JP2006187928A - Manufacturing method of foamed polyvinyl chloride wallpaper - Google Patents
Manufacturing method of foamed polyvinyl chloride wallpaper Download PDFInfo
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本発明は、意匠性、難燃性が改善された安価な発泡ポリ塩化ビニルを表層とする壁紙に関する。ここで、壁紙とは、建物の内装の化粧材として壁や天井に使われる化粧材のことである。 The present invention relates to a wallpaper whose surface layer is inexpensive foamed polyvinyl chloride with improved design and flame retardancy. Here, the wallpaper is a decorative material used for a wall or a ceiling as a decorative material for the interior of a building.
元来、ポリ塩化ビニルは物性に優れ、成形加工性がよく、可塑剤の添加により柔軟となり、発泡性がよく、且つ安価である等の理由で多くの分野で使用されており、特に壁装材においては、発泡ポリ塩化ビニルを表層として、紙を基層とする発泡ポリ塩化ビニル壁紙が広く使われている。そして、乳化重合ポリ塩化ビニル、いわゆるペーストレジンをコーターで紙にコーティングした壁紙、また、懸濁重合ポリ塩化ビニル、いわゆるストレートレジンをカレンダーで紙に積層した壁紙はどちらも広く知られている。また、多層のポリ塩化ビニルを用いる壁紙も知られている。紙表面に軟質ポリ塩化ビニルをカレンダー法で積層した積層物の上に、軟質ポリ塩化ビニルフィルムを積層し、下層のみ発泡させたもの(特許文献1)や、二層ともコーティング法により形成させた発泡軟質ポリ塩化ビニル壁紙(特許文献2)など提案されている。
近年、難燃性のレベルの高い壁紙が求められているが、発泡ポリ塩化ビニル壁紙の難燃性は、単位面積あたりの樹脂量に強い相関があり、樹脂量が多いほど難燃性が低下する。そして、難燃性を向上させるべく、単位面積当たりの樹脂量を少なくすると、発泡樹脂層の厚みが薄くなり、エンボス付与性などの意匠性が悪くなる。そのため、意匠性との兼ね合いで単位面積当たりの樹脂量の減少による難燃性の向上には限界がある。また、樹脂に発泡剤及び/又は無機質充填材を多量に配合することにより、単位面積当たり樹脂量を増やすことなく発泡樹脂層を厚くしてエンボス付与性を改善することができるが、この手段を採用すると、発泡剤及び/又は無機質充填材の多量配合によって、発泡後の製品の表面に面荒れが起こり、外観が悪くなる。
本発明は、意匠性と難燃性が高いレベルでバランスし、外観が良い発泡ポリ塩化ビニル壁紙を安価に製造する方法を提供することを目的とする。
In recent years, wallpaper with a high level of flame retardancy has been demanded, but the flame retardancy of expanded polyvinyl chloride wallpaper has a strong correlation with the amount of resin per unit area, and the flame retardance decreases as the amount of resin increases. To do. If the amount of resin per unit area is decreased to improve the flame retardancy, the thickness of the foamed resin layer is reduced, and the design properties such as embossability are deteriorated. Therefore, there is a limit to improvement in flame retardancy due to a decrease in the amount of resin per unit area in consideration of design properties. Further, by adding a large amount of a foaming agent and / or inorganic filler to the resin, the embossing property can be improved by increasing the thickness of the foamed resin layer without increasing the amount of resin per unit area. If it is adopted, the surface of the product after foaming is roughened due to a large amount of the foaming agent and / or inorganic filler, and the appearance is deteriorated.
An object of the present invention is to provide a method for producing a low-cost foamed polyvinyl chloride wallpaper that balances design and flame retardancy at a high level and has a good appearance.
すなわち、本発明は、(1)紙の表面に、懸濁重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物を、カレンダー法によって厚さ0.08〜0.16mmに積層して下層を形成させ、(2)この下層の表面に、乳化重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物を、コーティング法により厚さ0.02〜0.06mmに塗布して表面層を形成させ、(3)その後加熱発泡させることを特徴とする発泡ポリ塩化ビニル壁紙の製造方法である。上記の乳化重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物が、更に、ポリ塩化ビニル100質量部に対して10〜50質量部の炭酸カルシウムと5〜30質量部の二酸化チタンを含むのが好ましい。 That is, the present invention is as follows: (1) A composition comprising a suspension-polymerized polyvinyl chloride as a main component and a foaming agent is laminated on the surface of paper to a thickness of 0.08 to 0.16 mm by a calendering method. (2) A surface layer is formed on the surface of the lower layer by applying a composition mainly composed of emulsion-polymerized polyvinyl chloride and a foaming agent to a thickness of 0.02 to 0.06 mm by a coating method. (3) A method for producing a foamed polyvinyl chloride wallpaper, which is then heated and foamed. The composition mainly composed of the above-mentioned emulsion-polymerized polyvinyl chloride and containing a foaming agent further contains 10 to 50 parts by mass of calcium carbonate and 5 to 30 parts by mass of titanium dioxide with respect to 100 parts by mass of polyvinyl chloride. Is preferred.
本願発明によると、難燃性が良く、意匠性に優れた、外観が良い安価な発泡ポリ塩化ビニル壁紙を製造することができる。すなわち、紙表面に発泡ポリ塩化ビニル層を設けた壁紙について、発泡ポリ塩化ビニル層を多層にし、下層を懸濁重合ポリ塩化ビニルを用いてカレンダー法によって形成させたので、均一な厚みの層を安定性良く安価に形成できる。また、下層の上に表面層を設け、この表面層を乳化重合ポリ塩化ビニルを用いてコーティング法によって形成させたので、加熱発泡時に発泡倍率を大きくしても表面の面荒れを起こすことがなく、外観の良い壁紙が得られる。また発泡倍率を大きくすることが可能なために、未発泡時の表層の層厚を薄くしても良好にエンボス模様を現出できる。そして、未発泡時の下層の厚さを0.08〜0.16mm、未発泡時の表面層の厚さを0.02〜0.06mmにして、壁紙の面積当たりのポリ塩化ビニル量を少なくしたので、難燃性も維持できる。 According to the present invention, an inexpensive expanded polyvinyl chloride wallpaper having good flame retardancy, excellent design, and good appearance can be produced. That is, for wallpaper with a foamed polyvinyl chloride layer on the paper surface, the foamed polyvinyl chloride layer was made into a multilayer and the lower layer was formed by the calendar method using suspension-polymerized polyvinyl chloride. It can be formed stably and inexpensively. In addition, since a surface layer is provided on the lower layer and this surface layer is formed by a coating method using emulsion-polymerized polyvinyl chloride, the surface is not roughened even if the expansion ratio is increased during foaming by heating. , Wallpaper with good appearance can be obtained. Further, since the expansion ratio can be increased, an embossed pattern can be satisfactorily displayed even if the surface layer thickness when not foamed is reduced. Then, the thickness of the lower layer when not foamed is 0.08 to 0.16 mm, the thickness of the surface layer when not foamed is 0.02 to 0.06 mm, and the amount of polyvinyl chloride per area of the wallpaper is reduced. Therefore, flame retardancy can also be maintained.
本発明の製造法は、先ず、紙の表面に、懸濁重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物を、カレンダー法によって厚さ0.08〜0.16mmに積層して下層を形成させる。発泡剤及び/又は無機質充填材を配合したポリ塩化ビニルをカレンダー法で紙に積層する場合、積層加工が不安定になり、厚みむらが大きくなるため、樹脂層の厚みを0.08mm未満にするのは困難である。また、0.08mm未満ではエンボスによるエンボス付与を十分に行うことが困難である。また0.16mmを超えると、全体の厚みが厚くなり、難燃性が悪化する。この理由で特に好ましくは0.10mm〜0.14mmである。下層は2層以上にしてもよいが、発泡剤及び/又は無機質充填材を少量配合した場合でも、厚み0.06mm以下では同様に厚みむらが大きくなり、またカレンダー法による積層加工が不安定になるため、カレンダー法によってポリ塩化ビニル層を2層形成するのは、樹脂層が厚くなり満足できる難燃性は得られ難い。カレンダー法によるポリ塩化ビニルの紙への積層は公知の方法で行う。 In the production method of the present invention, first, a composition comprising a suspension-polymerized polyvinyl chloride as a main component and a foaming agent is laminated on a surface of paper to a thickness of 0.08 to 0.16 mm by a calender method, and a lower layer is formed. Let it form. When laminating polyvinyl chloride containing a foaming agent and / or inorganic filler on paper by the calender method, the laminating process becomes unstable and the thickness unevenness increases, so the thickness of the resin layer is made less than 0.08 mm. It is difficult. Moreover, if it is less than 0.08 mm, it is difficult to sufficiently provide embossing by embossing. Moreover, when it exceeds 0.16 mm, the whole thickness will become thick and a flame retardance will deteriorate. For this reason, the thickness is particularly preferably 0.10 mm to 0.14 mm. Although the lower layer may be two or more layers, even when a small amount of a foaming agent and / or an inorganic filler is blended, the thickness unevenness similarly increases at a thickness of 0.06 mm or less, and the laminating process by the calendar method is unstable. Therefore, forming the two polyvinyl chloride layers by the calendar method makes it difficult to obtain satisfactory flame retardancy because the resin layer becomes thick. Lamination of polyvinyl chloride on paper by the calendar method is performed by a known method.
本発明の製造方法では、上記した下層の表面に、乳化重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物を、コーティング法により厚さ0.02〜0.06mmに塗布して表面層を形成させる。乳化重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物をコーティング法で形成した層は、加熱発泡による面荒れが少ない。コーティング法によると、0.02mm程度までの薄い層の形成が可能であるが、0.02mm未満では上層に生じる厚みむらが目に付き易くなる。コーティング法で形成した層が0.06mmを超えると、全体の樹脂層の厚みが厚くなり、難燃性が悪化する。上記のコーティング法による表面層の形成はコーターによるなど公知のコーティング法で行う。また、所望によりマーブルプリント、艶調整表面処理、汚れ防止表面処理等を行う。 In the production method of the present invention, the surface layer is coated by applying a composition mainly composed of emulsion-polymerized polyvinyl chloride and a foaming agent to the surface of the lower layer described above to a thickness of 0.02 to 0.06 mm by a coating method. Let it form. A layer formed by a coating method using a composition mainly composed of emulsion-polymerized polyvinyl chloride and blended with a foaming agent has little surface roughness due to heat foaming. According to the coating method, it is possible to form a thin layer up to about 0.02 mm. However, if the thickness is less than 0.02 mm, the thickness unevenness generated in the upper layer is easily noticeable. When the layer formed by the coating method exceeds 0.06 mm, the thickness of the entire resin layer is increased, and the flame retardancy is deteriorated. Formation of the surface layer by the above coating method is performed by a known coating method such as by a coater. Further, marble printing, gloss adjustment surface treatment, antifouling surface treatment, and the like are performed as desired.
紙表面に上層及び表面層を形成させた後、発泡炉、ヒーター又は加温ロールで加熱して下層及び表面層の中の発泡剤を分解させ、下層及び表面層を発泡させる。そして、必要に応じてエンボスロールでエンボス加工し、所定長さに巻き取って壁紙製品となす。紙表面に発泡性ポリ塩化ビニル層を一層設けただけの壁紙材料を加熱発泡加工する場合には、発泡は外部から加熱して行なうため、ポリ塩化ビニル層の上部は過発泡で面荒れを起こしやすく、かつ発泡性ポリ塩化ビニル層の下部は発泡不足で本来期待される発泡倍率になっていない傾向がある。本発明方法では、紙の表面に、懸濁重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物で下層を形成し、その表面に乳化重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物で表面層を形成させたので、この恐れが少ない。 After the upper layer and the surface layer are formed on the paper surface, the lower layer and the surface layer are foamed by heating with a foaming furnace, a heater or a heating roll to decompose the foaming agent in the lower layer and the surface layer. And it embosses with an embossing roll as needed, winds up to predetermined length, and makes it a wallpaper product. When heating and foaming a wallpaper material that has only one foamable polyvinyl chloride layer on the paper surface, foaming is performed from the outside, so the top of the polyvinyl chloride layer is overfoamed and roughened. The lower part of the foamable polyvinyl chloride layer tends to be insufficient in foaming and does not have an expected expansion ratio. In the method of the present invention, a lower layer is formed on the surface of paper with a composition mainly composed of suspension-polymerized polyvinyl chloride and a foaming agent, and a composition mainly composed of emulsion-polymerized polyvinyl chloride and a foaming agent. Since the surface layer was formed by this, this fear is small.
本発明の壁紙の製造に用いる紙は、通常の壁紙の基材に使用する紙が用いられる。また本発明で用いるポリ塩化ビニルは、発泡性を重視するため、平均重合度が700〜1000程度のポリ塩化ビニルが用いられる。本発明では、下層に懸濁重合ポリ塩化ビニルを用い、表面層に乳化重合ポリ塩化ビニルを用いるが、これらはともに平均重合度700〜1000程度のものである。ポリ塩化ビニルとしては、塩化ビニル単独重合体、塩化ビニルと酢酸ビニルとの共重合体、ポリ塩化ビニルに他のポリマーをブレンド等したものが用いられる。 The paper used for the production of the wallpaper of the present invention is the paper used for the base material of ordinary wallpaper. Moreover, since the polyvinyl chloride used by this invention attaches importance to foamability, polyvinyl chloride with an average degree of polymerization of about 700-1000 is used. In the present invention, suspension-polymerized polyvinyl chloride is used for the lower layer, and emulsion-polymerized polyvinyl chloride is used for the surface layer, both of which have an average degree of polymerization of about 700 to 1000. As the polyvinyl chloride, a vinyl chloride homopolymer, a copolymer of vinyl chloride and vinyl acetate, a blend of polyvinyl chloride with another polymer, or the like is used.
本発明は、下層の形成には、懸濁重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物を用いる。また、表面層の形成には、乳化重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物を用いる。これらの発泡剤として熱分解型のアゾジカルボンアミド、4,4’−オキシビス(ベンゼンスルホニルヒドラジド)等が挙げられる。また、下層を形成する組成物には、懸濁重合ポリ塩化ビニル100質量部に対し0.5〜7質量部配合する。また、表面層を形成する組成物には、乳化重合ポリ塩化ビニル100質量部に対し0.5〜7質量部配合する。 In the present invention, a composition comprising a suspension-polymerized polyvinyl chloride as a main component and a foaming agent is used for forming the lower layer. For the formation of the surface layer, a composition mainly composed of emulsion-polymerized polyvinyl chloride and blended with a foaming agent is used. Examples of these foaming agents include pyrolytic azodicarbonamide, 4,4'-oxybis (benzenesulfonylhydrazide), and the like. Moreover, 0.5-7 mass parts is mix | blended with the composition which forms a lower layer with respect to 100 mass parts of suspension polymerization polyvinyl chloride. Moreover, 0.5-7 mass parts is mix | blended with the composition which forms a surface layer with respect to 100 mass parts of emulsion polymerization polyvinyl chloride.
下層を形成する組成物及び表面層を形成する組成物には、上記した発泡剤の他に可塑剤、安定剤、充填剤などを配合する。可塑剤としては、ジ−イソノニルフタレート、ジオクチルフタレートなどが挙げられる。高沸点の可塑剤は室内空気への揮散がほとんどないので、ジ−イソノニルフタレートが好ましく用いられる。配合量はポリ塩化ビニル100質量部に対して45〜80質量部である。また、ポリ塩化ビニル安定剤としてはBa−Zn系の金属石鹸、エポキシ化合物、亜リン酸トリエステル、β−ジケトン、ハイドロタルサイト、ゼオライト、多価アルコール等が挙げられる。Ba−Zn系の金属石鹸が、カレンダー加工用滑剤としての性能を持ち好ましい。 In addition to the above-mentioned foaming agent, a plasticizer, a stabilizer, a filler and the like are blended in the composition forming the lower layer and the composition forming the surface layer. Examples of the plasticizer include di-isononyl phthalate and dioctyl phthalate. Di-isononyl phthalate is preferably used because the high-boiling plasticizer has little volatilization into room air. A compounding quantity is 45-80 mass parts with respect to 100 mass parts of polyvinyl chloride. Examples of the polyvinyl chloride stabilizer include Ba-Zn metal soaps, epoxy compounds, phosphite triesters, β-diketones, hydrotalcites, zeolites, polyhydric alcohols, and the like. Ba-Zn-based metal soap is preferable because it has a performance as a lubricant for calendering.
充填剤としては、炭酸カルシウムと二酸化チタンの組合せが、充填剤と体質顔料の組む合わせとして好ましい。本発明では、発泡ポリ塩化ビニル層として下層と表面層とを設けるが、表面層のみ所定の色にし、下層は同一色にして連続生産すると生産効率が向上する。しかし、この方法を実施するには、表面層の隠蔽性が高いことが必要条件となる。そこで、本発明では表面層を形成する組成物に、隠蔽性は低いが安価でボリュームアップによるエンボス付与効果(意匠性向上効果)のある炭酸カルシウムと隠蔽性の高い二酸化チタンとを特定の範囲で添加する。これによって、下層を同一色にして連続生産することができる。表面層は、乳化重合ポリ塩化ビニル100質量部に対して10〜50質量部の炭酸カルシウムと5〜30質量部の二酸化チタンを含むのが好ましく、炭酸カルシウム10質量部未満では、ボリュームアップによる意匠性向上効果が不足し、50質量部を超えると面荒れが悪化する。二酸化チタン5質量部未満では隠蔽性が不足し、30質量部を超えると面荒れが悪化する。なお、下層の懸濁重合ポリ塩化ビニルには、ポリ塩化ビニル100質量部に対して無機充填剤(例えば、炭酸カルシウムと二酸化チタンの混合物)を60〜150質量部、なかんずく70〜120重量部配合するのが好ましい。 As the filler, a combination of calcium carbonate and titanium dioxide is preferable as a combination of the filler and extender. In the present invention, the lower layer and the surface layer are provided as the foamed polyvinyl chloride layer. However, if the surface layer is given a predetermined color and the lower layer is the same color, the production efficiency is improved. However, in order to carry out this method, it is a necessary condition that the surface layer has high concealability. Therefore, in the present invention, the composition for forming the surface layer includes calcium carbonate having a low concealing property but cheap and having an embossing effect (design improvement effect) by increasing the volume and titanium dioxide having a high concealing property within a specific range. Added. Thereby, the lower layer can be continuously produced with the same color. The surface layer preferably contains 10 to 50 parts by mass of calcium carbonate and 5 to 30 parts by mass of titanium dioxide with respect to 100 parts by mass of the emulsion-polymerized polyvinyl chloride. When the effect of improving the properties is insufficient and the amount exceeds 50 parts by mass, the surface roughness deteriorates. When the amount is less than 5 parts by mass of titanium dioxide, the concealability is insufficient, and when it exceeds 30 parts by mass, surface roughness is deteriorated. The lower layer suspension-polymerized polyvinyl chloride contains 60 to 150 parts by weight of inorganic filler (for example, a mixture of calcium carbonate and titanium dioxide) with respect to 100 parts by weight of polyvinyl chloride, especially 70 to 120 parts by weight. It is preferable to do this.
難燃剤は、特に必要としない。これは壁紙に要求される難燃性(ISO5660規定のコーンカロリーメーターによる)は、強制燃焼時の発熱量が問題とされるため、酸素遮断などで燃焼を遅らせるタイプの難燃剤(ハロゲン系、リン酸エステル系、アンチモン系の難燃剤)は配合する意味がないからである。吸熱型の難燃剤(水酸化マグネシウム、水酸化アルミニウムなど)は理論的には有効であるが、期待するほど効果は大きくない。 A flame retardant is not particularly required. This is because the flame retardancy required by wallpaper (using a cone calorimeter specified by ISO 5660) is a problem of the calorific value during forced combustion, so a flame retardant of a type that delays combustion by blocking oxygen (halogen, phosphorous, etc.) This is because there is no meaning to add an acid ester-based or antimony-based flame retardant. Endothermic flame retardants (magnesium hydroxide, aluminum hydroxide, etc.) are theoretically effective, but not as effective as expected.
本発明においては、上記のそれぞれの組成物に、更に添加剤を配合してもよい。抗菌及び防カビ剤として、シリカゲル銀、銀ゼオライト、りん酸ジルコニウム銀塩、リン酸カルシウム銀塩などの銀系、10,10’−オキシビスフェノキシアルシン、8−オキシキノリン銅、2−(4−チアゾリル)−ベンツイミダゾール、2−ベンツイミダゾールカルバミック酸メチール、2−n−オクチル−4−イソチアゾリル−3−オン、ビス(ピリジン−2−チオール−1−オキシド)亜鉛塩、2−ペリジチオール−1−オキサイドナトリウム塩、N,N’,N”−トリスヒドロキシエチルヘキサヒドロ−S−トリアジン等を配合してもよい。その他、必要に応じて、発泡セル調整剤、顔料、帯電防止剤、紫外線吸収剤、消臭剤、防カビ剤、抗菌剤、防虫剤等の薬剤を添加することができる。また、顔料、帯電防止剤、紫外線吸収剤、消臭剤、防カビ剤、抗菌剤、防虫剤等は、表面において効果を発揮するものであるので、表面層を形成する組成物のみへの添加でもよい。この表面層を形成する組成物のみへの添加により、コストを下げることができる。 In this invention, you may mix | blend an additive with said each composition further. As antibacterial and antifungal agents, silver-based 10,10'-oxybisphenoxyarsine, 8-oxyquinoline copper, 2- (4-thiazolyl) such as silica gel silver, silver zeolite, zirconium phosphate silver salt, calcium phosphate silver salt -Benzimidazole, methyl 2-benzimidazolecarbamic acid, 2-n-octyl-4-isothiazolyl-3-one, bis (pyridine-2-thiol-1-oxide) zinc salt, 2-peridithiol-1-oxide Sodium salt, N, N ′, N ″ -trishydroxyethylhexahydro-S-triazine, etc. may be blended. In addition, if necessary, foamed cell conditioner, pigment, antistatic agent, ultraviolet absorber, Agents such as deodorants, fungicides, antibacterial agents, insect repellents can be added, pigments, antistatic agents, UV absorption Deodorants, fungicides, antibacterial agents, insect repellents, etc. are effective on the surface, and may be added only to the composition forming the surface layer. The cost can be reduced by adding only to the above.
実施例1〜5、比較例1〜3
表1は、紙の表面に設ける下層の組成物、及び下層の表面に設ける表面層の組成物の各組成を示した表である。表2は、これらの組成物を用いて製造した壁紙並びにそれらの難燃性レベル、エンボス可能厚さ及び面荒れの評価を示した表である。Aは下層を形成するための組成物、B−1、B−2及びB−3は表面層を形成するための組成物である。
Examples 1-5, Comparative Examples 1-3
Table 1 is a table showing the compositions of the lower layer composition provided on the paper surface and the surface layer composition provided on the lower layer surface. Table 2 is a table showing the wallpaper manufactured using these compositions and the evaluation of their flame retardancy level, embossable thickness and surface roughness. A is a composition for forming a lower layer, and B-1, B-2 and B-3 are compositions for forming a surface layer.
壁紙の製造は次のようにして行った。
(1)紙の表面に下層を形成する工程
可塑剤50質量部に、安定剤2質量部及びアクリル系セル調整剤1質量部を添加し、良く攪拌して混合パックを作成し、これに懸濁重合ポリ塩化ビニル100質量部、発泡剤6質量部及び炭酸カルシウム70質量部を添加し、混合、混練して組成物Aを調製した。この混練物を、ロール温度160℃の4本カレンダーを用い表2に示した厚みにカレンダー成形し、秤量65g/m2の壁紙用普通紙に積層して下層を形成した。
(2)下層の表面に表面層を形成する工程
表1に示す所定量の可塑剤に、所定量の安定剤及びアクリル系セル調整剤を添加し、良く攪拌して混合パックを作成し、これに乳化重合ポリ塩化ビニル、発泡剤、炭酸カルシウム及び二酸化チタンを添加、混合して組成物B−1、組成物B−2及び組成物B−3を調製した。これらの組成物を、それぞれの下層の表面に、コーターで表2に示した厚さでコーティングし表面層を形成し、更に艶調整表面処理を施した。
(3)加熱発泡工程
上記で得た積層物を、200℃の発泡炉に入れて発泡させ、次いで、エンボスローラーでエンボスギャップを変えながらエンボスをして壁紙を製造した。
The wallpaper was manufactured as follows.
(1) Step of forming a lower layer on the surface of paper Add 50 parts by mass of a plasticizer with 2 parts by mass of a stabilizer and 1 part by mass of an acrylic cell regulator, and stir well to create a mixed pack. A composition A was prepared by adding 100 parts by mass of turbid polymerized polyvinyl chloride, 6 parts by mass of a foaming agent, and 70 parts by mass of calcium carbonate, mixing and kneading. This kneaded product was calendered to a thickness shown in Table 2 using a four calender roll having a roll temperature of 160 ° C., and laminated on plain paper for wallpaper having a weight of 65 g / m 2 to form a lower layer.
(2) Step of forming a surface layer on the surface of the lower layer To a predetermined amount of plasticizer shown in Table 1, a predetermined amount of stabilizer and acrylic cell conditioner are added, and stirred well to create a mixed pack. Emulsion-polymerized polyvinyl chloride, a foaming agent, calcium carbonate and titanium dioxide were added to and mixed to prepare Composition B-1, Composition B-2 and Composition B-3. These compositions were coated on the surface of each lower layer with a coater at the thickness shown in Table 2 to form a surface layer, and further subjected to gloss adjustment surface treatment.
(3) Heating and foaming process The laminate obtained above was put into a 200 ° C. foaming furnace and foamed, and then embossed with an embossing roller while changing the embossing gap to produce wallpaper.
表1において、乳化重合ポリ塩化ビニルは、PSL−675(鐘淵化学工業社製、平均重合度750)を用いた。懸濁重合ポリ塩化ビニルは、TK−800(信越化学工業社製、平均重合度800)を用いた。可塑剤はジ−イソノニルフタレートを用いた。安定剤はバリウムステアレート及びジンクステアレートの1:1の混合物を用いた。発泡剤はアゾジカルボンアミドと4,4’−オキシビスベンゼンスルホニルヒドラジンとの1:1の混合物を用いた。発泡セル調整剤はアクリル系セル調整剤(昭島化学工業社製300J)を用いた。炭酸カルシウムは日東粉化工業社製NS#100、二酸化チタンは日本ピグメント社製NVS−985(二酸化チタン75質量%)を用いた。 In Table 1, PSL-675 (manufactured by Kaneka Chemical Co., Ltd., average polymerization degree 750) was used as the emulsion polymerization polyvinyl chloride. As suspension polymerization polyvinyl chloride, TK-800 (manufactured by Shin-Etsu Chemical Co., Ltd., average polymerization degree 800) was used. Di-isononyl phthalate was used as the plasticizer. The stabilizer used was a 1: 1 mixture of barium stearate and zinc stearate. As the blowing agent, a 1: 1 mixture of azodicarbonamide and 4,4'-oxybisbenzenesulfonylhydrazine was used. As the foam cell regulator, an acrylic cell regulator (300J manufactured by Akishima Chemical Co., Ltd.) was used. NS # 100 manufactured by Nitto Flour Chemical Co., Ltd. was used as calcium carbonate, and NVS-985 (75% by mass of titanium dioxide) manufactured by Nippon Pigment was used as titanium dioxide.
表2に示す難燃性レベル、エンボス可能厚さ及び面荒れの評価は下記の方法にしたがった。
・難燃性レベルは、可燃物の単位面積当たり重量に拠った。可燃物質量(g/m2)で○は161.18未満を、△は161.18以上で263.15未満を、×は263.15以上を示す。×レベルでは、概ねISO5660規定のコーンカロリーメーター試験で発熱量8J以上となり、難燃壁紙の要件を満たさない。
・エンボス可能厚さは、エンボスロールの一番深い谷が、樹脂層に安定して接触する樹脂層の最大厚さを示す。○は1.2mm超で、高意匠性があることを示す。△は0.4mm以上1.2mm未満で、通常の意匠性レベルにあることを示す。×は0.4mm未満で、意匠性が貧弱なことを示す。
・面荒れは、エンボス可能厚さとなった部分での表面状態を目視にて評価した。○は良好、△はやや面荒れあり、×は面荒れがはっきり出ていることを示す。
The evaluation of flame retardancy level, embossable thickness and surface roughness shown in Table 2 was according to the following methods.
・ Flame retardance level was based on the weight per unit area of combustible material. In the amount of combustible material (g / m 2 ), ◯ indicates less than 161.18, Δ indicates 161.18 or more and less than 263.15, and x indicates 263.15 or more. In the x level, the calorific value of the cone calorimeter test defined by ISO 5660 is approximately 8 J or more, which does not satisfy the requirements for flame retardant wallpaper.
-Thickness which can be embossed shows the maximum thickness of the resin layer in which the deepest trough of an embossing roll contacts a resin layer stably. ○ is more than 1.2 mm, indicating that it has high design properties. Δ is 0.4 mm or more and less than 1.2 mm, indicating a normal design level. X is less than 0.4 mm, indicating that the design is poor.
-The surface roughness was evaluated by visual observation of the surface condition at the part where the embossable thickness was achieved. ○ is good, Δ is slightly rough, and x is clearly rough.
表2から分かるように、樹脂に炭酸カルシウム(無機充填材)を多量に配合した組成物Aのみの層を紙の表面に形成させ壁紙(比較例3)は、難燃性、エンボス性は良いが、面荒れが大きく、商品にならない。この組成物Aの層を下層とし、その表面に、乳化重合ポリ塩化ビニルを主体とし発泡剤を配合した組成物B−1,組成物B−2又は組成物B−3を0.02〜0.06mmに塗布して表面層を形成させ壁紙は、実施例1〜5にみるように難燃性、エンボス性に優れ、面荒れが少ない。ただ、炭酸カルシウムを多量に配合した組成物B−3を表面層にした実施例3は面荒れがやや多かった。また、下層及び表面層の目付を少くした実施例4はエンボス性がやや劣っていた。また、下層及び表面層の目付を多くした実施例5は難燃性がやや劣っていた。下層及び表面層の目付を更に多くすると、難燃性が著しく悪くなり、商品にならない(比較例1)。また、組成物B−2のみの層を紙の表面に形成させ壁紙(比較例2)は、エンボス性が良く、面荒れが少ないが、難燃性が著しく劣って商品にならない。 As can be seen from Table 2, the wallpaper (Comparative Example 3), in which a layer of only the composition A containing a large amount of calcium carbonate (inorganic filler) in the resin is formed on the surface of the paper, has good flame retardancy and embossability. However, the surface is so rough that it does not become a product. The composition A-1, the composition B-2 or the composition B-3, in which the layer of the composition A is a lower layer and the foaming agent is mainly composed of emulsion-polymerized polyvinyl chloride on the surface, is 0.02 to 0. The wallpaper is applied to a thickness of 0.06 mm to form a surface layer. As seen in Examples 1 to 5, the wallpaper has excellent flame retardancy and embossing properties, and has less surface roughness. However, Example 3 which used the composition B-3 which mix | blended calcium carbonate abundantly as the surface layer had a little surface roughness. Moreover, Example 4 which reduced the fabric weight of the lower layer and the surface layer was a little inferior in embossing property. Moreover, Example 5 which increased the fabric weight of a lower layer and a surface layer was a little inferior in flame retardance. When the basis weight of the lower layer and the surface layer is further increased, the flame retardancy is remarkably deteriorated and the product is not commercialized (Comparative Example 1). In addition, the wallpaper (Comparative Example 2) in which a layer of only the composition B-2 is formed on the paper surface has good embossing properties and little surface roughness, but the flame retardancy is extremely inferior and does not become a product.
Claims (2)
The composition mainly composed of emulsion-polymerized polyvinyl chloride and containing a foaming agent further contains 10 to 50 parts by mass of calcium carbonate and 5 to 30 parts by mass of titanium dioxide with respect to 100 parts by mass of polyvinyl chloride. The method for producing a foamed polyvinyl chloride wallpaper according to claim 1.
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JP2021070295A (en) * | 2019-11-01 | 2021-05-06 | 凸版印刷株式会社 | Decorative board |
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