusion compound with saturated or monounsaturated fatty acid in crystallization process, under freezing conditions crystallization,
And polyunsaturated fatty acid is more due to double bond, carbochain bends, and has certain space structure, is difficult to by urea clathration.Use
Filter method removes the clathrate that satisfied fatty acid and monounsaturated fatty acid are formed with carbamide, i.e. can get higher degree many not
Satisfied fatty acid.The separating effect of urea adduct method is affected by crystallization temperature and amount of urea, and crystallization temperature is the lowest, and carbamide is used
Measuring the most, products obtained therefrom purity is the highest, but product yield is the lowest.In order to improve product purity, repeatedly urea adduct method can be used.
Urea adduct method cost is relatively low, and application is relatively universal, but is difficult to by fatty acid close for double key number separately.
Embodiment 1
The preparation method of a kind of phase-change material with Petiolus Trachycarpi oil as raw material, comprises the steps:
(1) preparation of essence methyl ester: add Petiolus Trachycarpi oil and methanol that mol ratio is 1:2 in there-necked flask, stir (100r/min)
Add catalyst sodium methoxide when being heated to 50 DEG C to final concentration of mass percent 0.6%, take methyl ester after reaction 5min and carry out the mutually
Secondary ester exchange reaction, adds Petiolus Trachycarpi oil and methanol that mol ratio is 1:1, stirs (100r/min), adds catalyst at 50 DEG C
Feldalat NM, to final concentration of mass percent 0.2%, adds phosphoric acid solution after reaction 15min and is neutralized to neutrality, and stirring takes methyl ester
Phase, is washed, and is dried, and obtains essence methyl ester；
(2) preparation of saturated fatty acid methyl ester: use urea clathration partition method to separate essence methyl ester, add carbamide in there-necked flask
Being 1:2 with the mass ratio that mass percent is the ethanol of 95%, carbamide and ethanol, heated and stirred, condensing reflux, after carbamide dissolves
Adding smart methyl ester prepared by the step (1) of 45 DEG C, the mass ratio of essence methyl ester and carbamide is 1:1,70～90 DEG C of backflow 60min, falls
Enter in beaker with plastic film sealing, place 16h at 5 DEG C and carry out inclusion, vacuum filtration, isolated solid phase and liquid phase, solid phase
Adding water heating makes urine bag thing decompose, and adjusts pH value to 5～6 with the hydrochloric acid solution that concentration is 6mol/L, adds petroleum ether extraction 2
Secondary, anhydrous sodium sulfate is dried, and obtains saturated fatty acid methyl ester；
(3) preparation of phase-change material: saturated fatty acid methyl ester step (2) prepared and hexadecanol 2.5:1 in mass ratio are often
Temperature mixing, is combined into binary phase-change material.
Embodiment 2
The preparation method of a kind of phase-change material with Petiolus Trachycarpi oil as raw material, comprises the steps:
(1) preparation of essence methyl ester: add Petiolus Trachycarpi oil and methanol that mol ratio is 1:3.5 in there-necked flask, stir (100r/min),
Add catalyst sodium methoxide extremely final concentration of mass percent 0.6% when 65 DEG C, take methyl ester after reaction 10min and carry out second time ester mutually
Exchange reaction, adds Petiolus Trachycarpi oil and methanol that mol ratio is 1:2, stirs (100r/min), adds catalyst sodium methoxide at 65 DEG C
To final concentration of mass percent 0.3%, add phosphoric acid solution after reaction 25min and be neutralized to neutrality, be slowly stirred 5min, go
Methyl ester phase, washs with saturated aqueous common salt after removing unnecessary methanol, and anhydrous sodium sulfate is dried, and obtains essence methyl ester；
(2) preparation of saturated fatty acid methyl ester: use urea clathration partition method to separate essence methyl ester, add carbamide in there-necked flask
Being 1:2.7 with the mass ratio that mass percent is the ethanol of 95%, carbamide and ethanol, heated and stirred, condensing reflux, carbamide dissolves
The smart methyl ester of rear addition about 50 DEG C, the mass ratio of carbamide and essence methyl ester is 3.5:2, then 70～90 DEG C of backflow 60min, then
Pouring in beaker with plastic film sealing, place 18h and carry out inclusion at 5 DEG C, after inclusion is complete, vacuum filtration, isolated is solid
Phase and liquid phase, solid phase adds water heating makes urine bag thing decompose, and adjusts pH value to 5～6 with the hydrochloric acid solution that concentration is 6mol/L, adds
Entering petroleum ether extraction 2 times, anhydrous sodium sulfate is dried, and obtains saturated fatty acid methyl ester；
(3) preparation of phase-change material: saturated fatty acid methyl ester and hexadecanol 2.5:1 in mass ratio that step (2) prepares exist
Room temperature mixes, and prepares binary composite phase-change material.
Embodiment 3
The preparation method of a kind of phase-change material with Petiolus Trachycarpi oil as raw material, comprises the steps:
(1) preparation of essence methyl ester: using urea clathration partition method to separate essence methyl ester, adding mol ratio in there-necked flask is 1:5
Petiolus Trachycarpi oil and methanol, add catalyst sodium methoxide when being heated with stirring to 75 DEG C to final concentration of mass percent 0.6%, reaction
Take methyl ester after 5～15min and carry out second time ester exchange reaction mutually, add Petiolus Trachycarpi oil and methanol that mol ratio is 1:5, add at 75 DEG C
Catalyst sodium methoxide, to final concentration of mass percent 0.4%, adds phosphoric acid solution after reaction 30min and is neutralized to neutrality, stirring,
Take methyl ester phase, washed, be dried, obtain essence methyl ester；
(2) preparation of saturated fatty acid methyl ester: add carbamide in there-necked flask and mass percent is the ethanol of 95%, carbamide
Being 1:3.5 with the mass ratio of ethanol, heated and stirred, condensing reflux, carbamide adds essence prepared by the step (1) of 55 DEG C after dissolving
Methyl ester, the mass ratio of essence methyl ester and carbamide is 1:2.5,70～90 DEG C of backflow 60min, is subsequently poured in beaker and uses plastic film sealing,
Placing 24h at 5 DEG C and carry out inclusion, vacuum filtration, isolated solid phase and liquid phase, solid phase adds water heating makes urine bag thing decompose,
Adjust pH value to 5～6 with acid, extract and be dried, obtain saturated fatty acid methyl ester；
(3) preparation of phase-change material: saturated fatty acid methyl ester step (2) prepared and hexadecanol 2.5:1 in mass ratio are often
Temperature mixing, is combined into binary phase-change material.
Embodiment 4
Same as in Example 2, difference is:
Saturated fatty acid methyl ester and hexadecanol mass ratio are 5:1.
Embodiment 5
Same as in Example 2, difference is:
Saturated fatty acid methyl ester and hexadecanol mass ratio are 6:1.
Embodiment 6
Same as in Example 2, difference is:
Saturated fatty acid methyl ester and hexadecanol mass ratio are 7:1.
Embodiment 7
Same as in Example 2, difference is:
Saturated fatty acid methyl ester and hexadecanol mass ratio are 10:1.
Binary composite phase-change material embodiment 2, embodiment 4, embodiment 5, embodiment 6 and embodiment 7 prepared is surveyed
Its T fixedm(fusing point), Tc(crystallization temperature) and Hm(melting enthalpy), as shown in table 1.
Table 1 saturated fatty acid methyl ester-hexadecanol binary phase-change material
As shown in Table 1, its phase transition temperature of binary composite phase-change material that the present invention prepares is 22～27 DEG C, and latent heat of phase change is
160～190J/g.Such as, when being 7:1 for embodiment 6 saturated fatty acid methyl ester and hexadecanol mass ratio, this phase-change material is done
DSC tests, as it is shown in figure 1, this figure shows that the fusing point of binary phase-change material is 25.03 DEG C, crystallization temperature is 21.98 DEG C, molten
Melting enthalpy is 183.3J/g.
Above-listed detailed description is illustrating for possible embodiments of the present invention, and this embodiment also is not used to limit the special of the present invention
Profit scope, all equivalences done without departing from the present invention are implemented or change, are intended to be limited solely by the scope of patent protection of this case.
Claims (3)
1. the preparation method of the phase-change material with Petiolus Trachycarpi oil as raw material, it is characterised in that comprise the steps:
(1) preparation of essence methyl ester: add Petiolus Trachycarpi oil and methanol that mol ratio is 1:2～1:5 in reaction vessel, be heated with stirring to
Add catalyst sodium methoxide when 50～75 DEG C to final concentration of mass percent 0.6%, take methyl ester after reaction 5～15min and carry out the mutually
Secondary ester exchange reaction, adds Petiolus Trachycarpi oil and methanol that mol ratio is 1:1～1:5, adds catalyst sodium methoxide to end at 50～75 DEG C
Concentration is mass percent 0.2～0.4%, adds phosphoric acid solution and be neutralized to neutrality after reaction 15～30min, and stirring takes methyl ester phase,
Washed, be dried, obtained essence methyl ester；
(2) preparation of saturated fatty acid methyl ester: add carbamide in reaction vessel and mass percent is the ethanol solution of 95%,
The mass ratio of carbamide and ethanol is 1:2～1:3.5, heated and stirred, condensing reflux, and carbamide adds the described step of 45～55 DEG C after dissolving
Suddenly the smart methyl ester that prepared by (1), the mass ratio of essence methyl ester and carbamide is 1:1～1:2.5,70～90 DEG C of backflows, pours in container and seals,
Placing 16～24h at 5 DEG C and carry out inclusion, vacuum filtration, isolated solid phase and liquid phase, solid phase adds water heating makes urine bag thing divide
Solve, adjust pH value to 5～6 with acid, extract and be dried, obtain saturated fatty acid methyl ester；
(3) preparation of phase-change material: the saturated fatty acid methyl ester described step (2) prepared and hexadecanol are in mass ratio
2.5:1～10:1 mixes, and is combined into binary phase-change material.
The preparation method of the phase-change material with Petiolus Trachycarpi oil as raw material the most according to claim 1, it is characterised in that: described saturated fat
The mass ratio of fatty acid methyl esters and hexadecanol is 7:1.
The preparation method of the phase-change material with Petiolus Trachycarpi oil as raw material the most according to claim 1, it is characterised in that: phase transition temperature is
22～27 DEG C, latent heat of phase change is 160～190J/g.
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| CN109628069A (en) * | 2018-12-24 | 2019-04-16 | 北京三聚环保新材料股份有限公司 | A kind of phase-changing energy storage material and preparation method thereof |
| CN109628069B (en) * | 2018-12-24 | 2021-02-19 | 北京三聚环保新材料股份有限公司 | Phase-change energy storage material and preparation method thereof |
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| CN105925249B (en) | 2019-08-06 |
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