JP2018111760A - Composition for forming heat insulating layer and manufacturing method of heat insulating material - Google Patents
Composition for forming heat insulating layer and manufacturing method of heat insulating material Download PDFInfo
- Publication number
- JP2018111760A JP2018111760A JP2017002152A JP2017002152A JP2018111760A JP 2018111760 A JP2018111760 A JP 2018111760A JP 2017002152 A JP2017002152 A JP 2017002152A JP 2017002152 A JP2017002152 A JP 2017002152A JP 2018111760 A JP2018111760 A JP 2018111760A
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- Prior art keywords
- heat insulating
- resin
- forming
- composition
- mass
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 41
- 239000011810 insulating material Substances 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
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- 239000011347 resin Substances 0.000 claims abstract description 55
- 239000003094 microcapsule Substances 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 239000010410 layer Substances 0.000 claims description 46
- 239000011248 coating agent Substances 0.000 claims description 37
- 238000000576 coating method Methods 0.000 claims description 37
- 238000009413 insulation Methods 0.000 claims description 27
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- 230000015572 biosynthetic process Effects 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 11
- 239000011254 layer-forming composition Substances 0.000 claims description 9
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- 230000009477 glass transition Effects 0.000 claims description 6
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
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- KORSJDCBLAPZEQ-UHFFFAOYSA-N dicyclohexylmethane-4,4'-diisocyanate Chemical compound C1CC(N=C=O)CCC1CC1CCC(N=C=O)CC1 KORSJDCBLAPZEQ-UHFFFAOYSA-N 0.000 description 1
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- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- SWRGUMCEJHQWEE-UHFFFAOYSA-N ethanedihydrazide Chemical compound NNC(=O)C(=O)NN SWRGUMCEJHQWEE-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 238000007646 gravure printing Methods 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- MNNOXWOITSQLHM-UHFFFAOYSA-N hydrazinylmethylhydrazine Chemical compound NNCNN MNNOXWOITSQLHM-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
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- 238000007759 kiss coating Methods 0.000 description 1
- AYLRODJJLADBOB-QMMMGPOBSA-N methyl (2s)-2,6-diisocyanatohexanoate Chemical compound COC(=O)[C@@H](N=C=O)CCCCN=C=O AYLRODJJLADBOB-QMMMGPOBSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
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- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
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- OEIJHBUUFURJLI-UHFFFAOYSA-N octane-1,8-diol Chemical compound OCCCCCCCCO OEIJHBUUFURJLI-UHFFFAOYSA-N 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
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- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
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- 229920000570 polyether Polymers 0.000 description 1
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Landscapes
- Laminated Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
Abstract
Description
本発明は、基材の表面に断熱層を形成して断熱性に優れた複合材料(断熱材)を与える断熱層形成用組成物及び断熱材の製造方法に関する。 The present invention relates to a composition for forming a heat insulating layer which forms a heat insulating layer on the surface of a base material to give a composite material (heat insulating material) excellent in heat insulating properties, and a method for manufacturing the heat insulating material.
従来、樹脂ベースの断熱層が基材の表面に形成された複合材料は、断熱材として、建材、電気製品、食品、衣料、自動車等の分野で広く用いられている。このような断熱層を形成する材料としては、基材に塗布した後、乾燥に供せられる液体組成物、射出成形等に供する樹脂組成物等が一般的である。 Conventionally, a composite material in which a resin-based heat insulating layer is formed on the surface of a base material is widely used as a heat insulating material in the fields of building materials, electrical products, food, clothing, automobiles, and the like. As a material for forming such a heat insulating layer, a liquid composition that is applied to a substrate and then dried, a resin composition that is used for injection molding, or the like is generally used.
基材への塗布、乾燥等により、断熱層を与える液体組成物は、例えば、特許文献1及び2に開示されている。
特許文献1には、断熱性を有する化粧シート等の形成に用いられる組成物であって、バインダー樹脂100質量部に対して、中空粒子10〜120質量部、および溶剤もしくは分散剤50〜5000質量部が配合されている断熱性層形成用塗料組成物が開示されている。
また、特許文献2には、断熱性紙容器等の形成に用いられる断熱紙が開示されており、この断熱紙は、パルプを主原料とする紙基材の少なくとも片面に、アクリル樹脂を含む水溶液に空洞を有する中空粒子が分散している塗工組成物を用いて得られたことが記載されている。
The liquid composition which gives a heat insulation layer by application | coating to a base material, drying, etc. is disclosed by patent document 1 and 2, for example.
Patent Document 1 discloses a composition used for forming a decorative sheet or the like having heat insulation properties, and 10 to 120 parts by mass of hollow particles and 50 to 5000 parts by mass of a solvent or dispersant with respect to 100 parts by mass of the binder resin. A coating composition for forming a heat-insulating layer in which parts are blended is disclosed.
Patent Document 2 discloses a heat insulating paper used for forming a heat insulating paper container or the like, and this heat insulating paper is an aqueous solution containing an acrylic resin on at least one side of a paper base material mainly made of pulp. It is described that it was obtained using a coating composition in which hollow particles having cavities are dispersed.
本発明の課題は、保管時の経時安定性に優れ、塗膜の加熱により、熱膨張性マイクロカプセルが膨張して形成された膨張カプセル含有樹脂皮膜からなる断熱層を基材の表面に効率よく形成する断熱層形成用組成物及び断熱材の製造方法を提供することである。 An object of the present invention is excellent in stability over time during storage, and a heat insulating layer comprising an expanded capsule-containing resin film formed by expansion of thermally expandable microcapsules by heating of the coating film is efficiently applied to the surface of the substrate. It is providing the manufacturing method of the composition for heat insulation layer formation and heat insulating material to form.
本発明は、以下に示される。
1.皮膜形成用樹脂、膨張開始温度が80℃〜150℃である熱膨張性マイクロカプセル、アルコール及び水を、これらの合計を100質量%とした場合に、それぞれ、18〜40質量%、5〜22質量%、7〜20質量%及び30〜56質量%含有することを特徴とする断熱層形成用組成物。
2.上記皮膜形成用樹脂は、ガラス転移温度が−70℃〜−50℃のポリウレタン樹脂を含む上記項1に記載の断熱層形成用組成物。
3.上記熱膨張性マイクロカプセルは、熱可塑性の樹脂材料からなる外殻の内部に、液体化合物が内包されたものである上記項1又は2に記載の断熱層形成用組成物。
4.上記アルコールがイソプロピルアルコールを含む上記項1乃至3のいずれか一項に記載の断熱層形成用組成物。
5.断熱材の製造方法であって、
上記項1乃至4のいずれか一項に記載の断熱層形成用組成物を、基材の表面に塗布する工程と、得られた塗膜を加熱して、アルコール及び水を蒸発させるとともに、該塗膜に含まれる熱膨張性マイクロカプセルを膨張させつつ皮膜化する工程とを、順次、備えることを特徴とする断熱材の製造方法。
The present invention is shown below.
1. The resin for forming a film, the thermally expandable microcapsule having an expansion start temperature of 80 ° C. to 150 ° C., alcohol, and water are 18 to 40% by mass and 5 to 22 respectively when the total of these is 100% by mass. A composition for forming a heat insulating layer, comprising: mass%, 7 to 20 mass%, and 30 to 56 mass%.
2. Item 2. The heat insulating layer forming composition according to Item 1, wherein the film forming resin includes a polyurethane resin having a glass transition temperature of -70 ° C to -50 ° C.
3. Item 3. The composition for forming a heat insulation layer according to Item 1 or 2, wherein the thermally expandable microcapsule is obtained by encapsulating a liquid compound in an outer shell made of a thermoplastic resin material.
4). Item 4. The composition for forming a heat insulation layer according to any one of Items 1 to 3, wherein the alcohol contains isopropyl alcohol.
5). A method of manufacturing a heat insulating material,
The step of applying the composition for forming a heat insulating layer according to any one of Items 1 to 4 to the surface of the substrate, heating the obtained coating film to evaporate alcohol and water, A method for producing a heat insulating material, comprising sequentially forming a film while expanding the thermally expandable microcapsules contained in the coating film.
本発明の断熱層形成用組成物を用いて基材の表面に塗膜を形成した後、得られた塗膜を加熱することにより、熱膨張性マイクロカプセルを体積膨張させ、皮膜形成用樹脂からなる母相の中に膨張カプセルからなる分散相を含む膨張カプセル含有樹脂皮膜からなる断熱層を有する断熱材を製造することができる
本発明の断熱層形成用組成物は、保管中又は使用中に、特定の成分、例えば、熱膨張性マイクロカプセルが沈降して均一性が低下することを抑制することができ、保存安定性に優れる。従って、皮膜形成用樹脂及び熱膨張性マイクロカプセルの分散性が良好であるため、断熱材の製造時において、基材に塗布した場合には、皮膜形成用樹脂及び熱膨張性マイクロカプセルが均一に分布した塗膜が得られ、膨張カプセルのサイズのばらつきの小さい断熱層を備える断熱材を効率よく製造することができる。このような断熱材は、建築材料、電気製品、食品、衣料、自動車等の分野で広く利用することができる。
After forming a coating film on the surface of the substrate using the composition for forming a heat insulating layer of the present invention, by heating the obtained coating film, the thermally expandable microcapsules are volume-expanded, and the coating film forming resin is used. A heat insulating material having a heat insulating layer made of an expanded capsule-containing resin film containing a dispersed phase consisting of expanded capsules in the matrix phase can be produced. It is possible to suppress a specific component, for example, a thermally expandable microcapsule from settling and lowering the uniformity, and it is excellent in storage stability. Therefore, since the dispersibility of the film-forming resin and the heat-expandable microcapsules is good, the film-forming resin and the heat-expandable microcapsules are uniformly distributed when applied to the substrate during the production of the heat insulating material. A distributed coating film is obtained, and a heat insulating material including a heat insulating layer with small variation in the size of the expanded capsule can be efficiently produced. Such a heat insulating material can be widely used in the fields of building materials, electrical products, food, clothing, automobiles and the like.
本発明は、紙、樹脂フィルム、樹脂成形体、無機材料成形体等の被塗物(基材)の表面に、コーティング、スプレー等の、従来、公知の方法で塗布した後、塗膜を熱処理(加熱乾燥)することにより、断熱皮膜を形成するために好適な液状組成物であり、皮膜形成用樹脂、膨張開始温度が80℃〜150℃である熱膨張性マイクロカプセル、アルコール及び水を含有する断熱層形成用組成物である。塗膜の熱処理(加熱乾燥)により、熱膨張性マイクロカプセルが体積膨張して膨張カプセルとなり、この膨張カプセルが皮膜内部に分散相として存在し、断熱効果が付与される。
本発明の断熱層形成用組成物は、接着性改良剤、充填剤、粘度調整剤、酸化防止剤、紫外線吸収剤、安定剤、難燃剤、帯電防止剤、防カビ剤、着色剤等の他の成分を含有することができる。
In the present invention, a coating, spraying or the like is applied to the surface of an object to be coated (substrate) such as paper, a resin film, a resin molded body, an inorganic material molded body, and the like, and then the coating film is heat treated. A liquid composition suitable for forming a heat-insulating film by (heat drying), containing a film-forming resin, a thermally expandable microcapsule having an expansion start temperature of 80 ° C. to 150 ° C., alcohol and water It is a composition for heat insulation layer formation. By heat treatment (heat drying) of the coating film, the thermally expandable microcapsules are expanded in volume to become expanded capsules, and these expanded capsules exist as a dispersed phase inside the film, and a heat insulating effect is imparted.
The composition for forming a heat insulating layer of the present invention includes an adhesion improver, a filler, a viscosity modifier, an antioxidant, an ultraviolet absorber, a stabilizer, a flame retardant, an antistatic agent, an antifungal agent, a colorant and the like. The component of this can be contained.
以下、本発明の断熱層形成用組成物について、説明する。 Hereinafter, the composition for heat insulation layer formation of this invention is demonstrated.
上記皮膜形成用樹脂は、これを含む液状組成物を用いて得られた塗膜の加熱乾燥により、皮膜を形成するものであれば、特に限定されない。尚、本発明に係る皮膜形成用樹脂は、単一物質により皮膜を形成するもの、及び、2種以上の物質の反応等により皮膜を形成するもの、のいずれでもよく、後者の場合の組成物中の含有割合は、反応により形成された樹脂の量を用いて計算されたものとする。 The film-forming resin is not particularly limited as long as it forms a film by heating and drying a coating obtained using a liquid composition containing the resin. The film-forming resin according to the present invention may be either a film that forms a film by a single substance or a film that forms a film by reaction of two or more substances. The composition in the latter case It is assumed that the content ratio is calculated using the amount of resin formed by the reaction.
上記皮膜形成用樹脂としては、ウレタン樹脂、アクリル樹脂、スチレン樹脂、塩化ビニル樹脂、ポリエステル樹脂、アルキド樹脂、ポリアミド樹脂、ポリアミドイミド樹脂、ポリイミド樹脂、エポキシ樹脂、フェノキシ樹脂及びこれらのシリコーン変性物又はシラン変性物等が挙げられる。本発明においては、断熱層形成用組成物からなる塗膜の加熱乾燥により形成された皮膜の耐水性又は耐溶剤性、基材に対する密着性等を有する、ウレタン樹脂、アクリル樹脂、スチレン樹脂、塩化ビニル樹脂又はこれらの変性物等が好ましく、これらのうち、アルコール水溶液に溶解する又はアルコール水溶液中で分散性が良好なウレタン樹脂又はその変性物が特に好ましい。 Examples of the film-forming resin include urethane resin, acrylic resin, styrene resin, vinyl chloride resin, polyester resin, alkyd resin, polyamide resin, polyamideimide resin, polyimide resin, epoxy resin, phenoxy resin, and their silicone modified products or silanes. Examples include modified products. In the present invention, a urethane resin, an acrylic resin, a styrene resin, a chloride, etc. having water resistance or solvent resistance of a film formed by heating and drying a coating film comprising the heat insulating layer forming composition, adhesion to a substrate, and the like. A vinyl resin or a modified product thereof is preferable, and among these, a urethane resin which is dissolved in an alcohol aqueous solution or has good dispersibility in an alcohol aqueous solution or a modified product thereof is particularly preferable.
上記ウレタン樹脂としては、例えば、カルボキシル基を有し、分子末端にイソシアネート基を有するウレタンプレポリマー原料と、ヒドロキシル基及び重合性不飽和結合を有する化合物とを反応させて、上記イソシアネート基及び上記ヒドロキシル基によるウレタン結合を含むウレタンプレポリマーを得た後、このウレタンプレポリマーを、アルコール、水、中和剤及び鎖伸長剤を含む液中で分散させて、分子末端に重合性不飽和結合を有するウレタン樹脂原料を生成させ、次いで重合性不飽和結合の重合を行って得られた樹脂とすることができる。 As the urethane resin, for example, a urethane prepolymer raw material having a carboxyl group and having an isocyanate group at a molecular terminal is reacted with a compound having a hydroxyl group and a polymerizable unsaturated bond, and the isocyanate group and the hydroxyl group are reacted. After obtaining a urethane prepolymer containing a urethane bond due to a group, the urethane prepolymer is dispersed in a liquid containing alcohol, water, a neutralizing agent and a chain extender to have a polymerizable unsaturated bond at the molecular end. A resin obtained by generating a urethane resin raw material and then polymerizing a polymerizable unsaturated bond can be obtained.
上記ウレタンプレポリマー原料は、カルボキシル基を有するジオールと、ポリオールと、ポリイソシアネートとを反応させて得られたものとすることができ、好ましくは、イソシアネート基の当量をヒドロキシル基の合計当量より過剰とさせて得られたものである。
カルボキシル基を有するジオールとしては、α,α’−ジメチロールアルカン酸(グリセリン酸、ジメチロールプロピオン酸、ジメチロールブタン酸、2,2−ジメチロールペンタン酸等)、ジオキシマレイン酸、ジオキシフマル酸、酒石酸、2,6−ジオキシ安息香酸、4,4−ビス(ヒドロキシフェニル)吉草酸、4,4−ビス(ヒドロキシフェニル)酪酸等が挙げられる。
ポリオールとしては、エチレンオキサイド、プロピレンオキサイド、テトラヒドロフラン等を開環重合したポリエチレングリコール、ポリプロピレングリコール、ポリオキシテトラメチレンエーテルグリコール等のポリエーテルポリオール;エチレングリコール、ジエチレングリコール、トリエチレングリコール、1,2−プロパンジオール、1,3−プロパンジオール、1,3−ブタンジオール、1,4−ブタンジオール、ネオペンチルグリコール、ペンタンジオール、3−メチル−1,5−ペンタンジオール、1,6−ヘキサンジオール、オクタンジオール、1,4−ブチンジオール、ジプロピレングリコール、ビスフェノールA、水添ビスフェノールA等の飽和又は不飽和の低分子量グリコールと、アジピン酸、マレイン酸、フマル酸、無水フタル酸、イソフタル酸、テレフタル酸、コハク酸、シュウ酸、マロン酸、グルタル酸、ピメリン酸、アゼライン酸、セバシン酸、スベリン酸等の二塩基酸又はこれらに対応する酸無水物とを脱水縮合反応させて得られたポリエステルポリオール;ポリカーボネートポリオール等が挙げられる。
ポリイソシアネートとしては、ジフェニルメタンジイソシアネート、粗製ジフェニルメタンジイソシアネート、トリレンジイソシアネート、ナフタレンジイソシアネート、p−フェニレンジイソシアネート、キシレンジイソシアネート、テトラメチルキシリレンジイソシアネート、トリジンジイソシアネート等の芳香族イソシアネート;ヘキサメチレンジイソシアネート、リシンジイソシアネート、リシントリイソシアネート等の脂肪族イソシアネート;イソホロンジイソシアネート、シクロヘキシルジイソシアネート、水添化XDI、水添化MDI等の脂環式イソシアネート;上記イソシアネート化合物のウレタン変性体、2量体、3量体、カルボジイミド変性体、アロファネート変性体、ビューレット変性体、ウレア変性体、イソシアヌレート変性体、オキサゾリドン変性体、イソシアネート基末端プレポリマー等の変性イソシアネート等が挙げられる。
The urethane prepolymer raw material can be obtained by reacting a diol having a carboxyl group, a polyol, and a polyisocyanate. Preferably, the equivalent of the isocyanate group is more than the total equivalent of the hydroxyl group. It was obtained.
Examples of the diol having a carboxyl group include α, α′-dimethylolalkanoic acid (glyceric acid, dimethylolpropionic acid, dimethylolbutanoic acid, 2,2-dimethylolpentanoic acid, etc.), dioxymaleic acid, dioxyfumaric acid, Examples include tartaric acid, 2,6-dioxybenzoic acid, 4,4-bis (hydroxyphenyl) valeric acid, 4,4-bis (hydroxyphenyl) butyric acid, and the like.
Polyols include polyether polyols such as polyethylene glycol, polypropylene glycol, and polyoxytetramethylene ether glycol obtained by ring-opening polymerization of ethylene oxide, propylene oxide, tetrahydrofuran, etc .; ethylene glycol, diethylene glycol, triethylene glycol, 1,2-propanediol 1,3-propanediol, 1,3-butanediol, 1,4-butanediol, neopentyl glycol, pentanediol, 3-methyl-1,5-pentanediol, 1,6-hexanediol, octanediol, Saturated or unsaturated low molecular weight glycols such as 1,4-butynediol, dipropylene glycol, bisphenol A, hydrogenated bisphenol A, and adipic acid, maleic acid, fumaric acid Dehydration condensation with dibasic acids such as phthalic anhydride, isophthalic acid, terephthalic acid, succinic acid, oxalic acid, malonic acid, glutaric acid, pimelic acid, azelaic acid, sebacic acid, suberic acid or the corresponding acid anhydrides Polyester polyol obtained by reaction; polycarbonate polyol and the like.
Examples of polyisocyanates include diphenylmethane diisocyanate, crude diphenylmethane diisocyanate, tolylene diisocyanate, naphthalene diisocyanate, p-phenylene diisocyanate, xylene diisocyanate, tetramethylxylylene diisocyanate, and tolidine diisocyanate; hexamethylene diisocyanate, lysine diisocyanate, ricintri Aliphatic isocyanates such as isocyanates; Cycloaliphatic isocyanates such as isophorone diisocyanate, cyclohexyl diisocyanate, hydrogenated XDI, and hydrogenated MDI; Urethane modified products, dimers, trimers, carbodiimide modified products, and allophanates of the above isocyanate compounds Modified body, burette modified body, urea modified body, isocyanu Over preparative modified products, oxazolidone modified product, modified isocyanates such as isocyanate group-terminated prepolymer and the like.
その後、ウレタンプレポリマー原料と反応させる、ヒドロキシル基及び重合性不飽和結合を有する化合物としては、2−ヒドロキシプロピル(メタ)アクリレート、2−ヒドロキシブチル(メタ)アクリレート、4−ヒドロキシブチル(メタ)アクリレート、2−ヒドロキシ−3−フェノキシプロピル(メタ)アクリレート、2−ヒドロキシ−3−アクリロイルオキシプロピル(メタ)アクリレート、グリセリンジ(メタ)アクリレート、グリセリン(メタ)アクリレート、トリメチロールプロパンジアリルエーテル、グリセリンモノ(メタ)アクリレート、グリシドール/アクリル酸付加物、ペンタエリスリトールトリ(メタ)アクリレート、ペンタエリスリトールトリアリルエーテル、2−ヒドロキシエチルモノビニルエーテル、4−ヒドロキシブチルモノビニルエーテル、N−メチロールアクリルアミド、ポリプロピレングリコール(メタ)アクリレート、ポリエチレングリコール(メタ)アクリレート、ポリカプロラクトン(メタ)アクリレート等が挙げられる。これらは、得られるウレタンプレポリマーにイソシアネート基が若干残存する割合で用いられる。 Then, as a compound having a hydroxyl group and a polymerizable unsaturated bond to be reacted with the urethane prepolymer raw material, 2-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate , 2-hydroxy-3-phenoxypropyl (meth) acrylate, 2-hydroxy-3-acryloyloxypropyl (meth) acrylate, glycerol di (meth) acrylate, glycerol (meth) acrylate, trimethylolpropane diallyl ether, glycerol mono ( (Meth) acrylate, glycidol / acrylic acid adduct, pentaerythritol tri (meth) acrylate, pentaerythritol triallyl ether, 2-hydroxyethyl monovinyl ether, 4- B carboxybutyl monovinyl ether, N- methylol acrylamide, polypropylene glycol (meth) acrylate, polyethylene glycol (meth) acrylates, polycaprolactone (meth) acrylate. These are used in such a ratio that some isocyanate groups remain in the resulting urethane prepolymer.
次に、ウレタンプレポリマーを、エタノール、n−プロパノール、イソプロピルアルコール、n−ブタノール、イソブチルアルコール、sec−ブチルアルコール、tert−ブチルアルコール、n−ペンタノール、sec−アミルアルコール等のアルコール;水;水酸化ナトリウム、水酸化カリウム等のアルカリ金属の水酸化物、トリメチルアミン、トリエチルアミン、トリイソプロピルアミン、トリブチルアミン等の3級アミン、トリエタノールアミン、トリイソプロパノールアミン、N−アルキルジエタノールアミン、N,N’−ジアルキルモノエタノールアミン、N−アルキルジイソプロパノールアミン、N,N’−ジアルキルモノイソプロパノールアミン等のアルカノールアミン、アンモニア等の中和剤;及び、エチレンンジアミン、プロピレンジアミン、ヘキサメチレンジアミン、ジエチレントリアミン、トリエチレンテトラミン、イソホロンジアミン、ジシクロヘキシルメタン−4,4’−ジアミン等の脂肪族ジアミン;2−ヒドロキシエチルエチレンジアミン、2−ヒドロキシエチルプロピレンジアミン、ジ−2−ヒドロキシエチルエチレンジアミン、ジ−2−ヒドロキシエチルプロピレンジアミン、2−ヒドロキシプロピルエチレンジアミン、ジ−2−ヒドロキシプロピルエチレンジアミン等の分子内に水酸基を有するジアミン;メチレンジヒドラジン、エチレンジヒドラジン、プロピレンジヒドラジン等のアルキレンジヒドラジン、アジピン酸ジヒドラジド、シュウ酸ジヒドラジド、マロン酸ジヒドラジド、コハク酸ジヒドラジド、フタル酸ジヒドラジド、イタコン酸ジヒドラジド等の飽和又は不飽和ジヒドラジン;ダイマー酸のカルボキシル基をアミノ基に転化したダイマージアミン等の鎖伸長剤を含む液中で分散させて、分子末端に重合性不飽和結合を有するウレタン樹脂原料を生成させる。 Next, the urethane prepolymer is mixed with alcohol such as ethanol, n-propanol, isopropyl alcohol, n-butanol, isobutyl alcohol, sec-butyl alcohol, tert-butyl alcohol, n-pentanol, sec-amyl alcohol; water; water Alkali metal hydroxides such as sodium oxide and potassium hydroxide, tertiary amines such as trimethylamine, triethylamine, triisopropylamine and tributylamine, triethanolamine, triisopropanolamine, N-alkyldiethanolamine, N, N'-dialkyl Alkanolamines such as monoethanolamine, N-alkyldiisopropanolamine, N, N′-dialkylmonoisopropanolamine, neutralizing agents such as ammonia; and ethylenediamine Aliphatic diamines such as propylenediamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine, isophoronediamine, dicyclohexylmethane-4,4′-diamine; 2-hydroxyethylethylenediamine, 2-hydroxyethylpropylenediamine, di-2-hydroxy Diamines having a hydroxyl group in the molecule such as ethylethylenediamine, di-2-hydroxyethylpropylenediamine, 2-hydroxypropylethylenediamine, di-2-hydroxypropylethylenediamine; alkylene dimers such as methylenedihydrazine, ethylenedihydrazine, propylenedihydrazine Hydrazine, adipic acid dihydrazide, oxalic acid dihydrazide, malonic acid dihydrazide, succinic acid dihydrazide, phthalic acid dihydrazide, Saturated or unsaturated dihydrazine such as diacid dihydrazide; Urethane having a polymerizable unsaturated bond at the molecular end by dispersing in a solution containing a chain extender such as dimeramine converted from dimer acid carboxyl group to amino group A resin raw material is produced.
その後、ラジカル重合法等を利用して、ウレタン樹脂原料の重合性不飽和結合を重合させ、高分子量化されたウレタン樹脂の分散液を得ることができる。 Thereafter, a polymerizable unsaturated bond of the urethane resin raw material is polymerized using a radical polymerization method or the like to obtain a high molecular weight urethane resin dispersion.
上記皮膜形成用樹脂のガラス転移温度は、断熱層形成用組成物からなる塗膜を加熱乾燥した際の、熱膨張性マイクロカプセルの好ましい体積膨張性が得られることから、好ましくは−70℃〜−50℃であり、更に好ましくは−65℃〜−55℃である。 The glass transition temperature of the film-forming resin is preferably −70 ° C. to obtain a preferable volume expansion property of the heat-expandable microcapsule when the coating film made of the heat-insulating layer-forming composition is heat-dried. It is -50 degreeC, More preferably, it is -65 degreeC--55 degreeC.
上記熱膨張性マイクロカプセルは、好ましくは、加熱により占有体積を増す内包物質(気体、又は、固体若しくは液体であって加熱により気化するもの)が、樹脂材料からなる外殻の内部に封じ込められた粒子状マイクロカプセルであり、本発明に係る熱膨張性マイクロカプセルは、80℃〜150℃で加熱されると体積膨張するマイクロカプセルである。上記温度は、膨張開始温度であり、このような性質を有する熱膨張性マイクロカプセルが加熱されて膨張開始温度に達すると、内包物質が体積膨張し、外殻を構成する樹脂材料が軟化するため、内圧により膨張したカプセル(膨張カプセル)が得られる。本発明において、上記熱膨張性マイクロカプセルは、熱可塑性の樹脂材料(樹脂組成物)からなる外殻の内部に、液体化合物が内包されたものであることがより好ましい。 In the thermally expandable microcapsule, an encapsulated substance (a gas, or a solid or liquid that is vaporized by heating) that increases its occupied volume by heating is preferably enclosed in an outer shell made of a resin material. It is a particulate microcapsule, and the thermally expandable microcapsule according to the present invention is a microcapsule that expands in volume when heated at 80 ° C. to 150 ° C. The above temperature is an expansion start temperature, and when the thermally expandable microcapsule having such properties is heated to reach the expansion start temperature, the encapsulated substance expands in volume and the resin material constituting the outer shell softens. A capsule (expanded capsule) expanded by the internal pressure is obtained. In the present invention, the thermally expandable microcapsule is more preferably one in which a liquid compound is encapsulated inside an outer shell made of a thermoplastic resin material (resin composition).
上記熱膨張性マイクロカプセルを構成する内包物質である液体化合物は、上記熱膨張性マイクロカプセルの外殻を構成する樹脂材料の軟化温度以下の沸点(大気圧条件)を有するものが好ましく、例えば、n−ブタン、イソブタン、シクロブタン、n−ペンタン、イソペンタン、シクロペンタン、n−ヘキサン、2−メチルペンタン、2,2−ジメチルブタン、シクロヘキサン、n−ヘプタン、シクロヘプタン、n−オクタン、シクロオクタン等の炭化水素;C3F7OCH3、C4F9OCH3、C4F9OC2H5等のハイドロフルオロエーテル化合物等とすることができる。上記液体化合物は、1種のみであってよいし、2種以上であってもよい。上記液体化合物としては、炭化水素が好ましく、炭素原子数が4〜5の低沸点炭化水素を含むことが特に好ましい。また、外殻を構成する樹脂材料は、アクリロニトリル、メタクリロニトリル、アクリル酸アルキルエステル、メタクリル酸アルキルエステル、塩化ビニル、塩化ビニリデン、酢酸ビニル、芳香族ビニル化合物、アクリル酸、メタクリル酸、マレイン酸、フマル酸、イタコン酸、シトラコン酸、アクリルアミド、置換アクリルアミド、メタクリルアミド、置換メタクリルアミド、及び、2以上の重合性炭素−炭素不飽和結合を有する多官能性化合物から選ばれた少なくとも1種に由来する構造単位を含む熱可塑性樹脂を含有することが好ましい。この熱可塑性樹脂としては、例えば、ポリ塩化ビニリデン;塩化ビニリデン・アクリロニトリル共重合体、ポリアクリロニトリル、アクリロニトリル・メタクリル酸アルキルエステル共重合体等の、アクリロニトリル系(共)重合体;ポリメタクリル酸メチル等のアクリル系(共)重合体;ポリ塩化ビニル等が挙げられる。これらのうち、アクリロニトリル系(共)重合体が特に好ましい。上記樹脂材料(樹脂組成物)は、安定剤、紫外線吸収剤、酸化防止剤、帯電防止剤、難燃剤等の添加剤を含有することができる。 The liquid compound that is the inclusion substance constituting the thermally expandable microcapsule preferably has a boiling point (atmospheric pressure condition) that is not higher than the softening temperature of the resin material that constitutes the outer shell of the thermally expandable microcapsule. n-butane, isobutane, cyclobutane, n-pentane, isopentane, cyclopentane, n-hexane, 2-methylpentane, 2,2-dimethylbutane, cyclohexane, n-heptane, cycloheptane, n-octane, cyclooctane, etc. Hydrocarbon: Hydrofluoroether compounds such as C 3 F 7 OCH 3 , C 4 F 9 OCH 3 , C 4 F 9 OC 2 H 5 and the like. The liquid compound may be only one type or two or more types. As said liquid compound, a hydrocarbon is preferable and it is especially preferable that the C4-5 low boiling point hydrocarbon is included. In addition, the resin material constituting the outer shell is acrylonitrile, methacrylonitrile, alkyl acrylate ester, alkyl methacrylate ester, vinyl chloride, vinylidene chloride, vinyl acetate, aromatic vinyl compound, acrylic acid, methacrylic acid, maleic acid, Derived from at least one selected from fumaric acid, itaconic acid, citraconic acid, acrylamide, substituted acrylamide, methacrylamide, substituted methacrylamide, and a polyfunctional compound having two or more polymerizable carbon-carbon unsaturated bonds It is preferable to contain a thermoplastic resin containing a structural unit. Examples of this thermoplastic resin include polyvinylidene chloride; vinylidene chloride / acrylonitrile copolymer, polyacrylonitrile, acrylonitrile / methacrylic acid alkyl ester copolymer, and other acrylonitrile-based (co) polymers; polymethyl methacrylate, etc. Acrylic (co) polymers such as polyvinyl chloride. Of these, acrylonitrile-based (co) polymers are particularly preferred. The resin material (resin composition) can contain additives such as a stabilizer, an ultraviolet absorber, an antioxidant, an antistatic agent, and a flame retardant.
上記熱膨張性マイクロカプセルの形状は、球状又は楕円球状であり、熱機械分析(TMA)等により測定された粒子径は、適正な膨張率を与え、良好な断熱層を与えることから、好ましくは2μm以上、より好ましくは3〜40μm、更に好ましくは3〜30μmである。 The shape of the thermally expandable microcapsule is spherical or elliptical spherical, and the particle diameter measured by thermomechanical analysis (TMA) or the like preferably gives an appropriate expansion coefficient and preferably gives a good heat insulating layer. It is 2 μm or more, more preferably 3 to 40 μm, still more preferably 3 to 30 μm.
本発明の断熱層形成用組成物は、上記熱膨張性マイクロカプセルを、1種のみ含んでよいし、2種以上を含んでもよい。 The composition for forming a heat insulating layer of the present invention may contain only one kind of the above heat-expandable microcapsules, or may contain two or more kinds.
本発明の断熱層形成用組成物は、膨張開始温度が80℃未満又は150℃を超える、他の熱膨張性マイクロカプセルを、更に含有してもよい。この場合、他の熱膨張性マイクロカプセルの含有量の上限は、皮膜形成用樹脂及び熱膨張性マイクロカプセルの合計を100質量部としたときに、好ましくは15質量部である。 The composition for forming a heat insulation layer of the present invention may further contain other thermally expandable microcapsules having an expansion start temperature of less than 80 ° C or more than 150 ° C. In this case, the upper limit of the content of the other thermally expandable microcapsules is preferably 15 parts by mass when the total of the film-forming resin and the thermally expandable microcapsules is 100 parts by mass.
上記アルコールは、脂肪族アルコール、脂環式アルコール及び芳香族アルコールのいずれでもよく、また、モノオール及びポリオールのいずれでもよい。本発明において、上記アルコールは、好ましくは、水に溶解するアルコールであり、より好ましくは、炭素原子数が1〜4の脂肪族アルコールである。特に好ましくは、イソプロピルアルコールである。 The alcohol may be any of aliphatic alcohol, alicyclic alcohol and aromatic alcohol, and may be any of monool and polyol. In the present invention, the alcohol is preferably an alcohol that dissolves in water, and more preferably an aliphatic alcohol having 1 to 4 carbon atoms. Particularly preferred is isopropyl alcohol.
本発明の断熱層形成用組成物に含まれる皮膜形成用樹脂、熱膨張性マイクロカプセル、アルコール及び水の含有量は、保存安定性に優れ、膨張カプセルのサイズのばらつきの小さい断熱層を円滑に形成することができることから、これらの合計を100質量%とした場合に、それぞれ、18〜40質量%、5〜22質量%、7〜20質量%及び30〜56質量%であり、好ましくは20〜35質量%、8〜20質量%、8〜15質量%及び38〜55質量%、より好ましくは25〜30質量%、9.5〜16質量%、8.5〜13.5質量%及び42〜53質量%である。 The film-forming resin, heat-expandable microcapsule, alcohol and water contents contained in the heat-insulating layer-forming composition of the present invention are excellent in storage stability and smooth the heat-insulating layer with small variations in the size of the expanded capsule. Since it can form, when these sum is made into 100 mass%, it is 18-40 mass%, 5-22 mass%, 7-20 mass%, and 30-56 mass%, respectively, Preferably it is 20 -35 wt%, 8-20 wt%, 8-15 wt% and 38-55 wt%, more preferably 25-30 wt%, 9.5-16 wt%, 8.5-13.5 wt% and It is 42-53 mass%.
本発明の断熱層形成用組成物は、従来、公知の混合分散機、即ち、プラネタリーミキサー、アトライター、グレンミル、ニーダー、ロール、ディゾルバー等を用いて、原料成分を混合することにより製造することができる。 The heat insulating layer-forming composition of the present invention is conventionally produced by mixing raw material components using a known mixer / disperser, that is, a planetary mixer, attritor, glenmill, kneader, roll, dissolver, or the like. Can do.
本発明の断熱層形成用組成物は、基材の表面への断熱層形成に好適である。即ち、組成物を基材11の表面に塗布して塗膜を形成した後、得られた塗膜を加熱することにより、熱膨張性マイクロカプセルを体積膨張させるとともに樹脂皮膜を形成させ、皮膜形成用樹脂からなる母相の中に膨張カプセルからなる分散相を含む膨張カプセル含有樹脂皮膜からなる断熱層13を有する断熱材1を製造することができる(図1参照)。
他の使用方法としては、剥離可能なシート等の表面に塗膜を形成した後、得られた塗膜を加熱することにより、熱膨張性マイクロカプセルを体積膨張させ、皮膜形成用樹脂からなる母相の中に膨張カプセルからなる分散相を含む膨張カプセル含有樹脂皮膜の単体を製造することができる。
The composition for heat insulation layer formation of this invention is suitable for heat insulation layer formation to the surface of a base material. That is, after the composition is applied to the surface of the substrate 11 to form a coating film, the resulting coating film is heated to expand the thermally expandable microcapsules and form a resin film, thereby forming the film. The heat insulating material 1 which has the heat insulation layer 13 which consists of an expansion capsule containing resin film which contains the dispersed phase which consists of expansion capsules in the mother phase which consists of resin for resin can be manufactured (refer FIG. 1).
Another method of use is to form a coating film on the surface of a peelable sheet or the like, and then heat the resulting coating film to expand the volume of the thermally expandable microcapsules, thereby forming a matrix made of a film-forming resin. A single unit of an expanded capsule-containing resin film containing a dispersed phase composed of expanded capsules in the phase can be produced.
本発明の断熱層形成用組成物を用いて断熱材を製造する方法として、本発明では、断熱層形成用組成物を、基材の表面に塗布する工程(以下、「第1工程」という)と、得られた塗膜を加熱して、アルコール及び水を蒸発させるとともに、該塗膜に含まれる熱膨張性マイクロカプセルを膨張させつつ皮膜化する工程(以下、「第2工程」という)とを、順次、備える。 As a method for producing a heat insulating material using the heat insulating layer forming composition of the present invention, in the present invention, a step of applying the heat insulating layer forming composition to the surface of the substrate (hereinafter referred to as “first step”). And heating the obtained coating film to evaporate alcohol and water, and forming a film while expanding the thermally expandable microcapsules contained in the coating film (hereinafter referred to as “second process”); Are sequentially provided.
本発明に係る第1工程は、断熱層形成用組成物を、基材の表面の所定の部分に塗布する工程である。
上記基材は、有機材料及び無機材料のいずれを含むものでもよく、これらを組み合わせたものであってもよい。本発明においては、紙、樹脂フィルム、樹脂成形体、無機材料成形体等が好ましく用いられる。
The 1st process concerning this invention is a process of apply | coating the composition for heat insulation layer formation to the predetermined part of the surface of a base material.
The base material may contain either an organic material or an inorganic material, or may be a combination thereof. In the present invention, paper, resin film, resin molded body, inorganic material molded body and the like are preferably used.
第1工程において、組成物を基材に塗布する方法は、特に限定されない。通常、基材の構成材料、塗布部の表面形状等に応じて、コーティング(ディップコーティング、バーコーティング、ロールコーティング、グラビアコーティング、カーテンコーティング、キスコーティング等)、スプレー(エアレススプレー、エアスプレー等)、印刷(グラビア印刷、スクリーン印刷等)等から、適宜、選択される。
表面外観性に優れ、断熱性に優れた皮膜の形成に好適な塗膜の厚さは、通常、20μm以上、好ましくは30〜100μm、より好ましくは40〜80μmである。上記のように、本発明の断熱層形成用組成物は、保存安定性に優れ、熱膨張性マイクロカプセル等の特定の成分が沈降する等の不具合が抑制されるため、得られる塗膜に含まれる熱膨張性マイクロカプセルは、全体に渡って均一に分布している。
In the first step, the method for applying the composition to the substrate is not particularly limited. Usually, coating (dip coating, bar coating, roll coating, gravure coating, curtain coating, kiss coating, etc.), spray (airless spray, air spray, etc.) It is appropriately selected from printing (gravure printing, screen printing, etc.).
The thickness of the coating film suitable for forming a film having excellent surface appearance and excellent heat insulation is usually 20 μm or more, preferably 30 to 100 μm, more preferably 40 to 80 μm. As described above, the composition for forming a heat insulating layer of the present invention is excellent in storage stability, and is suppressed in problems such as precipitation of specific components such as thermally expandable microcapsules. The thermally expandable microcapsules to be distributed are uniformly distributed throughout.
本発明に係る第2工程は、塗膜を加熱して、アルコール及び水を蒸発させるとともに、塗膜に含まれる熱膨張性マイクロカプセルを体積膨張させつつ皮膜化する工程である。
塗膜の加熱方法は、特に限定されず、塗膜を所定の加熱温度条件下に曝す方法、塗膜を常温から所定の加熱温度まで昇温する方法等とすることができる。尚、上記の所定の加熱温度及びその加熱時間は、皮膜形成用樹脂の種類、熱膨張性マイクロカプセルの膨張開始温度等により、適宜、選択される。塗膜の加熱温度は、通常、100℃以上、好ましくは120℃〜150℃である。また、塗膜の加熱時間は、通常、30〜180秒間、好ましくは45〜120秒間である。このような加熱処理により、熱膨張性マイクロカプセルを膨張させ、塗膜の厚さに対して、好ましくは4〜16倍、より好ましくは7〜14倍の厚さの膨張カプセル含有樹脂皮膜を得ることができる。この膨張カプセル含有樹脂皮膜の厚さは、好ましくは200〜1000μm、より好ましくは300〜800μmである。また、この膨張カプセル含有樹脂皮膜に含まれる膨張カプセルのサイズ(平均径)は、好ましくは30〜100μm、より好ましくは50〜80μmである。
The second step according to the present invention is a step of heating the coating film to evaporate alcohol and water and forming a film while thermally expanding the thermally expandable microcapsules contained in the coating film.
The method for heating the coating film is not particularly limited, and may be a method for exposing the coating film to a predetermined heating temperature condition, a method for heating the coating film from room temperature to a predetermined heating temperature, or the like. The predetermined heating temperature and the heating time are appropriately selected depending on the type of the film-forming resin, the expansion start temperature of the thermally expandable microcapsules, and the like. The heating temperature of a coating film is 100 degreeC or more normally, Preferably it is 120 to 150 degreeC. Moreover, the heating time of a coating film is 30 to 180 second normally, Preferably it is 45 to 120 second. By such heat treatment, the thermally expandable microcapsule is expanded, and an expanded capsule-containing resin film having a thickness of preferably 4 to 16 times, more preferably 7 to 14 times the thickness of the coating film is obtained. be able to. The thickness of the expanded capsule-containing resin film is preferably 200 to 1000 μm, more preferably 300 to 800 μm. The size (average diameter) of the expanded capsules contained in the expanded capsule-containing resin film is preferably 30 to 100 μm, more preferably 50 to 80 μm.
第2工程により、図1に示す構造を有する断熱材1を製造することができるが、目的、用途等により、第1工程及び第2工程を繰り返して、より厚い断熱層としてもよい。また、他の工程を備えることにより、多様な構造を有する断熱材とすることができる。例えば、図1に示す断熱材1の断熱層13の表面に、その少なくとも一部を被覆する層を形成させてなる複合材料(図示せず)等とすることができる。 Although the heat insulating material 1 having the structure shown in FIG. 1 can be manufactured by the second step, the thicker heat insulating layer may be formed by repeating the first step and the second step depending on the purpose and application. Moreover, it can be set as the heat insulating material which has various structures by providing another process. For example, a composite material (not shown) formed by forming a layer covering at least a part of the surface of the heat insulating layer 13 of the heat insulating material 1 shown in FIG.
以下、本発明を実施例によって具体的に説明するが、本発明の主旨を超えない限り、本発明は、かかる実施例に限定されるものではない。 Hereinafter, the present invention will be specifically described by way of examples. However, the present invention is not limited to these examples unless it exceeds the gist of the present invention.
1.断熱層形成用組成物の原料
実施例及び比較例で用いた原料は、以下の通りである。
1. The raw material of the composition for heat insulation layer formation The raw material used by the Example and the comparative example is as follows.
1−1.皮膜形成用樹脂
下記樹脂成分を含むアルコール水溶液、水分散液又は水溶液を用いた。
(1)ポリウレタン樹脂のアルコール水溶液(A1)
ガラス転移温度が−60℃であるポリウレタン樹脂35質量%、イソプロピルアルコール9質量%及び水56質量%を含む荒川化学社製ポリウレタン樹脂「ユリアーノ W321」(商品名)を用いた。
(2)ポリウレタン樹脂の水分散液(A2)
ガラス転移温度が−38℃であるポリウレタン樹脂50質量%及び水50質量%を含む第一工業製薬社製非反応型ポリウレタン樹脂「スーパーフレックス E2000」(商品名)を用いた。
(3)アクリル樹脂の水溶液(A3)
ガラス転移温度が21℃であるアクリル樹脂40質量%を含む水溶液を用いた。
1-1. Film forming resin An alcohol aqueous solution, aqueous dispersion or aqueous solution containing the following resin components was used.
(1) Alcohol aqueous solution of polyurethane resin (A1)
A polyurethane resin “Yuriano W321” (trade name) manufactured by Arakawa Chemical Co., which contains 35% by mass of a polyurethane resin having a glass transition temperature of −60 ° C., 9% by mass of isopropyl alcohol and 56% by mass of water was used.
(2) Aqueous dispersion of polyurethane resin (A2)
A non-reactive polyurethane resin “Superflex E2000” (trade name) manufactured by Daiichi Kogyo Seiyaku Co., Ltd. containing 50% by mass of a polyurethane resin having a glass transition temperature of −38 ° C. and 50% by mass of water was used.
(3) Acrylic resin aqueous solution (A3)
An aqueous solution containing 40% by mass of an acrylic resin having a glass transition temperature of 21 ° C. was used.
1−2.熱膨張性マイクロカプセル
アクリロニトリル・メタクリレート共重合体からなる外殻の内部にイソブタンを含む、膨張開始温度が90℃であり、粒子径が3〜30μm(平均径10μm)である熱膨張性マイクロカプセルを用いた。
1−3.消泡剤
シリコーン化合物を用いた。
1-2. Thermally expandable microcapsule A thermally expandable microcapsule containing isobutane inside an outer shell made of acrylonitrile / methacrylate copolymer, having an expansion start temperature of 90 ° C. and a particle diameter of 3 to 30 μm (average diameter of 10 μm) Using.
1-3. Antifoaming agent A silicone compound was used.
2.断熱層形成用組成物の製造及び評価
表1に従って、断熱層形成用組成物を製造した。そして、断熱層形成用組成物及び基紙を用いて、断熱紙を製造した。
2. Manufacture and evaluation of the composition for heat insulation layer formation According to Table 1, the composition for heat insulation layer formation was manufactured. And the heat insulation paper was manufactured using the composition for heat insulation layer formation, and a base paper.
実施例1
78質量部のポリウレタン樹脂のアルコール水溶液(A1)と、12質量部の熱膨張性マイクロカプセルと、0.05質量部の消泡剤と、10質量部の20%イソプロピルアルコール水溶液とを混合して、断熱層形成用組成物(S1)を得た。この組成物を25℃で24時間静置し、保存安定性を評価した。分離、沈降若しくは増粘のないもの、あるいは、分離又は沈降があるが、攪拌すれば良好な分散状態となるものを「○」、分離若しくは沈降があり、撹拌しても元に戻らないもの、又は、増粘若しくはゲル化するものを「×」とした。
次に、厚さ275μmの基紙に、バーコート法により、組成物を塗布(塗膜の厚さ:50μm)し、大気中140℃で60〜90秒間加熱し、塗膜を乾燥させるとともに、熱膨張性マイクロカプセルを膨張させ、厚さ445〜505μmの皮膜(断熱層)を有する断熱紙を得た(図2参照)。得られた皮膜は、基紙に対して、密着性に優れていた。
その後、電子顕微鏡により、この断熱紙の表面観察を行い、皮膜が、n=10として算出された平均径が65μmである膨張カプセルを含むこと、及び、良好な発泡状態を有することを確認した(図3参照)。そして、断熱性を評価するため、図4に示す内容積200mLのポリプロピレン樹脂製カップ(市販品)30の側面全体に、上記断熱紙20の断熱層23側の面を貼り合わせて加熱飲料用の保温カップ50を作製した(図5参照)。次いで、この保温カップ50に熱湯(93℃)を注ぎ、上記内容積の約90%に相当する量(約180mL)となった瞬間の基紙21側の面の温度を、放射温度計により測定したところ、71.7℃であった。尚、断熱紙20を貼り合わせずにポリプロピレン樹脂製カップ30に熱湯(93℃)を注ぎ、側面の温度を測定した場合、89.7℃であった。
Example 1
An alcohol aqueous solution (A1) of 78 parts by mass of polyurethane resin, 12 parts by mass of thermally expandable microcapsules, 0.05 parts by mass of an antifoaming agent, and 10 parts by mass of 20% isopropyl alcohol aqueous solution were mixed. The composition for heat insulation layer formation (S1) was obtained. This composition was allowed to stand at 25 ° C. for 24 hours, and the storage stability was evaluated. There is no separation, sedimentation or thickening, or there is separation or sedimentation, but if it is stirred, it becomes a good dispersion state `` ○ '', there is separation or sedimentation, and it does not return to the original state even when stirring, Or the thing which thickens or gelatinizes was made into "x".
Next, the composition is applied to a base paper having a thickness of 275 μm by a bar coating method (the thickness of the coating film: 50 μm), heated in the atmosphere at 140 ° C. for 60 to 90 seconds, and the coating film is dried. The thermally expandable microcapsule was expanded to obtain a heat insulating paper having a film (heat insulating layer) having a thickness of 445 to 505 μm (see FIG. 2). The obtained film was excellent in adhesion to the base paper.
Thereafter, the surface of the heat-insulating paper was observed with an electron microscope, and it was confirmed that the film contained expanded capsules having an average diameter calculated as n = 10 of 65 μm and had a good foamed state ( (See FIG. 3). And in order to evaluate heat insulation, the surface by the side of the heat insulation layer 23 of the said heat insulation paper 20 is bonded to the whole side surface of the polypropylene resin cup (commercially available product) 30 having an internal volume of 200 mL shown in FIG. A heat retaining cup 50 was produced (see FIG. 5). Next, hot water (93 ° C.) is poured into the heat retaining cup 50, and the temperature of the surface on the side of the base paper 21 at the moment when it reaches an amount corresponding to about 90% of the internal volume (about 180 mL) is measured with a radiation thermometer. As a result, it was 71.7 degreeC. In addition, when hot water (93 degreeC) was poured into the polypropylene resin cup 30 without sticking the heat insulating paper 20, and the temperature of the side surface was measured, it was 89.7 degreeC.
実施例2〜5並びに比較例1及び2
表1に記載の原料を混合して、断熱層形成用組成物(S2)〜(S7)を製造し、その後、実施例1と同様にして、断熱紙及び保温カップを得た。そして、各種評価を行った。その結果を表1に示す。
Examples 2-5 and Comparative Examples 1 and 2
The raw materials shown in Table 1 were mixed to produce the heat insulating layer forming compositions (S2) to (S7), and then heat insulating paper and a heat retaining cup were obtained in the same manner as in Example 1. Various evaluations were performed. The results are shown in Table 1.
表1から明らかなように、実施例1〜5の組成物は、保存安定性に優れる。また、十分な断熱効果を得ることができた。一方、比較例1及び2の組成物は、保存安定性に劣っていた。 As is apparent from Table 1, the compositions of Examples 1 to 5 are excellent in storage stability. Moreover, sufficient heat insulation effect was able to be acquired. On the other hand, the compositions of Comparative Examples 1 and 2 were inferior in storage stability.
尚、本発明においては、上記の具体的実施例に示すものに限られず、目的、用途に応じて、本発明の範囲内で種々変更した実施例とすることができる。 In addition, in this invention, it can restrict to what is shown to said specific Example, It can be set as the Example variously changed within the range of this invention according to the objective and the use.
本発明の断熱層形成用組成物によれば、基材の表面に、断熱性に優れた皮膜を容易に形成することができる。本発明の断熱層形成用組成物を用いて得られた複合材料からなる断熱材は、例えば、−40℃〜100℃の範囲の温度に対する断熱効果に優れるため、建築材料、電気製品(冷蔵庫、保温庫等)、食品(加熱された飲料又は食品を収容する容器等)、衣料、自動車等の分野で広く利用することができる。 According to the composition for forming a heat insulating layer of the present invention, a film excellent in heat insulating properties can be easily formed on the surface of a substrate. A heat insulating material made of a composite material obtained using the composition for forming a heat insulating layer of the present invention is excellent in a heat insulating effect with respect to a temperature in the range of −40 ° C. to 100 ° C., for example. It can be widely used in fields such as a heat insulation box, food (a heated beverage or a container for containing food), clothing, automobiles, and the like.
1:断熱材、11:基材、13:断熱層、20:断熱紙、21:基紙、23:断熱層、30:樹脂製カップ、31:樹脂容器部、50:保温カップ 1: heat insulating material, 11: base material, 13: heat insulating layer, 20: heat insulating paper, 21: base paper, 23: heat insulating layer, 30: resin cup, 31: resin container part, 50: heat retaining cup
Claims (5)
請求項1乃至4のいずれか一項に記載の断熱層形成用組成物を、基材の表面に塗布する工程と、得られた塗膜を加熱して、アルコール及び水を蒸発させるとともに、該塗膜に含まれる熱膨張性マイクロカプセルを膨張させつつ皮膜化する工程とを、順次、備えることを特徴とする断熱材の製造方法。 A method of manufacturing a heat insulating material,
A step of applying the heat insulating layer forming composition according to any one of claims 1 to 4 to the surface of the substrate, heating the obtained coating film to evaporate alcohol and water, A method for producing a heat insulating material, comprising sequentially forming a film while expanding the thermally expandable microcapsules contained in the coating film.
Priority Applications (1)
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JP2017002152A JP6861409B2 (en) | 2017-01-10 | 2017-01-10 | A composition for forming a heat insulating layer used for forming a heat insulating layer of a container containing a heated beverage or food, and a method for producing a heat insulating layer of a container containing a heated beverage or food. |
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JP2020083407A (en) * | 2018-11-29 | 2020-06-04 | 東京インキ株式会社 | Microwave foam laminate, microwave foam package and manufacturing method of microwave foam package |
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JPS6239674A (en) * | 1985-08-12 | 1987-02-20 | Shikoku Kaken Kogyo Co Ltd | Method of forming heat insulating pattern coating compound composition and heat insulating pattern film of coating |
JP2002256251A (en) * | 2001-02-27 | 2002-09-11 | Dainichiseika Color & Chem Mfg Co Ltd | Composition comprising microcapsuled foaming agent and coating material |
JP2004345267A (en) * | 2003-05-23 | 2004-12-09 | Dainippon Printing Co Ltd | Thermal transfer image receiving sheet and its manufacturing method |
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JP2020083407A (en) * | 2018-11-29 | 2020-06-04 | 東京インキ株式会社 | Microwave foam laminate, microwave foam package and manufacturing method of microwave foam package |
JP7210244B2 (en) | 2018-11-29 | 2023-01-23 | 東京インキ株式会社 | MICROWAVE FOAM LAMINATE, MICROWAVE FOAM PACKAGE, AND METHOD FOR MANUFACTURING MICROWAVE FOAM PACKAGE |
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