JPH03124792A - Flame retarder for cellulosic material - Google Patents
Flame retarder for cellulosic materialInfo
- Publication number
- JPH03124792A JPH03124792A JP26370789A JP26370789A JPH03124792A JP H03124792 A JPH03124792 A JP H03124792A JP 26370789 A JP26370789 A JP 26370789A JP 26370789 A JP26370789 A JP 26370789A JP H03124792 A JPH03124792 A JP H03124792A
- Authority
- JP
- Japan
- Prior art keywords
- water
- flame retardant
- weight
- aqueous solution
- metal salt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 41
- 239000003063 flame retardant Substances 0.000 claims abstract description 47
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 26
- 150000003839 salts Chemical class 0.000 claims abstract description 26
- 229920005989 resin Polymers 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 25
- MBHRHUJRKGNOKX-UHFFFAOYSA-N [(4,6-diamino-1,3,5-triazin-2-yl)amino]methanol Chemical compound NC1=NC(N)=NC(NCO)=N1 MBHRHUJRKGNOKX-UHFFFAOYSA-N 0.000 claims abstract description 11
- VGGLHLAESQEWCR-UHFFFAOYSA-N N-(hydroxymethyl)urea Chemical compound NC(=O)NCO VGGLHLAESQEWCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 4
- 229920002678 cellulose Polymers 0.000 claims description 22
- 239000001913 cellulose Substances 0.000 claims description 22
- -1 alkali metal sulfamates Chemical class 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 17
- 239000000243 solution Substances 0.000 abstract description 12
- 239000007787 solid Substances 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 4
- 150000001340 alkali metals Chemical class 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract 3
- 150000001342 alkaline earth metals Chemical class 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 15
- YZVJHCGMTYDKFR-UHFFFAOYSA-L magnesium;disulfamate Chemical compound [Mg+2].NS([O-])(=O)=O.NS([O-])(=O)=O YZVJHCGMTYDKFR-UHFFFAOYSA-L 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 6
- 229920000877 Melamine resin Polymers 0.000 description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- NLXYLZCLIHHPMA-UHFFFAOYSA-K aluminum;trisulfamate Chemical compound [Al+3].NS([O-])(=O)=O.NS([O-])(=O)=O.NS([O-])(=O)=O NLXYLZCLIHHPMA-UHFFFAOYSA-K 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 159000000003 magnesium salts Chemical class 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- GEHMBYLTCISYNY-UHFFFAOYSA-N Ammonium sulfamate Chemical compound [NH4+].NS([O-])(=O)=O GEHMBYLTCISYNY-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 159000000009 barium salts Chemical class 0.000 description 1
- RSIPQRDGPVEGLE-UHFFFAOYSA-L calcium;disulfamate Chemical compound [Ca+2].NS([O-])(=O)=O.NS([O-])(=O)=O RSIPQRDGPVEGLE-UHFFFAOYSA-L 0.000 description 1
- LNEUSAPFBRDCPM-UHFFFAOYSA-N carbamimidoylazanium;sulfamate Chemical compound NC(N)=N.NS(O)(=O)=O LNEUSAPFBRDCPM-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000011120 plywood Substances 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical class NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 description 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical class NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Fireproofing Substances (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Paper (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は、セルロース系材料のための難燃剤に関する０
本発明にょる難燃剤は、難燃性化粧板用の含浸紙、壁紙
、障子紙等の紙材、木質合板類、木材、セルロース系繊
維等を主としたセルロース系材料の防炎処理に用いられ
る。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to flame retardants for cellulosic materials.
The flame retardant according to the present invention can be used for flame-retardant treatment of cellulose-based materials such as impregnated paper for flame-retardant decorative boards, wallpaper, paper materials such as shoji paper, wood plywood, wood, cellulose fibers, etc. It will be done.
〈従来の技術〉
特開昭６２−１２９３８２に記載されているスルファミ
ン酸マグネシウムをセルロース系材料に含浸処理するこ
とにより得られたセルロース系材料は、難燃性能のつい
てはすばらしい効果を示すが、耐水性９寸法安定性等に
乏しい。<Prior art> Cellulose-based materials obtained by impregnating cellulose-based materials with magnesium sulfamate described in JP-A No. 62-129382 exhibit excellent flame retardant properties, but have poor water resistance. 9 Poor dimensional stability etc.
特公昭６Ｊ−３９６３４に記載されているスルファミン
酸アルミニウムとメチロールメラミンを組み合せた難燃
剤は、これをつくるのに加熱が必要であり、また、得ら
れた液の常温安定性（可使時間）が短＜、難燃化性能が
不十分である。The flame retardant that is a combination of aluminum sulfamate and methylolmelamine described in Japanese Patent Publication No. 6J-39634 requires heating to produce, and the room temperature stability (pot life) of the resulting liquid is limited. Short <, flame retardant performance is insufficient.
スルファミン酸グアニジン、スルファミン酸アンモニウ
ム等は一般に使われているが、これらも、耐熱性に乏し
く、これらが含浸されたセルロース系材料は、加熱時に
着色を起し易く、難燃化性能も充分なものではない。Guanidine sulfamate, ammonium sulfamate, etc. are commonly used, but these also have poor heat resistance, and cellulose materials impregnated with these tend to become discolored when heated, and flame retardant performance is insufficient. isn't it.
〈発明が解決しようとする課題〉
本発明は、これらの問題を総合的に改良したものであり
、難燃剤溶液が安定であって、かつ含浸しやすく、また
その含浸によって得られたセルロース材料が、優れた難
燃性９寸法安定性、及び耐水性等を示す難燃剤組成物を
提供するものである。<Problems to be Solved by the Invention> The present invention comprehensively improves these problems by providing a flame retardant solution that is stable and easy to impregnate, and a cellulose material obtained by the impregnation. The present invention provides a flame retardant composition exhibiting excellent flame retardancy, dimensional stability, water resistance, and the like.
〈課題を解決するための手段〉
本発明によるセルロース系材料のための難燃剤は、メグ
・ロールメラミン及びメチロール尿素からなる群から選
ばれる１種又は２種以上の水溶性の樹脂と、アルカリ金
属スルファミン酸塩、アルカリ土類金属スルファミン酸
塩及びこれらのメチロール化合物からなる群から選ばれ
る１種又は２種以上の水溶性の金属塩とを、上記樹脂１
００重量部に対し上記金属塩１０〜２００重量部の比率
−に、そしてこれら樹脂と金属塩の合計として１５〜７
５重量％の濃度に含有する水溶液である。<Means for Solving the Problems> The flame retardant for cellulosic materials according to the present invention comprises one or more water-soluble resins selected from the group consisting of meg-roll melamine and methylol urea, and an alkali metal. One or more water-soluble metal salts selected from the group consisting of sulfamates, alkaline earth metal sulfamates, and methylol compounds thereof are added to the resin 1.
00 parts by weight to 10 to 200 parts by weight of the above metal salt, and the total amount of these resins and metal salts is 15 to 7 parts by weight.
It is an aqueous solution containing 5% by weight.
更に本発明によれば、この難燃剤水溶液を、セルロース
系材料の１００重量部に対し上記難燃剤水溶液中の金属
塩として１０〜１００重量部の比率となるようにセルロ
ース系材料に含浸させた後加熱乾燥することによって、
難燃化されたセルロース系材料が得られる。Further, according to the present invention, after impregnating the cellulosic material with this flame retardant aqueous solution at a ratio of 10 to 100 parts by weight as the metal salt in the flame retardant aqueous solution to 100 parts by weight of the cellulosic material, By heating and drying,
A flame-retardant cellulosic material is obtained.
本発明に用いられるメチロールメラミン、メチロール尿
素等の水溶性樹脂は、通常の方法、例えば、アルカリ性
の水性媒体中でメラミン、尿素をホルムアルデヒド、例
えば、ホルマリンと反応させることにより容易に得られ
る。場合によっては市販品を用いてもよい。The water-soluble resins such as methylolmelamine and methylolurea used in the present invention can be easily obtained by a conventional method, for example, by reacting melamine or urea with formaldehyde, such as formalin, in an alkaline aqueous medium. In some cases, commercially available products may be used.
メチロールメラミンとしては、メラミン１モルに対しメ
チロール基が１〜６モル付加したものが用いられる。ま
た、メチロール尿素とじては、尿素１モルに対し１〜２
モル付加したものが用いられる。これらメチロールメラ
ミンとメチロール尿素の混合物も用いることができる。As the methylol melamine, one in which 1 to 6 moles of methylol groups are added to 1 mole of melamine is used. In addition, for methylol urea, 1 to 2
A molar addition is used. A mixture of these methylolmelamine and methylolurea can also be used.
本発明に用いられる水溶性のアルカリ金属スルファミン
酸塩、アルカリ土類金属スルファミン酸塩等の好ましい
例としては、スルファミン酸のリチウム塩、ナトリウム
塩、カリウム塩、マグネシウム塩、カルシウム塩、バリ
ウム塩等が挙げられる。特に、マグネシウム塩、カルシ
ウム塩等が好ましい、これらスルファミン酸の金属塩の
メチロール化物は、通常の方法、例えば、上記スルファ
ミン酸の金属塩とホルマリンとを水中で反応させること
により、容易に得ることができる。これらメチロール化
物は、スルファミン酸塩のアミノ基１箇にホルムアルデ
ヒドが１又は２個付加した形態のものとして用いられる
。特に好ましいメチロール化物としては、１モルのスル
ファミン酸マグネシウム、スルファミン酸カルシウム等
に１〜４モルのホルムアルデヒドが付加したものが挙げ
られる。Preferred examples of water-soluble alkali metal sulfamates, alkaline earth metal sulfamates, etc. used in the present invention include lithium salts, sodium salts, potassium salts, magnesium salts, calcium salts, barium salts, etc. of sulfamic acid. Can be mentioned. In particular, methylolated products of metal salts of sulfamic acid, preferably magnesium salts, calcium salts, etc., can be easily obtained by conventional methods, for example, by reacting the metal salts of sulfamic acid and formalin in water. can. These methylol compounds are used in the form of a sulfamate having one or two formaldehyde added to one amino group. Particularly preferred methylol compounds include those obtained by adding 1 to 4 moles of formaldehyde to 1 mole of magnesium sulfamate, calcium sulfamate, or the like.
本発明の難燃剤水溶液は、上記水溶性の樹脂と水溶性の
金属塩とを水に溶解させることにより、或いはこれら成
分の水溶性を混合することにより、或いは更に、いずれ
か一方の成分の水溶液に他方の成分の固体を溶解させる
ことにより容易に得られる。The flame retardant aqueous solution of the present invention can be prepared by dissolving the above-mentioned water-soluble resin and water-soluble metal salt in water, or by mixing the water-solubility of these components, or by further preparing an aqueous solution of either one of the components. It can be easily obtained by dissolving the solid of the other component in .
本発明による好ましい難燃剤水溶液は、上記水溶性の樹
脂１００重量部に対し上記水溶性の金属塩１０〜２００
重量部の比率にこれら両成分を含有し、更にこれら両成
分を、固形分として１５〜７５重量％の濃度に含有する
。この水溶液としては、ｐＨ６〜８程度が好ましい。A preferable flame retardant aqueous solution according to the present invention contains 10 to 200 parts of the above water-soluble metal salt per 100 parts by weight of the above water-soluble resin.
These two components are contained in a ratio of parts by weight, and further, these two components are contained in a concentration of 15 to 75% by weight as solid content. This aqueous solution preferably has a pH of about 6 to 8.
本発明により、セルロース系材料を難燃化させることは
、セルロース系材料に、この難燃剤水溶液を、通常の寸
法、例えば、スプレー、塗布等により付着させたり、或
いは、加圧、減圧又は常圧下この水溶液中にセルロース
系材料を浸漬した後取り出し、そしてこれら難燃剤水溶
液が付着したセルロース系材料を乾燥することによって
容易に行うことができる。セルロース系材料に含有させ
る樹脂と金属塩の量は、この難燃剤水溶液のこれら両成
分の濃度を調節することにより、或いはこの水溶液の付
着量、含浸量等を調節することによって容易に調節する
ことができる。乾燥は、セルロース系材料の変質温度以
下、好ましくは常温〜１７０°Ｃ１特に好ましくは、
１００〜１５０°Ｃ近辺の温度で行うのがよい。According to the present invention, making a cellulosic material flame retardant can be achieved by attaching the flame retardant aqueous solution to the cellulosic material in a conventional manner, for example, by spraying, coating, etc., or by applying the flame retardant solution to the cellulosic material by applying it under pressure, reduced pressure, or normal pressure. This can be easily carried out by immersing the cellulose material in this aqueous solution, taking it out, and drying the cellulose material to which the flame retardant aqueous solution has adhered. The amounts of resin and metal salt contained in the cellulosic material can be easily adjusted by adjusting the concentrations of these two components in this aqueous flame retardant solution, or by adjusting the amount of adhesion, amount of impregnation, etc. of this aqueous solution. I can do it. The drying is carried out at a temperature below the deterioration temperature of the cellulosic material, preferably from room temperature to 170°C, particularly preferably,
It is preferable to carry out the process at a temperature around 100 to 150°C.
く作 用〉
スルファミン酸の金属塩、これらのメチロール化物等は
、燃焼時の加熱によりセルロース分子を炭素と水に分解
し、燃焼を防止する脱水作用をもっている。Effect> Metal salts of sulfamic acid, methylolated products, etc. of these have a dehydrating effect that decomposes cellulose molecules into carbon and water by heating during combustion and prevents combustion.
本発明の難燃剤水溶液の優れた安定性は、この液中に溶
解している金属塩の金属イオンが１価又は２価であって
、これにより溶解成分の三次元構造への変質が起りにく
いためであると考えられる。また、この水滴液のｐＨが
中性付近に調節されていることも、メチロールメラミン
、メチロール尿素等の三次元構造体への変質を起りに＜
＜シていると考えられる。The excellent stability of the flame retardant aqueous solution of the present invention is due to the fact that the metal ions of the metal salt dissolved in this solution are monovalent or divalent, which makes it difficult for the dissolved components to change into a three-dimensional structure. This is thought to be due to the In addition, the pH of this water droplet liquid is adjusted to around neutrality, which may cause deterioration into three-dimensional structures such as methylolmelamine and methylolurea.
<It is thought that
難燃剤水溶液に含有される水溶性金属塩の量が、水溶性
樹脂１００重量部に対し１０重量部以下では、高い難燃
性能を示す難燃剤水溶液が得られない０反対に２００重
量部以上にも多いと、安定性の高い難燃剤水溶液が得ら
れず、更に樹脂成分の相対比率が低下し、このような難
燃剤水溶液で処理されたセルロース系材料は耐水性に乏
しくなる。If the amount of the water-soluble metal salt contained in the flame retardant aqueous solution is less than 10 parts by weight per 100 parts by weight of the water-soluble resin, an aqueous flame retardant solution that exhibits high flame retardant performance cannot be obtained. If the flame retardant aqueous solution is too large, a highly stable aqueous flame retardant solution cannot be obtained, and the relative ratio of the resin components decreases, resulting in a cellulosic material treated with such an aqueous flame retardant solution having poor water resistance.
また、難燃剤水溶液中の樹脂と金属塩の合計濃度、即ち
固形分濃度が１５重量％以下のときにも、その水溶液は
安定性に乏しい０反対にこの固形分濃度芝７５重量％以
上にも高いと、その水溶液は透明性を失い、均一性に乏
しくなる。特に、この固形分濃度が１０重量％以下では
、セルロース系材料を難燃剤水溶液で処理する際、セル
ロース系材料を充分に難燃化せしめる量の固形分をセル
ロース系材料に含有させ難い。In addition, even when the total concentration of resin and metal salt in the flame retardant aqueous solution, that is, the solid content concentration, is less than 15% by weight, the aqueous solution has poor stability.On the contrary, even when the solid content concentration exceeds 75% by weight, the aqueous solution has poor stability. If it is high, the aqueous solution loses its transparency and becomes less homogeneous. In particular, if the solid content concentration is 10% by weight or less, when the cellulose material is treated with an aqueous flame retardant solution, it is difficult to make the cellulose material contain an amount of solid content that will sufficiently make the cellulose material flame retardant.
セルロース系材料を充分に難燃化せしめるには、セルロ
ース系材料１００重量部に対し難燃剤水溶液の金属塩成
分が１０〜１００重量部となるよう、また、樹脂成分は
５重量部以上５００重量部以下となるように、セルロー
ス系材料に含有させるのがよい、特に、樹脂成分の比率
として５重量部より少ないと、耐水性の高い難燃化セル
ロース系材料が得られない。In order to make the cellulose material sufficiently flame retardant, the metal salt component of the flame retardant aqueous solution should be 10 to 100 parts by weight per 100 parts by weight of the cellulose material, and the resin component should be 5 parts by weight or more and 500 parts by weight. It is preferable to include it in the cellulose-based material as shown below. In particular, if the proportion of the resin component is less than 5 parts by weight, a flame-retardant cellulose-based material with high water resistance cannot be obtained.
セルロース系材料に難燃剤水溶液を含浸させた後に行わ
れる乾燥の際、加熱を施すことにより、この難燃剤水溶
液に含まれていた樹脂成分に硬化を起こさせることがで
きる。この硬化反応は高温程迅速に進むが、セルロース
系材料の分解が起る如き高温は避けた方がよく、通常１
３０〜１５０℃位の温度が特に好ましい。When drying is performed after impregnating a cellulose-based material with an aqueous flame retardant solution, the resin component contained in the aqueous flame retardant solution can be cured by applying heat. This curing reaction proceeds more quickly at higher temperatures, but it is best to avoid high temperatures that would cause decomposition of cellulosic materials.
A temperature of about 30 to 150°C is particularly preferred.
〈実施例〉
セルロース系材料として、化学実験用１紙Ｎｏ、 ２を
用意した。<Example> Chemical experiment paper No. 1 and No. 2 were prepared as cellulose-based materials.
樹脂成分としては、メラミン１モルに対しホルムアルデ
ヒド１．７モルの比率に、水中でメラミンとホルマリン
とを反応させることにより得られた固形分濃度６０重量
％のメチロールメラミンの水溶液を用意した。As the resin component, an aqueous solution of methylolmelamine with a solid content concentration of 60% by weight, obtained by reacting melamine and formalin in water, was prepared at a ratio of 1.7 moles of formaldehyde to 1 mole of melamine.
金属塩成分としては、スルファミン酸マグネシウム（ｓ
ｕＡ−Ｍｇ）の５０重量％水溶液と、比較例に用いるた
めのスルファミン酸アルミニウム（ＳＭＡ−Ａｌ）の４
０重量％水溶液とを用意した。更に、スルファミン酸マ
グネシウムのメチロール化物としてモノメチロール化ス
ルファミン酸マグネシウム（Ｍ−ＳＭＡ−Ｍｇ）の５０
重量％水溶液を用意した。As a metal salt component, magnesium sulfamate (s
uA-Mg) and 4% of aluminum sulfamate (SMA-Al) for use in comparative examples.
A 0% by weight aqueous solution was prepared. Furthermore, 50% of monomethylolated magnesium sulfamate (M-SMA-Mg) was used as a methylolated magnesium sulfamate.
A wt% aqueous solution was prepared.
実施例１及び比較例１
上記用意された樹脂成分と金属塩成分とを、これら水溶
液の重量比率として第１表記載の比率に混合した後、安
定性のテストとして２０”Ｃで静置を続け、混合した水
溶液に白濁が現れる迄の時間を測定したところ、第１表
記載の結果が得られた。Example 1 and Comparative Example 1 After mixing the resin component and metal salt component prepared above in the weight ratio of these aqueous solutions as shown in Table 1, the mixture was left standing at 20"C as a stability test. The time required for the mixed aqueous solution to become cloudy was measured, and the results shown in Table 1 were obtained.
第１表
１００ １００ − −
２４１００ ５０ −
− ７２１００ ２０
− −２４０１００−１００−９６
１００−５０１６８
１００−１０２０
上記の結果は、メチロールメラミンとスルファミン酸ア
ルミニウムを含有する水溶液は安定性に乏しいが、本発
明によるメチロールメラミンとスルファミン酸マグネシ
ウム又はモノメチロール化スルファミン酸マグネシウム
を含有する水溶液は安定性が高いことを示している。Table 1 100 100 - -
24100 50 -
-72100 20
- -240100-100-96 100-50168 100-1020 The above results show that although the aqueous solution containing methylolmelamine and aluminum sulfamate is poor in stability, methylolmelamine and magnesium sulfamate or monomethylolated sulfamic acid according to the present invention Aqueous solutions containing magnesium have been shown to be highly stable.
実施例２及び比較例２
実施例１で得られた難燃剤水溶液Ａ、Ｂ、Ｃ及び比較例
のためのスルファミン酸マグネシウム単独５０重量％の
水溶液を用い、前記用意された１紙をこれら水溶液に浸
漬した後取り出し、余剰液を除いた後、１５０℃で５分
乾燥することにより、第２表記載の金属塩成分含有率の
１紙を得た。但し、スルファミン酸マグネシウム単独の
水溶液を用いた比較例では、常温で乾燥が行われた。Example 2 and Comparative Example 2 Using the flame retardant aqueous solutions A, B, and C obtained in Example 1 and a 50% by weight aqueous solution of magnesium sulfamate alone for the comparative example, the prepared piece of paper was immersed in these aqueous solutions. After immersion, the sample was taken out, excess liquid was removed, and the sample was dried at 150° C. for 5 minutes to obtain a paper having the metal salt component content listed in Table 2. However, in a comparative example using an aqueous solution of magnesium sulfamate alone, drying was performed at room temperature.
次いで、この含浸処理された１紙について、難燃性のテ
ストと耐水性のテストを行った。難燃性テストでは、１
紙に炎を１０秒接触させた後、炎を離し、自己消火性を
示したときを良好と、また、少しでも燃焼が続いたとき
を不良と判淀した。Next, this impregnated paper was subjected to a flame retardancy test and a water resistance test. In the flame retardant test, 1
After the flame was brought into contact with the paper for 10 seconds, the flame was removed and the paper was judged to be good if it exhibited self-extinguishing properties, and bad if combustion continued for even a short time.
耐水性のテストでは、２３℃、相対湿度８０％の室内に
２４時間放置したときの重量増加率を求め、吸湿率とし
で表わした。第２表にこれらテスト結果を示す。In the water resistance test, the weight increase rate when the sample was left in a room at 23° C. and 80% relative humidity for 24 hours was determined and expressed as the moisture absorption rate. Table 2 shows the results of these tests.
Ａ ２８
Ｂ １７
８
（比較例）
第２表
良好 １０
良好 ５
不良
０
ロール尿素の水溶性樹脂の水溶液と、水溶性のスルファ
ミン酸金属塩又はそのメチロール化物、或いはその水溶
液とを好ましい比率に、そして好ましい濃度になるよう
に混合するのみで、セルロース系材料に難燃化を施すた
めの安定性のよい難燃剤水溶液が得られる。A 28 B 17 8 (Comparative example) Table 2 Good 10 Good 5 Bad 0 An aqueous solution of a water-soluble resin of rolled urea and a water-soluble sulfamic acid metal salt or its methylol compound, or its aqueous solution in a preferred ratio, and A highly stable flame retardant aqueous solution for imparting flame retardancy to cellulosic materials can be obtained by simply mixing the two to achieve a desired concentration.
そして、この難燃剤水溶液をセルロース系材料に含浸さ
せた後、加熱乾燥させることにより、耐水性と難燃性に
優れるセルロース系材料が得られる。Then, by impregnating a cellulose material with this flame retardant aqueous solution and then heating and drying it, a cellulose material having excellent water resistance and flame retardancy can be obtained.
上記の結果は、比較例のスルファミン酸マグネシウム単
独の水溶液では、得られたセルロース系材料の耐水性が
乏しいが、本発明の難燃剤水溶液はセルロース系材料に
良好な難燃性を付与し、そしてこの難燃化させたセルロ
ース系材料は吸湿率が小さく、良好な耐水性を有するこ
とを示している。The above results demonstrate that the aqueous solution of magnesium sulfamate alone in the comparative example resulted in poor water resistance of the resulting cellulosic material, but the flame retardant aqueous solution of the present invention imparted good flame retardancy to the cellulosic material. This flame-retardant cellulosic material has a low moisture absorption rate, indicating that it has good water resistance.
〈発明の効果〉<Effect of the invention>
Claims (2)
群から選ばれる１種又は２種以上の水溶性の樹脂と、ア
ルカリ金属スルファミン酸塩、アルカリ土類金属スルフ
ァミン酸塩及びこれらのメチロール化合物からなる群か
ら選ばれる１種又は２種以上の水溶性の金属塩とを、上
記樹脂１００重量部に対し上記金属塩１０〜２００重量
部の比率に、そしてこれら樹脂と金属塩の合計として１
５〜７５重量％の濃度に含有するセルロース系材料のた
めの難燃剤水溶液。(1) One or more water-soluble resins selected from the group consisting of methylolmelamine and methylolurea, and one or more water-soluble resins selected from the group consisting of alkali metal sulfamates, alkaline earth metal sulfamates, and methylol compounds thereof. and one or more water-soluble metal salts in a ratio of 10 to 200 parts by weight per 100 parts by weight of the resin, and the total amount of these resins and metal salts is 1.
Aqueous flame retardant solutions for cellulosic materials containing concentrations of 5 to 75% by weight.
ス系材料１００重量部に対し、この難燃剤水溶液中の金
属塩の量として１０〜１００重量部の比率となるように
含浸させた後、得られたセルロース系材料を加熱乾燥す
ることを特徴とするセルロース系材料の難燃化方法。(2) The aqueous flame retardant solution according to claim (1) is impregnated with 100 parts by weight of the cellulose material so that the amount of metal salt in the aqueous flame retardant solution is 10 to 100 parts by weight. A method for making a cellulose-based material flame retardant, the method comprising: heating and drying the obtained cellulose-based material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26370789A JP2829300B2 (en) | 1989-10-09 | 1989-10-09 | Flame retardant for cellulosic materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26370789A JP2829300B2 (en) | 1989-10-09 | 1989-10-09 | Flame retardant for cellulosic materials |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03124792A true JPH03124792A (en) | 1991-05-28 |
| JP2829300B2 JP2829300B2 (en) | 1998-11-25 |
Family
ID=17393207
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26370789A Expired - Lifetime JP2829300B2 (en) | 1989-10-09 | 1989-10-09 | Flame retardant for cellulosic materials |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2829300B2 (en) |
-
1989
- 1989-10-09 JP JP26370789A patent/JP2829300B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP2829300B2 (en) | 1998-11-25 |
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