KR20130136599A - Method for producing microcapsule comprising phase change material and concrete composition using the same - Google Patents
Method for producing microcapsule comprising phase change material and concrete composition using the same Download PDFInfo
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- 239000004567 concrete Substances 0.000 title claims abstract description 32
- 239000000203 mixture Substances 0.000 title claims abstract description 20
- 239000012782 phase change material Substances 0.000 title claims abstract description 19
- 239000003094 microcapsule Substances 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000011162 core material Substances 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- 238000005338 heat storage Methods 0.000 claims description 36
- 239000011232 storage material Substances 0.000 claims description 25
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 18
- 229920000877 Melamine resin Polymers 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 239000012188 paraffin wax Substances 0.000 claims description 15
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 13
- 239000004568 cement Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002562 thickening agent Substances 0.000 claims description 6
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 5
- 239000004640 Melamine resin Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 230000001804 emulsifying effect Effects 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 4
- 239000000178 monomer Substances 0.000 claims description 4
- -1 Calcium Sulfur Aluminate Chemical class 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 230000000704 physical effect Effects 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 17
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000017525 heat dissipation Effects 0.000 description 5
- 239000004576 sand Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000002775 capsule Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000011398 Portland cement Substances 0.000 description 2
- 229920002522 Wood fibre Polymers 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002025 wood fiber Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910001341 Crude steel Inorganic materials 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000011396 hydraulic cement Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011257 shell material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
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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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
- E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
- E04B1/62—Insulation or other protection; Elements or use of specified material therefor
- E04B1/74—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
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- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
- Physics & Mathematics (AREA)
- Architecture (AREA)
- Civil Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Acoustics & Sound (AREA)
- Electromagnetism (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
Description
본 발명은 상변화 물질을 함유하는 마이크로캡슐 형태의 잠열축열재의 제조방법 및 이를 포함하여 제조된 콘크리트 조성물에 관한 것으로, 더욱 상세하게는 상변화 물질로서 파라핀계 왁스를 수용액에서 유화시킨 후 상기 유화액을 고분자 물질로 마이크로캡슐화하고, 생성된 마이크로캡슐을 콘크리트 조성물에 혼입해서 건축구조물에 필요한 잠열 축열재를 제조하는 것이다.The present invention relates to a method for producing a latent heat storage material in the form of microcapsules containing a phase change material and to a concrete composition prepared by the same. More specifically, the emulsion is prepared by emulsifying paraffin wax in an aqueous solution as a phase change material. Microencapsulation with a polymeric material, and the resulting microcapsules are incorporated into a concrete composition to produce latent heat storage materials for building structures.
에너지 절약은 근래에 이르러 지구온난화 문제를 해결하기 위한 기후협약 등의 영향으로 전 세계적인 이슈가 되고 있다.Energy conservation has become a global issue in recent years due to the impact of climate agreements on solving global warming problems.
단열재를 이용한 건축물의 단열 등 에너지 절약기술은 냉난방에 다양하게 이용하여 왔으며 많은 부분에서 에너지 절약에 기여하여 왔다. 현재 우리나라의 경우 건축물의 사용 중 국가 총 에너지의 약 20%를 소비하고 있으며, 영국 및 일본 등 냉난방이 더욱 발달한 선진국은 현재 약 26~28%를 사용하고 있어, 향후 지구기후 변화로 인해 약 38~40%의 에너지가 소비될 것으로 예측되고 있다. 또한 현재 영국 등에서는 열질량(Thermal Mass)을 활용하여 벽체 및 지붕의 열효율을 향상시키기 위한 개발이 지속되어 지고 있다. Energy-saving technologies, such as thermal insulation of buildings using insulation materials, have been used in various ways for heating and cooling, and have contributed to energy saving in many areas. Korea currently consumes about 20% of the country's total energy while using buildings, and advanced countries such as the United Kingdom and Japan are currently using about 26 ~ 28%. It is estimated that ~ 40% of energy will be consumed. In addition, in the UK, developments to improve thermal efficiency of walls and roofs using thermal mass have been continued.
즉, 같은 에너지량으로 더 많은 열효율이 발생될 수 있도록 하기 위한 연구가 요구되고 있으며, 축열재 이용 기술은 실내 냉난방을 위하여 사용된 에너지를 장시간 일정온도로 유지할 수 있도록 하여 에너지 사용 효율을 높이는 장점이 있다. 특히 기존의 온돌방식의 건축물이 콘크리트로 대체됨에 따라 건축물 벽의 축열기능이 낮아지게 되고 이로 인해 바닥과 벽간의 심한 온도차가 생겨 에너지 효율의 저하를 초래하게 되고 외기의 극심한 온도변화에도 실내온도를 일정하게 유지할 수 있는 축열 성능을 갖는 소재가 갈수록 요구되고 있다.That is, research is required to generate more thermal efficiency with the same amount of energy, and the heat storage material utilization technology has the advantage of increasing energy efficiency by maintaining energy used for indoor heating and cooling at a constant temperature for a long time. have. In particular, as the existing ondol-type buildings are replaced with concrete, the heat storage function of the building wall is lowered, which causes a severe temperature difference between the floor and the wall, resulting in a decrease in energy efficiency, and the indoor temperature is constant even in the extreme temperature change of the outside air. There is an increasing demand for materials having a heat storage performance that can be easily maintained.
따라서, 에너지 효율의 극대화를 위해서 상변화 물질(Phase Change Material, PCM)을 이용한 잠열 축열재의 제조에 많은 연구가 집중되고 있다. 상변화 물질은 특정 온도에서 온도의 변화 없이 상이 변하면서 많은 양의 열을 흡수하거나 방출하는 물질로서, 상기 흡수 및 방출열을 잠열(潛熱)이라 한다. 이러한 잠열을 이용하여 열에너지를 저장하는 방법인 잠열 축열법은 현열을 이용하여 열에너지를 저장하는 방법보다 단위 부피당 또는 단위 무게당 더 많은 양의 열을 저장할 수 있다.Therefore, much research has been focused on the production of latent heat storage materials using phase change materials (PCM) in order to maximize energy efficiency. A phase change material is a material that absorbs or releases a large amount of heat as the phase changes without changing the temperature at a specific temperature, and the heat of absorption and release is called latent heat. The latent heat storage method, which is a method of storing thermal energy using the latent heat, may store more heat per unit volume or unit weight than the method of storing thermal energy using sensible heat.
잠열 축열법에 사용되는 상변화 물질은 유기계와 무기계가 있으며 바람직하게는 큰 잠열, 원하는 온도범위에서의 흡열 및 발열, 좋은 열응답 속도, 장기간의 안정성 및 무독성과 같은 특성을 가져야 하며, 또한 경제적이고, 부식성이 없어야 한다. 그러나, 무기계 화합물은 과냉각이 심하고 상분리 현상이 발생하여 축열 및 방열 성능이 저하되는 등의 문제점이 있어 최근에는 유기계 화합물 중 저렴한 파라핀계 왁스가 상변화 물질로 상용화되고 있다.The phase change materials used in the latent heat storage method are organic and inorganic, and preferably have characteristics such as large latent heat, endothermic and exotherm at a desired temperature range, good heat response rate, long-term stability and nontoxicity, and are economical. It should not be corrosive. However, the inorganic compound has a problem of severe supercooling and phase separation phenomenon, such as deterioration of heat storage and heat dissipation performance. Recently, inexpensive paraffin wax among organic compounds has been commercialized as a phase change material.
상기 상변화 물질을 코팅하는 벽재 물질(shell material)은 유기계와 무기계가 있으며 건축자재에 적용하기 위해서는 기계적 물성이 우수하여야 하고 값이 저렴하여야 한다. 무기계로는 지올라이트 등과 같은 다공성 물질 등이 활용되고 있으며 유기계로는 나일론이나 멜라민 수지 등과 같은 고분자 물질 등이 사용되고 있다.The shell material coating the phase change material has an organic type and an inorganic type, and should be excellent in mechanical properties and inexpensive in order to be applied to building materials. Porous materials such as zeolite are used as the inorganic system, and polymer materials such as nylon and melamine resin are used as the organic system.
상기 상변화 물질을 잠열 축열재로 사용하기 위해서는 벽재 물질로 마이크로캡슐화 해야 하는데, 이 방법을 크게 분류하면 화학적 방법, 물리·화학적 방법 및 물리·기계적 방법의 3가지로 나눌 수 있으며, 어떤 방법을 사용할지는 상변화 물질과 벽재 물질의 종류 및 사용 목적 등을 고려하여 결정한다.In order to use the phase change material as a latent heat storage material, it is necessary to microencapsulate it as a wall material. If this method is largely classified, it can be divided into three types of chemical methods, physical and chemical methods, and physical and mechanical methods. The decision is made by considering the type of phase change material and wall material and the purpose of use.
습식공정에 의한 마이크로캡슐화 방법은 상변화 물질을 용매에서 유화시킨 후 벽재 모노머를 상변화 물질의 벽면에 코팅하여 경화시키는 공정이다. 이 경우 상변화 물질 유화액이나 벽재 모노머의 코팅 성능을 좋게 하기 위해서는 계면에너지의 조절이 필요하며 이를 위하여 계면활성제가 사용된다. 첨가되는 계면활성제의 특성에 따라서 마이크로캡슐화 성능이 좌우되고 벽재 물질의 코팅 두께 및 코팅의 균일성에 크게 영향을 미친다.The microencapsulation method by a wet process is a process of emulsifying a phase change material in a solvent and then coating and curing a wall monomer on a wall of the phase change material. In this case, in order to improve the coating performance of the phase change material emulsion or the wall monomer, it is necessary to control the interfacial energy. The nature of the surfactant added depends on the microencapsulation performance and greatly affects the coating thickness of the wall material and the uniformity of the coating.
본 발명은 상변화 물질인 파라핀계 왁스를 고분자 물질로 마이크로캡슐화할 때 계면에너지를 조절함으로써 방열 및 축열성이 개선된 잠열 축열재의 제조방법 및 이를 포함하여 제조된 콘크리트 조성물을 제공하고자 한다.The present invention provides a method for producing a latent heat storage material having improved heat dissipation and heat storage properties by controlling interfacial energy when microencapsulating a paraffin wax, which is a phase change material, with a polymer material, and a concrete composition prepared by the same.
상기 과제를 해결하기 위하여, 본 발명은 멜라민, 물, 포름알데히드의 혼합물을 가온 및 교반하여 벽재 물질을 제조하는 단계; 파라핀 왁스를 수용액에서 에멀션화하여 심물질을 제조하는 단계; 벽재 물질과 심물질을 투입하고, 아세트산을 정량 투입하여 교반한 후에 실온으로 냉각하는 단계를 포함하는 상변화 물질을 함유하는 마이크로캡슐 형태의 마이크로캡슐 형태의 잠열 축열재의 제조방법을 제공한다.In order to solve the above problems, the present invention comprises the steps of preparing a wall material by heating and stirring a mixture of melamine, water, formaldehyde; Preparing a core material by emulsifying paraffin wax in an aqueous solution; It provides a method for producing a latent heat storage material in the form of microcapsules containing a phase change material comprising the step of adding a wall material and a core material, and quantitatively adding acetic acid and stirring, followed by cooling to room temperature.
또한, 본 발명은 상기 제조방법으로 제조된 상변화 물질을 함유하는 마이크로캡슐 형태의 잠열 축열재를 포함하는 콘크리트 조성물을 제공한다. 상기 콘크리트 조성물은 전체가 100 중량부라 할 때, 결합재 21.5∼46.5 중량부, 잠열축열재 0.44∼2.72 중량부, 혼화제 0.11∼0.33 중량부, 골재 43.0∼63.0 중량부로 구성된다.In addition, the present invention provides a concrete composition comprising a latent heat storage material in the form of microcapsules containing a phase change material prepared by the manufacturing method. When the total weight of the concrete composition is 100 parts by weight, the binder is composed of 21.5 to 46.5 parts by weight, 0.44 to 2.72 parts by weight of latent heat storage material, 0.11 to 0.33 parts by weight of admixture, and 43.0 to 63.0 parts by weight of aggregate.
본 발명에 따른 잠열 축열재는 심물질을 벽재 물질로 마이크로캡슐화할 때 계면에너지를 조절함으로써 마이크로캡슐의 물성이 우수하며, 개선된 축, 방열성을 나타낸다.The latent heat storage material according to the present invention is excellent in the physical properties of the microcapsule by controlling the interfacial energy when microencapsulating the core material into the wall material, and exhibits improved axial and heat dissipation properties.
따라서, 본 발명의 잠열축열재가 포함하여 제조된 콘크리트를 건물의 벽체 및 슬래브에 설치하면 건물내부 및 외부로 이동하는 열의 손실을 최소화하며, 열이 전달되는 단면이 함께 줄어들어서 에너지 손실을 최소화할 수 있다.Therefore, when the concrete prepared by the latent heat storage material of the present invention is installed on the wall and the slab of the building to minimize the loss of heat to move inside and outside the building, the cross section through which heat is transferred can be reduced together to minimize the energy loss have.
도 1 내지 도 5는 본 발명에 의해 제조된 잠열 축열재의 전자현미경 사진이다.
도 6은 계면활성제 함량에 따른 잠열 축열재의 열 흡수 및 방출을 분석한 그래프이다.1 to 5 are electron micrographs of the latent heat storage material produced by the present invention.
6 is a graph analyzing the heat absorption and release of the latent heat storage material according to the surfactant content.
이하 구체적 실시예에 의해 본 발명을 설명하도록 하겠다.Hereinafter, the present invention will be described by specific examples.
본 발명에 따른 잠열 축열재의 제조방법은, 멜라민 11.2g, 물 28g, 포름알데히드(35～37%) 31g을 혼합한 후 55℃정도에서 15분간 교반하고 25～40℃로 냉각하여 벽재 물질을 제조하고, 정량의 물과 파라핀 왁스 온도를 70℃로 유지한 후 계면활성제를 정량 투입한 후 호모믹서에 의하여 격렬한 교반을 통하여 에멀젼화시켜 심물질을 제조한 후, 상기 벽재 물질과 심물질을 투입하고, 아세트산을 정량 투입하여 100분간 350 rpm의 속도로 교반한 후에 실온으로 냉각 후 건조하여 제조되는 것에 기술적 특징이 있다.Method for producing a latent heat storage material according to the present invention, after mixing melamine 11.2 g , water 28 g , formaldehyde (35-37 % ) 31 g , stirred at about 55 ℃ for 15 minutes and cooled to 25-40 ℃ wall material After preparing a water and paraffin wax temperature of 70 ℃ and quantitatively added surfactant and emulsified by vigorous stirring by a homomixer to prepare a core material, the wall material and core material There is a technical feature in that it is prepared by adding acetic acid in a fixed amount, stirring at a speed of 350 rpm for 100 minutes, and then cooling to room temperature and drying.
사용된 심물질은 녹는점이 55℃～65℃인 순도가 매우 높은 시약급 파라핀(Junsei, EP grade)을 추가 정제없이 사용하였다. 벽재에 사용된 시약들은 멜라민(Aldrich, 99%) 및 포름알데히드(Aldrich, 99+%)를 이용하였으며 중합 촉진제로서 아세트산(Junsei, 99.5%)을 사용하였으며 용매인 물은 실험실에서 제조된 증류수를 이용하였다.The core material used was a high purity reagent grade paraffin (Junsei, EP grade) with melting point of 55 ℃ ~ 65 ℃ without further purification. Reagents used for wall materials were melamine (Aldrich, 99%) and formaldehyde (Aldrich, 99 +%), and acetic acid (Junsei, 99.5%) was used as a polymerization accelerator. It was.
또한, 본 발명은 파라핀 에멀젼 계면에 멜라민 수지 모노머의 흡착이 용이하도록 적절한 계면활성제를 선택하는 데 있으며, 일 실시예로서 황산 도데실 나트륨(sodium dodecyl sulfate, SDS, Aldrich 99.5 %)을 사용하였다.In addition, the present invention is to select an appropriate surfactant to facilitate the adsorption of the melamine resin monomer on the paraffin emulsion interface, as an example was used sodium dodecyl sulfate (SDS, 99.5% Aldrich).
본 발명의 계면활성제는 0.5% ~ 1.5%의 농도로 사용될 수 있으며, 0.5% 미만을 첨가하였을 때에는 캡슐의 물성 및 열 흡수, 방출의 특성이 미비하며, 1.5%를 초과하는 경우 경제성이 떨어진다. Surfactant of the present invention can be used in a concentration of 0.5% to 1.5%, when the addition of less than 0.5% of the physical properties and heat absorption, the release characteristics of the capsule is insufficient, if it exceeds 1.5% is economical.
본 발명으로 제조된 잠열 축열재의 물성을 검토하기 위하여 각 상 간의 계면에너지를 측정하였다. 계면장력 측정은 Sessible Drop 법을 이용하였으며, 측정장치는 계면장력측정기(First Ten Angstrom, FTA-200)를 이용하였고, 계면장력의 수치적 계산은 ADSA(Axisymmetric Drop Shape Analysis)법에 의하였다.In order to examine the physical properties of the latent heat storage material produced by the present invention, the interfacial energy between each phase was measured. The interfacial tension was measured using the Sessible Drop method, and the measuring device was measured by the interfacial tension tester (First Ten Angstrom, FTA-200), and the numerical calculation of the interfacial tension was performed by the ASI (Axisymmetric Drop Shape Analysis) method.
제조된 마이크로 캡슐의 형태 및 표면은 Scanning Electron Microscope(Universal TA Instrument, TM-1000)를 이용하여 관찰하였으며, 내열성 및 축열 성능은 주사시차열 분석기(DSC)를 이용하여 관찰하였다.The shape and surface of the prepared microcapsules were observed using a Scanning Electron Microscope (Universal TA Instrument, TM-1000), and heat resistance and heat storage performance were observed using a scanning differential thermal analyzer (DSC).
본 발명의 마이크로캡슐의 제조에 있어서 계면활성제 투입 농도에 따른 캡슐의 형태는 도 1 내지 도 5에 나타내었다. In the preparation of the microcapsules of the present invention, the shape of the capsule according to the surfactant concentration is shown in FIGS. 1 to 5.
도 1 내지 도 5에 나타난 바와 같이, 마이크로로캡슐의 형상은 첨가된 SDS의 양에 따라서 크게 차이가 남을 알 수가 있었다. 즉, SDS의 투입 양이 적은 경우에 상대적으로 많은 경우에 비하여 캡슐 벽의 형태가 매우 불규칙하고 일그러져 있는 것으로 보아 0.1%(도 1) 및 0.2%(도 2)의 경우에는 벽재 형성이 잘 이루어지지 못하는 것으로 보인다. As shown in Figures 1 to 5, the shape of the microrocapsules was found to be significantly different depending on the amount of SDS added. That is, since the shape of the capsule wall is very irregular and distorted as compared to the case where the amount of SDS input is relatively small, the wall formation is not performed well in the case of 0.1% (FIG. 1) and 0.2% (FIG. 2). It doesn't seem to be possible.
한편 SDS 첨가량이 0.8%(도 4)의 경우에는 벽재가 상대적으로 균일한 두께로 구형으로 잘 이루어진 것을 관찰할 수 있었다.On the other hand, when the amount of SDS added 0.8% (Fig. 4) it was observed that the wall was made of a spherical well with a relatively uniform thickness.
또한 SDS가 1.2%(도 5)의 경우에는 벽재형성이 더욱 촉진되어진 것으로 관찰되었으며 특히 멜라민 수지 입자들이 표면에 코팅된 이외에도 엉겨서 표면에 돌기가 형성된 것으로 보아 SDS 첨가량이 많아질수록 벽재형성이 촉진되는 것으로 보인다.In addition, when the SDS is 1.2% (FIG. 5), it was observed that the wall re-formation was further promoted. In particular, the melamine resin particles were tangled in addition to the surface-coated surface to form projections on the surface. Seems to be.
본 발명의 마이크로캡슐의 제조에 있어서 첨가되는 계면활성제의 함량에 따른 잠열 축열재의 축방열 성능은 도 6에 나타내었다.The heat storage performance of the latent heat storage material according to the amount of surfactant added in the preparation of the microcapsules of the present invention is shown in FIG.
도 6에서 보면 SDS 농도 변화에 따라 열 흡수 및 방출에 매우 큰 차이가 있음을 알 수가 있다.In Figure 6 it can be seen that there is a very large difference in heat absorption and release according to the change in SDS concentration.
즉, SDS 증가가 상대적으로 적은 0.1%(도 6(a)) 및 0.2%(도 6(b))의 경우에는 본 발명에서 사용된 파라핀 왁스의 융점인 55-65℃에서 열 흡수 및 방출의 특성이 거의 나타나지 않고 있다. 그러나 SDS 량이 충분히 많은 0.8% 이상(도 6(d), (e) 및 (f))에서는 온도가 상승(가열) 및 하강(냉각)을 반복함에 따라서 심물질인 파라핀 왁스의 융점 부근에서 열 흡수 및 방출 현상이 나타남을 관찰할 수 있었다. 또한 SDS 투입량이 클수록 흡수 및 방출되는 열량의 차가 더욱 큼을 알 수가 있었다. 즉 SDS 함량이 높을수록 벽재형성이 잘 이루어지고, 따라서 캡슐화된 심물질의 파라핀 왁스에 의한 축방열 성능이 좋아지는 것으로 판단된다. 특히 SDS 함량이 가장 높은 1.2%의 경우가 가장 뚜렷한 축방열 곡선으로 보이고 있어, 가열 및 냉각을 여러번 반복하여도 열 충격에 의한 벽재의 손상이 거의 없는 충분한 물성의 축방열을 위한 마이크로캡슐이 잘 이루어지는 것으로 판단된다.That is, for 0.1% (FIG. 6 (a)) and 0.2% (FIG. 6 (b)), where the increase in SDS is relatively small, the heat absorption and emission at 55-65 ° C., the melting point of the paraffin wax used in the present invention There is almost no characteristic. However, at 0.8% or more (Figs. 6 (d), (e) and (f)) where the amount of SDS is sufficiently high, the heat absorption near the melting point of the paraffin wax, which is a core material, is repeated as the temperature is increased (heated) and lowered (cooled). And release phenomena were observed. Also, the larger the SDS input, the greater the difference in the amount of heat absorbed and released. In other words, the higher the SDS content, the better the wall reforming, and therefore, the better the axial heat radiation performance by the paraffin wax of the encapsulated core material. In particular, 1.2%, which has the highest SDS content, shows the most pronounced axial heat dissipation curve. Thus, even after repeated heating and cooling several times, microcapsules for axial heat dissipation of sufficient physical properties with little damage to the wall due to thermal shock are well formed. It seems to be.
또한, 본 발명은 상기 잠열 축열재를 경량콘크리트에 혼입해서 단열성능을 부여시키는 것으로 실시 예는 아래와 같다. In addition, the present invention is to provide the heat insulating performance by mixing the latent heat storage material in lightweight concrete, the embodiment is as follows.
본 실시예는 콘크리트 구조물의 외벽에 잠열 및 축열성능을 부여해서 단열성능을 향상시키는 경량콘크리트의 조성물에 관한 것으로, 상기 조성물은 전체가 100 중량부라 할 때, 결합재 21.5∼46.5 중량부, 잠열축열재 0.44∼2.72 중량부, 혼화제 0.11∼0.33 중량부, 골재 43.0∼63.0 중량부로 구성된다.The present embodiment relates to a composition of lightweight concrete for imparting latent heat and heat storage performance to an outer wall of a concrete structure to improve thermal insulation performance. When the composition is 100 parts by weight, the binder is 21.5 to 46.5 parts by weight, and latent heat storage material. 0.44 to 2.72 parts by weight, 0.11 to 0.33 parts by weight of admixtures, and 43.0 to 63.0 parts by weight of aggregates.
결합재는, 시멘트 20.0∼40.0 중량부, 팽창재로서 CSA(Calcium Sulfur Aluminate) 1∼5 중량부, 무수석고(CaSO4) 0.5∼1.5 중량부로 이루어질 수 있다.The binder may be composed of 20.0 to 40.0 parts by weight of cement, 1 to 5 parts by weight of Calcium Sulfur Aluminate (CSA), and 0.5 to 1.5 parts by weight of anhydrous gypsum (CaSO 4 ).
시멘트는 골재들을 결합시키고 모르타르의 강도를 증진시키는 역할을 한다. 본 실시예에서는 시멘트로서 보통 포틀란트 시멘트(1종), 조강 포틀란트 시멘트(2종), 알루미나 시멘트 등의 수경성 시멘트 중 하나를 선택하여 사용할 수 있으며, 경우에 따라서는 2 종류 이상의 시멘트를 혼합하여 사용할 수도 있다.Cement serves to bond aggregates and to enhance the strength of mortar. In this embodiment, one of hydraulic cements such as portland cement (1 type), crude steel portland cement (2 types), and alumina cement may be selected and used as cement. In some cases, two or more types of cement may be used. It can also be mixed and used.
본 실시예에서는 시멘트가 20∼40 중량부 사용되는데, 시멘트의 함유량이 높으면 강도 증진에는 효과가 있으나, 밀도와 열전도율이 높아져 열전도율이 높아지고, 시멘트의 함유량이 적으면 강도가 떨어지고 내구성이 감소하기 때문에, 경량콘크리트의 역학적 기능을 발휘하지 못할 수 있다.In the present embodiment, 20 to 40 parts by weight of cement is used, but a high content of cement is effective in improving strength, but a high density and thermal conductivity increases thermal conductivity, and a low content of cement reduces strength and decreases durability. The mechanical properties of lightweight concrete may not be achieved.
본 실시예에서는 기타 결합재로서, 경량콘크리트의 수축을 줄이기 위해 CSA계의 팽창재와 무수석고(CaSO4)를 각각 1∼5 중량부, 0.5∼1.5 중량부 사용할 수 있다. 팽창재의 사용량이 지나치게 많으면 경량콘크리트의 팽창을 심하게 유도시켜서 경량콘크리트의 균열 및 단면 탈락을 야기할 수 있다. 팽창재의 양이 너무 적으면 건조수축에 대한 저항성이 떨어져서 균열이 발생하게 되므로, 적절한 양의 팽창재를 첨가하는 것이 좋다.In this embodiment, in order to reduce shrinkage of lightweight concrete, CSA-based expansion material and anhydrous gypsum (CaSO 4 ) may be used in an amount of 1 to 5 parts by weight and 0.5 to 1.5 parts by weight, respectively. If the amount of the expansion material is excessively large, the expansion of the lightweight concrete may be severely induced, which may cause cracking and cross-sectional dropping of the lightweight concrete. If the amount of the expansion material is too small, the resistance to dry shrinkage is poor, so that cracking occurs, it is preferable to add an appropriate amount of expansion material.
잠열 축열재는 심물질(파라핀 왁스)과 벽재 물질(멜라민)로 구성된 것으로 0.44∼2.72 중량부로 이루어질 수 있다.The latent heat storage material is composed of a core material (paraffin wax) and a wall material (melamine) and may be 0.44 to 2.72 parts by weight.
혼화제는 멜라민계 유동화제 0.1∼0.3 중량부, 증점제 0.01∼0.03 중량부로 이루어질 수 있다.The admixture may be comprised of 0.1 to 0.3 parts by weight of melamine-based fluidizing agent and 0.01 to 0.03 parts by weight of thickener.
혼화제 중 멜라민계 유동화제는 경량콘크리트의 유동성을 유지시키고 타설시에 시공성을 향상시키는 역할을 한다. 또한, 배합수의 사용량을 줄여줌으로써 강도 증진 및 내구성 증진에 기여하게 된다. 멜라민계 유동화제의 사용량이 너무 많으면 그 효과가 떨어질 수 있으며, 사용량이 너무 적으면 감수 효과가 저하되는 문제가 발생할 수 있다.Melamine-based fluidizing agent in the admixture serves to maintain the fluidity of lightweight concrete and improve the workability when pouring. In addition, by reducing the amount of the blended water will contribute to the enhancement of strength and durability. If the amount of the melamine-based fluidizing agent is too high, the effect may be lowered. If the amount is too small, the effect of reducing the water-reducing effect may occur.
혼화제 중 증점제는 경량콘크리트에 점성을 부여하기 위한 것으로, 수화반응이 진행되는 동안 경량콘크리트의 처짐을 방지하는 역할을 한다. 증점제의 첨가량이 너무 많으면 점성이 높아져 뿜칠 작업시에 펌프의 막힘 현상이 발생할 수 있고, 마감 과정에서 경량콘크리트가 미장칼에 눌러 붙는 형상이 발생하여 마감이 어려워질 수 있다.The thickener in the admixture is to impart viscosity to the light concrete, and serves to prevent sagging of the light concrete during the hydration reaction. If the amount of thickener is added too much, the viscosity may increase, causing clogging of the pump during the spraying operation, and the finishing process may be difficult because the lightweight concrete is pressed onto the plastering knife.
골재는 규사 33∼53 중량부, 중공구체(中空求體)의 경량골재 10∼20 중량부로 이루어질 수 있다.Aggregate may be composed of 33 to 53 parts by weight of silica sand, 10 to 20 parts by weight of the lightweight aggregate of the hollow sphere (中空 求 體).
본 실시예에 따른 경량콘크리트는 채움재인 골재로서 규사와 경량골재를 사용한 것을 특징으로 한다. 일반적으로 규사는 강도 증진, 수축 저감, 경제성 향상을 위하여 모르타르 제조시에 많이 사용하는 골재의 하나이다. 규사는 0.21∼0.60mm 크기의 6호사를 33.0∼53.0 중량부의 범위에서 사용할 수 있다.Lightweight concrete according to the present embodiment is characterized in that using the silica sand and lightweight aggregate as a filler aggregate. In general, silica is one of the aggregates used in the production of mortar in order to increase strength, reduce shrinkage, and improve economic efficiency. The silica sand may use 6 yarns having a size of 0.21 to 0.60 mm in the range of 33.0 to 53.0 parts by weight.
또한, 경량콘크리트의 단열 효과를 증진시키기 위해 골재의 중앙이 비어 있는 경량골재를 사용할 수 있다. 경량골재의 비중은 0.35∼0.45g/cc, 열전도율은 0.11W/m℃, 융점은 1,300℃이고, 화학조성비는 Al2O3 30%, SiO2 50%, Fe2O3 6% 및 기타로 구성될 수 있다.In addition, in order to enhance the thermal insulation effect of lightweight concrete, it is possible to use a lightweight aggregate in which the center of the aggregate is empty. The specific gravity of lightweight aggregate is 0.35 ~ 0.45g / cc, thermal conductivity is 0.11W / m ℃, melting point is 1,300 ℃, and chemical composition ratio is 30% Al 2 O 3 , 50% SiO 2 , 6% Fe 2 O 3 and others. Can be configured.
경량골재의 사용량이 너무 많으면 배합시에 골재 분리 현상이 일어나 시공성이 떨어지고 강도가 현저히 저하될 수 있으며, 경량골재의 사용량이 너무 적으면 단열효과가 저감되어 단열재의 기능이 저하될 수 있다.If the amount of light aggregate is used too much, aggregate separation may occur at the time of blending, resulting in poor workability and the strength may be significantly reduced. If the amount of light aggregate is used too little, the insulation effect may be reduced and the function of the heat insulating material may be reduced.
본 실시예에 따른 경량콘크리트의 각 성분들의 함량범위를 정리하면 표 1과 같다.Table 1 summarizes the content range of each component of the lightweight concrete according to this embodiment.
한편, 본 실시예에 따른 경량콘크리트를 표 2와 같은 배합비로 제작하여 응결시간, 압축강도, 부착강도, 휨강도에 대해 시험하였으며, 그 결과는 표 3과 같다.On the other hand, the light weight concrete according to the present embodiment was produced in the mixing ratio as shown in Table 2 and tested for the setting time, compressive strength, adhesion strength, bending strength, the results are shown in Table 3.
시험 결과로부터, 본 실시예에 따른 경량콘크리트의 응결시간이 낮으나, 강도가 우수함을 알 수 있다.
From the test results, it can be seen that although the setting time of the lightweight concrete according to the present embodiment is low, the strength is excellent.
상기에서는 본 발명의 바람직한 실시예를 참조하여 설명하였지만, 해당 기술분야에서 통상의 지식을 가진 자라면 하기의 특허 청구의 범위에 기재된 본 발명의 사상 및 영역으로부터 벗어나지 않는 범위 내에서 본 발명을 다양하게 수정 및 변경시킬 수 있음을 이해할 수 있을 것이다.It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention as defined in the appended claims. It will be understood that the invention may be varied and varied without departing from the scope of the invention.
Claims (4)
파라핀 왁스를 수용액에서 에멀션화하여 심물질을 제조하는 단계;
상기 벽재 물질과 심물질을 투입하고, 아세트산을 투입하여 교반한 후에 실온으로 냉각하여 상변화 물질을 함유하는 마이크로캡슐 형태의 잠열 축열재를 제조하는 단계;를 포함하여 이루어지는 것을 특징으로 하는 마이크로캡슐 형태의 잠열 축열재 제조방법.
Warming and stirring a mixture of melamine, water and formaldehyde to produce a wall material;
Preparing a core material by emulsifying paraffin wax in an aqueous solution;
Microcapsule form characterized in that it comprises the step of adding the wall material and the core material, and by adding acetic acid, stirring and cooling to room temperature to produce a latent heat storage material in the form of microcapsules containing a phase change material; Method for producing latent heat storage material.
상기 멜라민, 물, 포름알데히드의 혼합물을 55정도에서 15분간 교반한 후, 2540로 냉각하여 벽재 물질을 제조하고, 파라핀 왁스를 수용액 70 온도 하에 유지한 후, 파라핀 에멀젼 계면에 멜라민 수지 모노머의 흡착이 용이하도록 황산 도데실 나트륨(sodium dodecyl sulfate, SDS, Aldrich 99.5 %)의 계면활성제 0.5중량% ~ 1.5중량부의 농도투입한 후, 교반을 통하여 에멀젼화시켜 심물질을 제조하는 단계 후, 상기 벽재 물질과 심물질을 투입하면서 아세트산을 투입하여 100분간 350 rpm의 속도로 교반한 후 실온으로 냉각 후 건조하여 제조하는 것을 특징으로 하는 마이크로캡슐 형태의 잠열 축열재 제조방법.
The method of claim 1,
The mixture of melamine, water and formaldehyde was stirred at about 55 minutes for 15 minutes, cooled to 2540 to prepare a wall material, the paraffin wax was maintained at 70 ° C. in water, and then adsorption of the melamine resin monomer on the paraffin emulsion interface was carried out. To facilitate the concentration of 0.5% to 1.5 parts by weight of a surfactant of sodium dodecyl sulfate (SDS, Aldrich 99.5%), and then emulsified by stirring to prepare a core material, the wall material and Method for producing a latent heat storage material of microcapsules type, characterized in that the acetic acid is added while stirring the core material and stirred at a speed of 350 rpm for 100 minutes and then cooled to room temperature and dried.
상기 콘크리트 조성물은 전체가 100 중량부라 할 때, 결합재 21.546.5 중량부, 잠열축열재 0.442.72 중량부, 혼화제 0.110.33 중량부, 골재 43.063.0 중량부로 구성되는 것을 특징으로 하는 마이크로캡슐 형태의 잠열 축열 콘크리트 조성물.
In the concrete composition comprising a latent heat storage material,
When the concrete composition is 100 parts by weight in total, a microcapsule form comprising a binder 21.546.5 parts by weight, latent heat storage material 0.442.72 parts by weight, admixture 0.110.33 parts by weight, aggregate 43.063.0 parts by weight Latent heat storage concrete composition.
상기 결합재는 시멘트 20.040.0 중량부, 팽창재로서 CSA(Calcium Sulfur Aluminate) 15 중량부, 무수석고(CaSO4) 0.51.5 중량부로 구성되며,
상기 잠열 축열재는 멜라민, 물, 포름알데히드의 혼합물로 구성된 벽재물질과 파라핀 왁스를 수용액에서 에멀션화한 심물질, 0.442.72 중량부로 구성되며,
상기 혼화제는 멜라민계 유동화제 0.10.3 중량부, 증점제 0.010.03 중량부로 구성되어 이루어지는 것을 특징으로 하는 마이크로캡슐 형태의 잠열 축열 콘크리트 조성물.
The method of claim 3,
The binder is composed of 20.040.0 parts by weight of cement, 15 parts by weight of Calcium Sulfur Aluminate (CSA) as an expanding material, and 0.51.5 parts by weight of anhydrous gypsum (CaSO 4 ),
The latent heat storage material is composed of a wall material consisting of a mixture of melamine, water, formaldehyde and core material emulsified in an aqueous solution of paraffin wax, 0.442.72 parts by weight,
The admixture is a latent heat storage concrete composition of the microcapsule type, characterized in that consisting of melamine-based fluidizing agent 0.10.3 parts by weight, thickener 0.010.03 parts by weight.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20160000086A (en) | 2014-06-23 | 2016-01-04 | 이화여자대학교 산학협력단 | Manufacturing method of concrete mixed with phase change material |
| KR20160046951A (en) | 2014-10-20 | 2016-05-02 | 한경대학교 산학협력단 | Light weight concrete using phase change material and manufacturing method thereof |
| KR20160107516A (en) * | 2015-03-04 | 2016-09-19 | 한국건설기술연구원 | Concrete cooling system |
| KR101666401B1 (en) | 2015-09-25 | 2016-10-14 | 한국과학기술연구원 | Double layered thermal energy storage capsules and method of manufacturing the same |
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- 2012-05-31 KR KR1020120058820A patent/KR20130136599A/en not_active Application Discontinuation
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20160000086A (en) | 2014-06-23 | 2016-01-04 | 이화여자대학교 산학협력단 | Manufacturing method of concrete mixed with phase change material |
| KR20160046951A (en) | 2014-10-20 | 2016-05-02 | 한경대학교 산학협력단 | Light weight concrete using phase change material and manufacturing method thereof |
| KR20160107516A (en) * | 2015-03-04 | 2016-09-19 | 한국건설기술연구원 | Concrete cooling system |
| KR101666401B1 (en) | 2015-09-25 | 2016-10-14 | 한국과학기술연구원 | Double layered thermal energy storage capsules and method of manufacturing the same |
| KR20220021224A (en) * | 2020-08-13 | 2022-02-22 | 명지대학교 산학협력단 | Method for manufacturing phase change nanocapsule and phase change nanocapsule manufactured using the same |
| KR20230064654A (en) * | 2021-11-03 | 2023-05-11 | 인천대학교 산학협력단 | High Thermal Conductivity PCM Heating generation Concrete composition using Magnetite Aggregate |
| KR102651041B1 (en) * | 2023-06-08 | 2024-03-25 | 주식회사 대하맨텍 | Phase change material microcapsule, method for manufacturing the same, and thermal energy storage concrete composite using the same |
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