CN110804422B - Preparation method of paraffin-cement-based shape-stabilized phase change material - Google Patents

Preparation method of paraffin-cement-based shape-stabilized phase change material Download PDF

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CN110804422B
CN110804422B CN201911125757.2A CN201911125757A CN110804422B CN 110804422 B CN110804422 B CN 110804422B CN 201911125757 A CN201911125757 A CN 201911125757A CN 110804422 B CN110804422 B CN 110804422B
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cement
paraffin
change material
based shape
phase
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CN110804422A (en
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杜银飞
刘谱晟
魏唐中
马聪
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Nanjing Xingyou Traffic Technology Co ltd
Central South University
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Nanjing Xingyou Traffic Technology Co ltd
Central South University
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    • 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
    • C09K5/063Materials absorbing or liberating heat during crystallisation; Heat storage materials

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

Abstract

The invention discloses a preparation method of a paraffin-cement-based shape-stabilized phase-change material. Because the hydration of the cement and the demulsification and precipitation of the paraffin emulsion are carried out simultaneously, the paraffin is uniformly dispersed in a hydration product to form a stable packaging system, and the prepared paraffin-cement-based shape-stabilized phase-change material is ensured not to leak when the phase change occurs; the paraffin-cement-based shape-stabilized phase change material prepared by the invention has the advantages of high phase change material packaging rate, good stability, simple preparation process, low cost and the like, and can be widely applied to various fields such as heat energy storage, building energy conservation and the like; by adding the superfine mineral admixture with the active effect, the thickening agent and the accelerating agent, the hydration speed, the hydration degree and the physical strength of the paraffin-cement-based shape-stabilized phase-change material are improved.

Description

Preparation method of paraffin-cement-based shape-stabilized phase change material
Technical Field
The invention belongs to the technical field of phase-change material preparation, and particularly relates to a preparation method of a paraffin-cement-based shape-stabilized phase-change material.
Background
The heat energy storage technology can improve the utilization efficiency of energy and relieve the contradiction between supply and demand of the energy, thereby attracting the attention of a plurality of scholars today when fossil energy is in short supply and the greenhouse effect is serious.
A phase change material is a material that can absorb or release a large amount of heat while undergoing a phase transition without changing or with little change in its temperature. Latent heat storage technology is a thermal energy storage technology developed by utilizing the characteristic of phase change materials. Common phase change materials are divided into solid-liquid phase change materials, solid-solid phase change materials, solid-gas phase change materials and liquid-gas phase change materials, and the solid-liquid phase change materials are considered to be the most feasible phase change materials with the most application value in consideration of volume change and phase change enthalpy during phase change. In order to prevent the solid-liquid phase change material from leaking during the phase change, some measures are generally taken to encapsulate the phase change material. For example, a phase change material is encapsulated by using a microcapsule wall material, or a phase change material is adsorbed by using a porous material, but these methods have disadvantages such as a low encapsulation rate of the phase change material and a high possibility of breaking a shell material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a paraffin-cement-based shape-stabilized phase change material, which utilizes the gelation property of cement and emulsifies the phase change material paraffin, uses paraffin emulsion to mix the cement, the cement and water in the emulsion have hydration reaction to accelerate emulsion breaking of the paraffin emulsion, and when the cement is finally hydrated, the paraffin is firmly encapsulated by a hydration product.
In order to achieve the purpose, the invention provides the following technical scheme:
the preparation method of the paraffin-cement-based shape-stabilized phase change material comprises the following steps:
(1) the paraffin-cement-based shape-stabilized phase change material comprises the following raw materials in parts by weight: 100 parts of cement, 30-80 parts of paraffin phase-change emulsion, 5-15 parts of mineral admixture, 1-5 parts of accelerator, 0.1-1 part of thickener, 0.1-5 parts of water reducer and 10-20 parts of water;
(2) weighing the dry materials in proportion, and putting the dry materials into a mixing pot for dry mixing;
(3) slowly pouring the paraffin phase-change emulsion and other liquid materials into a mixing pot;
(4) starting a cement paste mixer, firstly stirring at a low speed, then stirring at a high speed, and pouring the paste into a test mold after stirring;
(5) and after standard maintenance, crushing the test piece into powder or granules, and finishing the preparation of the paraffin-cement-based shape-stabilized phase-change material.
Preferably, in the step (1), the preparation process of the paraffin phase-change emulsion comprises the following steps: mixing and heating paraffin and an emulsifier to 60-100 ℃, slowly adding distilled water with the same temperature after the paraffin is completely melted, and stirring at the stirring speed of 1000-5000 rpm for 30-60 min for dispersing and emulsifying to prepare the paraffin phase-change emulsion.
According to a further technical scheme, the mass ratio of the paraffin to the emulsifier to the distilled water is 100: (10-30): (60-150).
According to a further technical scheme, the melting point of the paraffin is 30-80 ℃, and the emulsifier is one or a combination of span 20 and tween 80.
Preferably, in the step (1), the cement is one or more of portland cement, portland slag cement, portland pozzolana cement, portland fly ash cement, composite portland cement, sulphoaluminate cement, ferro-aluminate cement, phosphate cement and superfine cement;
the mineral admixture is one or a mixture of more of silica fume, fly ash, slag and limestone powder, and the fineness is higher than 1000 meshes;
the accelerating agent is one or more of an aluminum oxide clinker-carbonate accelerating agent, an aluminum oxide clinker-alunite accelerating agent, a water glass accelerating agent and an alkali-free accelerating agent;
the thickening agent is one or more of a propylene thickening agent, a cellulose thickening agent and a polysaccharide thickening agent;
the water reducing agent is one or more of a naphthalene water reducing agent, a lignin water reducing agent, an aliphatic water reducing agent and a polycarboxylic acid water reducing agent.
In the preferable scheme, in the step (2), the dry materials are weighed in proportion and put into a mixing pot for dry mixing for 1-2 min.
In the preferable scheme, in the step (4), the slurry is firstly stirred at a low speed for 2-3 min, is stopped for 15-30 s, is then stirred at a high speed for 2-3 min, and is then poured into a test mold.
Preferably, in the step (5), standard curing is required for 7-58 days.
The paraffin-cement-based shape-stabilized phase change material has the advantages of high phase change material packaging rate, good stability, simple preparation process, low cost and the like, and can be widely applied to various fields such as heat energy storage, building energy conservation and the like.
Compared with the prior art, the invention has the beneficial technical effects that:
1) as the hydration of the cement and the demulsification and precipitation of the paraffin emulsion are carried out simultaneously, the paraffin is uniformly dispersed in hydration products, a stable packaging system is formed, and the prepared paraffin-cement-based shape-stabilized phase-change material is ensured not to leak when the phase change occurs.
2) The paraffin-cement-based shape-stabilized phase change material prepared by the invention has the advantages of high phase change material packaging rate, good stability, simple preparation process, low cost and the like, and can be widely applied to various fields such as heat energy storage, building energy conservation and the like due to the excellent physical property, chemical stability and thermal stability of the cement material.
3) By adding the superfine mineral admixture with the active effect, the thickening agent and the accelerating agent, the hydration speed, the hydration degree and the physical strength of the paraffin-cement-based shape-stabilized phase-change material are improved.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
The paraffin-cement-based shape-stabilized phase change material prepared in the embodiment comprises the following raw materials: the cement is ordinary portland cement, the phase-change material is paraffin with a melting point of 60 ℃, the mineral admixture is silica fume, the accelerating agent is a red star I type accelerating agent belonging to aluminum oxide clinker-carbonate series, the thickening agent is polyacrylamide belonging to propylene series, the water reducing agent is a naphthalene series water reducing agent, and the emulsifier is span 20. The preparation method comprises the following specific steps:
s1, mixing 30g of paraffin and 8g of emulsifier, heating to 80 ℃, slowly adding 30g of distilled water with the same temperature after the paraffin is completely melted, stirring at the stirring speed of 1000rpm for 60min for dispersion and emulsification, and stirring to obtain a paraffin emulsion;
s2, weighing 100g of cement, 10g of silica fume, 5g of accelerating agent, 0.8g of thickening agent and 0.5g of water reducing agent, and putting into a mixing pot for dry mixing for 1 min;
s3, slowly pouring the prepared paraffin emulsion and 10g of water into a mixing pot;
s4, starting a cement paste mixer, firstly stirring at a low speed for 2min, stopping stirring for 15s, then stirring at a high speed for 2min, and then pouring the paste into a test mould;
and S5, after standard maintenance is carried out for 58 days, crushing the test piece into powder or granules, and preparing the paraffin-cement-based shape-stabilized phase-change material.
The prepared paraffin-cement-based shape-stabilized phase-change material is subjected to thermal performance test, the enthalpy value is 36.8J/g, and the enthalpy value is 34.2J/g after 100 times of temperature rise and drop circulation, so that the paraffin-cement-based shape-stabilized phase-change material has excellent heat storage capacity and thermal stability.
Example 2
The paraffin-cement-based shape-stabilized phase change material prepared in the embodiment comprises the following raw materials: the cement is sulphoaluminate cement, the phase-change material is paraffin with the melting point of 30 ℃, the mineral admixture is ultrafine fly ash, the accelerator is ART-SL12 alkali-free liquid accelerator, the thickener is cellulose ether belonging to cellulose system, the water reducing agent is polycarboxylic acid water reducing agent, and the emulsifier is Tween 80. The preparation method comprises the following specific steps:
s1, mixing 40g of paraffin and 6g of emulsifier, heating to 50 ℃, slowly adding 24g of distilled water with the same temperature after the paraffin is completely melted, stirring at a stirring speed of 5000rpm for 30min for dispersion and emulsification, and stirring to obtain a paraffin emulsion;
s2, weighing 100g of cement, 8g of ultrafine fly ash and 0.3g of thickening agent, and putting into a mixing pot for dry mixing for 1-2 min;
s3, adding the prepared paraffin emulsion, 2g of an accelerator, 0.8g of a water reducing agent and 15g of water into a mixing pot;
s4, starting a cement paste mixer, firstly stirring at a low speed for 2min, stopping stirring for 15s, then stirring at a high speed for 2min, and then pouring the paste into a test mould;
s5, after standard maintenance for 14 days, crushing the test piece into powder or particles, and finishing the preparation of the paraffin-cement-based shape-stabilized phase-change material.
The prepared paraffin-cement-based shape-stabilized phase-change material is subjected to thermal performance test, the enthalpy value is 33.7J/g, and the enthalpy value is 32.1J/g after 100 times of temperature rise and drop circulation, so that the paraffin-cement-based shape-stabilized phase-change material has excellent heat storage capacity and thermal stability.
Comparative example 1
The paraffin wax is finely ground, then the finely ground paraffin wax is used as an additive to be mixed with cement, and the other conditions are the same as in example 1.
And (3) performing thermal performance test on the prepared phase-change material, wherein the enthalpy value of the prepared phase-change material is 30.69J/g, and the enthalpy value of the prepared phase-change material after 100 times of temperature rise and drop cycles is 22.77J/g.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. Modifications and variations that may occur to those skilled in the art without departing from the spirit and scope of the invention are to be considered as within the scope of the invention.

Claims (6)

1. The preparation method of the paraffin-cement-based shape-stabilized phase change material comprises the following steps:
(1) the paraffin-cement-based shape-stabilized phase change material comprises the following raw materials in parts by weight: 100 parts of cement, 30-80 parts of paraffin phase-change emulsion, 5-15 parts of mineral admixture, 1-5 parts of accelerator, 0.1-1 part of thickener, 0.1-5 parts of water reducer and 10-20 parts of water;
(2) weighing the dry materials in proportion, and putting the dry materials into a mixing pot for dry mixing;
(3) slowly pouring the paraffin phase-change emulsion and other liquid materials into a mixing pot;
(4) starting a cement paste mixer, firstly stirring at a low speed, then stirring at a high speed, and pouring the paste into a test mold after stirring;
(5) after standard maintenance, crushing the test piece into powder or granules, and finishing the preparation of the paraffin-cement-based shape-stabilized phase-change material;
in the step (1), the preparation process of the paraffin phase-change emulsion comprises the following steps: mixing and heating paraffin and an emulsifier to 60-100 ℃, slowly adding distilled water with the same temperature after the paraffin is completely melted, and stirring at the stirring speed of 1000-5000 rpm for 30-60 min for dispersing and emulsifying to prepare a paraffin phase-change emulsion;
the mass ratio of the paraffin to the emulsifier to the distilled water is 100: (10-30): (60-150);
the melting point of the paraffin is 30-80 ℃; the emulsifier is one or the combination of two of span 20 and tween 80.
2. The method for preparing a paraffin-cement-based shaped phase change material according to claim 1, wherein in the step (1), the cement is one or more of portland cement, portland slag cement, portland pozzolana cement, portland fly ash cement, composite portland cement, sulphoaluminate cement, ferro-aluminate cement, phosphate cement, and ultra-fine cement;
the mineral admixture is one or a mixture of more of silica fume, fly ash, slag and limestone powder, and the fineness is higher than 1000 meshes;
the accelerating agent is one or more of an aluminum oxide clinker-carbonate accelerating agent, an aluminum oxide clinker-alunite accelerating agent, a water glass accelerating agent and an alkali-free accelerating agent;
the thickening agent is one or more of a propylene thickening agent, a cellulose thickening agent and a polysaccharide thickening agent;
the water reducing agent is one or more of a naphthalene water reducing agent, a lignin water reducing agent, an aliphatic water reducing agent and a polycarboxylic acid water reducing agent.
3. The preparation method of the paraffin-cement-based shape-stabilized phase change material as claimed in claim 1, wherein in the step (2), the dry materials are weighed in proportion and put into a mixing pot for dry mixing for 1-2 min.
4. The preparation method of the paraffin-cement-based shape-stabilized phase change material as claimed in claim 1, wherein in the step (4), the slurry is firstly stirred at a low speed for 2-3 min, then is stopped for 15-30 s, and then is stirred at a high speed for 2-3 min, and then is poured into a test mold.
5. The method for preparing the paraffin-cement-based shape-stabilized phase change material as claimed in claim 1, wherein in the step (5), standard curing is required for 7-58 days.
6. The paraffin-cement-based shape-stabilized phase-change material prepared by the preparation method of the paraffin-cement-based shape-stabilized phase-change material according to any one of claims 1 to 5.
CN201911125757.2A 2019-11-18 2019-11-18 Preparation method of paraffin-cement-based shape-stabilized phase change material Active CN110804422B (en)

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CN111337330A (en) * 2020-04-28 2020-06-26 福建江夏学院 Improved sealing method for cement soil permeation sample
CN113201314B (en) * 2021-04-22 2022-02-11 东南大学 Preparation method and application of C-S-H/PEG1000 phase-change composite material
CN113249096B (en) * 2021-05-17 2022-02-11 河北科技大学 Porous medium composite phase change material and preparation method and application thereof
CN113636798A (en) * 2021-08-13 2021-11-12 合肥工业大学 Preparation method of cement-based paraffin phase-change energy storage material
CN114471132B (en) * 2021-12-31 2023-10-24 山东汉博昱洲新材料有限公司 Additive for carbon mineralization product and preparation method and application thereof

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