JPH01234436A - Inorganic flame-retardant for thermoplastic resin - Google Patents
Inorganic flame-retardant for thermoplastic resinInfo
- Publication number
- JPH01234436A JPH01234436A JP5958188A JP5958188A JPH01234436A JP H01234436 A JPH01234436 A JP H01234436A JP 5958188 A JP5958188 A JP 5958188A JP 5958188 A JP5958188 A JP 5958188A JP H01234436 A JPH01234436 A JP H01234436A
- Authority
- JP
- Japan
- Prior art keywords
- magnesium hydroxide
- particle size
- resin
- size distribution
- retardant
- 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.)
- Pending
Links
- 229920005992 thermoplastic resin Polymers 0.000 title claims abstract description 15
- 239000012796 inorganic flame retardant Substances 0.000 title claims abstract description 6
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 40
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 40
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 39
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000009826 distribution Methods 0.000 claims abstract description 25
- 230000005540 biological transmission Effects 0.000 claims abstract description 14
- 230000000694 effects Effects 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000000691 measurement method Methods 0.000 claims description 10
- 229920005989 resin Polymers 0.000 abstract description 12
- 239000011347 resin Substances 0.000 abstract description 12
- 239000003945 anionic surfactant Substances 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 230000000704 physical effect Effects 0.000 description 13
- 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 description 10
- 239000003063 flame retardant Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 241001131796 Botaurus stellaris Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012756 surface treatment agent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- KAKVFSYQVNHFBS-UHFFFAOYSA-N (5-hydroxycyclopenten-1-yl)-phenylmethanone Chemical compound OC1CCC=C1C(=O)C1=CC=CC=C1 KAKVFSYQVNHFBS-UHFFFAOYSA-N 0.000 description 1
- IEKHISJGRIEHRE-UHFFFAOYSA-N 16-methylheptadecanoic acid;propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)CCCCCCCCCCCCCCC(O)=O.CC(C)CCCCCCCCCCCCCCC(O)=O.CC(C)CCCCCCCCCCCCCCC(O)=O IEKHISJGRIEHRE-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 238000007664 blowing Methods 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
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- -1 laurylbenzene sulfone Chemical class 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229940096992 potassium oleate Drugs 0.000 description 1
- 229940114930 potassium stearate Drugs 0.000 description 1
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 description 1
- FYFUQDOEHQSBFN-UHFFFAOYSA-M potassium;docosanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCCCCCC([O-])=O FYFUQDOEHQSBFN-UHFFFAOYSA-M 0.000 description 1
- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- CVYDEWKUJFCYJO-UHFFFAOYSA-M sodium;docosanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCCCCC([O-])=O CVYDEWKUJFCYJO-UHFFFAOYSA-M 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Fireproofing Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、水酸化マグネシウムからなる熱可塑性樹脂用
無機難燃剤に関し、特に低温ゼイ特性に優れた熱可塑性
樹脂用難燃剤に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an inorganic flame retardant for thermoplastic resins made of magnesium hydroxide, and particularly to a flame retardant for thermoplastic resins that has excellent low-temperature zeitage properties.
従来より、熱可塑性樹脂用難燃剤として、水酸化マグネ
シウムを利用することは、すでに広く知られており、近
年無公害な難燃剤として注目をあびている。現在まで熱
可塑性樹脂用難燃剤に適した水酸化マグネシウムについ
て、種々の提案が行われできた。The use of magnesium hydroxide as a flame retardant for thermoplastic resins has been widely known and has recently attracted attention as a non-polluting flame retardant. Until now, various proposals have been made regarding magnesium hydroxide suitable as a flame retardant for thermoplastic resins.
例えば、特開昭５１−８２３３４号公報には、メルトイ
ンデックス１０〜０．１ ｇ／１０分の熱可塑性樹脂５
５〜２５重量％と水酸化マグネシウム４５〜７５重量％
を配合した自消性樹脂組成物の押出又は射出成形におけ
る外観の悪さ、とくにシルバーストリークの発生を防止
するために比表面積が４５ｒｒｆ／ｇ以下の水酸化マグ
ネシウムを使用することが提案されている。For example, JP-A-51-82334 discloses that a thermoplastic resin with a melt index of 10 to 0.1 g/10 min.
5-25% by weight and magnesium hydroxide 45-75% by weight
It has been proposed to use magnesium hydroxide with a specific surface area of 45 rrf/g or less in order to prevent poor appearance, especially the occurrence of silver streaks, in extrusion or injection molding of self-extinguishing resin compositions containing .
また、特開昭５２−５９６４３号公報には、かさ密度が
０．３５〜０．７０ｇ／ｃｃで、比表面積が１０〜 ３
０ｎＴ／ｇであり、かつ結晶格子における〔１１０〕面
に垂直な方向の結晶子の厚みと（００１）面のそれとの
比が１．７〜２．７であるプラスチック充填剤の利用が
提案されている。Furthermore, JP-A-52-59643 discloses that the bulk density is 0.35 to 0.70 g/cc and the specific surface area is 10 to 3.
0 nT/g and the ratio of the crystallite thickness in the direction perpendicular to the [110] plane in the crystal lattice to that of the (001) plane is 1.7 to 2.7. ing.
更に、特公昭５２−４３６６３号公報には、平均粒径１
５μ以下、吸油量５０ｍ１／ｇ以下で、かつ活性値３０
■／ｇ以下の水酸化マグネシウムを熱可塑性樹脂に対し
て４０重量％−以上配合した難燃熱可塑性組成物の提案
がある。 ゛また更に、特開昭５４−８３９５
２号公報には、ＢＥＴ比表面積が約２０ｒｒｒ／ｇ以下
で、かつＢＥＴ比表比表面積／ブレー比法比表面積が１
〜約３の範囲にある水酸化マグネシウムについての提案
がある。Furthermore, in Japanese Patent Publication No. 52-43663, an average particle size of 1
5 μ or less, oil absorption amount of 50 m1/g or less, and activity value of 30
There is a proposal for a flame-retardant thermoplastic composition containing 40% by weight or more of magnesium hydroxide/g or less based on the thermoplastic resin.゛Furthermore, JP-A-54-8395
Publication No. 2 states that the BET specific surface area is approximately 20 rrr/g or less, and the BET specific surface area/Bree specific surface area is 1.
There are suggestions for magnesium hydroxide in the range of ~3.
更に、特開昭６２−１２３０１４号公報には、光透過式
液相沈降測定法による平均粒子径（ｄ）が０．２〜０．
８μで、該平均粒子径（ｄ）＋０．５μ以上の粒子径を
有する粒子の割合が重量比で全粒子重量の５０％以下、
かつ粒子の厚み分布が、厚’、＞０．０５μ以下の粒子
の数が２０％以下である薄板状の水酸化マグネシウムに
ついての提案がある。Furthermore, JP-A-62-123014 discloses that the average particle diameter (d) measured by a light transmission liquid phase sedimentation measurement method is 0.2 to 0.
8μ, the proportion of particles having a particle diameter of at least the average particle diameter (d) + 0.5μ is 50% or less of the total particle weight in terms of weight ratio,
There is also a proposal for a thin plate-like magnesium hydroxide in which the number of particles having a particle thickness distribution of >0.05μ or less is 20% or less.
しかし、上記の如き水酸化マグネシウムを特定するため
に用いられてきた因子によっては、樹脂に対する分散性
、成形性、成形物外観、難燃性もさることながら、優れ
た物理的性質、特に低温ゼイ化特性を付与することは困
難であった。熱可塑性樹脂の物理的性質の中で、低温ゼ
イ化特性は、重要な性質であり、とりわけ熱可塑性樹脂
用難燃剤として水酸化マグネシウムの使用が顕著な電線
ケーブル向用途では、屋外での使用割合が多く、特に冬
期においては、厳しい低温条件下にさらされる為、特に
重要な性質である。However, depending on the factors that have been used to specify magnesium hydroxide as mentioned above, in addition to its dispersibility in resin, moldability, molded product appearance, and flame retardance, it also has excellent physical properties, especially low-temperature resistance. It was difficult to impart chemical properties. Among the physical properties of thermoplastic resins, low-temperature gelatinization properties are an important property, especially in applications for electric wires and cables where the use of magnesium hydroxide as a flame retardant for thermoplastic resins is particularly important. This is an especially important property, especially in the winter, when the material is exposed to harsh low-temperature conditions.
本発明は、樹脂に対する分散性、成形性、成形物外観、
Ｈ燃性を損なうことなく、優れた物理的性質、特に低温
ゼイ化特性に優れた熱可塑性樹脂用難燃剤を提供するも
のである。The present invention focuses on dispersibility in resin, moldability, appearance of molded products,
The present invention provides a flame retardant for thermoplastic resins that has excellent physical properties, particularly low-temperature zeification properties, without impairing H flammability.
〔課題を解決するための手段〕 〔作用〕本発明者等は
、上記の如き問題点を解決すべく検討を重ねた結果、樹
脂に対する物理的性質付与性、特に低温ゼイ化特性に優
れた水酸化マグネシウムを与えるには、光透過式粒度分
布測定法による粒度分布と水酸化マグネシウムのＣ，Ａ
、Ａ、値（クエン酸活性価）を共に満足する必要がある
ことを発見した。すなわち、本発明は光透過式粒度分布
）９０％反応が約２５０秒以上である水酸化マグネシウ
ムからなることを特徴とする熱可望性樹脂用無機難燃剤
に係るものである。[Means for Solving the Problems] [Operation] As a result of repeated studies to solve the above-mentioned problems, the inventors of the present invention have developed a water solution that is excellent in imparting physical properties to resins, especially in low-temperature gelatinization properties. To give magnesium oxide, the particle size distribution by light transmission particle size distribution measurement method and C, A of magnesium hydroxide are determined.
, A, and value (citric acid activity value). That is, the present invention relates to an inorganic flame retardant for thermoplastic resins characterized by comprising magnesium hydroxide having a light transmission type particle size distribution (90% reaction) of about 250 seconds or more.
ここで使用する光透過式粒度分布測定法による粒度分布
とは、試料を媒体溶液（例えば、蒸留水。The particle size distribution measured by the light transmission particle size distribution measurement method used here means that the sample is measured in a medium solution (e.g., distilled water).
メタノール、エタノールの如きアルコール水溶液等）中
に分散懸濁させ、液相中での粒子の沈降伏況を特定時間
毎に光透過法で測定し、その沈降速度の差より粒子の粒
度分布を求めるものである。The particles are dispersed and suspended in an alcohol aqueous solution such as methanol or ethanol, and the sedimentation rate of the particles in the liquid phase is measured using a light transmission method at specific time intervals, and the particle size distribution of the particles is determined from the difference in the sedimentation rate. It is something.
また、Ｃ１＾、Ａ、値（クエン酸活性価）は、アルカリ
性粉末の活性度を測定する一般的な方法であり、その測
定方法は０．４Ｎのクエン酸溶液１００ｍ１を２００ｍ
１ｌ容ビーカーに採取し、液の温度を３０”Ｃ−１＝
０．２℃に調節し、回転子が回転してわずかに底が見え
る程度になるようにスターラーの回転数を合わせておく
。次にサンプルを採取しく水酸化マグネシウム９０％反
応の場合は、サンプル量１．２８９ｇ）ビーカーに投入
すると同時にストップウォッチをスタートさせ、１０秒
後にスターラーのスイッチを入れ回転を始め、あらかじ
めクエン酸溶液中に添加しておいたフェノールツクレイ
ンにより液がピンク色になるまでの時間を測定するもの
である。In addition, C1^, A, value (citric acid activity value) is a general method for measuring the activity of alkaline powder.
Collect the liquid in a 1L beaker and set the temperature of the liquid to 30"C-1=
Adjust the temperature to 0.2℃ and adjust the rotation speed of the stirrer so that the rotor rotates and the bottom is slightly visible. Next, take a sample (in the case of a 90% magnesium hydroxide reaction, the sample amount is 1.289 g), start the stopwatch at the same time as you add it to the beaker, turn on the stirrer after 10 seconds, start rotating, and add it to the citric acid solution in advance. The purpose is to measure the time it takes for the liquid to turn pink due to the addition of phenolskurein.
本発明で使用される水酸化マグネシウムは、通常のいず
れの製造方法によるものでも良い。例えば、海水または
苦汁に消石灰などのアルカリ性物質を添加して水酸化マ
グネシウムを得る方法、あるいは特開昭５２−１１５７
９９号公報に示される如く、塩基性塩化−もしくは硝酸
マグネシウムを水性媒体中において加圧条件下に加熱し
て水酸化マグネシウムを得る方法、また特開昭５６−１
０９８２０号公報に示される如く、１４００°Ｃ以上で
焼成した酸化マグネシウムを酸またはマグネシウム塩の
水懸濁スラリー中で水和して水酸化マグネシウムを得る
方法、更に特開昭６０−１５５５２９号公報に示される
如く、合成苦汁にアンモニアガスを吹き込んで反応させ
水酸化マグネシウムを得る方法などを選択して、製造さ
れる水酸化マグネシウムのうち、本発明の特定要件であ
る光透過式粒度分布測定法による粒度分布、がっＣ，Ａ
。The magnesium hydroxide used in the present invention may be produced by any conventional manufacturing method. For example, a method for obtaining magnesium hydroxide by adding an alkaline substance such as slaked lime to seawater or bittern, or JP-A-52-1157
As shown in Japanese Patent No. 99, a method for obtaining magnesium hydroxide by heating basic chloride or magnesium nitrate in an aqueous medium under pressurized conditions, and JP-A-56-1
As shown in Japanese Patent Publication No. 09820, a method for obtaining magnesium hydroxide by hydrating magnesium oxide calcined at 1400° C. or higher in a water suspension slurry of an acid or magnesium salt, and further disclosed in Japanese Patent Application Laid-open No. 155529/1982. As shown, among the magnesium hydroxide produced by selecting a method such as blowing ammonia gas into synthetic bittern and reacting it to obtain magnesium hydroxide, the magnesium hydroxide produced by the light transmission particle size distribution measurement method, which is a specific requirement of the present invention, is Particle size distribution, C, A
.
Ａ、値（クエン酸活性価）を満たす水酸化マグネシウム
である。A: Magnesium hydroxide that satisfies the value (citric acid activity value).
すなわち、本発明の水酸化マグネシウムは、光透過式粒
度分布測定法による粒度分布１μ以下の割合が約４０％
以上、好ましくは５０％以上で、Ｃ，Ａ、Ａ、 （クエ
ン酸活性価）９０％反応値が約２５０秒以上、好ましく
は３００秒以上の水酸化マグネシウムである。That is, in the magnesium hydroxide of the present invention, the proportion of particle size distribution of 1μ or less as measured by light transmission particle size distribution measurement method is about 40%.
Above, preferably 50% or more, C, A, A, (citric acid activity value) 90% reaction value is magnesium hydroxide of about 250 seconds or more, preferably 300 seconds or more.
つまり、光透過式粒度分布測定法による粒度分布１μ以
下の割合が４０％以下の場合、言い換えれば１μ以上の
割合が６０％を越える場合は、単一粒子のほとんどが１
μ以下の水酸化マグネシウム粉末が極度に凝集し、凝集
体として粒度分布が測定されていることを意味し、した
がって樹脂中においても分散が悪く、水酸化マグネシウ
ムの分散性が特に強く影響を与える物理的性質、特に低
温ゼイ化特性においては、好ましくない結果を与える。In other words, if the proportion of particle size distributions below 1μ in the light transmission particle size distribution measurement method is 40% or less, in other words, if the proportion of particles above 1μ exceeds 60%, most of the single particles are
This means that magnesium hydroxide powder with a particle size of less than μ is extremely agglomerated, and the particle size distribution is measured as an aggregate. Therefore, it is poorly dispersed even in resin, and the dispersibility of magnesium hydroxide has a particularly strong influence on physical properties. It gives unfavorable results in physical properties, especially low-temperature gelatinization properties.
また、上記粒度分布を満足する水酸化マグネシウムであ
ってもＣ，Ａ、Ａ、 （クエン酸活性価）９０％反応
値が２５０秒以下の場合には、ある程度の低温ゼイ化特
性は期待できるが、必ずしも満足できる特性値を与えず
、２５０秒以上好ましくは３００秒以上の水酸化マグネ
シウムが必要である。In addition, even if magnesium hydroxide satisfies the above particle size distribution, if the reaction value of C, A, A (citric acid activity value) 90% is 250 seconds or less, a certain degree of low-temperature zeification property can be expected. However, magnesium hydroxide does not necessarily give satisfactory characteristic values and requires a heating time of 250 seconds or more, preferably 300 seconds or more.
以上のように、従来水酸化マグネシウムを特定するため
に用いられてきた因子によっては樹脂の物理的性質、特
に優れた低温ゼイ化特性を付与するものではなかった。As mentioned above, depending on the factors conventionally used to specify magnesium hydroxide, the physical properties of the resin, particularly excellent low-temperature gelatinization properties, have not been imparted.
優れた低温ゼイ化特性を与えるには、本発明により特定
された光透過式粒度分布測定法による粒度分布およびＣ
，Ａ、Ａ、値（クエン酸活性価）を共に満足する水酸化
マグネシウムでしか与え得ない。In order to provide excellent low-temperature gelatinization properties, the particle size distribution determined by the light transmission particle size distribution measurement method specified by the present invention and C
, A, A, value (citric acid activity value) can only be provided with magnesium hydroxide.
本発明における水酸化マグネシウムは、そのまま難燃剤
として樹脂に混合使用できるが、樹脂との相容性９分散
性をさらに向上させるために、通常使用される表面処理
剤、例えばアニオン系界面活性剤やカップリング剤等で
表面処理することにより、成形性や成形体の物理的性質
により優れた難燃剤とすることができる。このようなア
ニオン系界面活性剤の具体例としては、ステアリン酸ナ
トリウム、ステアリン酸カリウム、オレイン酸ナトリウ
ム、オレイン酸カリウム、ラウリン酸ナトリウム、ラウ
リン酸カリウム、ベヘニン酸ナトリウム、ベヘニン酸酸
カリウム、ラウリルベンゼンスルホン酸ナトリウム等を
例示することができる。Magnesium hydroxide in the present invention can be mixed with resin as it is as a flame retardant, but in order to further improve the compatibility with the resin and the dispersibility, it is necessary to use commonly used surface treatment agents such as anionic surfactants. By surface-treating the flame retardant with a coupling agent or the like, it is possible to obtain a flame retardant with superior moldability and physical properties of the molded product. Specific examples of such anionic surfactants include sodium stearate, potassium stearate, sodium oleate, potassium oleate, sodium laurate, potassium laurate, sodium behenate, potassium behenate, and laurylbenzene sulfone. Examples include sodium acid.
また、カップリング剤の具体例としては、ビニルトリエ
トキシシラン、γ−グリシドキシプロピルトリメトキシ
シラン、γ−アミノプロピルトリエトキシシラン、Ｔ−
メタシクロキシプロピルトリメトキシシラン、イソプロ
ピルトリイソステアロイルチタネート、ビスジオクチル
パイロホスフェートオキシアセテートチタネート等を例
示することができる。Specific examples of coupling agents include vinyltriethoxysilane, γ-glycidoxypropyltrimethoxysilane, γ-aminopropyltriethoxysilane, T-
Examples include metacycloxypropyltrimethoxysilane, isopropyltriisostearoyl titanate, bisdioctylpyrophosphate oxyacetate titanate, and the like.
以下に本発明を実施例、比較例により更に詳しく説明す
る。The present invention will be explained in more detail below using Examples and Comparative Examples.
実施例１
光透過式粒度分布測定法による粒度分布１ｕ以下の割合
が５５％ Ｃ，Ａ、Ａ、 ９０％反応値が３２０秒の水
酸化マグネシウムをＥＶＡ樹脂（ＶＡ、 １９ｗｔ％）
１００部に対し、１３０部配合し、押出機で溶融混練し
ペレットを作った。このペレットを押出機で板状体に押
出成形し物性測定用の試料とした。その結果を第１表に
示す。Example 1 Magnesium hydroxide with a particle size distribution of 55% C, A, A, and a 90% reaction value of 320 seconds as measured by a light transmission particle size distribution measurement method was mixed with EVA resin (VA, 19 wt%)
For 100 parts, 130 parts were blended and melt-kneaded using an extruder to make pellets. This pellet was extruded into a plate shape using an extruder and used as a sample for measuring physical properties. The results are shown in Table 1.
実施例２〜６
実施例１と光透過式粒度分布測定法による粒度分布１μ
以下の割合およびＣ，Ａ、Ａ、 ９０％反応値がそれぞ
れ異なる水酸化マグネシウムを実施例１と同様の方法で
成形体とし物性測定した。その結果を第１表に示す。Examples 2 to 6 Example 1 and particle size distribution 1 μ by light transmission particle size distribution measurement method
Magnesium hydroxide having different proportions and C, A, A, and 90% reaction values as shown below were molded in the same manner as in Example 1, and physical properties were measured. The results are shown in Table 1.
比較例１〜３
本発明の特定要件の範囲から、粒度分布１μ以下の割合
およびＣ，Ａ、Ａ、値がそれぞれはずれる水酸化マグネ
シウムを実施例１と同様の方法で成形体とし物性測定し
た。その結果を第１表に示す。Comparative Examples 1 to 3 Magnesium hydroxide whose particle size distribution ratio of 1 μm or less and C, A, and A values each deviate from the range of the specific requirements of the present invention were made into molded bodies in the same manner as in Example 1, and their physical properties were measured. The results are shown in Table 1.
実施例７〜９
実施例１の水酸化子グネシウムを表面処理剤にて表面改
質したものについて実施例１と同様の方法で成形体とし
物性測定した。その結果を第１表に示す。Examples 7 to 9 The magnesium hydroxide obtained in Example 1 was surface-modified with a surface treatment agent, and the molded bodies were formed in the same manner as in Example 1 and their physical properties were measured. The results are shown in Table 1.
以上のように本発明による水酸化マグネシウムを熱可塑
性樹脂に使用することにより、樹脂に対する分散性、成
形性、成形物外観、難燃性を損なうことなく、優れた物
理的性質、特に低温ゼイ化特性に優れた成形体を得るこ
とが出来、その効果は非常に大きい。As described above, by using magnesium hydroxide according to the present invention in a thermoplastic resin, excellent physical properties, especially low-temperature zeification, can be achieved without impairing the dispersibility, moldability, appearance of molded products, and flame retardancy in the resin. A molded article with excellent properties can be obtained, and the effect is very large.
Claims (1)
の割合が約４０％以上で、かつＣ．Ａ．Ａ．（クエン酸
活性価）９０％反応値が約２５０秒以上である水酸化マ
グネシウムからなることを特徴とする熱可塑性樹脂用無
機難燃剤。(1) The proportion of particle size distribution of 1μ or less as measured by light transmission particle size distribution measurement method is about 40% or more, and C.I. A. A. (Citric acid activity value) An inorganic flame retardant for thermoplastic resins comprising magnesium hydroxide having a 90% reaction value of about 250 seconds or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5958188A JPH01234436A (en) | 1988-03-14 | 1988-03-14 | Inorganic flame-retardant for thermoplastic resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5958188A JPH01234436A (en) | 1988-03-14 | 1988-03-14 | Inorganic flame-retardant for thermoplastic resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01234436A true JPH01234436A (en) | 1989-09-19 |
Family
ID=13117339
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5958188A Pending JPH01234436A (en) | 1988-03-14 | 1988-03-14 | Inorganic flame-retardant for thermoplastic resin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01234436A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03137145A (en) * | 1989-10-23 | 1991-06-11 | Mitsubishi Petrochem Co Ltd | Ethylene-vinyl acetate copolymer composition |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5146341A (en) * | 1974-10-18 | 1976-04-20 | Mitsubishi Petrochemical Co | JISHOSEIJUSHISOSEIBUTSU |
| JPS62280242A (en) * | 1986-05-28 | 1987-12-05 | Idemitsu Petrochem Co Ltd | Polyethylene resin composition |
-
1988
- 1988-03-14 JP JP5958188A patent/JPH01234436A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5146341A (en) * | 1974-10-18 | 1976-04-20 | Mitsubishi Petrochemical Co | JISHOSEIJUSHISOSEIBUTSU |
| JPS62280242A (en) * | 1986-05-28 | 1987-12-05 | Idemitsu Petrochem Co Ltd | Polyethylene resin composition |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03137145A (en) * | 1989-10-23 | 1991-06-11 | Mitsubishi Petrochem Co Ltd | Ethylene-vinyl acetate copolymer composition |
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