CN111499311A - Compound fatty acid low-temperature phase change cement concrete material and preparation method thereof - Google Patents

Compound fatty acid low-temperature phase change cement concrete material and preparation method thereof Download PDF

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Publication number
CN111499311A
CN111499311A CN202010424510.7A CN202010424510A CN111499311A CN 111499311 A CN111499311 A CN 111499311A CN 202010424510 A CN202010424510 A CN 202010424510A CN 111499311 A CN111499311 A CN 111499311A
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phase change
preparation
fatty acid
concrete material
cement concrete
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Inventor
朱洪洲
代思
杨孝思
李夏
唐浩
谭祺琦
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Chongqing Jiaotong University
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Chongqing Jiaotong University
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/04Portland cements
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-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
    • C09K5/02Materials undergoing a change of physical state when used
    • C09K5/06Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474Uses not provided for elsewhere in C04B2111/00
    • C04B2111/0075Uses not provided for elsewhere in C04B2111/00 for road construction

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention belongs to the technical field of concrete materials, and discloses a compound fatty acid low-temperature phase-change cement concrete material and a preparation method thereof, wherein the compound fatty acid low-temperature phase-change cement concrete material is prepared from the following raw materials in parts by weight: 100 parts of ordinary Portland cement; 337 parts of limestone; 190 parts of river sand; 40 parts of tap water; and 20 parts of a shaped composite phase change material. The preparation method of the compound fatty acid low-temperature phase change cement concrete material comprises the following steps: weighing the raw materials according to the mixing ratio; pouring the shaped composite phase change material and river sand into a stirrer together, and stirring in advance; and adding portland cement, limestone and tap water, and mixing to obtain the compound fatty acid low-temperature phase change cement concrete material. The phase change concrete material can delay the time of starting ice condensation on the surface to a certain extent, thereby achieving the effect of ice condensation resistance.

Description

Compound fatty acid low-temperature phase change cement concrete material and preparation method thereof
Technical Field
The invention belongs to the technical field of concrete materials, and particularly relates to a compound fatty acid low-temperature phase change cement concrete material and a preparation method thereof.
Background
At present, the ice condensation phenomenon is easily generated on the surface of roads in part of areas in winter, the friction coefficient of the road surface is reduced by thin ice, great hidden danger is caused to the driving safety, and the development, research, application and popularization of the scientific and effective road surface ice and snow removing technology have very important social and economic values.
Phase Change Materials (PCM), also called phase change energy storage materials, belong to the category of energy materials, and refer to materials that can be used for energy storage by using a large amount of heat energy absorbed (released) when the phase change materials change states. The phase change process of the material is usually accompanied with the absorption and release of energy, and the energy is called latent heat of phase change and has good application value. The phase-change material is applied to the cement pavement so as to actively adjust the pavement temperature, and has wide application prospect and environmental friendliness. The cement road surface is subject to the influence of external factors such as repeated action of traffic load, climate condition change and the like in the using process, and the construction process of paving needs to be considered. Therefore, the performance requirement of the phase change material applied to the cement pavement is high. The existing single fatty acid material cannot meet the requirement of phase transition temperature. Therefore, a new compound fatty acid low-temperature phase change cement concrete material is needed to solve the problems in the prior art and meet the requirements of buildings.
In summary, the problems of the prior art are as follows: the phase transition temperature of the existing single fatty acid material is regularly changed along with the increase of the number of carbon atoms, the temperature is between-10 ℃ and 35 ℃, the requirement of the phase transition temperature (0-5 ℃) cannot be met, and the material is not suitable to be used as an anti-freezing phase transition material.
The difficulty of solving the technical problems is as follows: determining the theoretical lowest eutectic point of a fatty dibasic acid phase change system, preparing the binary phase change system, and exploring the long-term service performance of the compound fatty acid.
The significance of solving the technical problems is as follows: the phase transition temperature of the compound fatty acid is proper, the stability is good, and the compound fatty acid can be used as an anti-freezing phase transition material to prepare low-temperature phase transition concrete.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a compound fatty acid low-temperature phase change cement concrete material and a preparation method thereof.
The invention is realized in such a way that the compound fatty acid low-temperature phase-change cement concrete material is prepared from the following raw materials in parts by weight:
100 parts of Portland cement; 337 parts of limestone; 190 parts of river sand; 40 parts of tap water; and 20 parts of shaped composite Phase Change Materials (PCMs).
The invention also aims to provide a preparation method of the compound fatty acid low-temperature phase change cement concrete material, which comprises the following steps:
step one, weighing raw materials according to a mixing ratio;
pouring the shaped composite phase change material and river sand into a stirrer together, and stirring in advance;
and step three, adding portland cement, limestone and tap water, and mixing to obtain the compound fatty acid low-temperature phase change cement concrete material.
Further, the preparation method of the shaped composite phase change material comprises the following steps:
(1) preparation of a binary phase change system:
1) the raw materials comprise the following components in percentage by mass: n-octanoic acid and n-decanoic acid 1: 1;
2) the specific operation is as follows: mixing the raw materials according to the formula in a beaker, placing the beaker in a water bath environment at the temperature of 60 ℃, and stirring the mixture for 15min at the speed of 200r/min to obtain the octanoic acid-decanoic acid eutectic substance.
(2) Preparing expanded graphite:
and (3) placing the expandable graphite in an oven, drying for 2 hours at 100 ℃, taking out and spreading in a crucible, placing the crucible in a muffle furnace at 900 ℃ for calcining for 60s, taking out and cooling to prepare the completely expanded expandable graphite.
(3) Preparing a shaped composite phase change material:
1) placing the expanded graphite in a 100 ℃ oven for 2h, and fully drying;
2) weighing a certain mass of fully dried expanded graphite, adding the fully dried expanded graphite into a beaker, and pouring the octanoic acid-decanoic acid eutectic substance until the expanded graphite is completely submerged;
3) placing the beaker in a 60 ℃ water bath kettle, and stirring for 30min by a constant speed stirrer at the rotating speed of 160rad/min, wherein the expanded graphite on the wall of the beaker is scraped off;
4) pouring the stirred uniform mixture into a funnel, connecting a vacuum pump for suction filtration until no liquid drips at the bottom of the funnel, repeatedly washing the beaker by using filtrate, and performing suction filtration until no expanded graphite residue exists in the beaker;
5) and (3) putting the solid obtained by suction filtration into an oven for air blast drying at the temperature of 80 ℃, taking out and weighing at intervals of half an hour, and observing the surface drying state of the solid until the mass loss rate of the material is reduced and the sample is loose and granular, thus completing the preparation of the composite material.
In summary, the advantages and positive effects of the invention are: the invention adopts the caprylic-capric acid eutectic substance with the mass ratio of 1:1 as a proper anti-freezing ice phase-change material, and the eutectic substance has proper phase-change temperature and good stability. Meanwhile, the anti-icing phase-change material is in a liquid state at normal temperature, and the liquid phase-change material is directly doped into concrete to influence the hydration hardening of cement and directly influence the pavement performance. The phase change concrete is directly doped with 3 percent of PCMs (prestressed concrete) by mass based on common concrete, and the PCMs and fine aggregates are poured into a stirrer together and stirred in advance to obtain the compound fatty acid low-temperature phase change cement concrete material in order to avoid uneven stirring during stirring. The simulation ice condensation test proves that the time for the phase change concrete to start ice condensation on the surface can be delayed to a certain extent, so that the effect of resisting ice condensation is achieved.
Drawings
FIG. 1 is a flow chart of a preparation method of a compounded fatty acid low-temperature phase-change cement concrete material provided by an embodiment of the invention.
FIG. 2 is a DSC plot of the caprylic-capric acid eutectic before and after the phase transition cycle provided by the present invention.
FIG. 3 is an infrared spectrum of the octanoic acid-decanoic acid eutectic before and after phase transition according to the embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a compound fatty acid low-temperature phase change cement concrete material and a preparation method thereof, and the invention is described in detail below with reference to the accompanying drawings.
The compound fatty acid low-temperature phase change cement concrete material provided by the embodiment of the invention is prepared from the following raw materials in parts by weight: cement: 100 parts of Portland cement; coarse aggregate: 337 parts of limestone; fine aggregate: 190 parts of river sand; water: 40 parts of tap water; and 20 parts of shaped composite Phase Change Materials (PCMs).
As shown in fig. 1, the preparation method of the compounded fatty acid low-temperature phase change cement concrete material provided by the embodiment of the invention comprises the following steps:
s101: weighing the raw materials according to the mixing ratio;
s102: pouring the shaped composite phase change material and river sand into a stirrer together, and stirring in advance;
s103: and adding portland cement, limestone and tap water, and mixing to obtain the compound fatty acid low-temperature phase change cement concrete material.
The preparation method of the shaped composite phase change material provided by the embodiment of the invention comprises the following steps:
(1) preparation of a binary phase change system:
1) the raw materials comprise the following components in percentage by mass: n-octanoic acid and n-decanoic acid 1: 1;
2) the specific operation is as follows: mixing the raw materials according to the formula in a beaker, placing the beaker in a water bath environment at the temperature of 60 ℃, and stirring the mixture for 15min at the speed of 200r/min to obtain the octanoic acid-decanoic acid eutectic substance.
(2) Preparing expanded graphite:
and (3) placing the expandable graphite in an oven, drying for 2 hours at 100 ℃, taking out and spreading in a crucible, placing the crucible in a muffle furnace at 900 ℃ for calcining for 60s, taking out and cooling to prepare the completely expanded expandable graphite.
(3) Preparing a shaped composite phase change material:
1) placing the expanded graphite in a 100 ℃ oven for 2h, and fully drying;
2) weighing a certain mass of fully dried expanded graphite, adding the fully dried expanded graphite into a beaker, and pouring the octanoic acid-decanoic acid eutectic substance until the expanded graphite is completely submerged;
3) placing the beaker in a 60 ℃ water bath kettle, and stirring for 30min by a constant speed stirrer at the rotating speed of 160rad/min, wherein the expanded graphite on the wall of the beaker is scraped off;
4) pouring the stirred uniform mixture into a funnel, connecting a vacuum pump for suction filtration until no liquid drips at the bottom of the funnel, repeatedly washing the beaker by using filtrate, and performing suction filtration until no expanded graphite residue exists in the beaker;
5) and (3) putting the solid obtained by suction filtration into an oven for air blast drying at the temperature of 80 ℃, taking out and weighing at intervals of half an hour, and observing the surface drying state of the solid until the mass loss rate of the material is reduced and the sample is loose and granular, thus completing the preparation of the composite material.
The present invention will be further described with reference to the following examples.
Examples
Under the water bath environment of 60 ℃, mixing n-caprylic acid and n-capric acid in a mass ratio of 1:1 in a beaker, placing the beaker in the water bath environment of 60 ℃, and stirring for 15min at 200r/min to obtain an octanoic acid-capric acid eutectic; placing expandable graphite in an oven, drying for 2 hours at 100 ℃, taking out and spreading in a crucible, placing the crucible in a muffle furnace at 900 ℃ for calcining for 60s, taking out and cooling to prepare the completely expanded graphite; placing the expanded graphite in a 100 ℃ oven for 2h, and fully drying; weighing a certain mass of fully dried expanded graphite, adding the fully dried expanded graphite into a beaker, and pouring the octanoic acid-decanoic acid eutectic substance until the expanded graphite is completely submerged; placing the beaker in a 60 ℃ water bath kettle, and stirring for 30min by a constant speed stirrer at the rotating speed of 160rad/min, wherein the expanded graphite on the wall of the beaker is scraped off; pouring the stirred uniform mixture into a funnel, connecting a vacuum pump for suction filtration until no liquid drips at the bottom of the funnel, repeatedly washing the beaker by using filtrate, and performing suction filtration until no expanded graphite residue exists in the beaker; putting the solid obtained by suction filtration into an oven for air blast drying at the temperature of 80 ℃, taking out and weighing at intervals of half an hour, and observing until the mass loss rate of the material is reduced and the sample is loose and granular, namely the preparation of the composite material is finished; the mixing ratio is cement: coarse aggregate: fine aggregate: water 1: 3.37: 1.90: and (3) directly adding PCMs accounting for 3% of the total mass on the basis of 0.4, pouring the PCMs and fine aggregates into a stirrer together for stirring in advance in order to avoid uneven stirring in the preparation process, adding other materials, and stirring to obtain the compound fatty acid low-temperature phase change cement concrete material.
The present invention will be further described with reference to the experimental effects.
As shown in figure 2 by DSC curves of the caprylic-capric acid eutectic before and after the phase change cycle. From fig. 2, it can be seen that, in the process of temperature rise, the phase transition behavior of the caprylic-capric acid eutectic is basically not changed, and the phase transition behavior is changed to some extent in the process of temperature decrease, but the phase transition behavior has no obvious relation with the increase of the cycle number, and can be considered to be caused by test errors. Compared with four groups of DSC curves, the eutectic DSC curves which are not subjected to phase change circulation and 30 times of phase change circulation have larger difference, the phase change latent heat difference is larger, after the phase change circulation is carried out for 60 times and 90 times, the phase change behavior of the material is stabilized, the phase change latent heat is about 130J/g when the temperature is raised, and the phase change latent heat is about 115J/g when the temperature is lowered. The phase transition behavior is still in the proper phase transition temperature range as a whole.
As shown in the infrared spectrum before and after the phase transition of the caprylic-capric acid eutectic substance in figure 3. The wavelength of 2925cm < -1 > corresponds to a carbon-hydrogen bond (C-H) stretching vibration absorption peak, the wavelength of 1465cm < -1 > corresponds to a carbon-hydrogen bond (C-H) in-plane bending vibration absorption peak, 1430cm < -1 > is a hydroxyl (-OH) in-plane bending vibration absorption peak, and 940cm < -1 > is a hydroxyl (-OH) out-of-plane bending vibration absorption peak. The carbon-oxygen double bond (C ═ O) stretching vibration absorption peak appears at 1716 cm-1. The waveform of the caprylic-capric acid eutectic after 90 times of phase transition circulation is consistent with that before the phase transition circulation, and no new absorption peak appears or old peak disappears. This indicates that the properties of the eutectic did not change after 90 phase change cycles. The phase transition temperature of the caprylic-capric acid eutectic is suitable, the property is stable, and the caprylic-capric acid eutectic can be used as an anti-freezing phase transition material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (5)

1. The compound fatty acid low-temperature phase change cement concrete material is characterized by comprising 100 parts by weight of Portland cement, 337 parts by weight of limestone, 190 parts by weight of river sand, 40 parts by weight of tap water and 20 parts by weight of a shaping composite phase change material.
2. The preparation method of the compound fatty acid low-temperature phase change cement concrete material as claimed in claim 1, wherein the preparation method of the compound fatty acid low-temperature phase change cement concrete material comprises the following steps:
step one, weighing raw materials according to a mixing ratio;
pouring the shaped composite phase change material and river sand into a stirrer together, and stirring in advance;
and step three, adding portland cement, limestone and tap water, and mixing to obtain the compound fatty acid low-temperature phase change cement concrete material.
3. The preparation method of the compounded fatty acid low-temperature phase change cement concrete material as claimed in claim 2, wherein in the second step, the preparation method of the shaped composite phase change material comprises the following steps:
firstly, preparing a binary phase change system and expanded graphite;
secondly, preparing the shaped composite phase change material, wherein the specific preparation method comprises the following steps:
1) placing the expanded graphite in a 100 ℃ oven for 2h, and fully drying;
2) weighing a certain mass of fully dried expanded graphite, adding the fully dried expanded graphite into a beaker, and pouring the octanoic acid-decanoic acid eutectic substance until the expanded graphite is completely submerged;
3) placing the beaker in a 60 ℃ water bath kettle, and stirring for 30min by a constant speed stirrer at the rotating speed of 160rad/min, wherein the expanded graphite on the wall of the beaker is scraped off;
4) pouring the stirred uniform mixture into a funnel, connecting a vacuum pump for suction filtration until no liquid drips at the bottom of the funnel, repeatedly washing the beaker by using filtrate, and performing suction filtration until no expanded graphite residue exists in the beaker;
5) and (3) putting the solid obtained by suction filtration into an oven for air blast drying at the temperature of 80 ℃, taking out and weighing at intervals of half an hour, and observing the surface drying state of the solid until the mass loss rate of the material is reduced and the sample is loose and granular, thus completing the preparation of the composite material.
4. The preparation method of the compounded fatty acid low-temperature phase change cement concrete material as claimed in claim 3, wherein in the first step, the preparation method of the binary phase change system is as follows:
1) the raw materials comprise the following components in percentage by mass: n-octanoic acid and n-decanoic acid 1: 1;
2) the specific operation is as follows: mixing the raw materials according to the formula in a beaker, placing the beaker in a water bath environment at the temperature of 60 ℃, and stirring the mixture for 15min at the speed of 200r/min to obtain the octanoic acid-decanoic acid eutectic substance.
5. The preparation method of the compounded fatty acid low-temperature phase change cement concrete material as claimed in claim 3, wherein in the first step, the preparation method of the expanded graphite comprises the following steps:
and (3) placing the expandable graphite in an oven, drying for 2 hours at 100 ℃, taking out and spreading in a crucible, placing the crucible in a muffle furnace at 900 ℃ for calcining for 60s, taking out and cooling to prepare the completely expanded expandable graphite.
CN202010424510.7A 2020-05-19 2020-05-19 Compound fatty acid low-temperature phase change cement concrete material and preparation method thereof Pending CN111499311A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101239798A (en) * 2008-01-04 2008-08-13 华南理工大学 Organic matter/expandable graphite composite phase change heat-storing building material and preparation method thereof
DE102007062772A1 (en) * 2007-12-27 2009-07-02 Baerlocher Gmbh Fatty acid salt mixture as a water repellent for building materials

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007062772A1 (en) * 2007-12-27 2009-07-02 Baerlocher Gmbh Fatty acid salt mixture as a water repellent for building materials
CN101239798A (en) * 2008-01-04 2008-08-13 华南理工大学 Organic matter/expandable graphite composite phase change heat-storing building material and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王迎辉等: "正辛酸-肉豆蔻酸/膨胀石墨定形复合相变材料的制备和热物性", 《上海海事大学学报》 *
苟珊: "水泥路面抗凝冰低温相变材料开发与性能研究", 《中国学位论文全文数据库》 *

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