JPH0686704B2 - Flame-retardant method for cellulose materials - Google Patents
Flame-retardant method for cellulose materialsInfo
- Publication number
- JPH0686704B2 JPH0686704B2 JP60136857A JP13685785A JPH0686704B2 JP H0686704 B2 JPH0686704 B2 JP H0686704B2 JP 60136857 A JP60136857 A JP 60136857A JP 13685785 A JP13685785 A JP 13685785A JP H0686704 B2 JPH0686704 B2 JP H0686704B2
- Authority
- JP
- Japan
- Prior art keywords
- flame
- ammonium chloride
- retardant
- cellulosic material
- water
- 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.)
- Expired - Lifetime
Links
- 239000003063 flame retardant Substances 0.000 title claims description 20
- 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 title claims description 19
- 239000000463 material Substances 0.000 title claims description 17
- 238000000034 method Methods 0.000 title claims description 12
- 229920002678 cellulose Polymers 0.000 title description 3
- 239000001913 cellulose Substances 0.000 title description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 44
- 235000019270 ammonium chloride Nutrition 0.000 claims description 22
- 239000000126 substance Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 230000000979 retarding effect Effects 0.000 claims 1
- 229920000742 Cotton Polymers 0.000 description 17
- 239000004744 fabric Substances 0.000 description 15
- 150000001408 amides Chemical class 0.000 description 12
- GKTNLYAAZKKMTQ-UHFFFAOYSA-N n-[bis(dimethylamino)phosphinimyl]-n-methylmethanamine Chemical compound CN(C)P(=N)(N(C)C)N(C)C GKTNLYAAZKKMTQ-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 125000004122 cyclic group Chemical group 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000013638 trimer Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910001510 metal chloride Inorganic materials 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000004114 Ammonium polyphosphate Substances 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000002862 amidating effect Effects 0.000 description 1
- 230000009435 amidation Effects 0.000 description 1
- 238000007112 amidation reaction Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 1
- 229920001276 ammonium polyphosphate Polymers 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 235000009120 camo Nutrition 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
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 239000011093 chipboard Substances 0.000 description 1
- 150000001804 chlorine Chemical class 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000011094 fiberboard Substances 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229920001477 hydrophilic polymer Polymers 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000011087 paperboard Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 1
- 239000011120 plywood Substances 0.000 description 1
- 229920002627 poly(phosphazenes) Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 229940086066 potassium hydrogencarbonate Drugs 0.000 description 1
- VLYFRFHWUBBLRR-UHFFFAOYSA-L potassium;sodium;carbonate Chemical compound [Na+].[K+].[O-]C([O-])=O VLYFRFHWUBBLRR-UHFFFAOYSA-L 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910000031 sodium sesquicarbonate Inorganic materials 0.000 description 1
- 235000018341 sodium sesquicarbonate Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- WCTAGTRAWPDFQO-UHFFFAOYSA-K trisodium;hydrogen carbonate;carbonate Chemical compound [Na+].[Na+].[Na+].OC([O-])=O.[O-]C([O-])=O WCTAGTRAWPDFQO-UHFFFAOYSA-K 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Description
【発明の詳細な説明】 産業上の利用分野 本発明は塩化アンモニウムを含有するアミドフォスファ
ゼンを利用して木綿、麻、レーヨン、木板、合板、パー
チクルボード、ファイバーボード、チップボード、木毛
板、紙、板紙等のセルロース系物質を難燃化加工する方
法に関するものである。TECHNICAL FIELD The present invention utilizes amidophosphazene containing ammonium chloride to make cotton, hemp, rayon, wood board, plywood, particle board, fiber board, chip board, wood board, The present invention relates to a method for flame-retarding a cellulosic material such as paper and paperboard.
従来の技術 従来は、セルロース系物質の難燃化加工方法としては、
ポリリン酸アンモニウム、スルファミン酸グアニジン、
ホウ酸、ホウ砂等の水溶性難燃性物質を含浸させた後、
乾燥することにより難燃化加工がされているが、これら
の物質は水溶性であるため洗濯による難燃性の低下が著
しい。Conventional Technology Conventionally, as a flame retardant processing method for cellulosic materials,
Ammonium polyphosphate, guanidine sulfamate,
After impregnating a water-soluble flame-retardant substance such as boric acid or borax,
Although flame-retarded by drying, these substances are water-soluble, and thus the flame-retardant property is significantly reduced by washing.
本発明に使用するアミドフォスファゼンは水溶性の物質
であるが、これを水溶液としてセルロース系物質に含浸
させた後、乾燥し、更に加熱処理することにより重縮合
して水に不溶性の難燃性ポリマーを形成し、また一部は
セルロース分子と結合して、対象としたセルロース系物
質に対して耐久性のある難燃性を付与することができる
ことが知られている（米国特許第2,782,133号明細書、
米国特許第2,782,133号明細書、米国特許第3,617,220号
明細書、特公昭47−45636号公報参照）。The amide phosphazene used in the present invention is a water-soluble substance, which is impregnated with a cellulosic substance as an aqueous solution, dried, and then subjected to heat treatment to cause polycondensation to cause water-insoluble flame retardancy. It is known that a hydrophilic polymer can be formed and, in part, it can be combined with cellulose molecules to impart durable flame retardancy to the targeted cellulosic material (US Pat. No. 2,782,133). Specification,
See US Pat. No. 2,782,133, US Pat. No. 3,617,220, and Japanese Patent Publication No. 47-45636).
発明が解決しようとする問題点 アミドフォスファゼンはクロロフォスファゼンとアンモ
ニアとの反応によって生成するが、それは副生する大量
の塩化アンモニウムとの混合物として得られる。Problems to be Solved by the Invention Amidophosphazene is produced by the reaction of chlorophosphazene with ammonia, which is obtained as a mixture with a large amount of by-produced ammonium chloride.
塩化アンモニウムが混在したままのアミドフォスファゼ
ンを用いて難燃化処理を行なうと、処理した繊維が黄色
に着色し、また熱処理工程において塩化アンモニウムが
解離して、発生する塩化水素がセルロース製品の強度を
低下させると共に設備を腐食する。更にまた昇華した塩
化アンモニウムあるいは解離した塩化水素とアンモニウ
ムが再結合して生成する塩化アンモニウムは、使用する
装置の排気部分に閉塞を生ずる恐れがある。したがって
アミドフォスファゼンをセルロース製品の難燃化処理の
ために使用するためには、その前提としてアミドフォス
ファゼンと塩化アンモニウムを分離することが必要であ
る。When flame-retardant treatment is performed using amide phosphazene with ammonium chloride mixed, the treated fiber is colored yellow, and ammonium chloride is dissociated during the heat treatment process, resulting in hydrogen chloride generation of cellulose products. It reduces strength and corrodes equipment. Furthermore, sublimated ammonium chloride or ammonium chloride formed by recombination of dissociated hydrogen chloride and ammonium may cause blockage in the exhaust portion of the apparatus used. Therefore, in order to use amide phosphazene for the flame-retardant treatment of cellulosic products, it is necessary to separate amide phosphazene and ammonium chloride.
アミドフォスファゼンと塩化アンモニウムは、種々の溶
媒に対する性質が似ており、特に水に対しては両者とも
極めて易溶性である。両者を分離する方法としては、両
者をアンモニア水に溶かし、アルコールを加えてアミド
フォスファゼンを析出させる方法〔ジャーナル・オブ・
ポリマー・サイエンス（J.Polym.Sci.）、Ａ部（Part
A）、第３巻、第3343頁〜第3351頁（1965年）〕が知ら
れているが、この方法を実施するためには大量のアルコ
ールを必要とするので経済的に有利でない。Amidophosphazene and ammonium chloride have similar properties to various solvents, and both are extremely easily soluble especially in water. As a method for separating both, a method of dissolving both in ammonia water and adding alcohol to precipitate amide phosphazene [Journal of
Polymer Science (J.Polym.Sci.), Part A (Part
A), Volume 3, pp. 3343 to 3351 (1965)] is known, but it is not economically advantageous because a large amount of alcohol is required to carry out this method.
そこで本発明は、経済的に分離することができないアミ
ドフォスファゼンと塩化アンモニウムとの混合物を使用
して、経済的に有利に、しかもセルロース系物質の品質
を低下させることなく、セルロース系物質を難燃化する
方法を提供しようとするものである。Therefore, the present invention uses a mixture of amidophosphazene and ammonium chloride, which cannot be separated economically, to produce a cellulosic material economically advantageous and without degrading the quality of the cellulosic material. It is intended to provide a flame retardant method.
問題点を解決するための手段 本発明は、アミドフォスファゼンと塩化アンモニウムと
アルカリ性物質との混合物の水溶液をセルロース系物質
に含浸させ、乾燥し、120℃ないし220℃の温度に10秒な
いし30分間加熱し、次いで水洗することを特徴とするセ
ルロース系物質の難燃化方法である。Means for Solving the Problems According to the present invention, a cellulosic material is impregnated with an aqueous solution of a mixture of amidophosphazene, ammonium chloride and an alkaline substance, dried, and heated to a temperature of 120 ° C. to 220 ° C. for 10 seconds to 30 seconds. A method for making a cellulosic material flame-retardant is characterized by heating for minutes and then washing with water.
アミドフォスファゼンと塩化アンモニウムとアルカリ性
物質との混合水溶液をそのまま、例えばセルロース繊維
に含浸させてもよいが、この溶液を減圧処理して、ある
いは加熱してアンモニアガスを充分に揮散させた後の溶
液で繊維を処理してもよい。この際、必要以上に長時間
加熱することは、アミドフォスファゼンの加水分解を招
くので好ましくない。A mixed aqueous solution of amide phosphazene, ammonium chloride, and an alkaline substance may be directly impregnated into, for example, cellulose fibers, but this solution is subjected to reduced pressure treatment or after heating to sufficiently vaporize ammonia gas. The fibers may be treated with the solution. At this time, heating for an unnecessarily long time causes hydrolysis of amide phosphazene, which is not preferable.
本発明の要素について以下に詳説する。The elements of the present invention are described in detail below.
（アミドフォスファゼン） 本発明に使用するアミドフォスファゼンは、式 (-N=PCl2-)n （上式においてｎは３以上の整数である） で表わされるクロロフォスファゼンオリゴマーとアンモ
ニアとを反応させ、クロロフォスファゼンオリゴマー中
の塩素原子を-NH2によって置換することによって得られ
る〔アンナーレン・デア・ヒエミー（Ann.Chem.）第12
巻、第169頁（1939年）、ケミカル・インダストリー（C
hem.Ind.）1959年第748頁および特開昭48−51899号公報
参照〕。この-NH2による置換は完全に行なわれることが
好ましいが、少量の未置換塩素が残留（原料クロロフォ
スファゼンに結合している塩素のおよそ1/3以下）して
も難燃化剤としての使用は可能である。(Amidophosphazene) Amidophosphazene used in the present invention includes a chlorophosphazene oligomer represented by the formula (-N = PCl 2- ) n (n is an integer of 3 or more) and ammonia. reacting the bets, chlorine atom chloro polyphosphazene oligomer obtained by replacing -NH 2 [An'naren der Hiemi (Ann.Chem.) 12
Volume 169 (1939) Chemical Industry (C
hem.Ind.) 1959, page 748 and JP-A-48-51899). It is preferable that this replacement with -NH 2 be carried out completely, but even if a small amount of unsubstituted chlorine remains (about 1/3 or less of the chlorine bound to the raw material chlorophosphazene), it will still function as a flame retardant. Can be used.
アミド化に際しては副反応としてフォスファゼン分子間
で部分的な縮合が起こることもあるが、それによる縮合
物の混在も難燃化効果の妨げにならない。During amidation, partial condensation may occur between phosphazene molecules as a side reaction, and the condensate mixture due to this may not hinder the flame retardant effect.
ここに使用するクロロフォスファゼンオリゴマーは、五
塩化リンと塩化アンモニウムとの反応でつくられるもの
であって、その際に生成物は環状三量体 を主成分とし、その他に環状四量体および上記一般式に
おけるｎ≧５のオリゴマーを含む混合物である。The chlorophosphazene oligomer used here is formed by the reaction of phosphorus pentachloride and ammonium chloride, in which case the product is a cyclic trimer. And a cyclic tetramer and an oligomer of n ≧ 5 in the above general formula.
本発明においては、アミドフォスファゼンの原料として
このような混合物をそのまま使用してもよいが、例えば
特開昭58−130107号公報に開示されている方法に従って
分離された純環状トリマーあるいは純環状テトラマーを
使用して、難燃化剤としての性能の優れたアミドフォス
ファゼンを製造することもできる。In the present invention, such a mixture may be used as it is as a raw material for amide phosphazene, but for example, a pure cyclic trimer or a pure cyclic trimer separated according to the method disclosed in JP-A-58-130107. Tetramers can also be used to produce amide phosphazenes, which have excellent performance as flame retardants.
（アルカリ性物質） 本発明において使用されるアルカリ性物質としては、例
えば水酸化ナトリウム、水酸化カリウム、水酸化カルシ
ウム、炭酸ナトリウム、炭酸カリウム、炭酸水素ナトリ
ウム、炭酸水素カリウム、炭酸ナトリウムカリウム、セ
スキ炭酸ナトリウムなどをあげることができる。(Alkaline substance) Examples of the alkaline substance used in the present invention include sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate, potassium carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate, sodium potassium carbonate, sodium sesquicarbonate and the like. Can be raised.
本発明において使用されるこれらのアルカリ性物質の量
は、アミドフォスファゼンと塩化アンモニウムとの混合
物中の塩素イオンのほぼ当量が適当である。Appropriate amounts of these alkaline substances used in the present invention are approximately equivalent amounts of chloride ions in the mixture of amidophosphazene and ammonium chloride.
発明の作用 アミドフォスファゼンと塩化アンモニウムとの混合水溶
液に上記のアルカリ性物質を加えると、塩化アンモニウ
ムはアルカリ性物質によって分解され、生成するアンモ
ニアは自動的にあるいは減圧または加熱によって揮散除
去される。塩素イオンはアルカリ性物質中の金属イオン
と結合してセルロース系物質に無害な金属塩化物とな
り、これは被処理物の水洗工程において除去される。Effect of the Invention When the above alkaline substance is added to the mixed aqueous solution of amidophosphazene and ammonium chloride, ammonium chloride is decomposed by the alkaline substance, and the produced ammonia is volatilized and removed automatically or by decompression or heating. Chloride ions combine with metal ions in the alkaline substance to form a metal chloride that is harmless to the cellulosic material, and is removed in the step of washing the object to be treated with water.
（操作の指針） 以下にセルロース系物質の一例として綿布に対する処理
を述べる。(Guidelines for Operation) The treatment of cotton cloth will be described below as an example of the cellulosic material.
塩化アンモニウムを含有するアミドフォスファゼンとア
ルカリ性物質との混合水溶液をつくる。この際、水にア
ルコールを混ぜて用いてもよい。水溶液の濃度は最終的
に綿布に付着する難燃性ポリマーの期待量と、綿布を浸
漬したあとのピックアップ率によって異なるが、最終的
に綿布に付着する難燃性ポリマーの量は、綿布の重量の
２〜10％が適当である。次いで、この溶液を用いて綿布
を浸漬して絞り、次いで風乾によって予備乾燥する。さ
らにこの綿布を120〜220℃の温度で10秒ないし30分間、
好ましくは130〜170℃で２〜７分間キュアリングし、温
水洗浄して付着している水可溶性物（金属塩化物が主体
である）を除いた後に乾燥することにより、黄色着色な
らびに脆化がなく、難燃化効果が充分あり、また風合等
の点にも優れている難燃性綿布を作成することができ
る。A mixed aqueous solution of amidophosphazene containing ammonium chloride and an alkaline substance is prepared. At this time, alcohol may be mixed with water. The concentration of the aqueous solution depends on the expected amount of the flame-retardant polymer that eventually adheres to the cotton cloth and the pickup rate after the cotton cloth is dipped, but the amount of the flame-retardant polymer that finally adheres to the cotton cloth is the weight of the cotton cloth. 2 to 10% is suitable. A cotton cloth is then dipped and squeezed with this solution and then predried by air drying. In addition, this cotton cloth at a temperature of 120-220 ℃ for 10 seconds to 30 minutes,
Preferably, it is cured at 130 to 170 ° C. for 2 to 7 minutes, washed with warm water to remove the attached water-soluble substances (mainly metal chlorides), and then dried to prevent yellow coloring and embrittlement. It is possible to prepare a flame-retardant cotton cloth which has a sufficient flame-retardant effect and is also excellent in feeling and the like.
実施例 本発明をいっそう理解しやすくするために以下に実施例
を示すが、下記の実施例は本発明を制限するものではな
い。なお、実施例中の「部」および比較例中の「部」
は、いずれも「重量部」を意味する。Examples The following examples are provided to make the present invention easier to understand, but the following examples do not limit the present invention. In addition, "part" in Examples and "part" in Comparative Examples
Means "parts by weight".
実施例１ クロロフォスファゼンの環状三量体を完全にアミド化し
て得られるアミドフォスファゼン32.2部（塩化アンモニ
ウムの含有率56.4％）及び水酸化ナトリウム13.6部を水
154.2部に溶解した。この溶液に綿金巾布を浸漬し、ピ
ックアップ100％に絞り、風乾した。この綿布を160℃の
温度で３分間加熱したのち、60℃の温水で５分間洗浄し
て室温で乾燥した。綿布の重量は処理前より3.8％増加
していた。Example 1 32.2 parts (ammonium chloride content 56.4%) of amide phosphazene obtained by completely amidating the cyclic trimer of chlorophosphazene (ammonium chloride content 56.4%) and 13.6 parts of sodium hydroxide were added to water.
It dissolved in 154.2 parts. A cotton bandage was dipped in this solution, squeezed to 100% of the pickup, and air-dried. This cotton cloth was heated at a temperature of 160 ° C. for 3 minutes, washed with warm water of 60 ° C. for 5 minutes, and dried at room temperature. The weight of the cotton cloth increased by 3.8% from that before the treatment.
こうして得られた難燃性綿布は、繊維の脆化がなく、風
合がよく、またブンゼンバーナーの火にあてても炎上も
着火もせずに炭化し、アフターグローを示さなかった。The flame-retardant cotton cloth thus obtained did not embrittle the fibers, had a good texture, and did not burn or ignite even when exposed to the Bunsen burner, and did not show afterglow.
実施例２ 実施例１と同じ塩化アンモニウム含有アミドフォスファ
ゼン32.2部及び炭酸水素ナトリウム28.5部を水159.3部
に溶解し、軽く減圧しながら70℃の温度で30分間攪拌し
た。この溶液を用いて、実施例１と同様に綿布を処理し
たところ、得られた綿布の性質は実施例１の綿布とほと
んど同じであった。Example 2 The same ammonium chloride-containing amide phosphazene as in Example 1 (32.2 parts) and sodium hydrogencarbonate (28.5 parts) were dissolved in water (159.3 parts), and the mixture was stirred at 70 ° C. for 30 minutes while lightly reducing the pressure. When a cotton cloth was treated with this solution in the same manner as in Example 1, the properties of the obtained cotton cloth were almost the same as those of Example 1.
比較例１ 実施例１と同じ塩化アンモニウム含有アミドフォスファ
ゼン32.2部を水164.8部に溶解した溶液を用いて、水酸
化ナトリウムを使用しないで実施例１と同様に綿布を処
理した。Comparative Example 1 A cotton cloth was treated in the same manner as in Example 1 without using sodium hydroxide, using a solution prepared by dissolving 32.2 parts of the same ammonium chloride-containing amide phosphazene as in Example 1 in 164.8 parts of water.
得られた綿布は全面的に黄変、脆化し、風合は劣ってい
た。難燃化効果はほぼ同様であった。The obtained cotton cloth was entirely yellowed and brittle, and the texture was inferior. The flame retardant effect was almost the same.
発明の効果 本発明により、塩酸ガスによるセルロース系物質の脆化
を防止し、かつ風合、難燃化効果ともにすぐれた難燃性
セルロース系物質を得ることができる。EFFECTS OF THE INVENTION According to the present invention, it is possible to obtain a flame-retardant cellulosic material that prevents embrittlement of the cellulosic material due to hydrochloric acid gas, and that has excellent feeling and flame retardancy.
したがって本発明によれば、繊維処理工程における塩化
アンモニウム共存に伴う障害が排除されて、耐久性のあ
る難燃性セルロース系物質が得られる。Therefore, according to the present invention, the flame retardant cellulosic material having durability can be obtained by eliminating the obstacle caused by the coexistence of ammonium chloride in the fiber treatment step.
───────────────────────────────────────────────────── フロントページの続き 審査官 棚橋 留香 (56)参考文献 特開 昭54−45636（ＪＰ，Ａ) 特公 昭47−45636（ＪＰ，Ｂ１) ─────────────────────────────────────────────────── ─── Continuation of front page Examiner Ryuka Tanahashi (56) References JP 54-45636 (JP, A) JP 47-45636 (JP, B1)
Claims (2)
およびアルカリ性物質の混合水溶液をセルロース系物質
に含浸させ、乾燥し、120℃ないし220℃の温度に10秒な
いし30分間加熱し、次いで水洗することを特徴とするセ
ルロース系物質の難燃化方法。1. A method of impregnating a cellulosic material with a mixed aqueous solution of amidophosphazene, ammonium chloride and an alkaline substance, drying, heating to a temperature of 120 ° C. to 220 ° C. for 10 seconds to 30 minutes, and then washing with water. A method for making a cellulosic material flame-retardant.
が減圧または／および加熱によってアンモニアを発散さ
せた水溶液である特許請求の範囲第１項に記載のセルロ
ース系物質の難燃化方法。2. The method for flame retarding a cellulosic material according to claim 1, wherein the mixed aqueous solution with which the cellulosic material is impregnated is an aqueous solution in which ammonia is exhaled by pressure reduction and / or heating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60136857A JPH0686704B2 (en) | 1985-06-25 | 1985-06-25 | Flame-retardant method for cellulose materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60136857A JPH0686704B2 (en) | 1985-06-25 | 1985-06-25 | Flame-retardant method for cellulose materials |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61296177A JPS61296177A (en) | 1986-12-26 |
| JPH0686704B2 true JPH0686704B2 (en) | 1994-11-02 |
Family
ID=15185132
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60136857A Expired - Lifetime JPH0686704B2 (en) | 1985-06-25 | 1985-06-25 | Flame-retardant method for cellulose materials |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0686704B2 (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63264973A (en) * | 1987-04-15 | 1988-11-01 | 日東紡績株式会社 | Non-formaldehyde low shrinkable fabric |
| JPS63120173A (en) * | 1986-06-13 | 1988-05-24 | 日東紡績株式会社 | Method for processing knitted fabric |
| JPS6440674A (en) * | 1987-07-31 | 1989-02-10 | Wakayama Prefecture | Fire retardant processing of fiber with aminophosphazene derivative |
| JPS6440673A (en) * | 1987-07-31 | 1989-02-10 | Wakayama Prefecture | Fire retardant processing of fiber |
| JPH02216267A (en) * | 1988-10-12 | 1990-08-29 | Tango Orimono Kougiyoukumiai | Modifying processing of protein fiber product |
| JP2737296B2 (en) * | 1989-09-08 | 1998-04-08 | 日東紡績株式会社 | Processing method of cellulosic fabric |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL7803765A (en) * | 1978-04-10 | 1979-10-12 | Hoogovens Ijmuiden Bv | PROCESS FOR THE REMOVAL OF AMMONIA AND AMMONIUM SALTS FROM INDUSTRIAL WASTE WATER. |
-
1985
- 1985-06-25 JP JP60136857A patent/JPH0686704B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61296177A (en) | 1986-12-26 |
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