CN101838521B - Preparation method of aliphatic dibasic acid/bentonite composite phase change energy storage material - Google Patents
Preparation method of aliphatic dibasic acid/bentonite composite phase change energy storage material Download PDFInfo
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- CN101838521B CN101838521B CN2010101690754A CN201010169075A CN101838521B CN 101838521 B CN101838521 B CN 101838521B CN 2010101690754 A CN2010101690754 A CN 2010101690754A CN 201010169075 A CN201010169075 A CN 201010169075A CN 101838521 B CN101838521 B CN 101838521B
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Abstract
The invention relates to a preparation method of a composite phase change energy storage material by using bentonite as a base body and using aliphatic dibasic acid as a phase change energy storage body, which belongs to the technical field of the preparing technology of energy storage materials and comprises the steps of: putting the bentonite, CTAB (cetyltriethylammnonium bromide) and deionized water into a reaction container to heat and stir; modifying the bentonite; preparing a eutectic system of aliphatic dibasic acid by using myristic acid (MA) and palmitic acid (PA), or lauric acid (LA) and myristic acid (MA); heating 20% to 37% of eutectic mixture of the aliphatic dibasic acid, 26% to 42% of modified bentonite and 36% to 44% of absolute ethyl alcohol in the reaction container to 75 DEG C; stirring for 2 hours; and drying a product in the reaction container to constant weight to obtain the aliphatic dibasic acid/bentonite composite phase change material. The material has good heat storage capability and the stability of storing heat circulation, and can be used for the fields of using waste heat, residual heat and solar energy and the like.
Description
Technical field
The invention belongs to the energy-storage composite material field, being specifically related to a kind of is that base, binary lipid acid are the preparation method of the composite phase-change energy storage material of energy storage main body with the modification bentonite.
Background technology
At present, most inorganics phase change materials all have certain corrodibility, and in phase transition process, have shortcomings such as cold-peace is separated, and influence the ability and the work-ing life of its energy storage.And lipid acid corrodibility is little, and condensate depression is little in phase transition process, or does not almost have shortcomings such as cold-peace is separated, and its chemical property is also stable, low price, is comparatively ideal organic phase change energy storage material; But the transformation temperature of single fat acid is higher; Be difficult to adapt to the requirement of low temperature accumulator system, and the low shortcoming of organism phase change material ubiquity thermal conductivity, this causes its thermal storage performance in the application of heat reservoir poor; The heat accumulation capacity usage ratio is low, thereby has reduced the practical effect of its energy storage.Therefore, with the eutectic system of binary lipid acid material of main part, carry out compound with the high inorganics of thermal conductivity again and prepare novel composite phase-change energy storage material, for a new way has been created in the research and development of energy storage material as phase-change accumulation energy.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of binary lipid acid/bentonite composite phase-change energy storage material.
The present invention provides the preparation method of a kind of binary lipid acid and modification bentonite composite phase-change energy storage material, and this method has lower transformation temperature, is adapted to the requirement of low temperature accumulator system, and compound with the high inorganics bentonite of thermal conductivity.Concrete technological process and step are following:
The first step: bentonite organically-modified: its raw material moity and weight percent are:
Bentonite 32%～44%
Cetyl trimethylammonium bromide (CTAB) 12%～32%
Deionized water 26%～46%
Concrete operations are: take by weighing each raw material by above-mentioned prescription, at first an amount of bentonite, CTAB and deionized water are placed reaction vessel, be heated to 80 ℃, stirred 24 hours; Pass through suction filtration subsequently, and leach thing, in washing water, no longer contain the halogen ion with 80 ℃ deionized water wash; Place 80 ℃ baking oven to dry the product after the washing, can obtain having enlarged the modification bentonite of interlamellar spacing.
Second step: the eutectic system preparation of binary lipid acid: its raw material moity and weight percent are:
Myristic acid (MA) and palmitinic acid (PA) 58: 42, perhaps
LAURIC ACID 99 MIN (LA) and myristic acid (MA) 66: 34
Concrete operations are: take by weighing each raw material by above-mentioned formula rate, mix placing encloses container, heating whole fusions of mixture in container are liquid, and restir 2 hours is incubated 1 hour, makes the system thorough mixing even; Subsequently the mixture in the container is cooled to room temperature, takes out and, promptly get corresponding binary lipid acid eutectic miscellany its grinding.The 3rd step: the preparation of organic and inorganic composite phase-change material: its raw material is formed and weight percent is:
Made binary lipid acid eutectic miscellany 20%～37% of second step
The modification bentonite 26%～42% that the first step is made
Absolute ethyl alcohol 36%～44%
Concrete operations are: take by weighing each raw material by above-mentioned prescription, in the absolute ethyl alcohol adding reaction vessel with prepared modification bentonite of the first step and 2/3rds amounts, fully stirred 30 minutes; Place another container to mix wiring solution-forming with the absolute ethyl alcohol of 1/3rd amounts prepared binary lipid acid eutectic mixture of second step; The ethanolic soln that will be mixed with binary lipid acid eutectic mixture is subsequently poured in the reaction vessel that is mixed with modification bentonite dispersion liquid, is heated to 75 ℃, stirs 2 hours; After at last the product in the reaction vessel being dried to constant weight, promptly get binary lipid acid/bentonite composite phase-change material.
The characteristics of the inventive method: because the transformation temperature of single fat acid is higher; Be difficult to satisfy the requirement of low temperature accumulator system (＜100 ℃); The eutectic mixture that the present invention adopts the lipid acid binary system can reduce the transformation temperature of material as the phase change material main body, is suitable for the requirement of low temperature accumulator system.Shortcomings such as the plastic crystal that is had to existing energy storage material simultaneously, mistake is cold and be separated; Binary lipid acid phase change material and the high inorganics bentonite of thermal conductivity are carried out compound, through the liquid phase intercalation method binary lipid acid phase change material is inserted between the nanometer layer of bentonite and prepare the composite shape-setting phase-changing energy storage material.Enthalpy of phase change and the transformation temperature that experiment records LA-MA and MA-PA energy storage material after compound be respectively 132.38J/g, 36 ℃ and 97.95J/g, 32 ℃; Through continuous 800 times store thermal cycling after; The rate of fall-off of the two enthalpy of phase change is respectively 26.0% and 9.9%, and experimental result shows that the transformation temperature of matrix material decreases; And the rate of fall-off of material phase transformation enthalpy is less, and work-ing life is longer.
Embodiment
After specific embodiment of the present invention being described at present.
Embodiment one: takes by weighing bentonite 10g, CTAB7.42g, deionized water 10g, pours in the beaker of 250mL, stirred 24 hours in 80 ℃ of constant temperature, and suction filtration, and be washed till in the washing water not Halogen ion with 80 ℃ of zero(ppm) water.In 80 ℃ of baking ovens, dry, it is last for use to pulverize.Take by weighing myristic acid 2.95g, palmitinic acid 2.08g, it is mixed in the sealed vessel, being heated to whole fusions is liquid, stirs 2 hours and is incubated 1 hour, makes the system thorough mixing, is cooled to room temperature again, with its grind the eutectic mixture of myristic acid-palmitinic acid.Taking by weighing, modification bentonite 10g, absolute ethyl alcohol 15g fully stir after 30 minutes in beaker; Myristic acid-palmitinic acid eutectic mixture with 5g is dissolved in the absolute ethyl alcohol of 5g again; Pour in the dispersion liquid of modification bentonite, 75 ℃ of temperature controls stirred 2 hours; Product grinds and promptly gets myristic acid-palmitinic acid/bentonite composite phase-change material (PCM) after being dried to constant weight.
Detect with WCT-1A microcomputer differential thermal balance, the solubility curve peak value that records this material is 32 ℃, and latent heat of phase change is 97.95J/g.
Embodiment two: takes by weighing bentonite 10g, CTAB4.92g, deionized water 10g, pours in the beaker of 250mL, stirred 24 hours in 80 ℃ of constant temperature of magnetic force, and suction filtration, and be washed till in the washing water not Halogen ion with 80 ℃ of zero(ppm) water.In 80 ℃ of baking ovens, dry, it is last for use to pulverize.Take by weighing LAURIC ACID 99 MIN 3.12g, myristic acid 2.04g, it is mixed in the sealed vessel, being heated to whole fusions is liquid, stirs 2 hours and is incubated 1 hour, makes the system thorough mixing, is cooled to room temperature again, with its grind LAURIC ACID 99 MIN-myristic acid eutectic mixture.Taking by weighing, modification bentonite 10g, absolute ethyl alcohol 15g fully stir after 30 minutes in beaker; LAURIC ACID 99 MIN-myristic acid eutectic mixture with 5g is dissolved in the absolute ethyl alcohol of 5g again; Pour in the dispersion liquid of modification bentonite, 75 ℃ of temperature controls stirred 2 hours; Product grinds and promptly gets LAURIC ACID 99 MIN-myristic acid/bentonite composite phase-change material (PCM) after being dried to constant weight.
Detect with WCT-1A microcomputer differential thermal balance, the solubility curve peak value that records this material is 36 ℃, and latent heat of phase change is 132.38J/g.
Can know that from the foregoing description the binary lipid acid/bentonite composite phase-change energy storage material of the inventive method preparation has energy storage capacity preferably, its latent heat of phase change numerical value is higher, helps absorbing of used heat, waste heat.
Claims (1)
1. the preparation method of binary lipid acid/bentonite composite phase-change energy storage material is characterized in that having following technological process and step:
The first step: bentonite organically-modified: its raw material moity and weight percent are:
Bentonite 32%～44%
Cetyl trimethylammonium bromide 12%～32%
Deionized water 26%～46%
Concrete operations are: take by weighing each raw material by above-mentioned prescription, at first an amount of bentonite, CTAB and deionized water are placed reaction vessel, be heated to 80 ℃, stirred 24 hours; Pass through suction filtration subsequently, and leach thing, in washing water, no longer contain the halogen ion with 80 ℃ deionized water wash; Place 80 ℃ baking oven to dry the product after the washing, can obtain having enlarged the modification bentonite of interlamellar spacing;
Second step: the eutectic system preparation of binary lipid acid: its raw material moity and weight percent are:
Myristic acid and palmitinic acid 58: 42, perhaps
LAURIC ACID 99 MIN and myristic acid 66: 34
Concrete operations are: take by weighing each raw material by above-mentioned prescription, mix placing encloses container, heating whole fusions of mixture in container are liquid, restir 2 hours, and be incubated 1 hour, make the system thorough mixing even; Subsequently the mixture in the container is cooled to room temperature, takes out and it is ground and promptly get corresponding binary lipid acid eutectic miscellany;
The 3rd step: the preparation of binary lipid acid/bentonite composite phase-change material: its raw material is formed and weight percent is:
Made binary lipid acid eutectic miscellany 20%～37% of second step
The modification bentonite 26%～42% that the first step is made
Absolute ethyl alcohol 36%～44%
Concrete operations are: take by weighing each raw material by above-mentioned prescription, in the absolute ethyl alcohol adding reaction vessel with prepared modification bentonite of the first step and 2/3rds amounts, fully stirred 30 minutes; Place another container to mix wiring solution-forming with the absolute ethyl alcohol of 1/3rd amounts prepared binary lipid acid eutectic mixture of second step; The ethanolic soln that will be mixed with binary lipid acid eutectic mixture is subsequently poured in the reaction vessel that is mixed with modification bentonite dispersion liquid, is heated to 75 ℃, stirs 2 hours; At last with the product in the reaction vessel after being dried to constant weight, promptly get binary lipid acid/bentonite composite phase-change material.
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| CN105542723A (en) * | 2016-01-18 | 2016-05-04 | 苏州法斯特信息科技有限公司 | Nanometer composite phase-change textile material and preparation method thereof |
| CN105647482B (en) * | 2016-01-20 | 2018-10-30 | 福州大学 | A kind of ternary aliphatic acid/modified expanded vermiculite composite phase-change energy storage material |
| CN107619657A (en) * | 2016-07-16 | 2018-01-23 | 山东森森矿业新材料有限公司 | A kind of volcanic ash figuration composite phase-changing material and preparation method thereof |
| CN110408143A (en) * | 2019-06-27 | 2019-11-05 | 湖北英特吉新能源科技有限公司 | A kind of foaming figuration composite phase-changing material and preparation method thereof |
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