JPS6343964A - Inorganic powder having modified surface a resin composition containing the same - Google Patents

Inorganic powder having modified surface a resin composition containing the same

Info

Publication number
JPS6343964A
JPS6343964A JP61188098A JP18809886A JPS6343964A JP S6343964 A JPS6343964 A JP S6343964A JP 61188098 A JP61188098 A JP 61188098A JP 18809886 A JP18809886 A JP 18809886A JP S6343964 A JPS6343964 A JP S6343964A
Authority
JP
Japan
Prior art keywords
inorganic powder
powder
resin
modified inorganic
weight
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
Application number
JP61188098A
Other languages
Japanese (ja)
Inventor
Yasuhiro Onishi
康裕 大西
Hiroshi Yamanaka
山中 宏
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.)
Daihachi Chemical Industry Co Ltd
Original Assignee
Daihachi Chemical Industry Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Daihachi Chemical Industry Co Ltd filed Critical Daihachi Chemical Industry Co Ltd
Priority to JP61188098A priority Critical patent/JPS6343964A/en
Publication of JPS6343964A publication Critical patent/JPS6343964A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To provide a resin compsn. having excellent dispersibility, mechanical strength, electrical conductivity, magnetizability, flame retardance, etc., consisting of a resin and a specified inorg. powder having a modified surface. CONSTITUTION:A suspension obtd. by suspending inorg. powder having a particle size of 0.1-100mum (e.g., SiO2) in an equal volume or excees of an org. solvent (e.g., benzene) is mixed with 0.01-20wt% phosphorus-contg. silicon compd. of formula I [wherein R<1> and R<2> are each 1 1-18C alkyl, a (substd.) alkyl or a (substd.) aryl; Q is NH2 or a group of formula II, III or IV; R<3> is a 1-4C alkyl; l is 0-2; and a is 0 or 1]. The mixture is heated under reflux with stirring. The solid is separated from the liquid and dried under reduced pressure to obtain a surface-modified inorg. powder (B). A thermoplastic or thermosetting resin (1A) is blended with the component B.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、含燐ケイ素化合物により処理され。[Detailed description of the invention] (Industrial application field) The present invention is treated with a phosphorous-containing silicon compound.

各種樹脂中での分散性に優れた表面改質無機粉体。Surface-modified inorganic powder with excellent dispersibility in various resins.

および該粉体を含有する樹脂組成物に関する。and a resin composition containing the powder.

(従来の技術) 各種樹脂の強化、剛性の向上、熱伝導性の向上。(Conventional technology) Strengthening various resins, improving rigidity, and improving thermal conductivity.

導電性付与、帯磁性付与、難燃性の付与、増量などの目
的で、該樹脂に無機粉体を配合することが広く行われて
いる。しかし、樹脂中に無機粉体を配合すると■該樹脂
の成形性が悪くなるため配合量が制限される;■無機粉
体が充分に分散しないため、得られる成形品の各種性能
(例えば、難燃性、導電性、帯磁性)が充分ではない;
■無機粉体の不均一分散のため強度が低下する;などの
欠点がある。
It is widely practiced to blend inorganic powder into the resin for the purpose of imparting conductivity, magnetism, flame retardance, and increasing the amount of resin. However, when inorganic powder is blended into a resin, the moldability of the resin deteriorates, so the amount of inorganic powder added is limited; (flammability, conductivity, magnetism) are insufficient;
There are drawbacks such as: (1) strength decreases due to non-uniform dispersion of inorganic powder;

無機粉体や無機繊維を配合・含有する樹脂成形品の機械
的強度の低下を抑制するために、シランカップリング剤
が使用されている。例えば、アスベスト繊維やガラス繊
維をシランカップリング剤で処理するとこれらの繊維表
面にシランカップリング剤が化学的に結合し、その結果
、該繊維と樹脂とを混合したときの接着性が高まりa械
的強度が向上する。しかし、シランカップリング処理を
行っても無機粉体(無機繊維を含む)の樹脂への充填性
(混合しやすさ)や分散性はほとんど改善されない。無
機粉体を樹脂へ混合するときの加工性を高める(操作を
容易にする)目的で滑剤として長鎖脂肪酸やその塩が、
加工性を高めかつ無機粉体の分散性を向上させる目的で
チタンカップリング剤が用いられるが、いずれも無機粉
体の分散性が充分であるとはいえない。特開昭57−1
68954号公報には、このような無機粉体の処理剤と
してのような有機リン酸系化合物が開示されている。
Silane coupling agents are used to suppress a decrease in the mechanical strength of resin molded products that contain inorganic powder or inorganic fibers. For example, when asbestos fibers or glass fibers are treated with a silane coupling agent, the silane coupling agent chemically bonds to the surface of these fibers, resulting in increased adhesion when the fibers and resin are mixed, making it easier to use a machine. The target strength is improved. However, even if the silane coupling treatment is performed, the filling property (easiness of mixing) and dispersibility of the inorganic powder (including inorganic fibers) into the resin is hardly improved. Long chain fatty acids and their salts are used as lubricants to improve processability (facilitate operation) when mixing inorganic powder into resin.
Although titanium coupling agents are used for the purpose of increasing processability and improving the dispersibility of inorganic powder, none of them can be said to have sufficient dispersibility of inorganic powder. JP-A-57-1
No. 68954 discloses an organic phosphoric acid compound as a treatment agent for such an inorganic powder.

これは無機粉体が炭酸カルシウムであるときに樹脂中で
の分散性を充分に高める働きを有する。しかし、これを
炭酸カルシウム以外の無機粉体に適用すると2分子内に
2個の酸性OHiを有するため、該無機粉体の凝集をひ
きおこす。無機粉体表面に遊離の0■基が存在するよう
になる結果、樹脂と混合したときにゲル化を起こして樹
脂を劣化させる。さらに不飽和ポリエステル、エポキシ
樹脂などの熱硬化性樹脂に配合すると増粘現象をひきお
こし加工が困難になる。
This has the function of sufficiently increasing the dispersibility in the resin when the inorganic powder is calcium carbonate. However, if this is applied to inorganic powders other than calcium carbonate, the inorganic powders will agglomerate because there are two acidic OHi molecules in each molecule. As a result of the presence of free 0* groups on the surface of the inorganic powder, when mixed with a resin, gelation occurs and the resin deteriorates. Furthermore, when blended with thermosetting resins such as unsaturated polyesters and epoxy resins, a thickening phenomenon occurs and processing becomes difficult.

このように、樹脂に配合したときに充分な分散性を有し
、無機粉体配合樹脂組成物の機械的強度。
In this way, when blended with resin, it has sufficient dispersibility and the mechanical strength of the inorganic powder blended resin composition.

導電性、帯磁性、難燃性などの必要に応じた性能を充分
に確保できる無機粉体は、得られていないのが現状であ
る。
At present, inorganic powders that can sufficiently ensure required properties such as conductivity, magnetism, and flame retardance have not been obtained.

(発明が解決しようとする問題点) 本発明は、上記従来の欠点を解決するものであり、その
目的とするところは、各種樹脂と充分な親和性を有し該
樹脂中に混合されたときの分散性が良好であるため該樹
脂の機械的強度を低下させることなく、導電性、帯磁性
など必要に応じた機能を充分に付与しうる無機粉体を提
供することにある。本発明の他の目的は、適当な処理剤
でその表面が処理され樹脂中での分散性が高められた表
面改質無機粉体を提供することにある。本発明のさらに
他の目的は、上記表面改質無機粉体を含有する樹脂組成
物を提供することにある。
(Problems to be Solved by the Invention) The present invention solves the above-mentioned conventional drawbacks, and its purpose is to have sufficient affinity with various resins and when mixed in the resins. An object of the present invention is to provide an inorganic powder that has good dispersibility and can sufficiently impart necessary functions such as conductivity and magnetism without reducing the mechanical strength of the resin. Another object of the present invention is to provide a surface-modified inorganic powder whose surface is treated with a suitable treatment agent to improve its dispersibility in a resin. Still another object of the present invention is to provide a resin composition containing the above surface-modified inorganic powder.

(問題点を解決するための手段) 本発明の表面改質無機粉体は、無機粉体を下記式で示さ
れる含燐ケイ素化合物(I)により表面処理して得られ
、そのことにより上記目的が達成される。さらに本発明
の樹脂組成物は、無機粉体を下記式で示される含燐ケイ
素化合物(1)により表面処理して得られる表面改質無
機粉体および樹脂を含有し、そのことにより上記目的が
達成される: ここで R1およびR2はそれぞれ独立して。
(Means for Solving the Problems) The surface-modified inorganic powder of the present invention is obtained by surface-treating an inorganic powder with a phosphorus-containing silicon compound (I) represented by the following formula, thereby achieving the above-mentioned objectives. is achieved. Furthermore, the resin composition of the present invention contains a surface-modified inorganic powder obtained by surface-treating an inorganic powder with a phosphorus-containing silicon compound (1) represented by the following formula, and a resin, thereby achieving the above object. Achieved: where R1 and R2 are each independently.

炭素数1〜18のアルキル基、アリール基。C1-C18 alkyl group, aryl group.

置換アルキル基、および置換子り−ル基でなる群から選
択され;Qは または−C112CIl□−CO− であり、R3は炭素数1〜4のアルキル基であり;lは
0.1または2であり;そしてaは0または1である。
selected from the group consisting of substituted alkyl groups, and substituent groups; Q is or -C112CIl□-CO-, R3 is an alkyl group having 1 to 4 carbon atoms; l is 0.1 or 2 and a is 0 or 1.

本発明に用いられる含燐ケイ素化合物は、上記(I)式
で示される。それには1例えば2次の化合物が挙げられ
る。
The phosphorus-containing silicon compound used in the present invention is represented by the above formula (I). These include first, for example, second order compounds.

(CJsO) 2P −NH(C1l□)xsi (O
Czlls) x(CzlltO) tP −Nil 
 (CHz) sSi (OCzlls) x(C41
1tO) zP  NH(CIIz) ssi (OC
zlls) 3(CJ+tO)zr’  NH(CHz
hSi(OCzllsh(C611SO) zP  N
il  (Cllz) sSi (OCzlls) 3
(C211SO) zp −Nll−(CIl□)t 
 NH(Clh)isi(0(413)3(CJJ) 
zP −Nll−(C1l□)z  Ni1(CHz)
 zsi (OCRs) 3(C41190) 2P 
 Nll  (C1l□)z  Ni1(C1l□)+
Si (OCII:+) :1(CIlIIl?0)Z
P  Ntl  (CH2)2  N1((C1l□h
Si(OCHx)z(C611sO) zP  Nil
  (C1h) t  Nll (Cal□)3Si 
(OCH3) zI (Cm)l l ?) 2P  NH(C1l□)t−
NH(CII2)sSi(OCHz)3(C@H+ ?
O) zP  (CHz) 1si(OCII3) 3
(L;+tlhsOJzPClhC1l−GO(CHz
)zsi(OCIh)z上記含燐ケイ素化合物を用いて
表面処理がなされる無機粉体く本発明でいう無機粉体と
は、無機質の粉体、繊維、ウィスカーなどを包含する)
のII類は特に限定されない。無機粉体を配合すべき樹
脂に導電性、帯磁性、難燃性などの必要とする性能を付
与しうる素材が使用される。それには例えば、二酸化ケ
イ素(シリカ、石英、ホワイトカーボンなど)、水酸化
アルミニウム、水酸化マグネシウム、酸化チタン、酸化
マグネシウム、アルミナ、二酸化アンチモン、酸化鉄、
フェライト。
(CJsO) 2P -NH(C1l□)xsi (O
Czlls) x (CzlltO) tP -Nil
(CHz) sSi (OCzlls) x (C41
1tO) zP NH(CIIz) ssi (OC
zlls) 3(CJ+tO)zr' NH(CHz
hSi(OCzllsh(C611SO) zP N
il (Cllz) sSi (OCzlls) 3
(C211SO) zp -Nll-(CIl□)t
NH(Clh)isi(0(413)3(CJJ)
zP -Nll-(C1l□)z Ni1(CHz)
zsi (OCRs) 3 (C41190) 2P
Nll (C1l□)z Ni1(C1l□)+
Si (OCII:+) :1(CIlIIl?0)Z
P Ntl (CH2)2 N1((C1l□h
Si(OCHx)z(C611sO)zP Nil
(C1h) t Nll (Cal□)3Si
(OCH3) zI (Cm)l l? ) 2P NH(C1l□)t-
NH(CII2)sSi(OCHz)3(C@H+?
O) zP (CHz) 1si(OCII3) 3
(L;+tlhsOJzPClhC1l-GO(CHz
) zsi (OCIh)
Class II is not particularly limited. A material is used that can impart necessary properties such as conductivity, magnetism, and flame retardancy to the resin into which the inorganic powder is to be blended. Examples include silicon dioxide (silica, quartz, white carbon, etc.), aluminum hydroxide, magnesium hydroxide, titanium oxide, magnesium oxide, alumina, antimony dioxide, iron oxide,
Ferrite.

硫酸マグネシウム、炭酸カルシウム、クレイ、タルク、
アスベストマイカ、各種金属、ガラスなどがある。無機
粉体の粒径は、その目的により異なるが9通常0.1〜
100μmである。無機粉体が繊維状である場合もその
直径や繊維長は特に限定されないが1通常、それぞれ1
0〜100 p mおよびin會〜3 cmである。
Magnesium sulfate, calcium carbonate, clay, talc,
Examples include asbestos mica, various metals, and glass. The particle size of the inorganic powder varies depending on its purpose, but is usually 0.1 to 9.
It is 100 μm. Even if the inorganic powder is in the form of fibers, the diameter and fiber length are not particularly limited;
0-100 pm and in-person ~3 cm.

本発明の樹脂組成物に使用される樹脂も特に限定されな
い。その目的に応じて熱可塑性樹脂、熱硬化性樹脂、ゴ
ム系樹脂が使用されうる。その例としては、アルキド樹
脂、各種天然繊維、エポキシ樹脂、ポリアミド樹脂、熱
可塑性ポリエステル。
The resin used in the resin composition of the present invention is also not particularly limited. Thermoplastic resins, thermosetting resins, and rubber resins can be used depending on the purpose. Examples include alkyd resins, various natural fibers, epoxy resins, polyamide resins, thermoplastic polyesters.

ポリカーボネート、ポリエチレン、ポリブチレン。Polycarbonate, polyethylene, polybutylene.

ポリスチレン、スチレン−ブタジェン共重合体。Polystyrene, styrene-butadiene copolymer.

ポリプロピレン、スチレン−プロピレン共重合体。Polypropylene, styrene-propylene copolymer.

シリコーン樹脂、シリコーンゴム、 SBRゴム、ニト
リルゴム、天然ゴム、アクリル樹脂、フェノール樹脂、
ポリオキシメチレン、ポリウレタン、ポリスルホン、ポ
リスルフィドゴム、ニトロセルロース、エチルセルロー
ス、ビニル系樹脂(例エバ。
Silicone resin, silicone rubber, SBR rubber, nitrile rubber, natural rubber, acrylic resin, phenolic resin,
Polyoxymethylene, polyurethane, polysulfone, polysulfide rubber, nitrocellulose, ethylcellulose, vinyl resins (e.g. EVA).

ポリビニルブチレート塩化ビニル、酢酸ビニル含有重合
体)、酢酸セルロース1酪酸セルロース。
Polyvinyl butyrate (vinyl chloride, vinyl acetate-containing polymers), cellulose acetate, cellulose monobutyrate.

ビスコースレーヨン、ワックス、エチレン共重合体(例
えば、エチレン−酢酸ビニル共重合体、エチレン−アク
リル酸共重合体、エチレン−アクリル酸エステル共重合
体)などがある。
Examples include viscose rayon, wax, and ethylene copolymers (eg, ethylene-vinyl acetate copolymers, ethylene-acrylic acid copolymers, and ethylene-acrylic acid ester copolymers).

本発明の表面改質無機粉体は、前記無機粉体を前記含燐
ケイ素化合物とを湿式処理法または乾式処理法で処理す
ることにより得られる。湿式処理法では9例えばまず、
上記無機粉体を同容積以上の有機溶剤に懸濁させる。有
機溶剤としては通常。
The surface-modified inorganic powder of the present invention can be obtained by treating the inorganic powder with the phosphorus-containing silicon compound by a wet treatment method or a dry treatment method. In the wet processing method9, for example, first,
The above inorganic powder is suspended in the same volume or more of an organic solvent. Normal as an organic solvent.

アルコール、ベンゼン、トルエン、キシレンなどが用い
られる。このスラリー状の懸濁液に含燐ケイ素化合物を
加えて充分に攪拌を行う。含燐ケイ素化合物は無機粉体
に対して0.01〜20重量%、好ましくは0.1〜5
重量%の割合で添加される。過少であると無機粉体の樹
脂組成物中での分散効果が得られず、過剰であっても含
有量に比例した効果が得られないため無駄である。懸濁
液を充分に攪拌した後、これを昇温し攪拌下で加熱還流
を行う。次に、固液分離し、ケーキ状の粉体を取り出し
、乾燥させる。溶剤を充分に除去するために。
Alcohol, benzene, toluene, xylene, etc. are used. A phosphorous-containing silicon compound is added to this slurry-like suspension and thoroughly stirred. The phosphorus-containing silicon compound is 0.01 to 20% by weight, preferably 0.1 to 5% by weight based on the inorganic powder.
It is added in a proportion of % by weight. If the amount is too small, the effect of dispersing the inorganic powder in the resin composition cannot be obtained, and even if it is in excess, the effect proportional to the content cannot be obtained, which is wasteful. After the suspension is thoroughly stirred, the temperature of the suspension is raised, and the mixture is heated to reflux while being stirred. Next, solid-liquid separation is performed, and the cake-like powder is taken out and dried. To thoroughly remove the solvent.

減圧乾燥を行うことが推奨される。このような湿式処理
法を採用すると各粒子表面が均一に処理されるという利
点がある。
Drying under reduced pressure is recommended. Adoption of such a wet treatment method has the advantage that the surfaces of each particle are uniformly treated.

乾式処理法では2例えばまず、無機粉体を高速攪拌・昇
温が可能な粉体混合機(例えばヘンシェル形粉体混合n
)に仕込み、高速攪拌下、これに適当量の溶剤に溶解さ
せた含燐ケイ素化合物を噴射ノズルなどを用いて添加す
る。含燐ケイ素化合物の添加量は上記湿式処理法の場合
と同様である。
In the dry processing method, for example, first, a powder mixer capable of high-speed stirring and heating of inorganic powder (for example, Henschel type powder mixer n
), and a phosphorus-containing silicon compound dissolved in an appropriate amount of solvent is added thereto using a spray nozzle or the like under high-speed stirring. The amount of the phosphorous-containing silicon compound added is the same as in the case of the wet processing method described above.

粉体混合機で充分に混合した後、昇温し、溶剤を除去す
る。このような乾式処理法は、多量の溶剤を使用せず、
装置が簡単であり短時間で処理が可能であるためコスト
的に有利であるという利点がある。上記湿式処理法、乾
式処理法のいずれの方法で処理した場合も、粉体の処理
効果にはほとんど差がない。無機粉体の種類や形状に応
じて適宜処理方法を選択する。
After thoroughly mixing with a powder mixer, the temperature is raised and the solvent is removed. This dry processing method does not use large amounts of solvents,
It has the advantage of being cost-effective because the device is simple and processing can be done in a short time. There is almost no difference in the processing effect of the powder whether the powder is processed using the wet processing method or the dry processing method. An appropriate treatment method is selected depending on the type and shape of the inorganic powder.

(作用) このようにして得られる表面改質無機粉体は。(effect) The surface-modified inorganic powder obtained in this way is.

各種樹脂中に配合される。例えば、樹脂のa械的強度を
向上させるために表面処理したガラス繊維を、帯磁性を
付与するため表面処理したバリウムフェライト粉体を配
合する。磁気塗料中には1表面処理したα−酸化鉄粉体
を配合する。配合量は。
It is blended into various resins. For example, barium ferrite powder that has been surface-treated to impart magnetism is blended with glass fibers that have been surface-treated to improve the a-mechanical strength of the resin. A surface-treated α-iron oxide powder is blended into the magnetic paint. What is the blending amount?

無機粉体の種類やその使用目的に応して異なり。It varies depending on the type of inorganic powder and its purpose.

はぼ従来例に準する。This is based on the conventional example.

本発明の表面改質無機粉体においては、 (■)式の含
燐ケイ素化合物の−Si (OR’) xの部分が、従
来のシランカップリング剤と同様の機構で無機粉体表面
に化学的に結合している。この表面改質無機粉体が樹脂
中に混合されると、上記含燐ケイ素化合物のリン酸エス
テルの部分が樹脂と会合的に結合する。この点は、従来
のシランカップリング剤が、ビニル栽、アミノ基、メタ
クリルオキシ基などを有し、これらの基が樹脂と共有結
合する機構と異なる。リン酸エステルの部分が樹脂と会
合的に結合するということは、含燐ケイ素化合物と樹脂
、つまり表面改質無機粉体と樹脂との親和性が向上する
ことを意味する。さらに含燐ケイ素化合物は可塑剤とし
ての機能をも有する。その結果。
In the surface-modified inorganic powder of the present invention, the -Si (OR') are connected to each other. When this surface-modified inorganic powder is mixed into a resin, the phosphate ester portion of the phosphorus-containing silicon compound is associatively bonded to the resin. This point differs from the mechanism in which conventional silane coupling agents have vinyl groups, amino groups, methacryloxy groups, etc., and these groups are covalently bonded to the resin. The associative bonding of the phosphate ester moiety with the resin means that the affinity between the phosphorus-containing silicon compound and the resin, that is, the affinity between the surface-modified inorganic powder and the resin is improved. Furthermore, the phosphorus-containing silicon compound also has a function as a plasticizer. the result.

表面改質無機粉体は樹脂中に均一に分散しうる。The surface-modified inorganic powder can be uniformly dispersed in the resin.

表面改質無機粉体が配合された樹脂組成物は。A resin composition containing surface-modified inorganic powder.

例えば、射出成形、トランファ成形、圧縮成形。For example, injection molding, transfer molding, compression molding.

注型成形などにより所望の形状に成形されたり。It can be molded into the desired shape using cast molding, etc.

塗料として使用される。このように2本発明の表面改質
無機粉体が配合された樹脂組成物は、無機粉体がその中
に均一に分散されているため2例えば、可電性、帯磁性
、難燃性などの目的とする性能に優れ、かつ表面改質無
機粉体の混合により樹脂の機械的強度が低下することが
ない。
Used as a paint. In this way, the resin composition containing the surface-modified inorganic powder of the present invention has properties such as electroconductivity, magnetism, flame retardancy, etc. because the inorganic powder is uniformly dispersed therein. The resin has excellent performance as desired, and the mechanical strength of the resin does not decrease due to the mixing of the surface-modified inorganic powder.

(実施例) 以下に本発明を実施例につき説明する。(Example) The invention will be explained below with reference to examples.

叉施炎よ」 (A)表面改質無機粉体の調製:ヘンシエル形粉体混合
機に無機粉体として粒径3μmの水酸化アルミニウム粉
体(日本軽金属社製、 B−103)を100重量部仕
込んだ。これに高速攪拌下で下記の含燐ケイ素化合物0
.5重量部のイソプロパツール溶液をスプレーした。
(A) Preparation of surface-modified inorganic powder: 100 weight of aluminum hydroxide powder (manufactured by Nippon Light Metal Co., Ltd., B-103) with a particle size of 3 μm was added as an inorganic powder to a Henschel type powder mixer. I have prepared a section. The following phosphorus-containing silicon compound 0 was added to this under high-speed stirring.
.. A solution of 5 parts by weight of isopropanol was sprayed.

OClll0 il     l  :1 (Call l 7) 2P  CI□−CIl  C
O(CHz)ssi(OClh)sさらに攪拌を1時間
続けた後、120°Cに加熱しイソプロパツールを実質
的に除去し1表面改質熱機粉体を得た。
OClll0 ill l :1 (Call l 7) 2P CI□-CIl C
O(CHz)ssi(OClh)s After further stirring for 1 hour, the mixture was heated to 120°C to substantially remove isopropanol and obtain a surface-modified thermomechanical powder.

(B)表面改質無機粉体の性能評価=(八)項で得られ
た表面改質無機粉体を次の割合で含有する混合物を調製
し、その25℃における粘度をB形粘度計(ローター隘
3使用)を用いて測定した。粘度は11 、700cp
sであった。
(B) Performance evaluation of surface-modified inorganic powder = Prepare a mixture containing the surface-modified inorganic powder obtained in section (8) in the following ratio, and measure its viscosity at 25°C using a B-type viscometer ( The measurement was carried out using a rotor shaft 3). Viscosity is 11, 700cp
It was s.

星金側丘 塩化ビニル樹脂(ゼオン121)     150重量
部DOP                  90重
量部液状亜鉛系安定剤 (共同薬品社製KF80A−8)       5重量
部表面改質水酸化アルミニウム粉末 (@)項で調製)60重量部 尖立拠土」 含燐ケイ素化合物の量を1.0重■部として実施例1−
H^)項に準じて表面改質無機粉体を調製した。実施例
1−1(B)項と同様の操作で混合物を調製し、その粘
度を測定したところ、  9800cpsであった。
Star gold side hill vinyl chloride resin (Zeon 121) 150 parts by weight DOP 90 parts by weight Liquid zinc stabilizer (KF80A-8 manufactured by Kyodo Yakuhin Co., Ltd.) 5 parts by weight Surface-modified aluminum hydroxide powder (prepared in section @) 60 Example 1- with the amount of phosphorus-containing silicon compound being 1.0 parts by weight
Surface-modified inorganic powder was prepared according to Section H^). A mixture was prepared in the same manner as in Example 1-1(B), and its viscosity was measured to be 9800 cps.

l射吐上 実施例1−1の表面改質無機粉体の代わりに表面処理を
行っていない同質の水酸化アルミニウム粉体を配合した
混合物を調製し、その粘度を測定したところ、 15.
700cpsであった。
1. When a mixture was prepared in which a homogeneous aluminum hydroxide powder without surface treatment was mixed in place of the surface-modified inorganic powder of Example 1-1, the viscosity of the mixture was measured.15.
It was 700 cps.

実施例1−1.1−2および比較例1から9本発明の表
面改質無機粉体を樹脂中に配合すると1表面未処理熱機
粉体を利用したときに比べて粘度が著しく降下し、成形
などの操作が容易になされうろことがわかる。
Example 1-1.1-2 and Comparative Examples 1 to 9 When the surface-modified inorganic powder of the present invention is blended into a resin, the viscosity decreases significantly compared to when a surface-untreated thermomechanical powder is used. It can be seen that operations such as molding can be easily performed.

スl」LL」 アルミナ粉体(日本軽金属社製; A−34) 100
重量部を、下記の含燐ケイ素化合物0.5重量部を用い
実施例1(A)項に準じて処理し1表面改質熱機粉体を
得た: 得られた表面改質無機粉体100重量部および硬化剤(
油化シェル製;エビキュア126) 24重量部を加え
て、減圧下で20分間脱泡・混合した。この混合物の粘
度を実施例1(B)項に阜して測定したところ1200
cpsであった。この混合物を5日間放置したが沈降を
生じなかった。
Alumina powder (manufactured by Nippon Light Metal Co., Ltd.; A-34) 100
Part by weight was treated according to Example 1 (A) using 0.5 part by weight of the following phosphorous-containing silicon compound to obtain 1 surface-modified thermomechanical powder: Obtained surface-modified inorganic powder 100 Parts by weight and curing agent (
24 parts by weight of Ebicure 126) manufactured by Yuka Shell Co., Ltd. were added, and the mixture was defoamed and mixed for 20 minutes under reduced pressure. The viscosity of this mixture was measured according to Example 1 (B) and was 1200.
It was cps. This mixture was allowed to stand for 5 days, but no sedimentation occurred.

尖庭炭1」 含燐ケイ素化合物の量を1.0重量部としたこと以外は
実施例2−1と同様に表面改質無機粉体を調製した。実
施例2−1の表面改質無機粉体の代わりに、この表面改
質無機粉体を用いて同様の混合物を調製し、その粘度を
測定したところ720cpsであった。この混合物を5
日間放置したが沈降を生じなかった。
Senniwa charcoal 1'' A surface-modified inorganic powder was prepared in the same manner as in Example 2-1 except that the amount of the phosphorous-containing silicon compound was 1.0 parts by weight. A similar mixture was prepared using this surface-modified inorganic powder in place of the surface-modified inorganic powder of Example 2-1, and its viscosity was measured to be 720 cps. Add this mixture to 5
Although it was left to stand for several days, no sedimentation occurred.

此fil生先 表面改質無機粉体の代わりに表面処理を行っていない同
質のアルミナ粉体(日本軽金属社製;^−34)を用い
て、実施例1−1に準じて混合物を調製した。その粘度
を測定したところ15.500cpsであった。この混
合物を5日間放置したところ、固形成分の沈降が生じた
A mixture was prepared according to Example 1-1 using a homogeneous alumina powder (manufactured by Nippon Light Metal Co., Ltd.; ^-34) without surface treatment instead of this fil raw material surface-modified inorganic powder. . The viscosity was measured and found to be 15.500 cps. When this mixture was left to stand for 5 days, sedimentation of solid components occurred.

実施例2−1.2−2および比較例2から1本発明の表
面処理が行われた無機粉体を樹脂中に配合すると1表面
未処理無機粉体を利用したときに比べて低粘度であり、
かつ沈降を生じることなく安定に保存しうろことが明ら
かである。
From Example 2-1.2-2 and Comparative Example 2, when the inorganic powder subjected to the surface treatment of the present invention is blended into the resin, the viscosity is lower than when the surface-untreated inorganic powder is used. can be,
It is also clear that it can be stored stably without sedimentation.

尖施炭主 (A)表面改質無機粉体の調製:高速形ミキサーに水酸
化アルミニウム粉体(昭和軽金属社製;ト32) 10
0重量部を仕込んだ、これに下記の含燐ケイ素化合物の
10%メタノール溶液5重量部を加え。
Preparation of surface-modified inorganic powder (A): Aluminum hydroxide powder (manufactured by Showa Light Metal Co., Ltd.; 32) in a high-speed mixer 10
0 parts by weight was charged, and 5 parts by weight of a 10% methanol solution of the following phosphorus-containing silicon compound was added thereto.

高速攪拌を30分間行った: 温度を120℃に上げてメタノールを除去・乾燥し。High speed stirring was performed for 30 minutes: Raise the temperature to 120°C to remove methanol and dry.

表面改質無機粉体を得た。A surface-modified inorganic powder was obtained.

(B)表面改質無機粉体の性能評価:不飽和ポリエステ
ル(日本触媒化学社製; S−355LT) 100重
量部に9本実施例(A)項で得られた表面改質無機粉体
140重量部をフィラーとして添加した。この混合物の
粘度を実施例1(B)項に阜じて測定した。
(B) Performance evaluation of surface-modified inorganic powder: 9 parts per 100 parts by weight of unsaturated polyester (manufactured by Nippon Shokubai Kagaku Co., Ltd.; S-355LT) 140 parts of the surface-modified inorganic powder obtained in Example (A) Parts by weight were added as filler. The viscosity of this mixture was measured according to Example 1 (B).

同様の混合物を2組準備し、さらにスチレン15重量部
および25重量部をそれぞれ添加し、各々の粘度を測定
した。その結果を表1に示す。比較例3−1および3−
2の結果もあわせて表1に示す。
Two sets of similar mixtures were prepared, 15 parts by weight and 25 parts by weight of styrene were added, respectively, and the viscosity of each was measured. The results are shown in Table 1. Comparative Examples 3-1 and 3-
The results of No. 2 are also shown in Table 1.

ル較侃1ユ 実施例3(A)項で得られた表面改質無機粉体の代わり
に表面処理を行っていない同質の水酸化アルミニウム粉
体を用い、実施例3に準じて混合物を調製し、その粘度
を測定した。
Example 3 A mixture was prepared according to Example 3 using homogeneous aluminum hydroxide powder without surface treatment in place of the surface-modified inorganic powder obtained in Section (A). and its viscosity was measured.

(以下余白) 此皇13u C1□1lzs 0P(OH)zを用いたこと以外は、
実施例3と同様である。
(Left below) Except for using Kono 13u C1□1lzs 0P(OH)z,
This is the same as in Example 3.

表1 実施例3(A)項で得られた表面改質無機粉体140重
量部と不飽和ポリエステル(日本触媒化学社製;S−3
55LT) 100重撥部とを均一に混合し、これをガ
ラスマット(# 150)に含浸させた。このような含
浸ガラスマット3枚を積層し軽く圧縮した後、 110
℃で2時間アフターキュアーを行い、成形体を調製した
。このような成形体を4枚準備し、その1枚を用い1曲
げ強度保持率をJISに−6911の方法で測定した。
Table 1 140 parts by weight of the surface-modified inorganic powder obtained in Example 3 (A) and unsaturated polyester (manufactured by Nippon Shokubai Kagaku Co., Ltd.; S-3
55LT) were mixed uniformly with 100 parts, and a glass mat (#150) was impregnated with this. After laminating three such impregnated glass mats and lightly compressing them, 110
After-curing was performed at ℃ for 2 hours to prepare a molded article. Four such molded bodies were prepared, and one of the molded bodies was used to measure the 1-bending strength retention rate using the JIS-6911 method.

残りの3枚を70℃に保管し、20時間後。The remaining three sheets were stored at 70°C for 20 hours.

40時間後および80時間後に1枚ずつ取り出して同様
の方法で測定を行なった。成形直後の曲げ強度を100
%とし、20時間後、40時間後および80時間後の曲
げ強度の百分率を算出した。その結果を表2に示す。比
較例4−1および4−2の結果もあわせて表2に示す。
After 40 hours and 80 hours, each piece was taken out and measured in the same manner. The bending strength immediately after forming is 100
%, and the percentage of bending strength after 20 hours, 40 hours, and 80 hours was calculated. The results are shown in Table 2. The results of Comparative Examples 4-1 and 4-2 are also shown in Table 2.

止較■(ユ 実施例3(八)項で得られた表面改質無機粉体の代わり
に表面処理を行なっていない同質の水酸化アルミニウム
粉体を用い、実施例4に準じて成形体を調製し9曲げ強
度を測定した。
Comparison ■ (U) A molded body was produced according to Example 4, using a homogeneous aluminum hydroxide powder without surface treatment in place of the surface-modified inorganic powder obtained in Example 3 (8). 9 bending strengths were measured.

C+zflzs 0P(OH)zを用いて表面改質無機
粉体を調製した。これを用い、実施例4に準じて成形体
を調製し2曲げ強度を測定した。
A surface-modified inorganic powder was prepared using C+zflzs 0P(OH)z. Using this, a molded body was prepared according to Example 4, and the 2-bending strength was measured.

表2 (^)表面改質無機粉体の調製;高速形ミキサーに水酸
化アルミニウム粉体(日本軽金属社製;B2O2) 1
00重量部を仕込んだ。高速攪拌しながら。
Table 2 (^) Preparation of surface-modified inorganic powder; Aluminum hydroxide powder (manufactured by Nippon Light Metal Co., Ltd.; B2O2) 1 in a high-speed mixer
00 parts by weight were charged. While stirring at high speed.

これに下記の含燐ケイ素化合物1重量部を加えて充分に
混合した。
1 part by weight of the following phosphorus-containing silicon compound was added to this and thoroughly mixed.

(CzHsO) zP−NH−(CHz) zsi (
OCzHs) 3これを130℃に加温して1時間乾燥
し1表面改質無機粉体を得た。
(CzHsO) zP-NH-(CHz) zsi (
OCzHs) 3 This was heated to 130°C and dried for 1 hour to obtain 1 surface-modified inorganic powder.

CB)表面改質無機粉体含有樹脂成形品の性能評価:エ
チレンー酢酸ビニル共重合樹脂(三井ポリケミカル社製
;エバフレックスr’−2805)  100重量部8
本実施例(A)項で得られた表面改質無機粉体120重
量部、酸化防止剤(入内新興社製;ツクラック300)
 1.3重量部およびステアリン酸2.6重量部を75
℃の混練ロールで30分混練し、100°C2100k
g / cjの条件でプレス成形を行った。この成形体
の引張強度を軟質塩化ビニルの試験法(JISK−67
23)に準じて測定した。その結果を表3に示す。表3
において、100%モジェラスとは、試験片の100%
伸長時における単位面積(龍2)あたりの引張力(kg
)をいう。実施例5−2〜5−4および比較例5の結果
もあわせて表3に示す。
CB) Performance evaluation of resin molded product containing surface-modified inorganic powder: Ethylene-vinyl acetate copolymer resin (manufactured by Mitsui Polychemical Co., Ltd.; Evaflex r'-2805) 100 parts by weight 8
120 parts by weight of the surface-modified inorganic powder obtained in Example (A), antioxidant (manufactured by Iruuchi Shinko Co., Ltd.; Tsukurak 300)
75 parts by weight of 1.3 parts by weight and 2.6 parts by weight of stearic acid.
Knead for 30 minutes with a kneading roll at 100°C 2100k
Press molding was performed under the conditions of g/cj. The tensile strength of this molded body was determined using the soft vinyl chloride test method (JISK-67).
23). The results are shown in Table 3. Table 3
, 100% modella means 100% of the test piece.
Tensile force (kg) per unit area (Ryu 2) during elongation
). The results of Examples 5-2 to 5-4 and Comparative Example 5 are also shown in Table 3.

実上皿工」 含燐ケイ素化合物として次の化合物を使用したこと以外
は実施例S−tと同様である。
Practical Plate Crafts'' This was the same as Example S-t except that the following compound was used as the phosphorus-containing silicon compound.

(C41190) zP−Nll−(CHり JH(C
1l□) :IS i (QC)13) s実隻撚工」 含燐ケイ素化合物として次の化合物を使用したこと以外
は実施例5−1と同様である。
(C41190) zP-Nll-(CHri JH(C
1l□) : IS i (QC) 13) s Actual Twisting Work The same as Example 5-1 except that the following compound was used as the phosphorus-containing silicon compound.

(CJsO) zP−Nl(−(CHz) zNH(C
Il□)isi (OCII:l) 3裏上與】」 含燐ケイ素化合物として次の化合物を使用したこと以外
は実施例5−1と同様である。
(CJsO) zP-Nl(-(CHz) zNH(C
Il□)isi (OCII:l) 3 Uraage 與】" The same as Example 5-1 except that the following compound was used as the phosphorus-containing silicon compound.

表面改質無機粉体の代わりに表面処理を行っていない同
質の水酸化アルミニウム粉体を用い、実施例5−1に準
じて成形体を調製した。この成形体を比較例5−1と同
様の方法で評価した。
A molded body was prepared according to Example 5-1 using a homogeneous aluminum hydroxide powder without surface treatment in place of the surface-modified inorganic powder. This molded article was evaluated in the same manner as Comparative Example 5-1.

(以下余白) 表3 表3より1本発明の表面改質無機粉体を含有する組成物
を用いて得られる成形体は1表面未処理無機粉体を含有
する組成物を用いて得られる成形体に比べて、引張強度
、伸びともに優れていることが明らかである。
(Leaving space below) Table 3 From Table 3, 1 molded product obtained using the composition containing the surface-modified inorganic powder of the present invention is 1 molded product obtained using the composition containing the surface-untreated inorganic powder. It is clear that both tensile strength and elongation are superior to that of the body.

裏血五l」 (A)表面改質無機粉体の調製:粒径0.4μIのγ−
Fe、O,粉体100重量部およびトルエン500重量
部をホモミキサー(特殊機械工業社製)に仕込み、これ
に下記の含燐ケイ素化合物2重量部を加えて1時間撹拌
した。
(A) Preparation of surface-modified inorganic powder: γ-
100 parts by weight of Fe, O, powder and 500 parts by weight of toluene were placed in a homo mixer (manufactured by Tokushu Kikai Kogyo Co., Ltd.), and 2 parts by weight of the following phosphorus-containing silicon compound were added thereto and stirred for 1 hour.

これを濾過して溶剤を除き、100℃で1時間乾燥して
表面改質無機粉体を得た。
This was filtered to remove the solvent and dried at 100° C. for 1 hour to obtain a surface-modified inorganic powder.

(B)表面改質無機粉体を含む磁気記録媒体の性能評価
二次の処方により磁性塗料を調製した。
(B) Performance evaluation of magnetic recording media containing surface-modified inorganic powder A magnetic paint was prepared using the following recipe.

磁性■料配合割合: (A)項で得られた表面改質無機粉体 100重量部 塩化ビニル−酢酸ビニル共重合体 15重量部ジオクチ
ルフタレート      5重量部トルエン     
      122重量部メチルエチルケトン    
  110重量部この磁性塗料をポリエステルフィルム
に塗布し。
Magnetic material mixing ratio: 100 parts by weight of the surface-modified inorganic powder obtained in section (A) 15 parts by weight of vinyl chloride-vinyl acetate copolymer Dioctyl phthalate 5 parts by weight Toluene
122 parts by weight methyl ethyl ketone
110 parts by weight of this magnetic paint was applied to a polyester film.

配向、乾燥させて磁気記録媒体を得た。この磁気記録媒
体の保磁力(llc)および配向度を測定した。
A magnetic recording medium was obtained by orientation and drying. The coercive force (llc) and degree of orientation of this magnetic recording medium were measured.

次に、  10KIIzにおける出力を測定し、これを
基準(OdB)とし、後述の実施例6−1および比較例
6との比較を行った。その結果を表4に示す。前記10
にIlzにおける出力の比較は「電気特性」の項に記載
した。実施例6−2および比較例6の結果もあわせて表
4に示す。
Next, the output at 10 KIIz was measured, and this was used as a reference (OdB) for comparison with Example 6-1 and Comparative Example 6, which will be described later. The results are shown in Table 4. Said 10
A comparison of the output in Ilz is described in the "Electrical Characteristics" section. The results of Example 6-2 and Comparative Example 6 are also shown in Table 4.

遍1粗彰( 含燐ケイ素化合物として次の化合物を使用したこと以外
は実施例6−1と同様である。
Same as Example 6-1 except that the following compound was used as the phosphorus-containing silicon compound.

o     C1h  O II     I   II (Cell+tO) 2P −C1lz −CIl−C
O(C11□)+5i(OCIIi) z上較適i 表面改質無機粉体の代わりに表面処理を行っていない同
質のγ−Fe20.粉体を用いて磁性塗料を調製し、得
られた磁気媒体の性能評価を行った。
o C1h O II I II (Cell+tO) 2P -C1lz -CIl-C
O(C11□)+5i(OCIIi) z upper calibration i Instead of surface-modified inorganic powder, homogeneous γ-Fe20. without surface treatment. A magnetic paint was prepared using powder, and the performance of the obtained magnetic medium was evaluated.

(以下余白) 表4から9本発明の表面改質無機粉体を含有する組成物
を用いた磁気記録媒体は、従来の磁気記録媒体に比較し
て保磁力が高く、かつ磁気記録媒体として必要な高周波
領域における出力が5〜6dBも高いことがわかる。
(The following are blank spaces) Tables 4 to 9 Magnetic recording media using compositions containing the surface-modified inorganic powder of the present invention have higher coercive force than conventional magnetic recording media, and are necessary as magnetic recording media. It can be seen that the output in the high frequency region is as high as 5 to 6 dB.

夫施貫ユ」 (A)表面改質無機粉体の調製:異方性バリウムフェラ
イト粉体(粒径1.2μm)100重量部をヘンシルミ
キサーで低速攪拌し、これに下記の含燐ケイ素化合物0
.5重量部を3倍量のメタノールに溶解させたメタノー
ル溶液を、5分間かけて徐々に滴下・混合した。
(A) Preparation of surface-modified inorganic powder: 100 parts by weight of anisotropic barium ferrite powder (particle size 1.2 μm) was stirred at low speed with a Henshil mixer, and the following phosphorus-containing silicon was added to it. Compound 0
.. A methanol solution in which 5 parts by weight were dissolved in 3 times the amount of methanol was gradually added dropwise and mixed over 5 minutes.

(CsHI 70) 2P−NH−(CH2) 2−N
11 (C112) zsi (OCR:l) :1さ
らに、これを1時間高速撹拌し、この間冷々に昇温し溶
剤を除去して表面改質無機粉体を得た。
(CsHI 70) 2P-NH-(CH2) 2-N
11 (C112) zsi (OCR:l): 1 This was further stirred at high speed for 1 hour, during which time the temperature was raised slowly and the solvent was removed to obtain a surface-modified inorganic powder.

(B)表面改質無機粉体を含むプラスチック磁石の性能
評価二(^)項で得られた表面改質無機粉体(表面改質
異方性バリウムフェライト)を85重量部、そしてナイ
ロン6を15重組部押出機に仕込み。
(B) Performance evaluation of plastic magnets containing surface-modified inorganic powder 85 parts by weight of the surface-modified inorganic powder (surface-modified anisotropic barium ferrite) obtained in Section 2(^), and nylon 6. Load into a 15-layer extruder.

混練してペレット化した。このペレットを、磁場発生装
置の付設された射出成形機に仕込み、キャビティ内充填
と同時にコイル磁場1.5万ガウスをかけ配量着磁を行
った。この試験片(プラスチック磁石)についての各試
験結果を表5に示す、実  ・施例7−2〜7−3.お
よび比較例7−1〜7−2の結果もあわせて表5に示す
The mixture was kneaded and pelletized. The pellets were placed in an injection molding machine equipped with a magnetic field generator, and at the same time as the cavity was filled, a coil magnetic field of 15,000 Gauss was applied for metered magnetization. The test results for this test piece (plastic magnet) are shown in Table 5. Examples 7-2 to 7-3. Table 5 also shows the results of Comparative Examples 7-1 and 7-2.

大指開1」 含燐ケイ素化合物として次の化合物を使用したこと以外
は実施例7−1と同様である。
Big Finger Opening 1" The same as Example 7-1 except that the following compound was used as the phosphorus-containing silicon compound.

(C4H90) zP−NH−(CHz) ssi (
OC2H5) 3災胤桝1」 含燐ケイ素化合物として次の化合物を使用したこと以外
は実施例7−1と同様である。
(C4H90) zP-NH-(CHz) ssi (
OC2H5) 3 disasters 1'' Same as Example 7-1 except that the following compound was used as the phosphorus-containing silicon compound.

を較±1ユ 本発明の含燐ケイ素化合物の代わりに従来のチタンカッ
プリング剤(味の素社製、 TTS )  0.5重量
部を使用したこと以外は実施例?−1と同様である。
Example 1 except that 0.5 parts by weight of a conventional titanium coupling agent (manufactured by Ajinomoto Co., Ltd., TTS) was used instead of the phosphorus-containing silicon compound of the present invention. -1 is the same.

此μm1L」 表面改質無機粉体の代わりに表面処理を行っていない同
質の異方性バリウムフェライト粉体を用いてプラスチッ
ク!8石を調製したこと以外は実施例?−1と同様であ
る。
"This μm 1L" is made of plastic using homogeneous anisotropic barium ferrite powder without surface treatment instead of surface-modified inorganic powder! Is this an example except that 8 stones were prepared? -1 is the same.

(以下余白) 表5から1本発明の表面改質無機粉体を用いたプラスチ
ック磁石は、従来の表面処理剤によって処理されたある
いは表面未処理の無機粉体を含むプラスチック磁石に比
べ、残留磁束密度、保磁力。
(Left below) From Table 5, plastic magnets using the surface-modified inorganic powder of the present invention have a higher residual magnetic flux than plastic magnets containing inorganic powder that has been treated with a conventional surface treatment agent or whose surface has not been treated. Density, coercive force.

最大エネルギー積および配向性に優れていることがわか
る。このような磁石としての性質のみならず、 fJi
?J1強度や引張強度にも優れていることが明らかであ
る。
It can be seen that the maximum energy product and orientation are excellent. In addition to these magnetic properties, fJi
? It is clear that it is also excellent in J1 strength and tensile strength.

(発明の効果) 本発明によれば、このように、各種樹脂中での分散性に
優れた表面改質無機粉体およびそれを含有する樹脂組成
物が得られる。本発明の表面改質無機粉体は、樹脂中に
均一に分散するため樹脂組成物の機械的強度を低下させ
ることがないのはもちろんのこと、導電性、帯磁性、難
燃性など必要に応じた効果を充分に付与しうる。このよ
うな表面改質無機粉体およびそれを含有する樹脂組成物
は1強化プラスチック複合製品、難燃材、プラスチック
磁石、磁気記録媒体など各種製品に有効に利用されうる
(Effects of the Invention) According to the present invention, a surface-modified inorganic powder having excellent dispersibility in various resins and a resin composition containing the same can be obtained. Since the surface-modified inorganic powder of the present invention is uniformly dispersed in the resin, it does not reduce the mechanical strength of the resin composition, and also has the necessary properties such as conductivity, magnetism, and flame retardancy. The corresponding effect can be sufficiently imparted. Such surface-modified inorganic powders and resin compositions containing the same can be effectively used in various products such as reinforced plastic composite products, flame retardants, plastic magnets, and magnetic recording media.

Claims (1)

【特許請求の範囲】 1、無機粉体を下記式で示される含燐ケイ素化合物(
I )により表面処理して得られる表面改質無機粉体:▲
数式、化学式、表等があります▼( I ) ここで、R^1およびR^2はそれぞれ独立して、炭素
数1〜18のアルキル基、アリール基、置換アルキル基
、および置換アリール基でなる群から選択され;Qは−
NH−、−NH(CH_2)_2NH−、▲数式、化学
式、表等があります▼または▲数式、化学式、表等があ
ります▼ であり;R^3は炭素数1〜4のアルキル基であり;l
は0、1または2であり;そしてaは0または1である
。 2、無機粉体を下記式で示される含燐ケイ素化合物(
I )により表面処理して得られる表面改質無機粉体およ
び樹脂を含有する組成物: ▲数式、化学式、表等があります▼( I ) ここで、R^1およびR^2それぞれ独立して、炭素数
1〜18のアルキル基、アリール基、置換アルキル基、
および置換アリール基でなる群から選択され;Qは−N
H−、−NH(CH_2)_2NH−、▲数式、化学式
、表等があります▼または▲数式、化学式、表等があり
ます▼ であり;R^3は炭素数1〜4のアルキル基であり;l
は0、1または2であり;そしてaは0または1である
[Claims] 1. The inorganic powder is a phosphorous-containing silicon compound represented by the following formula (
Surface-modified inorganic powder obtained by surface treatment by I): ▲
There are mathematical formulas, chemical formulas, tables, etc. ▼ (I) Here, R^1 and R^2 are each independently an alkyl group, an aryl group, a substituted alkyl group, and a substituted aryl group having 1 to 18 carbon atoms. selected from the group; Q is −
NH-, -NH(CH_2)_2NH-, ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼ or ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼; R^3 is an alkyl group with 1 to 4 carbon atoms; l
is 0, 1 or 2; and a is 0 or 1. 2. Inorganic powder is converted into a phosphorous-containing silicon compound represented by the following formula (
Composition containing surface-modified inorganic powder and resin obtained by surface treatment by I): ▲There are mathematical formulas, chemical formulas, tables, etc.▼(I) Here, R^1 and R^2 are each independently , an alkyl group having 1 to 18 carbon atoms, an aryl group, a substituted alkyl group,
and a substituted aryl group; Q is -N
H-, -NH(CH_2)_2NH-, ▲There are mathematical formulas, chemical formulas, tables, etc.▼ or ▲There are mathematical formulas, chemical formulas, tables, etc.▼; R^3 is an alkyl group with 1 to 4 carbon atoms; l
is 0, 1 or 2; and a is 0 or 1.
JP61188098A 1986-08-11 1986-08-11 Inorganic powder having modified surface a resin composition containing the same Pending JPS6343964A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP61188098A JPS6343964A (en) 1986-08-11 1986-08-11 Inorganic powder having modified surface a resin composition containing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP61188098A JPS6343964A (en) 1986-08-11 1986-08-11 Inorganic powder having modified surface a resin composition containing the same

Publications (1)

Publication Number Publication Date
JPS6343964A true JPS6343964A (en) 1988-02-25

Family

ID=16217665

Family Applications (1)

Application Number Title Priority Date Filing Date
JP61188098A Pending JPS6343964A (en) 1986-08-11 1986-08-11 Inorganic powder having modified surface a resin composition containing the same

Country Status (1)

Country Link
JP (1) JPS6343964A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0678561A3 (en) * 1994-04-22 1998-07-22 BASF Aktiengesellschaft Metal pigments twice passivated in a gaseous phase
WO2004052897A1 (en) * 2002-12-10 2004-06-24 Nippon Unicar Company Limited Phosphorus-containing organosilicon compounds, process for production thereof, and resin compositions or coating compositions containing the same
JP2007031259A (en) * 2005-06-22 2007-02-08 Nissan Motor Co Ltd Metal oxide particle composite, metal oxide composite sol, and method for producing metal oxide composite sol
JP2009518510A (en) * 2005-12-05 2009-05-07 スリーエム イノベイティブ プロパティズ カンパニー Flame retardant polymer composition
JP2013184945A (en) * 2012-03-09 2013-09-19 National Institute Of Advanced Industrial Science & Technology Iminophosphorane compound, process for producing the same, and method of modifying surface of base material using the same
US9249033B2 (en) * 2007-03-14 2016-02-02 Toda Kogyo Corporation Ferrite particles for bonded magnets, resin composition for bonded magnets, and molded product comprising the same
WO2017063096A1 (en) * 2015-10-16 2017-04-20 Nanograde Ag Solution-processable hri inorganic/organic hybrid optical films
CN113429435A (en) * 2021-06-30 2021-09-24 成都硅宝科技股份有限公司 Silane coupling agent containing phosphorus and nitrogen and preparation method thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0678561A3 (en) * 1994-04-22 1998-07-22 BASF Aktiengesellschaft Metal pigments twice passivated in a gaseous phase
WO2004052897A1 (en) * 2002-12-10 2004-06-24 Nippon Unicar Company Limited Phosphorus-containing organosilicon compounds, process for production thereof, and resin compositions or coating compositions containing the same
JPWO2004052897A1 (en) * 2002-12-10 2006-04-13 東レ・ダウコーニング株式会社 Phosphorus-containing organosilicon compound, method for producing the same, and resin composition or coating composition containing the same
US7223880B2 (en) 2002-12-10 2007-05-29 Nippon Unicar Company Limited Phosphorus-containing organosilicon compound, a method for producing the same, and a resin composition or a coating composition containing the same
JP4553734B2 (en) * 2002-12-10 2010-09-29 東レ・ダウコーニング株式会社 Phosphorus-containing organosilicon compound, method for producing the same, and resin composition or coating composition containing the same
JP2007031259A (en) * 2005-06-22 2007-02-08 Nissan Motor Co Ltd Metal oxide particle composite, metal oxide composite sol, and method for producing metal oxide composite sol
JP2009518510A (en) * 2005-12-05 2009-05-07 スリーエム イノベイティブ プロパティズ カンパニー Flame retardant polymer composition
US9249033B2 (en) * 2007-03-14 2016-02-02 Toda Kogyo Corporation Ferrite particles for bonded magnets, resin composition for bonded magnets, and molded product comprising the same
JP2013184945A (en) * 2012-03-09 2013-09-19 National Institute Of Advanced Industrial Science & Technology Iminophosphorane compound, process for producing the same, and method of modifying surface of base material using the same
WO2017063096A1 (en) * 2015-10-16 2017-04-20 Nanograde Ag Solution-processable hri inorganic/organic hybrid optical films
KR20180072681A (en) * 2015-10-16 2018-06-29 아반타마 아게 Solution-processable HRI inorganic / organic hybrid optical film
CN113429435A (en) * 2021-06-30 2021-09-24 成都硅宝科技股份有限公司 Silane coupling agent containing phosphorus and nitrogen and preparation method thereof

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