JP2014162807A - Flame-retardant composition, flame-retarding method using the same, and flame-retardant material - Google Patents
Flame-retardant composition, flame-retarding method using the same, and flame-retardant material Download PDFInfo
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- JP2014162807A JP2014162807A JP2013032181A JP2013032181A JP2014162807A JP 2014162807 A JP2014162807 A JP 2014162807A JP 2013032181 A JP2013032181 A JP 2013032181A JP 2013032181 A JP2013032181 A JP 2013032181A JP 2014162807 A JP2014162807 A JP 2014162807A
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- flame retardant
- retardant composition
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- flame
- saccharide
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Abstract
Description
本発明は、ケイ素化合物および糖類を含有する難燃組成物、それを用いた難燃化処理方法およびそれにより得られた難燃材料に関する。本発明の難燃組成物は、木材、紙、織布、不織布、樹脂の難燃化に好適に用いられる。 The present invention relates to a flame retardant composition containing a silicon compound and a saccharide, a flame retardant treatment method using the same, and a flame retardant material obtained thereby. The flame-retardant composition of the present invention is suitably used for flame-retarding wood, paper, woven fabric, nonwoven fabric, and resin.
ケイ酸ナトリウム（ケイ酸ソーダ）の高濃度水溶液である水ガラスなどのケイ素化合物は古くから段ボールやベニヤ板などの防火剤（難燃剤）として用いられてきた。
具体的には、水ガラスは接着剤の機能も有することから、防火剤と接着材の機能を併用し、水ガラスを浸透させた紙や木材同士を貼り合せて段ボールやベニヤ板などが加工されてきた。
一方、基材の表面に水ガラスを塗布して難燃性を有する塗膜を形成しようとしても、溶質成分が無機質であるため、基材の表面で粉体化してしまい塗膜が形成されず、十分な難燃性能が得られない。このように水ガラス単独では塗膜剤にはならず、塗膜化するためのバインダーが求められていた。
Silicon compounds such as water glass, which is a high-concentration aqueous solution of sodium silicate (sodium silicate), have long been used as fireproofing agents (flame retardants) for corrugated cardboard and plywood.
Specifically, since water glass also has the function of an adhesive, the function of a fire retardant and an adhesive is used in combination, and paper and wood that have been infiltrated with water glass are bonded together to process cardboard, plywood, etc. It was.
On the other hand, even when trying to form a flame retardant coating film by applying water glass on the surface of the substrate, the solute component is inorganic, so it is powdered on the surface of the substrate and the coating film is not formed. Insufficient flame retardant performance is obtained. Thus, water glass alone does not become a coating agent, but a binder for forming a coating film has been demanded.
一方、特開２００５−１１２７００号公報（特許文献１）、特開２００６−２１９３２９号公報（特許文献２）および特開２００９−２９１０３号公報（特許文献３）には、ホウ素化合物の水溶液、液状組成物および重合体を用いた難燃化技術が開示されている。
また、特開２００６−２３３００６号公報（特許文献４）には、本発明の有効成分である糖類が難燃効果を有することが記載されている。すなわち、樹脂中に糖類化合物が存在していると、糖類化合物は燃焼時の高温時に水酸基が脱水し、水を放出して冷却効果を発揮するとともに、チャー（炭化層）を生成して断熱皮膜を形成することが記載されている。しかし、一般的にチャーは不定形に生成するため、内部を完全につつんで保護する形の皮膜にはなりにくいという欠点があった。
On the other hand, JP 2005-112700 A (Patent Document 1), JP 2006-219329 A (Patent Document 2) and JP 2009-29103 A (Patent Document 3) disclose an aqueous solution and a liquid composition of a boron compound. Flame retardant technology using products and polymers is disclosed.
JP-A-2006-233006 (Patent Document 4) describes that the saccharide which is an active ingredient of the present invention has a flame retardant effect. In other words, if a saccharide compound is present in the resin, the saccharide compound dehydrates at high temperatures during combustion, releases water and exhibits a cooling effect, and also forms a char (carbonized layer) to form a heat insulating film. Is described. However, since char is generally formed in an indefinite shape, there is a drawback that it is difficult to form a film that completely protects the inside by being completely wrapped.
さらに、特開２０１１−１６２７４３号公報（特許文献５）には、ホウ素化合物と糖類との併用およびその高い難燃性能の向上（付与）効果に記載されている。
しかしながら、ホウ酸塩の一部は、欧州などで環境規制の対象になりつつあり、今後の使用できなくなる可能性がある。
すなわち、ホウ素はＰＲＴＲ法第１種指定化学物質で、使用に当たって含有量の把握が必要である。また、水質汚濁防止法ではホウ素に関する水質基準が定められており、環境中への漏出には注意が必要である。欧州の環境規制であるＲｏＨＳ指令やＲＥＡＣＨ規則などでも、ホウ素化合物の規制が強化されつつあり、今後使用できなくなる可能性がある。
Furthermore, JP 2011-162743 A (Patent Document 5) describes the combined use of a boron compound and a saccharide and the improvement (giving) effect of high flame retardancy.
However, some borates are becoming subject to environmental regulations in Europe and the like, and may become unusable in the future.
In other words, boron is a PRTR method type 1 designated chemical substance, and it is necessary to grasp its content before use. In addition, the Water Pollution Control Law sets the water quality standard for boron, and caution is required for leakage into the environment. The RoHS directive and REACH regulations, which are environmental regulations in Europe, are becoming more restrictive for boron compounds and may become unusable in the future.
また、特開２００９−５２１３５０号公報（特許文献６）には、本発明の有効成分であるケイ酸塩を含む、耐久性および耐熱性に優れた有機質発泡プラスチック成型体が記載され、ケイ酸塩の反応の遅延剤として本発明の有効成分である糖類が記載されている。
しかしながら、上記の先行技術において、ケイ酸化合物と糖質との併用およびその高い難燃性能の向上（付与）効果については記載されていない。
JP-A-2009-521350 (Patent Document 6) describes an organic foamed plastic molded article excellent in durability and heat resistance, which contains a silicate which is an active ingredient of the present invention. As the reaction retarder, saccharides which are active ingredients of the present invention are described.
However, the above prior art does not describe the combined use of a silicate compound and a saccharide and the improvement (giving) effect of its high flame retardancy.
本発明は、木材、紙、織布、不織布および樹脂に高い難燃性能を付与し得る液状または粉末状の難燃組成物、それを用いた低コストでかつ簡便な難燃化処理方法およびそれにより得られた難燃材料を提供することを課題とする。 The present invention relates to a liquid or powder flame retardant composition capable of imparting high flame retardant performance to wood, paper, woven fabric, nonwoven fabric and resin, a low-cost and simple flame retardant treatment method using the same, and It is an object to provide a flame retardant material obtained by the above.
本発明者は、上記の課題を解決するために鋭意研究を重ねた結果、ケイ素化合物、特にケイ酸ナトリウムと糖類とを併用することにより、難燃性能の付与効果が飛躍的に増大し、これまで難燃効果が低かった有機ポリマーにも適用できることを見出し、本発明を完成するに到った。 As a result of intensive research in order to solve the above-mentioned problems, the present inventors have dramatically increased the effect of imparting flame retardancy by using a silicon compound, particularly sodium silicate and a saccharide in combination. The present invention has been completed by finding that the present invention can be applied to organic polymers having a low flame retardant effect.
かくして、本発明によれば、ケイ酸、ケイ酸塩またはそれらの混合物から選択されるケイ素化合物と、糖類とを相乗効果を奏する割合で含有することを特徴とする難燃組成物が提供される。 Thus, according to the present invention, there is provided a flame retardant composition characterized by containing a silicon compound selected from silicic acid, silicate or a mixture thereof and a saccharide in a synergistic ratio. .
また、本発明によれば、上記の難燃組成物で難燃化対象材料を処理して、難燃材料を得ることを特徴とする難燃化処理方法が提供される。
さらに、本発明によれば、上記の難燃化処理方法により得られた難燃材料が提供される。
Moreover, according to this invention, the flame-retardant processing method characterized by obtaining a flame-retardant material by processing a flame-retardant target material with said flame-retardant composition is provided.
Furthermore, according to this invention, the flame-retardant material obtained by said flame-retarding processing method is provided.
本発明によれば、木材、紙、織布、不織布および樹脂に高い難燃性能を付与し得る液状または粉末状の難燃組成物、それを用いた低コストでかつ簡便な難燃化処理方法およびそれにより得られた難燃材料を提供することができる。
すなわち、本発明の難燃組成物は、これを樹脂などに配合することにより、優れた難燃性を有する樹脂材料を提供することができる。
実施例に示すように、ケイ素化合物と糖類を併用する難燃組成物は、ホウ素化合物と糖類とを併用する難燃組成物に比較して、少量の塗布量で同等の難燃性を発揮することを見出した。
According to the present invention, a liquid or powdery flame retardant composition capable of imparting high flame retardant performance to wood, paper, woven fabric, nonwoven fabric and resin, and a low-cost and simple flame retardant treatment method using the same And the flame-retardant material obtained by it can be provided.
That is, the flame retardant composition of the present invention can provide a resin material having excellent flame retardancy by blending it with a resin or the like.
As shown in the Examples, the flame retardant composition using a silicon compound and a saccharide together exhibits the same flame retardancy with a small amount of application compared to the flame retardant composition using a boron compound and a saccharide together. I found out.
本発明では、セルロースと同じ炭水化物である糖類を併用することにより、接炎時に表面に炭化層を生じ難い有機ポリマーであっても、その表面に緻密な炭化層が形成され、顕著な難燃効果が発現するものと考えられる。
本発明のケイ素化合物と糖類とを併用する難燃性組成物は、ホウ素化合物と糖類とを併用する難燃性組成物と同等の高い難燃性を発揮するが、上記のようにホウ酸塩の一部が環境規制の対象になりつつあることを考えると、その代替えとして有望である。
また、ケイ素化合物の価格（数十円／ｋｇ）は、ホウ素化合物の価格（数百円／ｋｇ）よりも１桁以上安価であり、ケイ素化合物を用いる本発明は、経済的にも優位性がある。
In the present invention, by using a saccharide which is the same carbohydrate as cellulose, a dense carbonized layer is formed on the surface of the organic polymer which is difficult to generate a carbonized layer on the surface at the time of flame contact. Is considered to be expressed.
The flame retardant composition in which the silicon compound and saccharide of the present invention are used in combination exhibits high flame retardancy equivalent to the flame retardant composition in which the boron compound and saccharide are used in combination. Considering that some of these are becoming subject to environmental regulations, it is a promising alternative.
Further, the price of silicon compounds (tens of yen / kg) is one digit or more cheaper than the price of boron compounds (several hundred yen / kg), and the present invention using silicon compounds is economically superior. is there.
また、本発明の難燃組成物は、
（１）ケイ素化合物が、ケイ酸ナトリウム（Ｎａ2Ｏ・ｎＳｉＯ2・ｘＨ2Ｏ）であり、かつ糖類が、グルコースおよびフルクトースから選択される単糖類、スクロース（ショ糖）、トレハロース、セロビオースおよびα−シクロデキストリンから選択される少糖類またはデンプン、グルコマンナンおよびヒドロキシプロピルメチルセルロースから選択される多糖類である、
（２）相乗効果を奏する割合が、ケイ素化合物１００部に対して、糖類が単糖類または少糖類であるとき糖類３〜１５００部または糖類が多糖類であるとき糖類１〜１５００部の割合である、
（３）ケイ素化合物１００部中に２０〜９５部の水を含み、Ｎａ／Ｓｉのモル比で０．４〜１．５の範囲にある水溶液に、糖類が単糖類または少糖類であるとき、ケイ素化合物１００部に対して糖類１〜８０部、または糖類が多糖類であるときケイ素化合物１００部に対して糖類１〜３０部を添加して、溶解せしめた液状の難燃組成物である、および
（４）難燃組成物が、ケイ素化合物と糖類とを混合するか、または上記の液状の難燃組成物を蒸発乾固することにより得られた粉末状の難燃組成物である
のいずれか１つの条件を満足する場合に、上記の優れた効果をさらに発揮する。
Moreover, the flame retardant composition of the present invention comprises:
(1) A monosaccharide, sucrose (sucrose), trehalose, cellobiose and α in which the silicon compound is sodium silicate (Na 2 O · nSiO 2 · xH 2 O) and the saccharide is selected from glucose and fructose A oligosaccharide selected from cyclodextrins or a polysaccharide selected from starch, glucomannan and hydroxypropylmethylcellulose;
(2) The ratio of producing a synergistic effect is the ratio of 3 to 1500 parts of saccharide when the saccharide is a monosaccharide or oligosaccharide, or 1 to 1500 parts of saccharide when the saccharide is a polysaccharide, relative to 100 parts of the silicon compound. ,
(3) When the saccharide is a monosaccharide or oligosaccharide in an aqueous solution containing 20 to 95 parts of water in 100 parts of a silicon compound and having a Na / Si molar ratio in the range of 0.4 to 1.5, 1 to 80 parts of saccharide with respect to 100 parts of silicon compound, or 1 to 30 parts of saccharide with respect to 100 parts of silicon compound when saccharide is a polysaccharide, and is a liquid flame retardant composition dissolved. And (4) The flame retardant composition is a powdery flame retardant composition obtained by mixing a silicon compound and a saccharide or evaporating and drying the liquid flame retardant composition. The above excellent effect is further exhibited when one of the conditions is satisfied.
さらに、本発明の難燃化処理方法は、
（１）難燃化対象材料が、木材、紙、織布、不織布および樹脂から選択される材料である、
（２）難燃組成物が水溶液、水性懸濁液およびコロイド溶液から選択される液状の難燃組成物でありかつ難燃化対象材料が木材、紙、織布、不織布および樹脂から選択される材料であるとき、該液状の難燃組成物を該材料に塗布または含浸させること、
難燃組成物が粉末状の難燃組成物でありかつ難燃化対象材料が樹脂であるとき、該粉末状の難燃組成物を該樹脂に添加し溶融混練すること、または
難燃化対象材料が樹脂であるとき、難燃組成物の粉末状の構成成分を該樹脂に個別に添加して溶融混練すること
からなる、および
（３）塗布が難燃化対象材料の重量増加率で５〜４００％または付着量で０．００４〜１．５ｇ／ｃｍ2になるように行われ、含浸が前記難燃化対象材料の１ｋｇ当り５０ｇ以上の含浸量になるように行われ、また添加が前記樹脂１００部に対して５〜３０部の添加量になるように行われる
のいずれか１つの条件を満足する場合に、上記の優れた効果をさらに発揮する。
Furthermore, the flame retardant treatment method of the present invention comprises:
(1) The material to be flame retardant is a material selected from wood, paper, woven fabric, non-woven fabric, and resin.
(2) The flame retardant composition is a liquid flame retardant composition selected from an aqueous solution, an aqueous suspension and a colloidal solution, and the material to be flame retardant is selected from wood, paper, woven fabric, nonwoven fabric and resin. When it is a material, applying or impregnating the liquid flame retardant composition to the material;
When the flame retardant composition is a powdered flame retardant composition and the material to be flame retardant is a resin, the powdered flame retardant composition is added to the resin and melt-kneaded, or the flame retardant target When the material is a resin, the powdery component of the flame retardant composition is individually added to the resin and melt-kneaded. (3) The coating is 5% by weight increase rate of the material to be flame retardant. done so as to 0.004~1.5g / cm 2 at 400% or adhesion amount is performed so impregnated is 1kg per 50g or more impregnation amount of the flame retardant material of interest, also is added The above excellent effects are further exhibited when any one of the conditions of 5 to 30 parts of the resin is performed so as to be added in an amount of 5 to 30 parts.
本発明の難燃組成物は、ケイ酸、ケイ酸塩またはそれらの混合物から選択されるケイ素化合物と、糖類とを相乗効果を奏する割合で含有することを特徴とする。
本発明において「難燃」とは燃え難いこと、「難燃化」とは燃え難くすること、「難燃組成物（「難燃剤」ともいう）」とは材料を燃え難くするための添加剤を意味する。
材料およびその用途によっては法令が整備され、「難燃」に関する詳細な基準や評価方法が規格化されている。
それらの中で、炎を伴った燃焼ができないことを意味する「不燃」、火が燃え広がらないことを意味する「防炎」、その他「防火」および「耐火」などの用語が使われているが、本発明では、これらの用語をすべて含めて「難燃」と定義する。
The flame retardant composition of the present invention is characterized by containing a silicon compound selected from silicic acid, silicate, or a mixture thereof, and a saccharide in a ratio that exhibits a synergistic effect.
In the present invention, “flame retardant” means that it is difficult to burn, “flame retardant” means that it is difficult to burn, and “flame retardant composition (also referred to as“ flame retardant ”) means an additive for making material difficult to burn. Means.
Depending on the material and its application, laws and regulations have been established, and detailed standards and evaluation methods for "flame retardants" have been standardized.
Among them, terms such as “non-combustible”, which means that combustion with flames cannot be performed, “flame-proof” which means that fire does not burn and spread, and “fireproof” and “fireproof” are used. However, in the present invention, all these terms are included and defined as “flame retardant”.
ケイ酸、ケイ酸塩またはそれらの混合物から選択されるケイ素化合物は、工業的に入手し得るものであれば特に限定されず、例えば、ケイ酸塩としては、ＪＩＳ Ｋ１４０８に規定されるＮａ2Ｏ・ｎＳｉＯ2・ｘＨ2Ｏの化学式で表わされるケイ酸ナトリウム（ケイ酸ソーダ、工業的には「水ガラス」ともいう）が挙げられる。
上記のＪＩＳで規格された市販の水ガラスは、４０〜６０％程度のＨ2Ｏを含み、本発明では、これを水で希釈して、水を蒸発させて濃縮して、または蒸発乾固して固体にして用いることができる。
また、他のケイ酸塩としては、ケイ酸リチウム、ケイ酸カリウムなどが挙げられる。
ケイ素化合物としては、本発明の効果および入手し易さなどの点で、ケイ酸ナトリウムが特に好ましい。
The silicon compound selected from silicic acid, silicate or a mixture thereof is not particularly limited as long as it is industrially available. Examples of silicate include Na 2 O defined in JIS K1408. · nSiO 2 · xH 2 O in formula sodium silicate (sodium silicate, for industrial also referred to as "water glass") represented by the like.
The commercial water glass standardized by the above JIS contains about 40 to 60% of H 2 O. In the present invention, this is diluted with water, evaporated to evaporate the water, or evaporated to dryness. And can be used as a solid.
Examples of other silicates include lithium silicate and potassium silicate.
As the silicon compound, sodium silicate is particularly preferable in terms of the effects of the present invention and availability.
糖類は、ケイ素化合物との併用により本発明の効果を発揮し得る糖類であり、工業的に入手し得るものであれば特に限定されず、低コストで入手し易いものが特に好ましい。
このような糖類は、単糖類、少糖類（オリゴ糖）および多糖類に分類される。
The saccharide is a saccharide that can exhibit the effects of the present invention when used in combination with a silicon compound, and is not particularly limited as long as it is industrially available, and those that are easily available at low cost are particularly preferable.
Such saccharides are classified into monosaccharides, oligosaccharides (oligosaccharides) and polysaccharides.
単糖類としては、
グリセルアルデヒドのようなトリオース（三炭糖）、エリトロース、トレオースなどのテトロース（四炭糖）、リボース、リキソース、キシロース、アラビノース、アピオースなどのペントース（五炭糖）、アロース、タロース、グロース、グルコース（ブドウ糖）、アルトロース、マンノース、ガラクトース、イドースなどのヘキソース（六炭糖）などのアルドース；
ジヒドロキシアセトンのようなトリオース（三炭糖）、エリトルロースのようなテトロース（四炭糖）、リブロース、キシルロースなどのペントース（五炭糖）、プシコース、フルクトース（果糖）、ソルボース、タガトースなどのヘキソース（六炭糖）、セドヘプツロース、コリオースなどのヘプトース（七炭糖）などのケトースが挙げられる。
As monosaccharides,
Triose (tricarbon sugar) such as glyceraldehyde, Tetrose (tetracarbon sugar) such as erythrose and threose, Pentose (pentose sugar) such as ribose, lyxose, xylose, arabinose, apiose, allose, talose, growth, glucose (Dextrose), aldoses such as hexose (hexose) such as altrose, mannose, galactose, idose;
Hexoses such as triose such as dihydroxyacetone, tetrose such as erythrulose, pentose such as ribulose and xylulose, psicose, fructose, fructose, sorbose and tagatose (Carbon sugar), ketose such as heptose (seven carbon sugar) such as sedoheptulose and coliose.
少糖類としては、
トレハロース、イソトレハロース、コージビオース、ソホロース、ニゲロース、ラミナリビオース、マルトース（麦芽糖）、セロビオース、イソマルトース、ゲンチオビオース、ラクトース（乳糖）、スクロース（ショ糖）などの二糖類；
フルクオリゴ糖、ガラクオリゴ糖、乳果オリゴ糖、デオキシリボース、フコース、ラムノース、グルクロン酸、ガラクツロン酸、グルコサミン、ガラクトサミン、グリセリン、キシリトール、ソルビトール、アスコルビン酸（ビタミンＣ）、グルクロノラクトン、グルコノラクトン、α−シクロデキストリンなどのオリゴ糖が挙げられる。
As oligosaccharides,
Disaccharides such as trehalose, isotrehalose, cordobiose, sophorose, nigerose, laminaribiose, maltose (maltose), cellobiose, isomaltose, gentiobiose, lactose (lactose), sucrose (sucrose);
Fructooligosaccharide, galactooligosaccharide, dairy oligosaccharide, deoxyribose, fucose, rhamnose, glucuronic acid, galacturonic acid, glucosamine, galactosamine, glycerin, xylitol, sorbitol, ascorbic acid (vitamin C), glucuronolactone, gluconolactone, α -Oligosaccharides such as cyclodextrins.
多糖類としては、デンプン、アミロース、アミロペクチン、グリコーゲン、セルロース、ヒドロキシプロピルメチルセルロース、ペクチン、グルコマンナン、ポリデキストロースなどが挙げられる。 Examples of the polysaccharide include starch, amylose, amylopectin, glycogen, cellulose, hydroxypropylmethylcellulose, pectin, glucomannan, polydextrose and the like.
これらの糖類の中でも、グルコースおよびフルクトースから選択される単糖類、スクロース（ショ糖）、トレハロース、セロビオースおよびα−シクロデキストリンから選択される少糖類またはデンプン、グルコマンナンおよびヒドロキシプロピルメチルセルロースから選択される多糖類が特に好ましい。 Among these saccharides, monosaccharides selected from glucose and fructose, sucrose (sucrose), trehalose, cellobiose and oligosaccharides selected from α-cyclodextrin or starch, glucomannan and hydroxypropyl methylcellulose Saccharides are particularly preferred.
ケイ素化合物と糖類との相乗効果を奏する割合は、ケイ素化合物１００部に対して、糖類が単糖類または少糖類であるとき糖類１〜１５００部、好ましくは３〜１５００部、より好ましくは１０〜１５０部または糖類が多糖類であるとき糖類１〜１５００部、好ましくは１〜３０部の割合である。
配合割合が上記の範囲内であれば、本発明の優れた効果が得られる。
本発明において「部」とは重量部を意味する。
When the saccharide is a monosaccharide or oligosaccharide, the proportion of the synergistic effect between the silicon compound and the saccharide is 1 to 1500 parts, preferably 3 to 1500 parts, more preferably 10 to 150, when the saccharide is a monosaccharide or oligosaccharide. When the part or saccharide is a polysaccharide, the ratio is 1 to 1500 parts, preferably 1 to 30 parts.
When the blending ratio is within the above range, the excellent effect of the present invention can be obtained.
In the present invention, “parts” means parts by weight.
本発明の難燃性組成物は、ケイ素化合物１００部中に２０〜９５部の水を含み、Ｎａ／Ｓｉのモル比で０．４〜１．５の範囲にある水溶液に、前記糖類が単糖類または少糖類であるとき、ケイ素化合物１００部に対して糖類１〜８０部、または前記糖類が多糖類であるときケイ素化合物１００部に対して糖類１〜３０部を添加して、溶解せしめた液状の難燃組成物であるのが好ましい。
配合割合が上記の範囲内であれば、本発明の優れた効果が得られる。
本発明の液状の難燃組成物は、水溶液、水性懸濁液、コロイド溶液のいずれであってもよい。
The flame retardant composition of the present invention contains 20 to 95 parts of water in 100 parts of a silicon compound, and the saccharide is simply contained in an aqueous solution having a Na / Si molar ratio in the range of 0.4 to 1.5. When it is a saccharide or oligosaccharide, 1 to 80 parts of saccharide is added to 100 parts of silicon compound, or when the saccharide is a polysaccharide, 1 to 30 parts of saccharide is added to 100 parts of silicon compound and dissolved. A liquid flame retardant composition is preferred.
When the blending ratio is within the above range, the excellent effect of the present invention can be obtained.
The liquid flame retardant composition of the present invention may be an aqueous solution, an aqueous suspension, or a colloidal solution.
本発明の難燃組成物は、本発明の効果を阻害しない範囲で、付加効果を発揮する添加剤を含んでいてもよい。
液状の難燃組成物の場合、このような添加剤としては、例えば、塗膜形成剤、浸透剤が挙げられる。
浸透剤は、難燃成分を難燃化対象材料、特に樹脂内部まで浸透させる効果を有する。
このような塗膜形成剤としては、水性ポリウレタンエマルション、エチレン−酢酸ビニル共重合体（ＥＶＡ）エマルション、エチレン−アクリル酸共重合体（ＥＥＡ）エマルションなどが挙げられる。
塗膜形成剤の添加量は、難燃組成物が水溶液のとき、２〜１５重量％程度、好ましくは２〜５重量％である。
The flame retardant composition of the present invention may contain an additive exhibiting an additional effect as long as the effects of the present invention are not impaired.
In the case of a liquid flame retardant composition, examples of such additives include a film-forming agent and a penetrating agent.
The penetrant has an effect of allowing the flame retardant component to penetrate into the material to be flame retardant, particularly into the resin.
Examples of such a film-forming agent include an aqueous polyurethane emulsion, an ethylene-vinyl acetate copolymer (EVA) emulsion, and an ethylene-acrylic acid copolymer (EEA) emulsion.
When the flame retardant composition is an aqueous solution, the amount of the film forming agent added is about 2 to 15% by weight, preferably 2 to 5% by weight.
浸透剤は、難燃化対象材料へのケイ素化合物の含浸を促進する効果を有する。
このような浸透剤としては、メタノール、エタノール、プロパノール、ブタノール、ペンタノール、ヘキサノールなどのアルコール；エチレングリコール、プロピレングリコールのようなジオール；グリセリンのようなトリオール；炭素数３〜１１のアルジトール（グリシトールともいう）のようなポリオール、ポリフェノール類、界面張力を低下させる作用のある界面活性剤などが挙げられる。
浸透剤の添加量は、難燃組成物が水溶液のとき、１〜１０重量％程度、好ましくは１〜３重量％である。
The penetrant has an effect of promoting the impregnation of the silicon compound into the flame retardant material.
Examples of such penetrants include alcohols such as methanol, ethanol, propanol, butanol, pentanol, and hexanol; diols such as ethylene glycol and propylene glycol; triols such as glycerin; alditols having 3 to 11 carbon atoms (also called glycitol). Polyol), polyphenols, and surfactants having an action of reducing interfacial tension.
When the flame retardant composition is an aqueous solution, the amount of penetrant added is about 1 to 10% by weight, preferably 1 to 3% by weight.
また、本発明の難燃性組成物は、ケイ酸、ケイ酸塩またはそれらの混合物から選択されるケイ素化合物と糖類とを混合するか、または上記の液状の難燃組成物を蒸発乾固することにより得られた粉末状の難燃組成物であるのが好ましい。
蒸発乾固は、公知の方法により行うことができるが、スプレードライ法（噴霧乾燥法）が特に好ましい。「スプレードライ法」とは、液体を微細な霧状にして、熱風中に噴霧し、瞬間的に乾燥させて粉体を得る方法である。具体的には、実施例において詳述する。
Moreover, the flame retardant composition of the present invention is a mixture of a silicon compound selected from silicic acid, silicate or a mixture thereof and a saccharide, or the above liquid flame retardant composition is evaporated to dryness. It is preferable that it is a powdery flame-retardant composition obtained by this.
Evaporation to dryness can be performed by a known method, but spray drying (spray drying) is particularly preferred. The “spray drying method” is a method in which a liquid is made into a fine mist, sprayed in hot air, and instantaneously dried to obtain a powder. Specifically, it will be described in detail in Examples.
本発明によれば、上記の難燃組成物で難燃化対象材料を処理して、難燃材料を得ることことからなる難燃化処理方法およびそれにより得られた難燃材料が提供される。 According to the present invention, a flame retardant treatment method comprising obtaining a flame retardant material by treating a flame retardant target material with the above flame retardant composition, and a flame retardant material obtained thereby are provided. .
難燃化対象材料は、木材、紙、織布、不織布および樹脂から選択される材料であるのが好ましい。このような材料としては、例えば、
杉材、エゾマツ、ヒノキ、キリ、ベニヤ、ケヤキ、ＳＰＦ集成材（スプルス（エゾマツ）、パイン（マツ）、ファー（モミ）を貼り合わせた合材）、竹などの木材；
和紙、ふすま紙、洋紙などの紙；
綿布、ポリエステル織布、ポリプロピレン織布、ナイロン織布、アクリル織布、ビニロン織布、アラミド織布、ポリエチレンテレフタレート（ＰＥＴ）織布などの織布；
ポリエステル不織布、ポリプロピレン不織布、ナイロン不織布、アクリル不織布、ビニロン不織布、アラミド不織布などの不織布；
The flame retardant material is preferably a material selected from wood, paper, woven fabric, non-woven fabric and resin. As such a material, for example,
Wood such as cedar, Japanese pine, Japanese cypress, Japanese cypress, veneer, Japanese zelkova, SPF laminated timber (a mixture of spruce, pine, pine, fir) and bamboo;
Japanese paper, bran paper, western paper, etc .;
Woven fabrics such as cotton fabric, polyester woven fabric, polypropylene woven fabric, nylon woven fabric, acrylic woven fabric, vinylon woven fabric, aramid woven fabric, polyethylene terephthalate (PET) woven fabric;
Nonwoven fabrics such as polyester nonwoven fabric, polypropylene nonwoven fabric, nylon nonwoven fabric, acrylic nonwoven fabric, vinylon nonwoven fabric, and aramid nonwoven fabric;
ポリプロピレン、ポリエチレン、ポリウレタン（硬質、軟質）、ポリスチレン、塩化ビニル、ポリカーボネート、フェノール樹脂、尿素樹脂、メラミン樹脂、酢酸ビニル樹脂、メタクリル樹脂、エポキシ樹脂、アクリル樹脂、ポリウレタン（硬質、軟質）、塩化ビニル樹脂、ポリ塩化ビニリデン、ポリテトラフルオロエチレン（ＰＴＦＥ）樹脂、ＡＢＳ（アクリロニトリルブタジエンスチレン）樹脂、ＡＳ（アクリロニトリルスチレン）樹脂、ポリアセタール、変性ポリフェニレンエーテル樹脂、ポリブチレンテレフタラート樹脂、ブタジエンゴム、ネオプレン（クロロプレン）ゴム、スチレンブタジエンゴム（ＳＢＲ）、ブタジエンアクリロニトリルゴム（ＮＢＲ）、イソブテンイソプレンゴム、ポリ酢酸ビニル、ポリエチレンテレフタレート（ＰＥＴ）およびこれらの複合材料の成形体およびフィルム
が挙げられる。
上記のように、本発明における「木材」は、厚板状、薄板状、粉砕品、粉状にした木を張り合わせや成形により加工した木質材料および薄板、粉砕品、粉状の木材に樹脂を注入して成形性をもたせた木質材料を含む。
Polypropylene, polyethylene, polyurethane (hard, soft), polystyrene, vinyl chloride, polycarbonate, phenol resin, urea resin, melamine resin, vinyl acetate resin, methacrylic resin, epoxy resin, acrylic resin, polyurethane (hard, soft), vinyl chloride resin , Polyvinylidene chloride, polytetrafluoroethylene (PTFE) resin, ABS (acrylonitrile butadiene styrene) resin, AS (acrylonitrile styrene) resin, polyacetal, modified polyphenylene ether resin, polybutylene terephthalate resin, butadiene rubber, neoprene (chloroprene) rubber , Styrene butadiene rubber (SBR), butadiene acrylonitrile rubber (NBR), isobutene isoprene rubber, polyvinyl acetate, polyethylene terephthalate Preparative (PET) and moldings of these composites and films.
As described above, the term “wood” in the present invention refers to a wood material and a thin plate, a pulverized product, and a powdered wood obtained by processing a thick plate, thin plate, pulverized product, and powdered wood by pasting or molding. Contains wood material that has been cast to give formability.
本発明の難燃組成物による処理は、
難燃組成物が水溶液、水性懸濁液およびコロイド溶液から選択される液状の難燃組成物でありかつ難燃化対象材料が木材、紙、織布、不織布および樹脂から選択される材料であるとき、液状の難燃組成物を材料に塗布または含浸させること、
難燃組成物が粉末状の難燃組成物でありかつ難燃化対象材料が樹脂であるとき、粉末状の難燃組成物を樹脂に添加し溶融混練すること、または
難燃化対象材料が樹脂であるとき、難燃組成物の粉末状の構成成分を樹脂に個別に添加して溶融混練すること
からなるのが好ましい。
The treatment with the flame retardant composition of the present invention comprises:
The flame retardant composition is a liquid flame retardant composition selected from aqueous solutions, aqueous suspensions and colloidal solutions, and the material to be flame retardant is a material selected from wood, paper, woven fabric, non-woven fabric and resin. When applying or impregnating the material with a liquid flame retardant composition,
When the flame retardant composition is a powdered flame retardant composition and the flame retardant material is a resin, the powder flame retardant composition is added to the resin and melt-kneaded, or the flame retardant material is When it is a resin, it is preferable that the powdery constituents of the flame retardant composition are individually added to the resin and melt kneaded.
液状の難燃組成物を難燃化対象材料に含浸または塗布するには、公知の方法を適用することができる。
含浸は、加熱下および／または加圧下で行うのが好ましい。その条件は、難燃化対象材料の種類や形状などにより適宜設定すればよい。例えば、液状の難燃組成物の調製時における加熱温度またはそれ以上の温度が好ましく、通常、２〜２０気圧程度の圧力が好ましい。
含浸量は、液状の難燃組成物の濃度などにもよるが、難燃化対象材料の１ｋｇ当り５０ｇ以上、好ましくは５００〜２０００ｇである。
含浸量が上記の範囲内であれば、本発明の優れた効果が得られる。
In order to impregnate or apply the liquid flame retardant composition to the flame retardant material, a known method can be applied.
The impregnation is preferably performed under heating and / or pressure. The conditions may be set as appropriate depending on the type and shape of the flame retardant material. For example, a heating temperature or higher at the time of preparing the liquid flame retardant composition is preferable, and a pressure of about 2 to 20 atm is usually preferable.
Although the amount of impregnation depends on the concentration of the liquid flame retardant composition, it is 50 g or more, preferably 500 to 2000 g per kg of the flame retardant material.
If the amount of impregnation is within the above range, the excellent effect of the present invention can be obtained.
塗布方法およびその条件は、難燃化対象材料の種類や形状、液状の難燃組成物の性状などにより適宜設定すればよく、刷毛、ブレードなどを用いた塗布、噴霧などの公知の方法が挙げられる。液状の難燃組成物が高粘度である場合には、バターナイフ様のブレードを用いた方法が好ましい。
塗布量（乾燥後）は、難燃化対象材料の種類や形状などによるが、難燃化対象材料の重量増加率で５〜４００％程度、好ましくは６０〜８０％、付着量で０．００４〜１．５ｇ／ｃｍ2程度、好ましくは０．０１〜０．１ｇ／ｃｍ2である。
塗布量が上記の範囲内であれば、本発明の優れた効果が得られる。
また、所望の難燃性能を得るために１回の塗布で不足の場合には、塗布・乾燥の工程を繰り返してもよい。
The application method and its conditions may be set as appropriate depending on the type and shape of the material to be flame retardant, the properties of the liquid flame retardant composition, etc., and include known methods such as application using a brush, a blade, and spraying. It is done. When the liquid flame retardant composition has a high viscosity, a method using a butter knife-like blade is preferable.
The coating amount (after drying) depends on the type and shape of the material to be flame retardant, but the weight increase rate of the material to be flame retardant is about 5 to 400%, preferably 60 to 80%, and the amount of adhesion is 0.004. to 1.5 g / cm 2 or so, preferably from 0.01 to 0.1 g / cm 2.
When the coating amount is within the above range, the excellent effect of the present invention can be obtained.
In addition, in order to obtain a desired flame retardancy, when the application is insufficient in one application, the application / drying process may be repeated.
液状の難燃組成物を難燃化対象材料に含浸または塗布した後、液状の難燃組成物の溶媒である水を除去するために乾燥してもよい。
乾燥方法およびその条件は、液状の難燃組成物の溶媒である水が除去され、難燃成分および難燃化対象材料が変質、変形しない限り特に限定されず、適宜設定すればよい。
After impregnating or applying the liquid flame retardant composition to the flame retardant material, the material may be dried to remove water which is a solvent of the liquid flame retardant composition.
The drying method and the conditions thereof are not particularly limited as long as water as a solvent of the liquid flame retardant composition is removed, and the flame retardant component and the flame retardant material are not altered or deformed, and may be set as appropriate.
粉末状の難燃組成物と樹脂とを溶融混練する方法、難燃組成物の構成成分を樹脂に個別に添加して溶融混練する方法は、公知の方法を適用することができる。また、溶融混練された樹脂は、通常、公知の方法で所望の形状に成形することができる。
溶融混練には、例えば二軸混練機、成形には例えば押出成形機または射出成形機を用いることができる。
Known methods can be applied to the method of melt-kneading the powdered flame-retardant composition and the resin, and the method of individually adding the components of the flame-retardant composition to the resin and melt-kneading. The melt-kneaded resin can be usually formed into a desired shape by a known method.
For example, a twin-screw kneader can be used for the melt kneading, and an extrusion molding machine or an injection molding machine can be used for the molding.
粉末状の難燃組成物または難燃組成物の構成成分の総量の配合量は、樹脂材料の種類や要求される難燃性などにより適宜設定すればよく、通常、樹脂１００部に対して５〜３０部程度、好ましくは１５〜２０部である。
配合量が上記の範囲内であれば、本発明の優れた効果が得られる。
What is necessary is just to set suitably the compounding quantity of the powdery flame retardant composition or the total amount of the structural component of a flame retardant composition by the kind of resin material, the flame retardance requested | required, etc., and normally 5 parts with respect to 100 parts of resin About 30 parts, preferably 15-20 parts.
When the blending amount is within the above range, the excellent effect of the present invention can be obtained.
本発明を以下の実施例および比較例からなる試験例によりさらに詳しく説明するが、これらの実施例により本発明が限定されるものではない。
以下の説明において、特に断りのない限り「部」は「重量部」を意味する。
The present invention will be described in more detail with reference to test examples including the following examples and comparative examples, but the present invention is not limited to these examples.
In the following description, “parts” means “parts by weight” unless otherwise specified.
（試験例１）
水ガラス１００部（Ｎａ2Ｏ濃度：１４．９重量％、ＳｉＯ2濃度：３１．７８重量％、モル比Ｎａ2Ｏ／ＳｉＯ2：２．２、冨士化学株式会社製、製品名：１号水ガラス５０°、以下同様）に、ショ糖（ＨＩＲＡＮＯ社製、上白糖、以下同様）２５部を添加・溶解させて水溶液を得た。
水ガラス１００部にショ糖１０部、５部、２．５部、１．６部および１．３部をそれぞれ添加したこと以外は上記と同様にして水溶液を得た。
得られたショ糖を含む水ガラスの水溶液難燃性能を、水ガラスおよびショ糖水溶液（水１００部に対してショ糖１７部を添加・溶解した水溶液）と比較評価した。
(Test Example 1)
100 parts of water glass (Na 2 O concentration: 14.9% by weight, SiO 2 concentration: 31.78% by weight, molar ratio Na 2 O / SiO 2 : 2.2, manufactured by Fuji Chemical Co., Ltd., product name: No. 1 An aqueous solution was obtained by adding and dissolving 25 parts of sucrose (manufactured by HIRANO, super white sugar, the same applies hereinafter) to water glass 50 °, the same applies hereinafter.
An aqueous solution was obtained in the same manner as above except that 10 parts, 5 parts, 2.5 parts, 1.6 parts and 1.3 parts of sucrose were added to 100 parts of water glass.
The aqueous solution flame retardant performance of the obtained water glass containing sucrose was compared with water glass and a sucrose aqueous solution (an aqueous solution in which 17 parts of sucrose was added to and dissolved in 100 parts of water).
難燃（耐火）性能の評価を、消防法施行規則第４条の３第３〜７項に規定された防炎物品の防炎性能試験基準（ＪＩＳ規格Ａ１３２２に相当）の４５°メッケルバーナー法に基づいて実施した。
具体的には、試験体（約３００ｍｍ×２００ｍｍ）を水平面から４５°傾け、炎長６５ｍｍのメッケルバーナーで試験体の下部から２分間、試験体が着火せず貫通しない場合には連続して最長１２〜１４分間まで接炎（加熱）し、その際の炭化長、炭化面積、貫通時間および加熱中の試験体上面の温度変化を調べた。
The 45 ° Meckel burner method of flameproof performance test standards (corresponding to JIS standard A1322) of flameproof articles defined in Article 4-3, Paragraphs 3 to 7 of the Fire Service Act Enforcement Regulations. Based on.
Specifically, the specimen (approx. 300 mm x 200 mm) is tilted 45 ° from the horizontal plane, and if the specimen does not ignite and does not penetrate for 2 minutes from the bottom of the specimen with a 65 mm flame length, it will continue to be the longest. Flame contact (heating) was performed for 12 to 14 minutes, and carbonization length, carbonization area, penetration time, and temperature change of the upper surface of the test specimen during heating were examined.
介護用マットや住宅用断熱材に使用される硬質ウレタンフォーム（厚さ１０ｍｍ、密度０．０５ｇ／ｃｍ3）からなる試験体の表面に、ふすま・障子のり用の刷毛（毛足３０ｍｍ×幅７３ｍｍ）を用いて、各水溶液を塗布・乾燥した。
予め試験体の重量を計量しておき、その塗布・乾燥後の重量とから重量増加率（ＷＰＧ：％）および難燃成分の付着量（ｇ／ｃｍ2）を求めた。
得られた結果を表１および２にまとめて示す。
Brushes for bran and paper shoji (30 mm bristle foot x 73 mm width) on the surface of a test piece made of rigid urethane foam (thickness 10 mm, density 0.05 g / cm 3 ) used for nursing mats and thermal insulation for housing ) Was used to apply and dry each aqueous solution.
The weight of the specimen was measured in advance, and the weight increase rate (WPG:%) and the amount of flame retardant component adhered (g / cm 2 ) were determined from the weight after coating and drying.
The obtained results are summarized in Tables 1 and 2.
未貫通の試験体について、接炎状態で背面（接炎面と反対の表面）の温度を１２分間継続してモニターした。
得られた結果を図１に示す。
About the unpenetrated test body, the temperature of the back surface (surface opposite to the flame contact surface) was continuously monitored for 12 minutes in the flame contact state.
The obtained results are shown in FIG.
（試験例２）
ショ糖の代わりにトレハロース（林原社製、トレハ）を用いたこと以外は、試験例１と同様にして、水溶液を調製し、それらを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表１および２にまとめて示す。
未貫通の試験体について、接炎状態で背面（接炎面と反対の表面）の温度を１２分間継続してモニターした。
得られた結果を図２に示す。
(Test Example 2)
Except for using trehalose (manufactured by Hayashibara Co., Ltd., Treha) instead of sucrose, aqueous solutions were prepared in the same manner as in Test Example 1, and applied to a rigid urethane foam and dried to evaluate flame retardancy. .
The obtained results are summarized in Tables 1 and 2.
About the unpenetrated test body, the temperature of the back surface (surface opposite to the flame contact surface) was continuously monitored for 12 minutes in the flame contact state.
The obtained results are shown in FIG.
（試験例３）
ショ糖の代わりにグルコース（ブドウ糖、和光純薬社製）を用いたこと以外は、試験例１と同様にして、水溶液を調製し、それらを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表１および２にまとめて示す。
未貫通の試験体について、接炎状態で背面（接炎面と反対の表面）の温度を１２分間継続してモニターした。
得られた結果を図２に示す。
(Test Example 3)
Except that glucose (glucose, manufactured by Wako Pure Chemical Industries, Ltd.) was used instead of sucrose, an aqueous solution was prepared in the same manner as in Test Example 1, and the flame retardant performance was obtained by applying and drying them on a rigid urethane foam. evaluated.
The obtained results are summarized in Tables 1 and 2.
About the unpenetrated test body, the temperature of the back surface (surface opposite to the flame contact surface) was continuously monitored for 12 minutes in the flame contact state.
The obtained results are shown in FIG.
（試験例４）
ショ糖の代わりにフルクトース（果糖、和光純薬社製）を用いたこと以外は、試験例１と同様にして、水溶液を調製し、それらを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表１および２にまとめて示す。
(Test Example 4)
Except that fructose (fructose, manufactured by Wako Pure Chemical Industries, Ltd.) was used instead of sucrose, an aqueous solution was prepared in the same manner as in Test Example 1, and these were applied to a rigid urethane foam and dried to obtain flame retardant performance. evaluated.
The obtained results are summarized in Tables 1 and 2.
（試験例５）
ショ糖の代わりにデンプン（幸田商店製、馬鈴薯片栗粉、以下同様）を用い、添加量を６部、３部および１部としたこと以外は、試験例１と同様にして、水溶液を調製し、それらを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表１および２にまとめて示す。
未貫通の試験体について、接炎状態で背面（接炎面と反対の表面）の温度を１２分間継続してモニターした。
得られた結果を図３に示す。
(Test Example 5)
An aqueous solution was prepared in the same manner as in Test Example 1 except that starch (made by Koda Shoten, potato potato starch, hereinafter the same) was used instead of sucrose, and the addition amount was 6 parts, 3 parts and 1 part, They were applied to a rigid urethane foam and dried to evaluate flame retardancy.
The obtained results are summarized in Tables 1 and 2.
About the unpenetrated test body, the temperature of the back surface (surface opposite to the flame contact surface) was continuously monitored for 12 minutes in the flame contact state.
The obtained results are shown in FIG.
（試験例６）
ショ糖の代わりにグルコマンナン（清水化学社製、レオレックスＬＭ）を用い、添加量を６部、３部および１部としたこと以外は、試験例１と同様にして、水溶液を調製し、それらを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表１および２にまとめて示す。
(Test Example 6)
An aqueous solution was prepared in the same manner as in Test Example 1, except that glucomannan (manufactured by Shimizu Chemical Co., Ltd., ROLEX LM) was used instead of sucrose, and the addition amount was 6 parts, 3 parts and 1 part. They were applied to a rigid urethane foam and dried to evaluate flame retardancy.
The obtained results are summarized in Tables 1 and 2.
（試験例７）
ショ糖の代わりにヒドロキシプロピルメチルセルロース（水溶性セルロース、信越化学製、メトローズ６０ＳＨ）を用い、添加量を６部、３部および１部としたこと以外は、試験例１と同様にして、水溶液を調製し、それらを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表１および２にまとめて示す。
(Test Example 7)
An aqueous solution was prepared in the same manner as in Test Example 1, except that hydroxypropylmethylcellulose (water-soluble cellulose, manufactured by Shin-Etsu Chemical Co., Ltd., Metrose 60SH) was used instead of sucrose, and the addition amount was 6 parts, 3 parts and 1 part. They were prepared and applied to a rigid urethane foam and dried to evaluate flame retardancy.
The obtained results are summarized in Tables 1 and 2.
（試験例８）
ショ糖の代わりにセロビオース（松谷化学製、セロビオース９０）を用いたこと以外は、試験例１と同様にして、水溶液を調製し、それらを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表１および２にまとめて示す。
(Test Example 8)
Except for using cellobiose (manufactured by Matsutani Chemical, cellobiose 90) instead of sucrose, prepare an aqueous solution in the same manner as in Test Example 1, and apply and dry them to rigid urethane foam to evaluate flame retardancy. did.
The obtained results are summarized in Tables 1 and 2.
（試験例９）
ショ糖の代わりにデンプン５部を用い、硬質ウレタンフォームの代わりにポリプロピレン板（厚さ１ｍｍ）を用いたこと以外は、試験例１と同様にして、水溶液を調製し、それをポリプロピレン板に塗布・乾燥して難燃性能を評価した。
表３に示すように、一部の試験において、基材・難燃剤間に塗布するプライマーとして、ポリプロピレン（ＰＰ）用接着剤（コニシ株式会社製、製品名：ボンドウルトラ多用途ＳＵ、以下同様）を塗布量３０重量部で塗布した。
得られた結果を表３および４にまとめて示す。
(Test Example 9)
An aqueous solution was prepared and applied to the polypropylene plate in the same manner as in Test Example 1, except that 5 parts of starch was used instead of sucrose, and a polypropylene plate (thickness 1 mm) was used instead of rigid urethane foam. -Dried and evaluated flame retardant performance.
As shown in Table 3, in some tests, as a primer to be applied between the base material and the flame retardant, an adhesive for polypropylene (PP) (manufactured by Konishi Co., Ltd., product name: Bond Ultra Multipurpose SU, the same applies hereinafter) Was applied at a coating amount of 30 parts by weight.
The results obtained are summarized in Tables 3 and 4.
（試験例１０）
ポリプロピレン板の代わりにポリエチレン板（厚さ１ｍｍ）を用いたこと以外は、試験例９と同様にして、水溶液を調製し、それをポリエチレン板に塗布・乾燥して難燃性能を評価した。
表３に示すように、一部の試験において、基材・難燃剤間に塗布するプライマーとして、ポリプロピレン（ＰＰ）用接着剤を塗布量３０重量部で塗布した。
得られた結果を表３および４にまとめて示す。
(Test Example 10)
An aqueous solution was prepared in the same manner as in Test Example 9 except that a polyethylene plate (thickness 1 mm) was used instead of the polypropylene plate, and the flame retardant performance was evaluated by applying and drying the solution on a polyethylene plate.
As shown in Table 3, in some tests, an adhesive for polypropylene (PP) was applied at a coating amount of 30 parts by weight as a primer to be applied between the base material and the flame retardant.
The results obtained are summarized in Tables 3 and 4.
（試験例１１）
ポリプロピレン板の代わりに硬質ウレタンフォーム（厚さ１０ｍｍ）を用いたこと以外は、試験例９と同様にして、水溶液を調製し、それを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表３および４にまとめて示す。
(Test Example 11)
Except that a rigid urethane foam (thickness 10 mm) was used instead of the polypropylene plate, an aqueous solution was prepared in the same manner as in Test Example 9, and applied to the rigid urethane foam and dried to evaluate the flame retardant performance. .
The results obtained are summarized in Tables 3 and 4.
（試験例１２）
ポリプロピレン板の代わりに軟質ウレタンフォーム（厚さ１０ｍｍ）を用いたこと以外は、試験例９と同様にして、水溶液を調製し、それを軟質ウレタンフォームに塗布または含浸・乾燥して難燃性能を評価した。
得られた結果を表３および４にまとめて示す。
(Test Example 12)
Except that a flexible urethane foam (thickness 10 mm) was used instead of the polypropylene plate, an aqueous solution was prepared in the same manner as in Test Example 9, and applied or impregnated / dried to the flexible urethane foam to achieve flame retardancy. evaluated.
The results obtained are summarized in Tables 3 and 4.
（試験例１３）
ポリプロピレン板の代わりにポリプロピレン不織布（日本製紙クレシア製、キムテックス、厚さ０．７ｍｍ）を用いたこと以外は、試験例９と同様にして、水溶液を調製し、それをポリプロピレン不織布に塗布または含浸・乾燥して難燃性能を評価した。
得られた結果を表３および４にまとめて示す。
(Test Example 13)
An aqueous solution was prepared in the same manner as in Test Example 9 except that a polypropylene nonwoven fabric (Nippon Paper Crecia, Kimtex, thickness 0.7 mm) was used instead of the polypropylene plate, and an aqueous solution was applied or impregnated on the polypropylene nonwoven fabric. -Dried and evaluated flame retardant performance.
The results obtained are summarized in Tables 3 and 4.
また、難燃性能の評価を、ＦＭＶＳＳ３０２（米国自動車安全基準の燃焼性試験）に基づいて実施した。
具体的には、上記と同様にして作成した試験体（３０５ｍｍ×３０５ｍｍ）をＵ字枠に挟んで水平にし、試験体の真下１８．８ｍｍの位置にバーナー口を設置し、１５秒間接炎（炎長１９ｍｍ）し、炎が試験体の点火端から３８ｍｍおよび３２５ｍｍの線を通過する間の時間を測定した。また、試験体の点火端から２８７ｍｍの位置まで燃焼が継続しない場合には、消炎までの時間と試験体の点火端から長さを測定した。これらの測定から、燃焼時間（秒）および燃焼速度（ｍｍ／秒）を求めた。
未処理のポリプロピレン不織布は燃焼時間８８秒および燃焼速度６９ｍｍ／秒であったが、デンプンを含む水ガラスを塗布・乾燥した試験体は着火せず、燃焼時間０秒および燃焼速度０ｍｍ／秒であった。
また、水ガラスおよびデンプン水溶液をそれぞれ塗布・乾燥した試験体は、それぞれ燃焼時間８１秒および７７秒、燃焼速度４３ｍｍ／秒および燃焼速度５０ｍｍ／秒であった。
In addition, the evaluation of flame retardancy was carried out based on FMVSS302 (American Automobile Safety Standard Flammability Test).
Specifically, a test specimen (305 mm × 305 mm) prepared in the same manner as described above was placed horizontally with a U-shaped frame, a burner port was installed at a position 18.8 mm directly below the test specimen, and a 15-second indirect flame ( The flame length was 19 mm) and the time during which the flame passed through the 38 mm and 325 mm lines from the ignition end of the specimen was measured. Moreover, when combustion did not continue to the position of 287 mm from the ignition end of the test body, the time to extinction and the length from the ignition end of the test body were measured. From these measurements, the burning time (seconds) and burning rate (mm / sec) were determined.
The untreated polypropylene non-woven fabric had a burning time of 88 seconds and a burning speed of 69 mm / second, but the test specimen coated with water-containing starch and dried did not ignite, and had a burning time of 0 seconds and a burning speed of 0 mm / second. It was.
Moreover, the test body which apply | coated and dried the water glass and the starch aqueous solution, respectively had a burning time of 81 seconds and 77 seconds, a burning speed of 43 mm / sec, and a burning speed of 50 mm / sec.
（試験例１４）
ポリプロピレン板の代わりにポリウレタンフィルム（厚さ０．３ｍｍ）を用いたこと以外は、試験例９と同様にして、水溶液を調製し、それをポリウレタンフィルム不織布に塗布または含浸・乾燥して難燃性能を評価した。
得られた結果を表３および４にまとめて示す。
(Test Example 14)
Except that a polyurethane film (thickness 0.3 mm) was used instead of the polypropylene plate, an aqueous solution was prepared in the same manner as in Test Example 9, and applied to, or impregnated with, and dried on a polyurethane film nonwoven fabric to give flame retardancy. Evaluated.
The results obtained are summarized in Tables 3 and 4.
（試験例１５）
ポリプロピレン板の代わりに発泡ポリスチレンフォーム板（厚さ１０ｍｍ）を用いたこと以外は、試験例９と同様にして、水溶液を調製し、それを発泡ポリスチレンフォーム板に塗布・乾燥して難燃性能を評価した。
得られた結果を表３および４にまとめて示す。
(Test Example 15)
Except that a foamed polystyrene foam plate (thickness 10 mm) was used instead of the polypropylene plate, an aqueous solution was prepared in the same manner as in Test Example 9, and applied to the foamed polystyrene foam plate and dried to provide flame retardancy. evaluated.
The results obtained are summarized in Tables 3 and 4.
（試験例１６）
デンプンの代わりにα−シクロデキストリン（Ｃ36Ｈ60Ｏ30、分子量９７３、純正化学製）を用いたこと以外は、試験例９と同様にして、水溶液を調製し、それをポリプロピレン板に塗布・乾燥して難燃性能を評価した。
表３に示すように、一部の試験において、基材・難燃剤間に塗布するプライマーとして、ポリプロピレン（ＰＰ）用接着剤を塗布量３０重量部で塗布した。
得られた結果を表３および４にまとめて示す。
(Test Example 16)
An aqueous solution was prepared in the same manner as in Test Example 9 except that α-cyclodextrin (C 36 H 60 O 30 , molecular weight 973, manufactured by Junsei Kagaku) was used instead of starch, and this was applied to a polypropylene plate. It dried and evaluated flame retardancy.
As shown in Table 3, in some tests, an adhesive for polypropylene (PP) was applied at a coating amount of 30 parts by weight as a primer to be applied between the base material and the flame retardant.
The results obtained are summarized in Tables 3 and 4.
（試験例１７）
デンプン５部を含有する水ガラスを、付着量０．０２５ｇ／ｃｍ2になるようにポリプロピレン板（厚さ１ｍｍ）に塗布したこと以外は、試験例９と同様にして、難燃性能を評価した。
表３に示すように、基材・難燃剤間に塗布するプライマーとして、ポリプロピレン（ＰＰ）用接着剤を塗布量３０重量部で塗布した。
得られた結果を表３および４にまとめて示す。
(Test Example 17)
Flame retardant performance was evaluated in the same manner as in Test Example 9 except that water glass containing 5 parts of starch was applied to a polypropylene plate (thickness 1 mm) so that the adhesion amount was 0.025 g / cm 2 . .
As shown in Table 3, as a primer to be applied between the base material and the flame retardant, an adhesive for polypropylene (PP) was applied at an application amount of 30 parts by weight.
The results obtained are summarized in Tables 3 and 4.
（試験例１８）
デンプン５部を含有する水ガラスを、付着量０．０２５ｇ／ｃｍ2になるようにポリプロピレン板（厚さ０．７５ｍｍ）に塗布したこと以外は、試験例９と同様にして、難燃性能を評価した。
表３に示すように、基材・難燃剤間に塗布するプライマーとして、ポリプロピレン（ＰＰ）用接着剤を塗布量３０重量部で塗布した。
得られた結果を表３および４にまとめて示す。
(Test Example 18)
Flame retardant performance was obtained in the same manner as in Test Example 9, except that water glass containing 5 parts of starch was applied to a polypropylene plate (thickness: 0.75 mm) so that the adhesion amount was 0.025 g / cm 2. evaluated.
As shown in Table 3, as a primer to be applied between the base material and the flame retardant, an adhesive for polypropylene (PP) was applied at an application amount of 30 parts by weight.
The results obtained are summarized in Tables 3 and 4.
（試験例１９）
水ガラス（Ｎａ2Ｏ濃度：１７．７３重量％、ＳｉＯ2濃度：３５．５８重量％、モル比Ｎａ2Ｏ／ＳｉＯ2：２．１３、冨士化学株式会社製、品種：１号５９°）６０部および水４０部を含む水ガラス水溶液を用いたこと以外は、試験例１と同様にして、ショ糖を添加・溶解させて水溶液を調製し、それを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表５および６にまとめて示す。
(Test Example 19)
Water glass (Na 2 O concentration: 17.73 wt%, SiO 2 concentration: 35.58 wt%, molar ratio Na 2 O / SiO 2 : 2.13, manufactured by Fuji Chemical Co., Ltd., variety: No. 59 °) Except that a water glass aqueous solution containing 60 parts and 40 parts of water was used, an aqueous solution was prepared by adding and dissolving sucrose in the same manner as in Test Example 1, and applying and drying the solution to a rigid urethane foam. Flame retardant performance was evaluated.
The results obtained are summarized in Tables 5 and 6.
（試験例２０）
ショ糖の代わりにデンプン５部を用いたこと以外は、試験例１９と同様にして、水溶液を調製し、それをポリプロピレン板（厚さ１ｍｍ）に塗布・乾燥して難燃性能を評価した。
得られた結果を表５および６にまとめて示す。
(Test Example 20)
An aqueous solution was prepared in the same manner as in Test Example 19 except that 5 parts of starch was used instead of sucrose, and this was applied to a polypropylene plate (thickness 1 mm) and dried to evaluate flame retardancy.
The results obtained are summarized in Tables 5 and 6.
（試験例２１）
水ガラス（Ｎａ2Ｏ濃度：１１．７２重量％、ＳｉＯ2濃度：２８．６５重量％、モル比Ｎａ2Ｏ／ＳｉＯ2：２．５２、冨士化学株式会社製、品種：２号）７５部および水２５部を含む水ガラス水溶液を用いたこと以外は、試験例１と同様にして、ショ糖を添加・溶解させて水溶液を調製し、それを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表５および６にまとめて示す。
(Test Example 21)
75 parts of water glass (Na 2 O concentration: 11.72% by weight, SiO 2 concentration: 28.65% by weight, molar ratio Na 2 O / SiO 2 : 2.52, manufactured by Fuji Chemical Co., Ltd., type: 2) In addition, except that a water glass aqueous solution containing 25 parts of water was used, an aqueous solution was prepared by adding and dissolving sucrose in the same manner as in Test Example 1, and applied to a rigid urethane foam and dried to make it flame retardant. Performance was evaluated.
The results obtained are summarized in Tables 5 and 6.
（試験例２２）
ショ糖の代わりにデンプン５部を用いたこと以外は、試験例２１と同様にして、水溶液を調製し、それをポリプロピレン板（厚さ１ｍｍ）に塗布・乾燥して難燃性能を評価した。
得られた結果を表５および６にまとめて示す。
(Test Example 22)
Except that 5 parts of starch was used instead of sucrose, an aqueous solution was prepared in the same manner as in Test Example 21, and applied to a polypropylene plate (thickness 1 mm) and dried to evaluate flame retardancy.
The results obtained are summarized in Tables 5 and 6.
（試験例２３）
水ガラス（Ｎａ2Ｏ濃度：９．３３重量％、ＳｉＯ2濃度：２８．８６重量％、モル比Ｎａ2Ｏ／ＳｉＯ2：３．１９、冨士化学株式会社製、品種：３号）８０部および水２０部を含む水ガラス水溶液を用いたこと以外は、試験例１と同様にして、ショ糖を添加・溶解させて水溶液を調製し、それを硬質ウレタンフォームに塗布・乾燥して難燃性能を評価した。
得られた結果を表５および６にまとめて示す。
(Test Example 23)
80 parts of water glass (Na 2 O concentration: 9.33% by weight, SiO 2 concentration: 28.86% by weight, molar ratio Na 2 O / SiO 2 : 3.19, manufactured by Fuji Chemical Co., Ltd., variety: No. 3) Except that a water glass aqueous solution containing 20 parts of water and water was used, an aqueous solution was prepared by adding and dissolving sucrose in the same manner as in Test Example 1, and applied to a rigid urethane foam and dried to make it flame retardant. Performance was evaluated.
The results obtained are summarized in Tables 5 and 6.
（試験例２４）
ショ糖の代わりにデンプン５部を用いたこと以外は、試験例２３と同様にして、水溶液を調製し、それをポリプロピレン板（厚さ１ｍｍ）に塗布・乾燥して難燃性能を評価した。
得られた結果を表５および６にまとめて示す。
(Test Example 24)
Except for using 5 parts of starch instead of sucrose, an aqueous solution was prepared in the same manner as in Test Example 23, and applied to a polypropylene plate (thickness 1 mm) and dried to evaluate flame retardancy.
The results obtained are summarized in Tables 5 and 6.
（試験例２５）
水ガラス（Ｎａ2Ｏ濃度：９．９重量％、ＳｉＯ2濃度：３０．２１重量％、モル比Ｎａ2Ｏ／ＳｉＯ2：３．１５、冨士化学株式会社製、品種：３号）８０部、水２０部およびデンプン５部を含む水溶液を用いたこと、ならびに硬質ウレタンフォームの代わりにポリプロピレン板（厚さ１ｍｍ）を用いたこと以外は、試験例１と同様にして、難燃性能を評価した。
得られた結果を表５および６にまとめて示す。
(Test Example 25)
80 parts of water glass (Na 2 O concentration: 9.9 wt%, SiO 2 concentration: 30.21 wt%, molar ratio Na 2 O / SiO 2 : 3.15, manufactured by Fuji Chemical Co., Ltd., variety: No. 3) The flame retardant performance was evaluated in the same manner as in Test Example 1 except that an aqueous solution containing 20 parts of water and 5 parts of starch was used, and a polypropylene plate (thickness 1 mm) was used instead of the rigid urethane foam. did.
The results obtained are summarized in Tables 5 and 6.
（試験例２６）
水ガラス（Ｎａ2Ｏ濃度：７．５重量％、ＳｉＯ2濃度：２４．５重量％、モル比Ｎａ2Ｏ／ＳｉＯ2：３．３７、冨士化学株式会社製、品種：特３号）１００部およびデンプン５部を含む水溶液を用いたこと、ならびに硬質ウレタンフォームの代わりにポリプロピレン板（厚さ１ｍｍ）を用いたこと以外は、試験例１と同様にして、難燃性能を評価した。
得られた結果を表５および６にまとめて示す。
(Test Example 26)
Water glass (Na 2 O concentration: 7.5% by weight, SiO 2 concentration: 24.5% by weight, molar ratio Na 2 O / SiO 2 : 3.37, manufactured by Fuji Chemical Co., Ltd., variety: No. 3) 100 The flame retardant performance was evaluated in the same manner as in Test Example 1, except that an aqueous solution containing 5 parts of starch and 5 parts of starch was used, and a polypropylene plate (thickness 1 mm) was used instead of the rigid urethane foam.
The results obtained are summarized in Tables 5 and 6.
（試験例２７）
水ガラス（Ｎａ2Ｏ濃度：５．８重量％、ＳｉＯ2濃度：２２．５重量％、モル比Ｎａ2Ｏ／ＳｉＯ2：４、冨士化学株式会社製、品種：特３号）１００部およびデンプン５部を含む水溶液を用いたこと、ならびに硬質ウレタンフォームの代わりにポリプロピレン板（厚さ１ｍｍ）を用いたこと以外は、試験例１と同様にして、難燃性能を評価した。
得られた結果を表５および６にまとめて示す。
(Test Example 27)
100 parts of water glass (Na 2 O concentration: 5.8 wt%, SiO 2 concentration: 22.5 wt%, molar ratio Na 2 O / SiO 2 : 4, manufactured by Fuji Chemical Co., Ltd., variety: No. 3) and Flame retardancy was evaluated in the same manner as in Test Example 1 except that an aqueous solution containing 5 parts of starch was used and a polypropylene plate (thickness 1 mm) was used instead of the rigid urethane foam.
The results obtained are summarized in Tables 5 and 6.
（試験例２８）
試験例１９で用いた水ガラス（Ｎａ2Ｏ濃度：１７．７３重量％、ＳｉＯ2濃度：３５．５８重量％、モル比Ｎａ2Ｏ／ＳｉＯ2：２．１３、冨士化学株式会社製、品種：１号５９°）２００ｋｇを、次の条件でスプレードライ法により蒸発乾固（粒体化）した。
装置：日本化学機械製造株式会社製
ノズル径：０．８４ｍｍ
スワール：ＳＣ
噴霧圧力：１２０ｋｇｆ／ｃｍ2（１２ＭＰａ）
噴霧量：約１００Ｌ／ｈ
熱風量：４０Ｎｍ3／ｍｉｎ．
熱風温度：１６０℃
排風温度：７９．６〜８４．１℃（コーン部）
７５．１〜８０．７℃（サイクロン部）
(Test Example 28)
Water glass used in Test Example 19 (Na 2 O concentration: 17.73 wt%, SiO 2 concentration: 35.58 wt%, molar ratio Na 2 O / SiO 2 : 2.13, manufactured by Fuji Chemical Co., Ltd., variety 1: 59 °) 200 kg was evaporated to dryness (granulated) by the spray drying method under the following conditions.
Apparatus: Nippon Chemical Machinery Manufacturing Co., Ltd. Nozzle diameter: 0.84 mm
Swirl: SC
Spray pressure: 120 kgf / cm 2 (12 MPa)
Spray amount: about 100 L / h
Hot air volume: 40 Nm 3 / min.
Hot air temperature: 160 ° C
Exhaust air temperature: 79.6-84.1 ° C. (cone part)
75.1-80.7 ° C (Cyclone part)
次の物性値を有するきれいな球形の粒子が得られた（パウダー回収量１０３ｋｇ）。
水分量：７％（３００℃×１時間の乾燥減量値）
粒度：１０〜３０μｍ（電子顕微鏡写真より計測）
平均粒径：１４．３μｍ
嵩比重：０．９３（さわり比重）
０．７２（みかけ比重）
このように、本発明のケイ素化合物の水溶液を公知の方法により蒸発乾固（粒体化）することができた。
Clean spherical particles having the following physical property values were obtained (powder recovery amount: 103 kg).
Water content: 7% (300 ° C x 1 hour loss on drying)
Particle size: 10-30 μm (measured from electron micrograph)
Average particle size: 14.3 μm
Bulk specific gravity: 0.93 (touch specific gravity)
0.72 (apparent specific gravity)
Thus, the aqueous solution of the silicon compound of the present invention could be evaporated and dried (granulated) by a known method.
得られた粉末１２部およびデンプン３部を、加熱溶融した低密度ポリエチレン樹脂（住友化学社製、以下同様）１００部に配合して、溶融混練により配合物を均一に分散させた。次いで、押出成型機（Ｈｉｔｚ日立造船製）を用いて、得られた混練物を厚さ１ｍｍの板状に成形し、ポリエチレン板の試験体を得て、試験例１と同様にして難燃性能を評価した。
得られた結果を表７および８にまとめて示す。
12 parts of the obtained powder and 3 parts of starch were blended into 100 parts of a heat-melted low-density polyethylene resin (manufactured by Sumitomo Chemical Co., Ltd., hereinafter the same), and the blend was uniformly dispersed by melt kneading. Next, using an extrusion molding machine (manufactured by Hitz Hitachi Zosen), the obtained kneaded material was formed into a 1 mm thick plate to obtain a test piece of a polyethylene plate. Evaluated.
The results obtained are summarized in Tables 7 and 8.
（試験例２９）
低密度ポリエチレン樹脂の代わりにポリプロピレン樹脂（住友化学社製、以下同様）を用いたこと以外は、試験例２８と同様にして、ポリプロピレン板の試験体の難燃性能を評価した。
得られた結果を表７および８にまとめて示す。
(Test Example 29)
The flame retardant performance of the test specimen of the polypropylene plate was evaluated in the same manner as in Test Example 28 except that a polypropylene resin (manufactured by Sumitomo Chemical Co., Ltd., the same applies below) was used instead of the low density polyethylene resin.
The results obtained are summarized in Tables 7 and 8.
（試験例３０）
水ガラスの粉末１８部およびデンプン５部を用いたこと以外は、試験例２８と同様にして、ポリエチレン板の試験体の難燃性能を評価した。
得られた結果を表７および８にまとめて示す。
(Test Example 30)
Except that 18 parts of water glass powder and 5 parts of starch were used, the flame retardancy performance of the polyethylene plate specimen was evaluated in the same manner as in Test Example 28.
The results obtained are summarized in Tables 7 and 8.
（試験例３１）
低密度ポリエチレン樹脂の代わりにポリプロピレン樹脂を用いたこと以外は、試験例３０と同様にして、ポリプロピレン板の試験体の難燃性能を評価した。
得られた結果を表７および８にまとめて示す。
(Test Example 31)
The flame retardant performance of the test specimen of the polypropylene plate was evaluated in the same manner as in Test Example 30, except that a polypropylene resin was used instead of the low density polyethylene resin.
The results obtained are summarized in Tables 7 and 8.
Claims (10)
前記難燃組成物が水溶液、水性懸濁液およびコロイド溶液から選択される液状の難燃組成物でありかつ前記難燃化対象材料が木材、紙、織布、不織布および樹脂から選択される材料であるとき、該液状の難燃組成物を該材料に塗布または含浸させること、
前記難燃組成物が粉末状の難燃組成物でありかつ前記難燃化対象材料が樹脂であるとき、該粉末状の難燃組成物を該樹脂に添加し溶融混練すること、または
前記難燃化対象材料が樹脂であるとき、前記難燃組成物の粉末状の構成成分を該樹脂に個別に添加して溶融混練すること
からなる請求項６または７に記載の難燃化処理方法。 The process is
The flame retardant composition is a liquid flame retardant composition selected from an aqueous solution, an aqueous suspension and a colloidal solution, and the material to be flame retardant is selected from wood, paper, woven fabric, nonwoven fabric and resin. When the material is applied or impregnated with the liquid flame retardant composition,
When the flame retardant composition is a powdered flame retardant composition and the flame retardant material is a resin, the powdered flame retardant composition is added to the resin and melt-kneaded, or The flame retardant treatment method according to claim 6 or 7, wherein when the material to be combusted is a resin, powdery components of the flame retardant composition are individually added to the resin and melt-kneaded.
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