JPH06157032A - Composite metal oxide, its production and its use - Google Patents

Composite metal oxide, its production and its use

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Publication number
JPH06157032A
JPH06157032A JP4103725A JP10372592A JPH06157032A JP H06157032 A JPH06157032 A JP H06157032A JP 4103725 A JP4103725 A JP 4103725A JP 10372592 A JP10372592 A JP 10372592A JP H06157032 A JPH06157032 A JP H06157032A
Authority
JP
Japan
Prior art keywords
resin
rubber
formula
metal oxide
magnesium oxide
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
Application number
JP4103725A
Other languages
Japanese (ja)
Other versions
JP3384816B2 (en
Inventor
Shigeo Miyata
茂男 宮田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
KAISUI KAGAKU KENKYUSHO KK
Sea Water Chemical Institute Inc
Original Assignee
KAISUI KAGAKU KENKYUSHO KK
Sea Water Chemical Institute Inc
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Publication date
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Priority to JP10372592A priority Critical patent/JP3384816B2/en
Publication of JPH06157032A publication Critical patent/JPH06157032A/en
Application granted granted Critical
Publication of JP3384816B2 publication Critical patent/JP3384816B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02Compounds of alkaline earth metals or magnesium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/02Oxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00Compounds of manganese
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/50Solid solutions
    • C01P2002/52Solid solutions containing elements as dopants
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/50Solid solutions
    • C01P2002/52Solid solutions containing elements as dopants
    • C01P2002/54Solid solutions containing elements as dopants one element only
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/22Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Compounds Of Iron (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

PURPOSE:To produce the composite metal oxide exhibiting excellent characteristics as a thickening agent, a thermal stabilizer, etc., for resins, etc., by calcining a magnesium hydroxide solid solution of the formula at a prescribed temperature. CONSTITUTION:A magnesium hydroxide solid solution of formula: Mg1-xM<2+>x(OH2)2 (M<2+> is selected from Mn<2+>, Fe<2+>, Co<2+>, Ni<2+>, Cu<2+> and Zn<2+>; x is 0.001-0.5) is calcined at 400-1000 deg.C to produce a magnesium oxide solid solution of formula: Mg1-xM<2+>Ox. 0.001-20 pts.wt. of the composite metal oxide is compounded with 100 pts.wt. of a resin, etc., to provide a resin composition and/or a rubber composition.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、新規な複合金属酸化
物、その製造方法およびその使用に関する。さらに詳し
くは、酸化マグネシウムよりも優れた熱安定性、耐候
性、加硫性、増粘性等を付与できる新規な複合金属酸化
物、その製造方法および該複合金属酸化物を配合してな
る熱安定性、加硫性、増粘性等に優れた樹脂および/ま
たはゴム組成物に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a novel mixed metal oxide, a method for producing the same and use thereof. More specifically, a novel composite metal oxide capable of imparting thermal stability, weather resistance, vulcanizability, thickening property, etc. superior to magnesium oxide, a method for producing the same, and a heat stability obtained by blending the composite metal oxide. TECHNICAL FIELD The present invention relates to a resin and / or rubber composition having excellent properties, vulcanizability, thickening property, and the like.

【0002】[0002]

【従来の技術】酸化マグネシウムは、比較的安価、比較
的安定、比較的強い塩基性、無毒性等の特徴があるた
め、種々の分野で使用されてきた。例えばクロロプレン
とかクロロスルホン化ポリエチレン等のハロゲン化ゴム
の加硫時の受酸剤、ポリ塩化ビニルの熱安定剤および耐
候性改良剤、FRPの増粘剤、ABS、EVA等の樹脂
中に存在するまたは熱分解時に発生する酸性物質の中和
剤、セラミック原料、電磁鋼板の焼鈍分離剤等に使用さ
れてきた。
2. Description of the Related Art Magnesium oxide has been used in various fields because it is relatively inexpensive, relatively stable, relatively basic, and nontoxic. For example, it is present in acid acceptors during vulcanization of halogenated rubbers such as chloroprene and chlorosulfonated polyethylene, heat stabilizers and weather resistance improvers of polyvinyl chloride, thickeners of FRP, and resins such as ABS and EVA. It has also been used as a neutralizing agent for acidic substances generated during thermal decomposition, a ceramic raw material, an annealing separator for electromagnetic steel sheets, and the like.

【0003】しかし酸化マグネシウムは、凝集し易く、
樹脂やゴム中での分散が悪い。このため、酸、ハロゲン
の中和、増粘といった本来の機能を十分に発揮できな
い。その上、樹脂やゴムの機械的強度、外観を損なうこ
とが多い。また吸湿性が強く、種々のトラブルを起こし
易い。凝集を殆ど生じない高分散性の酸化マグネシウム
の新規な製造方法も提案された(特開平2−14141
8号公報)。しかし酸性物質との反応性はまだ十分満足
できるものではなく、また樹脂中に未反応の酸化マグネ
シウムが残存する傾向、および吸湿性が大であるという
欠点も解消されるものではない。
However, magnesium oxide easily aggregates,
Poor dispersion in resin or rubber. Therefore, the original functions of neutralizing acid and halogen and thickening cannot be sufficiently exerted. In addition, the mechanical strength and appearance of resins and rubber are often impaired. In addition, it has a high hygroscopic property and is apt to cause various troubles. A novel method for producing highly dispersible magnesium oxide which hardly causes agglomeration has also been proposed (JP-A-2-14141).
No. 8). However, the reactivity with an acidic substance is not yet sufficiently satisfactory, and the disadvantages that unreacted magnesium oxide remains in the resin and that the hygroscopicity is large cannot be solved.

【0004】[0004]

【発明が解決しようとする課題】酸化マグネシウムは、
本質的な欠点として耐水性、耐酸性に乏しく、樹脂やゴ
ム中で吸水するため、樹脂やゴムを膨潤させて本来の製
品特性を損なうことが多い。また樹脂やゴム製の容器に
酸化マグネシウムを使用した場合、酸性物質を入れると
徐徐に酸化マグネシウムが酸性物質中に溶出するという
問題をも有している。このため高レベルの耐水性が要求
される場合、例えば水道のパッキン、貯水池のライニン
グ材として使用するゴム、塩ビ製電線、窓枠、パイプ等
には有毒な鉛化合物が止むをえず使用されている。従っ
て酸化マグネシウム本来の利点である低毒性を維持し
て、酸やハロゲンに対する反応性をさらに高めることが
でき、しかも酸化マグネシウム本来の欠点である吸湿性
を改善できる新規な化合物が望まれてきた。
DISCLOSURE OF THE INVENTION Magnesium oxide is
As an essential drawback, it is poor in water resistance and acid resistance and absorbs water in resin or rubber, so that the resin or rubber is often swollen and the original product characteristics are impaired. Further, when magnesium oxide is used in a resin or rubber container, when an acidic substance is added, magnesium oxide is gradually eluted into the acidic substance. For this reason, when a high level of water resistance is required, for example, toxic lead compounds are inevitably used in water packing, rubber used as lining material for reservoirs, PVC electric wires, window frames, pipes, etc. There is. Therefore, there has been a demand for a novel compound which can maintain the low toxicity which is the original advantage of magnesium oxide and can further enhance the reactivity with respect to an acid or a halogen, and can improve the hygroscopicity which is the inherent drawback of magnesium oxide.

【0005】[0005]

【課題を解決するための手段】本発明は、BET比表面
積5〜300m2/gである式(1) Mg1-x2+ xO (1) (式中、M2+はMn2+、Fe2+、Co2+、Ni2+、Cu
2+およびZn2+からなる群から選ばれた二価金属イオン
の少なくとも一種を示し、xは0.001<x<0.5の
範囲の数を示す)の酸化マグネシウム系固溶体、および
該固溶体を有効成分として含有する樹脂および/または
ゴム用受酸剤(熱安定剤、増粘剤を含む)を提供する。
さらに本発明は樹脂および/またはゴム100重量部に
対し、上記酸化マグネシウム系固溶体を0.001〜2
0重量部配合した樹脂および/またはゴム組成物を提供
する。本発明はさらに、式(3) Mg1-x2+(OH)2 (3) (式中、M2+とxは式(1)と同じ意味を表す)の水酸
化マグネシウム系固溶体を約400〜1000℃で焼成
することからなる上記酸化マグネシウム系固溶体の製造
方法を提供する。
According to the present invention, a BET specific surface area of 5 to 300 m 2 / g is given by the formula (1) Mg 1-x M 2+ x O (1) (wherein M 2+ is Mn 2 + , Fe 2+ , Co 2+ , Ni 2+ , Cu
2+ and Zn 2+, which represents at least one divalent metal ion selected from the group consisting of 2+ and Zn 2+ , and x represents a number in the range of 0.001 <x <0.5), and a solid solution thereof, An acid-accepting agent (including a heat stabilizer and a thickening agent) for a resin and / or rubber, which contains as an active ingredient.
Further, in the present invention, the magnesium oxide solid solution is added to 0.001 to 2 parts by weight with respect to 100 parts by weight of resin and / or rubber.
A resin and / or rubber composition blended with 0 part by weight is provided. The present invention further provides a magnesium hydroxide-based solid solution of the formula (3) Mg 1-x M 2+ (OH) 2 (3) (wherein M 2+ and x have the same meaning as in the formula (1)). Provided is a method for producing the above magnesium oxide-based solid solution, which comprises firing at about 400 to 1000 ° C.

【0006】本発明者は、酸化マグネシウムの欠点であ
る耐水性、耐酸性不良を克服すべく鋭意研究に努めてき
た。その結果、酸化マグネシウムの耐水性等の不良は、
酸化マグネシウム固有の物性に起因するものであり、酸
化マグネシウムである限りこの欠点を著しく改善するこ
とは困難であると考えるに至り、さらに研究を進めた。
The present inventor has conducted earnest research to overcome the drawbacks of magnesium oxide, such as poor water resistance and poor acid resistance. As a result, the poor water resistance of magnesium oxide
This is due to the physical properties peculiar to magnesium oxide, and as far as magnesium oxide is concerned, it has been thought that it would be difficult to remedy this drawback significantly, and further research was conducted.

【0007】その結果、本発明者が先に発明した下記式
(3) Mg1-x2+ x(OH)2 (3) (式中、M2+はMn2+、Fe2+、Co2+、Ni2+、Cu
2+およびZn2+からなる群から選ばれた二価金属イオン
の少なくとも一種を示し、xは0.001<x<0.5の
範囲の数を示す)の水酸化マグネシウム系固溶体を約4
00〜1000℃で焼成すると酸化マグネシウム系固溶
体となること、しかもこの酸化マグネシウム系固溶体が
酸化マグネシウムよりも優れた耐水性、耐酸性を示すこ
とを発見するに至った。さらにこの酸化マグネシウム系
固溶体は、酸化マグネシウムよりも酸やハロゲンに対し
て反応性が優れているという意外な特徴をも発見した。
As a result, the following formula (3) Mg 1-x M 2+ x (OH) 2 (3) previously invented by the present inventor (in the formula, M 2+ is Mn 2+ , Fe 2+ , Co 2+ , Ni 2+ , Cu
2+ and Zn 2+ represents at least one divalent metal ion selected from the group consisting of 2+ and Zn 2+ , and x represents a number in the range of 0.001 <x <0.5), and a magnesium hydroxide solid solution of about 4
It has been discovered that a magnesium oxide-based solid solution is obtained by firing at 00 to 1000 ° C., and that this magnesium oxide-based solid solution exhibits superior water resistance and acid resistance to magnesium oxide. Further, they have also discovered an unexpected characteristic that this magnesium oxide-based solid solution has a higher reactivity with acids and halogens than magnesium oxide.

【0008】本発明の式(1)で表される酸化マグネシ
ウム系固溶体の粉末X線回折パターンは酸化マグネシウ
ムと実質的に同じであり、M2+O(M2+は式(1)のM
2+と同じ意味を表す)に相当する回折パターンは現れな
い。酸化マグネシウムにM2+Oが固溶しているため、そ
の固溶量と固溶したM2+の種類によりわずかに回折角度
がシフトする。M2+Oの固溶量xが大きくなるほど、耐
水性、耐酸性が向上し、酸やハロゲンに対する反応性、
増粘性および焼結性が向上する傾向にある。しかし、x
が0.5以上になると酸化マグネシウムよりも反応性が
低下する。従って、xの範囲としては好ましくは0.0
1≦x<0.5、さらに好ましくは0.03≦x<0.3
である。
The powder X-ray diffraction pattern of the magnesium oxide type solid solution represented by the formula (1) of the present invention is substantially the same as that of magnesium oxide, and M 2+ O (M 2+ is M of the formula (1)).
2+ ) has the same meaning) and no diffraction pattern appears. Since M 2+ O is solid-dissolved in magnesium oxide, the diffraction angle slightly shifts depending on the amount of solid solution and the type of M 2+ dissolved. The larger the solid solution amount x of M 2+ O, the higher the water resistance and acid resistance, and the reactivity to acid and halogen,
The viscosity increase and the sinterability tend to be improved. But x
Is 0.5 or more, the reactivity becomes lower than that of magnesium oxide. Therefore, the range of x is preferably 0.0
1 ≦ x <0.5, more preferably 0.03 ≦ x <0.3
Is.

【0009】式(1)のM2+の中では、ニッケルの耐水
性、耐酸性が優れている。M2+が亜鉛の場合はニッケル
程耐水性、耐酸性の改善は顕著でないが、酸化マグネシ
ウムよりも優れた白色度、酸やハロゲンに対する反応性
を示すと共に、樹脂特に塩化ビニルの熱安定剤として用
いた場合に酸化マグネシウムの赤色系着色を著しく抑え
る等の特徴を示す。上記特徴を有する酸化マグネシウム
系固溶体は式(2) Mg1-x(Niおよび/またはZn)xO (2) (式中、xは式(1)と同じ意味を表す)で表される。
Among M 2+ of the formula (1), nickel has excellent water resistance and acid resistance. When M 2+ is zinc, the water resistance and acid resistance are not so much improved as that of nickel, but it shows superior whiteness and reactivity to acids and halogens than magnesium oxide, and as a heat stabilizer for resins, especially vinyl chloride. When used, it exhibits features such as remarkably suppressing reddish coloring of magnesium oxide. The magnesium oxide-based solid solution having the above characteristics is represented by the formula (2) Mg 1-x (Ni and / or Zn) x O (2) (where x represents the same meaning as in the formula (1)).

【0010】本発明の酸化マグネシウム系固溶体は、そ
の能力を最大限発揮させるために凝集が殆ど無く、樹脂
やゴム中で高分散性であることが好ましい。このような
特性を発揮させるためには、平均2次粒子径が好ましく
は0.1〜2μm、特に好ましくは0.1〜1.0μmで
あり、BET比表面積が5m2/g以上、好ましくは1
0m2/g以上であり、特に好ましくは20m2/g〜3
00m2/gである。
The magnesium oxide-based solid solution of the present invention is preferably highly dispersible in resins and rubbers with almost no aggregation in order to maximize its ability. In order to exert such characteristics, the average secondary particle diameter is preferably 0.1 to 2 μm, particularly preferably 0.1 to 1.0 μm, and the BET specific surface area is 5 m 2 / g or more, preferably 1
It is at 0m 2 / g or more, and particularly preferably 20m 2 / g~3
It is 00 m 2 / g.

【0011】本発明の酸化マグネシウム系固溶体は、そ
のまま用いることができると共に、高級脂肪酸、高級脂
肪酸の金属塩、アニオン系界面活性剤、リン酸エステ
ル、シラン系、チタネート系、アルミニウム系カップリ
ング剤、多価アルコールと脂肪酸のエステル等の表面処
理剤で表面処理して用いてもよい。
The magnesium oxide-based solid solution of the present invention can be used as it is, and higher fatty acids, metal salts of higher fatty acids, anionic surfactants, phosphoric acid esters, silane-based, titanate-based, aluminum-based coupling agents, You may use after surface-treating with surface-treating agents, such as ester of polyhydric alcohol and fatty acid.

【0012】表面処理剤として好ましく用いられるもの
を例示すると次の通りである。ステアリン酸、オレイン
酸、エルカ酸、パルミチン酸、ラウリン酸、ベヘニン酸
等の炭素数10以上の高級脂肪酸類;前記高級脂肪酸類
のMg、Ca、Zn、Al、Na等の塩類;ステアリル
アルコール、オレイルアルコール等の高級アルコールの
硫酸エステル塩;ポリエチレングリコールエーテルの硫
酸エステル塩;アミド結合硫酸エステル塩、エステル結
合硫酸エステル塩、エステル結合スルホネート、アミド
結合スルホン酸塩、エーテル結合スルホン酸塩、エーテ
ル結合アルキルアリルスルホン酸塩、エステル結合アル
キルアリルスルホン酸塩、アミド結合アルキルアリルス
ルホン酸塩等のアニオン系界面活性剤類;オルトリン酸
とオレイルアルコール、ステアリルアルコール等のモノ
またはジエステルまたは両者の混合物であって、それら
の酸型またはアルカリ金属塩またはアミン塩等のリン酸
エステル類;ビニルエトキシシラン、ビニル−トリス
(2−メトキシ−エトキシ)シラン、ガンマ−メタクリ
ロキシプロピルトリメトキシシラン、ガンマ−アミノプ
ロピルトリメトキシシラン、ベ−タ−(3、4−エポキ
シシクロヘキシル)エチルトリメトキシシラン、ガンマ
−グリシドキシプロピルトリメトキシシラン、ガンマ−
メルカプトプロピルトリメトキシシラン等のシランカッ
プリング剤類;イソプロピルトリイソステアロイルチタ
ネート、イソプロピルトリス(ジオクチルパイロフォス
フェート)チタネート、イソプロピルトリデシルベンゼ
ンスルホニルチタネート等のチタネート系カップリング
剤類;アセトアルコキシアルミニウムジイソプロピレー
ト等のアルミニウム系カップリング剤類;グリセリンモ
ノステアレート、グリセリンモノオレエート等のアルコ
ールと脂肪酸のエステル類。
Examples of the surface treatment agent preferably used are as follows. Higher fatty acids having 10 or more carbon atoms such as stearic acid, oleic acid, erucic acid, palmitic acid, lauric acid and behenic acid; salts of the higher fatty acids such as Mg, Ca, Zn, Al and Na; stearyl alcohol, oleyl Sulfate ester salts of higher alcohols such as alcohols; Sulfate ester salts of polyethylene glycol ethers; Amide bond sulfate ester salts, ester bond sulfate ester salts, ester bond sulfonates, amide bond sulfonates, ether bond sulfonates, ether bond alkyl allyls Anionic surfactants such as sulfonates, ester-bonded alkylallylsulfonates, amide-bonded alkylallylsulfonates; mono- or diesters of orthophosphoric acid and oleyl alcohol, stearyl alcohol, etc., or a mixture of both, Phosphates such as acid type or alkali metal salts or amine salts; vinylethoxysilane, vinyl-tris (2-methoxy-ethoxy) silane, gamma-methacryloxypropyltrimethoxysilane, gamma-aminopropyltrimethoxy Silane, beta- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-
Silane coupling agents such as mercaptopropyltrimethoxysilane; titanate coupling agents such as isopropyl triisostearoyl titanate, isopropyl tris (dioctyl pyrophosphate) titanate, isopropyl tridecylbenzenesulfonyl titanate; acetoalkoxyaluminum diisopropylate Aluminum-based coupling agents such as; esters of alcohols and fatty acids such as glycerin monostearate and glycerin monooleate.

【0013】表面処理剤による式(1)の酸化マグネシ
ウム系固溶体の表面コーティング処理は、それ自体公知
の方法により実施できる。例えば、酸化マグネシウム系
固溶体の粉末をヘンシェルミキサー等の混合機により十
分撹拌下に表面処理剤を液状、エマルジョン状、固形状
で加え、加熱または非加熱下に十分に混合すればよい。
表面処理剤の添加量は、適宜選択できるが、通常酸化マ
グネシウム系固溶体の重量に基づいて約0.1〜約10
重量%である。表面処理した後は、造粒、乾燥、粉砕、
分級等の手段を適宜選択して実施し、最終製品の形態と
される。
The surface coating treatment of the magnesium oxide type solid solution of the formula (1) with the surface treating agent can be carried out by a method known per se. For example, the surface treatment agent may be added in the form of liquid, emulsion or solid with sufficient stirring of a magnesium oxide solid solution powder with a mixer such as a Henschel mixer, and the mixture may be sufficiently mixed with or without heating.
The addition amount of the surface treatment agent can be appropriately selected, but is usually about 0.1 to about 10 based on the weight of the magnesium oxide solid solution.
% By weight. After surface treatment, granulation, drying, crushing,
Means such as classification are appropriately selected and implemented to obtain the final product form.

【0014】本発明の酸化マグネシウム系固溶体は、酸
化マグネシウムと同様に強い塩基性を示し、したがって
酸、ハロゲンと良く反応し、それらを中和し不活性化す
る。このため、樹脂やゴム中に存在するモノマー、製造
工程、添加剤、チーグラーナッタ触媒やフリーデルクラ
フト触媒等の触媒、後ハロゲン化、熱分解等に由来する
ハロゲン、酸性物質と反応して、これらを不活性化し、
その結果として樹脂やゴムの耐熱性、耐紫外線性等の耐
候性等を改善する。
The magnesium oxide-based solid solution of the present invention exhibits strong basicity like magnesium oxide, and therefore reacts well with acids and halogens to neutralize and inactivate them. Therefore, it reacts with monomers present in resins and rubbers, manufacturing processes, additives, catalysts such as Ziegler-Natta catalysts and Friedel-Crafts catalysts, halogens derived from post-halogenation, thermal decomposition, etc. Inactivate the
As a result, the heat resistance of resins and rubbers, weather resistance such as ultraviolet resistance, etc. are improved.

【0015】この様な利用分野の具体的例としては、例
えば、ポリエチレン、ポリプロピレン、4−メチルペン
テン−1、EPDM等のチーグラーナッタ触媒で重合さ
れた樹脂またはゴム中に残存する触媒残渣の中和、AB
S中の酸性成分の中和、ポリアセタール中のフリーデル
クラフト触媒残渣の中和、有機ハロゲン系難燃剤から遊
離してくるハロゲンの中和、ポリアミド中の酸性成分の
中和、ポリ塩化ビニルの熱安定剤(脱離してくるHCl
の中和)、ポリ塩化ビニリデンの熱安定剤、ポリ酢酸ビ
ニルおよびエチレンと酢酸ビニルとの共重合体から遊離
する酢酸の中和による熱安定化と酢酸臭の除去、ポリフ
ェニレンサルファイドの熱安定剤(発生する硫化水素の
中和、不活性化)、クロロプレンゴム、ハロゲン化ブチ
ルゴム、クロロスルホン化ポリエチレンゴム、エピクロ
ルヒドリンゴム、フッ素ゴム、塩素化ポリエチレン等の
ハロゲン化ゴムの加硫時の受酸剤、FRPに使用するポ
リエステル、フェノール樹脂等の増粘剤等が例示され
る。
Specific examples of such fields of use include neutralization of catalyst residues remaining in a resin or rubber polymerized with a Ziegler-Natta catalyst such as polyethylene, polypropylene, 4-methylpentene-1, EPDM. , AB
Neutralization of acidic components in S, neutralization of Friedel-Crafts catalyst residues in polyacetal, neutralization of halogens liberated from organic halogen flame retardants, neutralization of acidic components in polyamide, heat of polyvinyl chloride Stabilizer (desorbed HCl
Neutralization), heat stabilizer for polyvinylidene chloride, heat stabilization by neutralization of acetic acid liberated from polyvinyl acetate and copolymers of ethylene and vinyl acetate and removal of acetic acid odor, heat stabilizer for polyphenylene sulfide ( Neutralization and inactivation of generated hydrogen sulfide), chloroprene rubber, halogenated butyl rubber, chlorosulfonated polyethylene rubber, epichlorohydrin rubber, fluorine rubber, acid acceptor for vulcanization of halogenated rubber such as chlorinated polyethylene, FRP Examples of the thickeners such as polyester and phenol resin used for the above.

【0016】本発明で用いる式(1)の酸化マグネシウ
ム系固溶体は、本発明者の発明にかかる式(3) Mg1-x2+ x(OH)2 (3) (式中、M2+とxは式(1)と同じ意味を表す)で示さ
れる水酸化マグネシウム系固溶体を約400〜1000
℃で約0.1〜10時間、大気、窒素、ヘリウム、アル
ゴン等の雰囲気下または真空下に焼成することにより製
造される。
The magnesium oxide type solid solution of the formula (1) used in the present invention is represented by the formula (3) Mg 1-x M 2+ x (OH) 2 (3) (wherein M 2 + And x represent the same meaning as in the formula (1)), and the magnesium hydroxide solid solution represented by the formula (1) is about 400 to 1000.
It is produced by baking at 0.1 ° C. for about 0.1 to 10 hours in the atmosphere, atmosphere of nitrogen, helium, argon or the like or under vacuum.

【0017】式(3)の水酸化マグネシウム系固溶体
は、種々の方法で製造される。例えばMgイオンとM2+
イオンとを含有する水溶液にMgとM2+との合計当量に
対しほぼ1当量以下、好ましくは0.95当量以下のア
ルカリを、好ましくは約40℃以下で撹拌下に加えて沈
澱させる共沈法で製造される。他の方法として、酸化マ
グネシウムおよび/または水酸化マグネシウムとM2+
含有する水溶液を混合し、反応させる方法によっても製
造される。さらに他の方法として、マグネシウムとM2+
のアルコラートの加水分解によるゾルーゲル法によって
も製造される。前記反応生成物はさらに結晶成長、分散
を改良するためにオートクレーブを用いて母液または塩
化カルシウムや塩化ナトリウムの共存下または非共存下
に約100〜250℃で加温、加圧してもよい。
The magnesium hydroxide-based solid solution of the formula (3) can be produced by various methods. For example, Mg ion and M 2+
Coprecipitation in which an aqueous solution containing ions is added with an alkali of about 1 equivalent or less, preferably 0.95 equivalent or less with respect to the total equivalent of Mg and M 2+ , with stirring, preferably at about 40 ° C. or less, with stirring. Manufactured by law. As another method, it can also be produced by a method of mixing magnesium oxide and / or magnesium hydroxide with an aqueous solution containing M 2+ and reacting them. Yet another method is magnesium and M 2+
It is also produced by the sol-gel method by hydrolysis of the alcoholate. The reaction product may be further heated and pressurized at about 100 to 250 ° C. in the presence or absence of mother liquor or calcium chloride or sodium chloride in an autoclave in order to improve crystal growth and dispersion.

【0018】本発明で用いられる樹脂およびゴムの例と
しては、例えばポリエチレン、エチレンと他のα−オレ
フィンとの共重合体、エチレンと酢酸ビニル、アクリル
酸エチルまたはアクリル酸メチルとの共重合体、ポリプ
ロピレン、プロピレンと他のα−オレフィンとの共重合
体、ポリブテン−1、4−メチルペンテン−1、ポリス
チレン、スチレンとアクリロニトリル、エチレンとプロ
ピレンジエンゴムまたはブタジエンとの共重合体、ポリ
酢酸ビニル、ポリビニルアルコール、ポリアクリレー
ト、ポリメタクリレート、ポリウレタン、ポリエステ
ル、ポリエーテル、ポリアミド、ABS、ポリカーボネ
ート、ポリフェニレンサルファイド等の熱可塑性樹脂、
フェノール樹脂、メラミン樹脂、エポキシ樹脂、不飽和
ポリエステル樹脂、アルキド樹脂等の熱硬化性樹脂、E
PDM、SBR、NBR、ブチルゴム、クロロプレンゴ
ム、イソプレンゴム、クロロスルホン化ポリエチレンゴ
ム、シリコンゴム、フッ素ゴム、塩素化ブチルゴム、臭
素化ブチルゴム、エピクロルヒドリンゴム、塩素化ポリ
エチレン等が例示される。
Examples of the resins and rubbers used in the present invention include polyethylene, copolymers of ethylene with other α-olefins, copolymers of ethylene with vinyl acetate, ethyl acrylate or methyl acrylate, Polypropylene, copolymer of propylene and other α-olefins, polybutene-1,4-methylpentene-1, polystyrene, styrene and acrylonitrile, copolymer of ethylene and propylene diene rubber or butadiene, polyvinyl acetate, polyvinyl Thermoplastic resins such as alcohol, polyacrylate, polymethacrylate, polyurethane, polyester, polyether, polyamide, ABS, polycarbonate, polyphenylene sulfide,
Thermosetting resin such as phenol resin, melamine resin, epoxy resin, unsaturated polyester resin, alkyd resin, E
PDM, SBR, NBR, butyl rubber, chloroprene rubber, isoprene rubber, chlorosulfonated polyethylene rubber, silicone rubber, fluororubber, chlorinated butyl rubber, brominated butyl rubber, epichlorohydrin rubber, chlorinated polyethylene and the like are exemplified.

【0019】本発明において、樹脂および/またはゴム
に対する式(1)の酸化マグネシウム系固溶体の配合量
は、樹脂やゴムの種類、および含有するハロゲンおよび
酸の種類によって適宜変更される。通常樹脂および/ま
たはゴム100重量部に対して表面処理した、または処
理しない式(1)酸化マグネシウム系固溶体の約0.0
01〜約20重量部、好ましくは約0.01〜約10重
量部が配合される。
In the present invention, the compounding amount of the magnesium oxide type solid solution of the formula (1) with respect to the resin and / or the rubber is appropriately changed depending on the kind of the resin or the rubber and the kind of the halogen and the acid contained therein. Approximately 0.0 of the magnesium oxide solid solution of the formula (1) surface treated or not treated with 100 parts by weight of resin and / or rubber.
01 to about 20 parts by weight, preferably about 0.01 to about 10 parts by weight is blended.

【0020】樹脂および/またはゴムと式(1)の酸化
マグネシウム系固溶体との混合、混練方法には特別の制
約はなく、両者を均一に混合できる方法であればよい。
例えば、一軸または二軸押出機、ロール、バンバリミキ
サー等により混合、混練される。成形方法にも特別の制
約はなく、樹脂およびゴムの種類、所望成形品の種類等
に応じてそれ自体公知の成形手段を任意に採用できる。
例えば射出成形、押出成形、ブロー成形、プレス成形、
回転成形、カレンダー成形、シートフォーミング成形、
トランスファー成形、積層成形、真空成形等である。
There are no particular restrictions on the method of mixing and kneading the resin and / or rubber with the magnesium oxide-based solid solution of the formula (1), as long as they can be uniformly mixed.
For example, they are mixed and kneaded by a single-screw or twin-screw extruder, a roll, a Banbury mixer, or the like. There is no particular restriction on the molding method, and any known molding means can be arbitrarily adopted depending on the types of resin and rubber, the type of desired molded product, and the like.
For example, injection molding, extrusion molding, blow molding, press molding,
Rotational molding, calendar molding, sheet forming molding,
Examples include transfer molding, laminated molding, and vacuum molding.

【0021】本発明の熱伝導性樹脂および/またはゴム
組成物は、上記成分以外にも慣用の他の添加剤を配合し
てもよい。このような添加剤としては、例えば酸化防止
剤、紫外線吸収剤、加硫剤、加硫促進剤、帯電防止剤、
顔料、滑剤、架橋剤、亜鉛の有機酸塩類、β−ジケトン
類、有機錫類、フォスファイト類、多価アルコールの部
分エステル類等の塩化ビニルの熱安定剤、発泡剤、可塑
剤、充填剤等が例示される。
The heat conductive resin and / or rubber composition of the present invention may contain other conventional additives in addition to the above components. Examples of such additives include antioxidants, ultraviolet absorbers, vulcanizing agents, vulcanization accelerators, antistatic agents,
Pigment, lubricant, cross-linking agent, organic salt of zinc, β-diketone, organotin, phosphite, vinyl ester heat stabilizer such as partial ester of polyhydric alcohol, foaming agent, plasticizer, filler Etc. are illustrated.

【0022】本発明の複合金属酸化物は、樹脂および/
またはゴム類に配合して、それらに含まれる酸性物質お
よび/またはハロゲンと速やかにかつ長時間反応して熱
安定性を改善したり、ハロゲン含有ゴムの加硫に作用し
たり、不飽和ポリエステルのプレゲル形成に作用した
り、塩ビ等の熱安定性、耐候性を延長したり、樹脂とか
ゴムの臭いを除去したりする作用を有しており、樹脂お
よび/またはゴム用受酸剤、加硫剤、増粘剤、熱安定
剤、消臭剤、耐候性改良剤として有用である。
The composite metal oxide of the present invention is a resin and / or
Alternatively, it may be blended with rubbers to react with acidic substances and / or halogens contained in them rapidly and for a long time to improve thermal stability, to act on vulcanization of halogen-containing rubbers, and to It acts to form a pregel, extends the thermal stability and weather resistance of PVC, etc., and removes the odor of resin and rubber. Acid acceptors for resins and / or rubber, vulcanization It is useful as an agent, a thickener, a heat stabilizer, a deodorant, and a weather resistance improver.

【0023】以下実施例に基づき本発明をより詳細に説
明する。以下の各例において、部は特に断りの無い限り
重量部を意味する。 実施例1、2 塩化マグネシウムと硝酸亜鉛の混合水溶液(Mg2+
1.9モル/リットル、Zn2+=0.035モル/リット
ル、20℃)5リットルを約10リットルのステンレス
製丸型反応槽に入れ、ケミスターラーで撹拌しつつ、2
モル/リットルの水酸化カルシウム(20℃)を4.3
5リットル(MgとZnの合計当量の約0.9当量に相
当)加えて反応させた。得られた白色沈澱を含むスラリ
ーを反応母液と共にオートクレーブに入れ、110℃で
2時間加温加圧処理した。その合計、脱水、水洗、乾
燥、粉砕した。この物の化学組成はMg0.98Zn
0.02(OH)2である、粉末X線の回折パターンはMg
(OH)2と同様の回折パターンを示した。
The present invention will be described in more detail based on the following examples. In the following examples, parts mean parts by weight unless otherwise specified. Examples 1 and 2 Mixed aqueous solution of magnesium chloride and zinc nitrate (Mg 2+ =
1.9 mol / l, Zn 2+ = 0.035 mol / l, 20 ° C.) 5 liters were placed in a stainless steel round reaction tank of about 10 liters, and stirred with a chemistirrer.
Mol / l calcium hydroxide (20 ° C) 4.3
5 liters (corresponding to about 0.9 equivalent of the total equivalent of Mg and Zn) were added and reacted. The slurry containing the obtained white precipitate was put into an autoclave together with the reaction mother liquor, and heated and pressurized at 110 ° C. for 2 hours. The total, dehydration, washing with water, drying and crushing were carried out. The chemical composition of this product is Mg 0.98 Zn
The powder X-ray diffraction pattern of 0.02 (OH) 2 is Mg
The diffraction pattern was similar to that of (OH) 2 .

【0024】この複合金属水酸化物を空気雰囲気中シリ
コニット炉を用いて500℃、5分間(実施例1)、7
50℃、30分間(実施例2)それぞれ焼成した。得ら
れた複合金属酸化物の化学組成、粉末X線回折、BET
比表面積、平均2次粒子径を測定した。結果を表1に示
す。
This composite metal hydroxide was heated in an atmosphere of silicon using a silicon knit furnace at 500 ° C. for 5 minutes (Example 1), 7
Firing was performed at 50 ° C. for 30 minutes (Example 2). Chemical composition, powder X-ray diffraction, BET of the obtained composite metal oxide
The specific surface area and the average secondary particle diameter were measured. The results are shown in Table 1.

【0025】以下の例を含め、化学組成はキレート滴定
法により、BET比表面積は窒素吸着法により、平均2
次粒子径は試料をアルコールに加えて超音波で十分分散
させた後マイクロトラック粒度分析計によりそれぞれ測
定した。
Including the following examples, the chemical composition was determined by the chelate titration method, and the BET specific surface area was determined by the nitrogen adsorption method on average of 2
The secondary particle diameter was measured by a Microtrac particle size analyzer after the sample was added to alcohol and sufficiently dispersed by ultrasonic waves.

【0026】実施例3、4 塩化マグネシウムと塩化ニッケルの混合水溶液(Mg2+
=1.73モル/リットル、Ni2+=0.27モル/リッ
トル、15℃)5リットルを約10リットルのステンレ
ス製丸型反応槽に入れ、ケミスターラーで撹拌しつつ、
2モル/リットルの水酸化カルシウム(15℃)を4.
5リットル(MgとZnの合計当量の約0.9当量に相
当)加えて反応させた。得られた白色沈澱を含むスラリ
ーを反応母液と共にオートクレーブに入れ、120℃で
1時間加温加圧処理した。その合計、脱水、水洗、乾
燥、粉砕した。この物の化学組成はMg0.85Ni
0.15(OH)2であった。粉末X線回折パターンはMg
(OH)2と同様の回折パターンを示した。
Examples 3, 4 Mixed aqueous solution of magnesium chloride and nickel chloride (Mg 2+
= 1.73 mol / l, Ni 2+ = 0.27 mol / l, 15 ° C.) 5 liters were placed in a stainless steel round reaction tank of about 10 liters, and stirred with a chemister stirrer,
2. Add 2 mol / l calcium hydroxide (15 ° C) 4.
5 liters (corresponding to about 0.9 equivalent of the total equivalent of Mg and Zn) were added and reacted. The slurry containing the obtained white precipitate was put into an autoclave together with the reaction mother liquor, and heated and pressurized at 120 ° C. for 1 hour. The total, dehydration, washing with water, drying and crushing were carried out. The chemical composition of this product is Mg 0.85 Ni
It was 0.15 (OH) 2 . Powder X-ray diffraction pattern is Mg
The diffraction pattern was similar to that of (OH) 2 .

【0027】この複合金属水酸化物を空気雰囲気中シリ
コニット炉を用いて500℃、5分間(実施例3)、7
50℃、30分間(実施例4)それぞれ焼成した。得ら
れた複合金属酸化物の化学組成、粉末X線回折、BET
比表面積、平均2次粒子径を測定した。結果を表1に示
す。
This composite metal hydroxide was heated in an air atmosphere using a silicon knit furnace at 500 ° C. for 5 minutes (Example 3), 7
Firing was performed at 50 ° C. for 30 minutes (Example 4). Chemical composition, powder X-ray diffraction, BET of the obtained composite metal oxide
The specific surface area and the average secondary particle diameter were measured. The results are shown in Table 1.

【0028】実施例5 砂濾過、脱炭酸処理した海水150リットル(Mg2+
0.052モル/リットル、12℃)を容量200リッ
トルの反応槽に入れ、撹拌機で撹拌しつつ塩化第2銅を
0.15モル加え、溶解した。1モル/リットルの水酸
化カルシウムを7.02リットル(MgとCaの合計当
量の0.88当量に相当、15℃)加えて反応させた。
濾過、脱水後、2モル/リットルの塩化カルシウム水溶
液に乳化し、100℃で1時間加熱した。その後脱水、
水洗、乾燥、粉砕した。この物の化学組成はMg0.96
0.04(OH)2であった。粉末X線回折パターンはM
g(OH)2と同様のパターンを示した。
Example 5 150 liters of seawater filtered with sand and decarbonated (Mg 2+ =
(0.052 mol / liter, 12 ° C.) was placed in a reaction tank having a capacity of 200 liters, and 0.15 mol of cupric chloride was added and dissolved while stirring with a stirrer. 7.02 liters (corresponding to 0.88 equivalents of the total equivalents of Mg and Ca, 15 ° C.) of 1 mol / liter of calcium hydroxide was added and reacted.
After filtration and dehydration, the mixture was emulsified in a 2 mol / liter calcium chloride aqueous solution and heated at 100 ° C. for 1 hour. Then dehydration,
Washed with water, dried and crushed. The chemical composition of this product is Mg 0.96 C
It was u 0.04 (OH) 2 . Powder X-ray diffraction pattern is M
It showed a pattern similar to g (OH) 2 .

【0029】この複合金属水酸化物を空気中、シリコニ
ット炉を用いて、750℃で30分間焼成した。この酸
化物の試験結果を表1に示す。
This composite metal hydroxide was fired in air at 750 ° C. for 30 minutes using a silicon knit furnace. The test results of this oxide are shown in Table 1.

【0030】実施例6 沸騰させた後、窒素ガスを吹込み脱酸素処理した脱イオ
ン水に硝酸マグネシウムと塩化コバルトを溶解し、Mg
2+=1.0モル/リットル、Co2+=0.20モル/リッ
トルの混合水溶液6リットルを、容量10リットルの反
応槽に入れ撹拌しながら、窒素ガス雰囲気中で4モル/
リットルの水酸化ナトリウムを3リットル(20℃)加
えて反応させた。反応物を母液と共に窒素ガス雰囲気中
98℃で3時間加熱後、濾過、水洗、乾燥、粉砕した。
この物の化学組成はMg0.80Co0.20(OH)2であっ
た。粉末X線回折パターンは、Mg(OH)2と同様の
パターンを示した。
Example 6 Magnesium nitrate and cobalt chloride were dissolved in deionized water which had been deoxidized by blowing nitrogen gas after boiling,
6 liters of a mixed aqueous solution of 2+ = 1.0 mol / liter and Co 2+ = 0.20 mol / liter was placed in a reaction tank having a volume of 10 liters while stirring and 4 mol / liter in a nitrogen gas atmosphere.
3 liters of sodium hydroxide (20 ° C.) was added and reacted. The reaction product was heated with a mother liquor in a nitrogen gas atmosphere at 98 ° C. for 3 hours, then filtered, washed with water, dried and pulverized.
The chemical composition of this product was Mg 0.80 Co 0.20 (OH) 2 . The powder X-ray diffraction pattern showed the same pattern as Mg (OH) 2 .

【0031】この複合金属水酸化物を窒素雰囲気中、シ
リコニット炉を用いて、450℃で5分間焼成した。こ
の酸化物の試験結果を表1に示す。
This composite metal hydroxide was fired at 450 ° C. for 5 minutes in a nitrogen atmosphere using a silicon knit furnace. The test results of this oxide are shown in Table 1.

【0032】実施例7、8 脱酸素処理した脱イオン水に塩化マグネシウムと塩化マ
ンガン(実施例7)または硫酸第1鉄(実施例8)を溶
解した混合水溶液4リットル(15℃)を容量10リッ
トルの反応槽に入れ、撹拌しながら脱酸素処理した2モ
ル/リットルの水酸化ナトリウム4リットルを加えて反
応させた。得られた反応物を母液と共にオートクレーブ
に入れ、140℃で2時間加温加圧後、濾過、水洗、乾
燥、粉砕した。以上の操作は全て窒素ガス雰囲気下で実
施した。この物の化学組成はMg0.90Mn0.10(OH)
2(実施例7)およびMg0.90Fe0.10(OH)2(実施
例8)であった。これらの粉末X線回折パターンはMg
(OH)2と同様のパターンを示した。これらの複合金
属水酸化物をシリコニット炉を用いて窒素雰囲気中、8
00℃で30分間焼成した。試験結果を表1に示す。
Examples 7 and 8 4 liters (15 ° C.) of a mixed aqueous solution prepared by dissolving magnesium chloride and manganese chloride (Example 7) or ferrous sulfate (Example 8) in deionized water that had been deoxygenated had a volume of 10 It was placed in a liter reaction tank, and 4 liters of 2 mol / liter sodium hydroxide deoxidized while stirring was added and reacted. The obtained reaction product was placed in an autoclave together with the mother liquor, and heated and pressurized at 140 ° C. for 2 hours, filtered, washed with water, dried and pulverized. All the above operations were carried out under a nitrogen gas atmosphere. The chemical composition of this product is Mg 0.90 Mn 0.10 (OH)
2 (Example 7) and Mg 0.90 Fe 0.10 (OH) 2 (Example 8). These powder X-ray diffraction patterns are Mg
A pattern similar to that of (OH) 2 was shown. These composite metal hydroxides were placed in a silicon atmosphere in a nitrogen atmosphere at 8
It was baked at 00 ° C. for 30 minutes. The test results are shown in Table 1.

【0033】比較例1、2 市販の高活性酸化マグネシウムおよび中活性酸化マグネ
シウム2種類の試験結果を表1に示す。
Comparative Examples 1 and 2 Table 1 shows the test results of two types of commercially available high activity magnesium oxide and medium activity magnesium oxide.

【0034】比較例3 実施例1において、Mg2+=1.1モル/リットル、Z
2+=0.3モル/リットルの混合水溶液(10℃)6
リットルと、2モル/リットルの水酸化カルシウム(1
0℃)3リットルとを反応させた以外は、実施例1と同
様に操作して水酸化物を製造した。得られた水酸化物の
粉末X線回折パターンは、水酸化マグネシウムと同様の
Mg1-xZnx(OH)2と(0.3−x)Zn(OH)
1.6Cl0.4との混合物のパターンを示した。Zn/Mg
のモル比は0.30であった。この物を500℃で5分
間焼成した物の試験結果を表1に示す。
Comparative Example 3 In Example 1, Mg 2+ = 1.1 mol / liter, Z
n 2+ = 0.3 mol / liter mixed aqueous solution (10 ° C.) 6
Liter and 2 mol / liter calcium hydroxide (1
Hydroxide was produced in the same manner as in Example 1 except that 3 liters (0 ° C.) were reacted. The powder X-ray diffraction pattern of the obtained hydroxide is similar to that of magnesium hydroxide: Mg 1-x Zn x (OH) 2 and (0.3-x) Zn (OH) 2.
The pattern of the mixture with 1.6 Cl 0.4 was shown. Zn / Mg
The molar ratio of was 0.30. Table 1 shows the test results of the product obtained by firing the product at 500 ° C. for 5 minutes.

【0035】比較例4 実施例3において、混合水溶液としてMg2+=0.54
モル/リットル、Ni2+=1.26モル/リットルを用
いた以外は実施例3と同様に操作して水酸化物を得た。
この物の化学組成はMg0.30Ni0.70(OH)2であっ
た。粉末X線回折パターンはMg(OH)2と同様であ
った。この複合水酸化物を窒素雰囲気中、500℃で5
分間焼成した。酸化物の試験結果を表1に示す。
Comparative Example 4 In Example 3, Mg 2+ = 0.54 as a mixed aqueous solution.
A hydroxide was obtained in the same manner as in Example 3 except that mol / liter and Ni 2+ = 1.26 mol / liter were used.
The chemical composition of this product was Mg 0.30 Ni 0.70 (OH) 2 . The powder X-ray diffraction pattern was similar to that of Mg (OH) 2 . This composite hydroxide is heated at 500 ° C in a nitrogen atmosphere at 5 ° C.
Bake for minutes. The oxide test results are shown in Table 1.

【0036】 表1 例 粉末X線回折 BET比表面積 平均2次粒子径 (m2/g) (μm) 実施例1 MgOと同じ 181 0.24 2 MgOと同じ 42 0.27 3 MgOと同じ 220 0.31 4 MgOと同じ 40 0.33 5 MgOと同じ 44 0.30 6 MgOと同じ 212 0.72 7 MgOと同じ 34 0.63 8 MgOと同じ 32 0.48 比較例1 MgOと同じ 148 5.52 2 MgOと同じ 32 4.16 3 MgOとZnO 126 1.73 4 MgOと同じ 141 0.46Table 1 Example Powder X-ray diffraction BET specific surface area Average secondary particle size (M 2 / g) (μm) Example 1 Same as MgO 181 0.22 2 Same as MgO 42 0.27 3 Same as MgO 220 0.31 4 Same as MgO 40 0.33 5 Same as MgO 44 44. 30 6 Same as MgO 212 0.72 7 Same as MgO 34 0.63 8 Same as MgO 32 0.48 Comparative Example 1 Same as MgO 148 5.52 2 Same as MgO 32 4.16 3 MgO and ZnO 126 1. 73 4 Same as MgO 141 0.46

【0037】実施例9(クロロプレンゴムの受酸剤) クロロプレンゴムに受酸剤として、表2に示す酸化マグ
ネシウム系化合物を下記の通りに配合した。 クロロプレンゴム(昭和電工デュポン(株)製、Neoprene GS) 100部 受酸剤 4部 酸化亜鉛(正同化学(株)製、亜鉛華1号) 5部 ステアリン酸(和光純薬(株)製、試薬1級) 1部 カーボンブラック(東海電極(株)製、シーストS) 30部 上記配合物を、オープンロールを用いて均一に混合後、
ムーニースコーチ試験を行うと共に、153℃で30分
間プレス加硫して物性を測定した。試験結果を表2に示
す。
Example 9 (Acid acceptor for chloroprene rubber) Magnesium oxide compounds shown in Table 2 were blended as an acid acceptor with chloroprene rubber as follows. Chloroprene rubber (Showa Denko DuPont Co., Ltd., Neoprene GS) 100 parts Acid acceptor 4 parts Zinc oxide (Shodo Chemical Co., Ltd., Zinc Hua No. 1) 5 parts Stearic acid (Wako Pure Chemical Industries, Ltd., Reagent grade 1) 1 part Carbon black (Tokai Electrode Co., Ltd., Seast S) 30 parts After uniformly mixing the above components using an open roll,
A Mooney scorch test was conducted, and physical properties were measured by press vulcanization at 153 ° C. for 30 minutes. The test results are shown in Table 2.

【0038】本発明の酸化マグネシウム系固溶体は、酸
化マグネシウムと比較して、著しく改善された貯蔵安定
性(ムーニースコーチ性)を示すと共に、加硫後のゴム
物性が改善されていた。特に耐水性、圧縮永久歪、モジ
ュラスが改善されていた。
The magnesium oxide-based solid solution of the present invention exhibited significantly improved storage stability (mooney scorch property) and improved rubber physical properties after vulcanization, as compared with magnesium oxide. In particular, water resistance, compression set, and modulus were improved.

【0039】 表2 酸化マグネシウム系化合物の種類 実施例 比較例 1 3 6 1 3 4 貯蔵安定性 オリジナル 最小粘度Vm(ムーニー) 30.4 30.9 29.9 29.0 29.2 29.5 T5 34.8 35.7 34.0 31.2 30.7 26.2 T35 62.0 65.7 61.8 50.5 48.0 36.5 加硫ゴムの物性 100%モジュラス 30 32 30 27 26 24 300%モジュラス 125 130 114 109 102 95 引張強さ 215 220 219 207 199 190 伸び(%) 520 518 522 540 558 565 硬度 66 67 67 65 64 62 圧縮永久歪(%) 54.6 53.2 54.5 56.3 57.0 57.9 耐水性 9.5 6.2 5.3 10.6 10.4 4.5 注:貯蔵安定性;ムーニースコーチ、125℃ 圧縮永久歪;100℃、22時間後 耐水性;70℃で7日間浸漬後の体積増加率(%)。 単位:モジュラス(kgf/cm2)、引張強さ(kg
f/cm2
Table 2 Types of magnesium oxide compounds Examples Comparative Example 1 3 6 1 3 4 Storage stability Original minimum viscosity Vm (Moonie) 30.4 30.9 29.9 29.0 29.2 29.5 T 5 34.8 35.7 34.0 31.2 30.7 26.2 T 35 62.0 65.7 61.8 50.5 48.0 36.5 Physical properties of vulcanized rubber 100% modulus 30 32 30 27 26 24 300% modulus 125 130 114 109 102 95 Tensile strength 215 220 219 207 199 190 Elongation (%) 520 518 522 540 558 565 Hardness 66 67 67 65 64 62 Compression set (%) 54.6 53.2 54.5 56.3 57.0 57.9 Water resistance 9.5 6.2 5.3 10.6 10.4 4.5 Note: Storage stability; Mooney scorch, 125 ° C Compression set; 100 ° C, after 22 hours Water resistance; 7 at 70 ° C Volume increase rate (%) after immersion for a day. Unit: modulus (kgf / cm 2 ), tensile strength (kg
f / cm 2 )

【0040】実施例10(ポリエステル樹脂の増粘剤と
しての利用) ポリエステル樹脂のSMC(シートモールディングコン
パウンド)用増粘剤としての性能を調べるため、不飽和
ポリエステル樹脂(日本触媒(株)製、エポラックN−2
1)100部、炭酸カルシウム(日東粉化(株)製、NS
−100)、酸化マグネシウム系増粘剤1.0部をホモ
ジナイザーで2分間混合後、30℃のオーブンに入れ、
粘度の経時変化をブルックフィールド粘度計を用いて測
定した。試験結果を図1に示す。図1中、記号1は実施
例2の複合金属酸化物を添加した場合、記号2は実施例
4の複合金属酸化物を添加した場合を示す。記号3は比
較例2で使用した市販酸化マグネシウムを添加した場合
を示す。理想的な増粘剤としては、初期粘度が低く、そ
の後S字型のシャープな増粘性を示し、かつ最終到達粘
度が高いことである。図1から、本発明の酸化マグネシ
ウム系固溶体は、市販酸化マグネシウムよりも理想に近
い増粘剤であることがわかる。
Example 10 (Use of Polyester Resin as Thickening Agent) In order to investigate the performance of the polyester resin as a thickening agent for SMC (sheet molding compound), unsaturated polyester resin (Nippon Shokubai Co., Ltd., Epolak) was used. N-2
1) 100 parts, calcium carbonate (Nitto Koka Co., Ltd., NS
-100), 1.0 part of the magnesium oxide-based thickener was mixed with a homogenizer for 2 minutes and then placed in an oven at 30 ° C.
The change in viscosity with time was measured using a Brookfield viscometer. The test results are shown in FIG. 1, symbol 1 shows the case where the composite metal oxide of Example 2 was added, and symbol 2 shows the case where the composite metal oxide of Example 4 was added. Reference numeral 3 shows the case where the commercially available magnesium oxide used in Comparative Example 2 was added. An ideal thickener is one that has a low initial viscosity, then shows a sharp S-shaped thickening, and has a high final viscosity. From FIG. 1, it can be seen that the magnesium oxide-based solid solution of the present invention is a thickener that is closer to the ideal than the commercially available magnesium oxide.

【0041】実施例11(EVAからの酢酸発生の抑制
と酢酸臭の抑制) EVA(三井デュポン(株)製、ELVALOY 74
1)100部に、酸化マグネシウム系化合物0.5部を
混合し、オープンロールを用いて約140℃で混練して
試料とした。この試料1.0gを窒素ガスフロー下にD
TA装置を用いて、200℃に昇温し、60分間維持し
て、熱分解により発生した酢酸を脱イオン水に吸収さ
せ、水酸化ナトリウムで中和滴定し、酢酸の量を定量し
た。試験結果を表3に示す。
Example 11 (Suppression of acetic acid generation from EVA and suppression of acetic acid odor) EVA (manufactured by Mitsui DuPont Co., Ltd., ELVALOY 74)
1) 0.5 part of a magnesium oxide compound was mixed with 100 parts and kneaded at about 140 ° C. using an open roll to prepare a sample. 1.0 g of this sample was placed under a nitrogen gas flow to obtain D
Using a TA device, the temperature was raised to 200 ° C. and maintained for 60 minutes, the acetic acid generated by thermal decomposition was absorbed in deionized water, and the amount of acetic acid was quantified by neutralization titration with sodium hydroxide. The test results are shown in Table 3.

【0042】 表3 MgO系化合物 酢酸発生量(mg/g−試料) 実施例1の試料 2.1 比較例1の試料 3.4 ブランク 5.8Table 3 MgO compound acetic acid generation amount (mg / g-sample) Sample of Example 1 2.1 Sample of Comparative Example 1 3.4 Blank 5.8

【0043】実施例12 下記配合のポリ塩化ビニル ポリ塩化ビニル(信越化学(株)製、分子量700) 100部 ステアリン酸亜鉛(正同化学(株)製) 0.5部 酸化マグネシウム系化合物 1.0部 をオープンロールを用い、170℃で混練した。このシ
ートの一部を試料として、180℃でコンゴーレッド法
(JIS K6723−1969)により熱安定時間を
測定した。試験結果を表4に示す。
Example 12 Polyvinyl chloride having the following composition Polyvinyl chloride (manufactured by Shin-Etsu Chemical Co., Ltd., molecular weight 700) 100 parts Zinc stearate (manufactured by Shodo Chemical Co., Ltd.) 0.5 parts Magnesium oxide compound 1. 0 part was kneaded at 170 ° C. using an open roll. Using a part of this sheet as a sample, the heat stabilization time was measured at 180 ° C. by the Congo red method (JIS K6723-1969). The test results are shown in Table 4.

【0044】 表4 MgO系熱安定剤 熱安定時間(分) Mg0.98Zn0.02O 18.7 Mg0.76Cu0.04O 20.6 Mg0.85Ni0.15O 19.4 MgO 12.1 無添加 4.9 表4から、本発明の酸化マグネシウム系固溶体は、酸化
マグネシウムに比して優れた熱安定性を示すことがわか
る。
[0044] 4.9 Table Table 4 MgO-based heat stabilizer thermal stabilization time (min) Mg 0.98 Zn 0.02 O 18.7 Mg 0.76 Cu 0.04 O 20.6 Mg 0.85 Ni 0.15 O 19.4 MgO 12.1 no addition From 4, it can be seen that the magnesium oxide-based solid solution of the present invention exhibits excellent thermal stability as compared with magnesium oxide.

【0045】[0045]

【発明の効果】本発明によれば、低毒性を維持して酸、
ハロゲンに対する反応性に優れ、かつ吸湿性の改善され
た新規な酸化マグネシウム系固溶体が提供される。該酸
化マグネシウム系固溶体は、樹脂および/またはゴム用
受酸剤、増粘剤、熱安定剤、消臭剤、耐候性改良剤とし
ての優れた特性を呈する。更に本発明によれば、上記酸
化マグネシウム系固溶体を配合した樹脂および/または
ゴム組成物が提供される。
According to the present invention, acid, which maintains low toxicity,
Provided is a novel magnesium oxide-based solid solution having excellent reactivity with halogen and improved hygroscopicity. The magnesium oxide-based solid solution exhibits excellent properties as an acid acceptor for resins and / or rubbers, a thickener, a heat stabilizer, a deodorant, and a weather resistance improver. Further, according to the present invention, there is provided a resin and / or rubber composition containing the above magnesium oxide-based solid solution.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明の酸化マグネシウム系固溶体が有する増
粘効果を示すグラフである。
FIG. 1 is a graph showing the thickening effect of the magnesium oxide-based solid solution of the present invention.

【符号の説明】[Explanation of symbols]

1 実施例2の複合金属酸化物 2 実施例4の複合金属酸化物 3 比較例2の市販酸化マグネシウム 1 Composite metal oxide of Example 2 2 Composite metal oxide of Example 4 3 Commercially available magnesium oxide of Comparative Example 2

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 FI 技術表示箇所 C08L 21/00 LBB 8218−4J 101/00 LSZ 7242−4J C09C 3/08 PBT 8218−4J ─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. 5 Identification code Internal reference number FI Technical display location C08L 21/00 LBB 8218-4J 101/00 LSZ 7242-4J C09C 3/08 PBT 8218-4J

Claims (8)

【特許請求の範囲】[Claims] 【請求項1】 100重量部の樹脂と0.001〜20
重量部の式(1) Mg1-x2+ xO (1) (式中、M2+はMn2+、Fe2+、Co2+、Ni2+、Cu
2+およびZn2+からなる群から選ばれた二価金属イオン
の少なくとも一種を示し、xは0.001<x<0.5の
範囲の数を示す)の酸化マグネシウム系固溶体である複
合金属酸化物とからなる樹脂および/またはゴム組成
物。
1. 100 parts by weight of resin and 0.001-20
Parts by weight of formula (1) Mg 1-x M 2+ x O (1) (wherein M 2+ is Mn 2+ , Fe 2+ , Co 2+ , Ni 2+ , Cu
2+ and Zn 2+ represents at least one divalent metal ion selected from the group consisting of 2+ and Zn 2+ , and x represents a number in the range of 0.001 <x <0.5). A resin and / or rubber composition comprising an oxide.
【請求項2】 式(1)の複合金属酸化物が、式(2) Mg1-x(Ni2+および/またはZn2+xO (2) (式中、xは式(1)と同じ意味を表す)の複合金属酸
化物である請求項1記載の樹脂および/またはゴム組成
物。。
2. The complex metal oxide of the formula (1) has the formula (2) Mg 1-x (Ni 2+ and / or Zn 2+ ) x O (2) (where x is the formula (1)). A resin and / or rubber composition according to claim 1, which is a mixed metal oxide having the same meaning as in (1) above. .
【請求項3】 式(1)の複合金属酸化物が、高級脂肪
酸類、リン酸エステル、シラン、チタネートおよびアル
ミニウム系カップリング剤、および多価アルコールと脂
肪酸のエステル類、高級脂肪酸の金属塩からなる群から
選ばれた表面処理剤の少なくとも一種で表面処理されて
なる請求項1記載の樹脂および/またはゴム組成物。
3. The complex metal oxide of the formula (1) comprises higher fatty acids, phosphoric acid esters, silanes, titanates and aluminum-based coupling agents, and esters of polyhydric alcohols and fatty acids and metal salts of higher fatty acids. The resin and / or rubber composition according to claim 1, which is surface-treated with at least one surface-treating agent selected from the group consisting of:
【請求項4】 ゴムが、クロロプレンゴム、クロロスル
ホン化ポリエチレンゴム、エピクロルヒドリンゴム、塩
素化または臭素化ブチルゴム、塩素化ポリエチレンゴム
およびフッ素ゴムから選ばれた少なくとも一種のゴムで
あり、複合金属酸化物が、該ゴムの受酸剤または加硫剤
である請求項1記載の樹脂および/またはゴム組成物。
4. The rubber is at least one rubber selected from chloroprene rubber, chlorosulfonated polyethylene rubber, epichlorohydrin rubber, chlorinated or brominated butyl rubber, chlorinated polyethylene rubber and fluororubber, and the composite metal oxide is The resin and / or rubber composition according to claim 1, which is an acid acceptor or a vulcanizing agent for the rubber.
【請求項5】 樹脂が、不飽和ポリエステル樹脂、ビニ
ル樹脂、フェノール樹脂から選ばれた少なくとも一種の
樹脂であり、複合金属酸化物が、該樹脂の増粘剤である
請求項1記載の樹脂および/またはゴム組成物。
5. The resin according to claim 1, wherein the resin is at least one resin selected from unsaturated polyester resin, vinyl resin and phenol resin, and the composite metal oxide is a thickener for the resin. / Or a rubber composition.
【請求項6】 BET比表面積が5〜300m2/gで
ある式(1) Mg1-x2+ xO (1) (式中、M2+はMn2+、Fe2+、Co2+、Ni2+、Cu
2+およびZn2+からなる群から選ばれた二価金属イオン
の少なくとも一種を示し、xは0.001<x<0.5の
範囲の数を示す)の酸化マグネシウム系固溶体である複
合金属酸化物。
6. A formula (1) Mg 1-x M 2+ x O (1) having a BET specific surface area of 5 to 300 m 2 / g (wherein M 2+ is Mn 2+ , Fe 2+ , Co) 2+ , Ni 2+ , Cu
2+ and Zn 2+ represents at least one divalent metal ion selected from the group consisting of 2+ and Zn 2+ , and x represents a number in the range of 0.001 <x <0.5). Oxide.
【請求項7】 マイクロトラック法で測定した平均2次
粒子径が0.1〜2.0μmである請求項6記載の複合金
属酸化物。
7. The composite metal oxide according to claim 6, which has an average secondary particle diameter of 0.1 to 2.0 μm measured by the Microtrac method.
【請求項8】 式(3) Mg1-x2+ x(OH)2 (3) の水酸化マグネシウム系固溶体を約400〜1000℃
で焼成することからなる請求項6記載複合金属酸化物の
製造方法。
8. A magnesium hydroxide-based solid solution of the formula (3) Mg 1-x M 2+ x (OH) 2 (3) is added at about 400 to 1000 ° C.
The method for producing a composite metal oxide according to claim 6, which comprises firing at.
JP10372592A 1992-03-30 1992-03-30 Composite metal oxide-containing resin composition and method for producing the oxide Expired - Fee Related JP3384816B2 (en)

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Cited By (9)

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US5759509A (en) * 1995-03-17 1998-06-02 Tateho Chemical Industries Co., Ltd. Metal hydroxide and oxide solid solutions having high aspect ratios and their processes for production
US5891945A (en) * 1995-06-02 1999-04-06 Tateho Chemical Industries, Co., Ltd. Magnesium hydroxide solid solutions, their production method and use
JP2003096298A (en) * 2001-09-25 2003-04-03 Toray Ind Inc Polyphenylene sulfide resin composition and condenser part
JP2003096299A (en) * 2001-09-25 2003-04-03 Toray Ind Inc Polyphenylene sulfide resin composition for resin molding and molded product
JP2005330641A (en) * 2004-04-23 2005-12-02 Chisso Corp Deodorant fiber, fiber molded article using the same, and fiber product
JP2008243707A (en) * 2007-03-28 2008-10-09 Ube Material Industries Ltd Zinc containing magnesium oxide calcined powder
JP2013194233A (en) * 2012-03-22 2013-09-30 Hitachi Cable Ltd Chlorine-containing resin composition, method for producing the same, and resin molded body, electric wire and cable using the same
JP2015124318A (en) * 2013-12-26 2015-07-06 東ソー株式会社 Chlorosulfonated polyolefin composition
EP2980021B1 (en) 2013-03-25 2018-10-10 Konoshima Chemical Co., Ltd. Magnesium oxide particles, resin composition, rubber composition, and molded article

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5759509A (en) * 1995-03-17 1998-06-02 Tateho Chemical Industries Co., Ltd. Metal hydroxide and oxide solid solutions having high aspect ratios and their processes for production
US5891945A (en) * 1995-06-02 1999-04-06 Tateho Chemical Industries, Co., Ltd. Magnesium hydroxide solid solutions, their production method and use
JP2003096298A (en) * 2001-09-25 2003-04-03 Toray Ind Inc Polyphenylene sulfide resin composition and condenser part
JP2003096299A (en) * 2001-09-25 2003-04-03 Toray Ind Inc Polyphenylene sulfide resin composition for resin molding and molded product
JP2005330641A (en) * 2004-04-23 2005-12-02 Chisso Corp Deodorant fiber, fiber molded article using the same, and fiber product
JP2008243707A (en) * 2007-03-28 2008-10-09 Ube Material Industries Ltd Zinc containing magnesium oxide calcined powder
KR101444462B1 (en) * 2007-03-28 2014-09-24 우베 마테리알즈 가부시키가이샤 Fired zinc-containing magnesium oxide powder
JP2013194233A (en) * 2012-03-22 2013-09-30 Hitachi Cable Ltd Chlorine-containing resin composition, method for producing the same, and resin molded body, electric wire and cable using the same
EP2980021B1 (en) 2013-03-25 2018-10-10 Konoshima Chemical Co., Ltd. Magnesium oxide particles, resin composition, rubber composition, and molded article
JP2015124318A (en) * 2013-12-26 2015-07-06 東ソー株式会社 Chlorosulfonated polyolefin composition

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