JPS58183737A - Surface-treated filler - Google Patents

Surface-treated filler

Info

Publication number
JPS58183737A
JPS58183737A JP6546082A JP6546082A JPS58183737A JP S58183737 A JPS58183737 A JP S58183737A JP 6546082 A JP6546082 A JP 6546082A JP 6546082 A JP6546082 A JP 6546082A JP S58183737 A JPS58183737 A JP S58183737A
Authority
JP
Japan
Prior art keywords
carboxylic acid
filler
acid ester
unsaturated carboxylic
hydroxyl
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
JP6546082A
Other languages
Japanese (ja)
Other versions
JPS6313450B2 (en
Inventor
Jiro Saito
斉藤 二郎
Takahiro Hirai
平井 隆宥
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.)
Calp Kogyo KK
Original Assignee
Calp Kogyo KK
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 Calp Kogyo KK filed Critical Calp Kogyo KK
Priority to JP6546082A priority Critical patent/JPS58183737A/en
Publication of JPS58183737A publication Critical patent/JPS58183737A/en
Publication of JPS6313450B2 publication Critical patent/JPS6313450B2/ja
Granted legal-status Critical Current

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  • Compositions Of Macromolecular Compounds (AREA)

Abstract

PURPOSE:To provide the titled filler capable of improving the moldability of a resin composition and reducing the temperature dependency of its flowability, and suitable as a modifier for synthetic resins and rubbers, by coating the surface of a filler with a hydroxyl-containing carboxylic acid ester. CONSTITUTION:The objective filler coated with a hydroxyl-containing carboxylic acid ester and optionally an unsaturated carboxylic acid, can be prepared by charging (A) a hydroxyl-containing carboxylic acid ester (preferably an unsaturated carboxylic acid lower hydroxyalkyl ester such as 2-hydroxyethyl methacrylate) and optionally 10-50wt% of an unsaturated carboxylic acid such as (meth) acrylic acid and (B) a filler such as ground limestone, etc. in e.g. a heat kneader, and mixing e.g. at 100-150 deg.C for 5-15min if necessary adding a lubricant, a radical generator, a pigment, and an antistatic agent to the mixture. EFFECT:The flow of the resin composition in the mold can be made uniform, and the molded product has little deformation and warpage.

Description

【発明の詳細な説明】 本発明は表向処理充填剤に関し、詳しくは特定の被膜を
表面に形成した表面処理充填剤に関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a surface-treated filler, and more particularly to a surface-treated filler having a specific coating formed on its surface.

無機および/または有橋充填剤はポリオレフィン、ボり
塩化ビニルなどの合成樹脂の機械的強度。
Inorganic and/or bridged fillers improve the mechanical strength of synthetic resins such as polyolefins and polyvinyl chloride.

熱的性實や塗装性、さらには成形性を改良する目的で使
用されているほか、炭酸カルシウム、クレーなどの無機
充填剤は塗料、インキ等の成分などとして広く利用され
ている。九とえば、ポリオレフィンの改質を目的として
°炭酸カルシウム、炭酸マグネシウム、亜硫酸カルシウ
ム、硫酸ノくリウム。
In addition to being used to improve thermal properties, paintability, and even moldability, inorganic fillers such as calcium carbonate and clay are widely used as components of paints, inks, and the like. For example, °calcium carbonate, magnesium carbonate, calcium sulfite, norium sulfate for the purpose of modifying polyolefins.

シリカ、タルク、ケイソウ上、木粉、セルロース等の充
填剤が用いられてお抄、これら充填剤の粒子−けポリオ
レフィンと混練するに先立って有機酸などの表面処理剤
によって表面処理をして分散性の向上が図られている。
Fillers such as silica, talc, diatom, wood flour, and cellulose are used in papermaking, and the particles of these fillers are surface-treated and dispersed with a surface treatment agent such as an organic acid before being kneaded with the polyolefin. Improvements are being made in this area.

しかしながら、有機酸で表面処理をした充填剤をポリオ
レフィンに配合したものii変色しやすく、70−マー
クの発生や成形品にソリが発生するほか塗装性の改善が
十分でないという欠点がある。
However, when a filler whose surface has been treated with an organic acid is blended with a polyolefin, it is easily discolored, causes 70-marks and warps on molded products, and has the disadvantage that the paintability is not sufficiently improved.

そこで本発明者らは、このような欠点のない表+MJ処
理充填剤を開発すべく検討を重ねた結果、本発明に到−
したのである。
Therefore, the present inventors conducted repeated studies to develop a table + MJ treated filler that does not have such drawbacks, and as a result, they arrived at the present invention.
That's what I did.

本発明はヒドロキシル基を有するカルボン酸エステルの
被膜を表面に形成してなる表面処理充填剤に関する。さ
らに、本発明はヒドロキシル基を有スルカルボン酸エス
テルおよび不飽和カルボン酸の被膜を表面に形成してな
る表面処理充填剤に関する。
The present invention relates to a surface-treated filler having a surface coated with a carboxylic acid ester having a hydroxyl group. Furthermore, the present invention relates to a surface-treated filler formed by forming a film of a sulfurcarboxylic acid ester having a hydroxyl group and an unsaturated carboxylic acid on the surface.

本発明に用いる充填剤としては特に制限はなく、たとえ
ば0aOO,I Mg0O1、BaOOB等の炭酸塩;
OaO、MgO,Bad、  All0. 、  Ti
on 、 ZnO等の酸化物;0a(OH)1. Mg
(OH)、 、  ム1(OH’)、 e ”a(01
10m等の水酸化物;0a804 、  Mg80. 
、  Ba804等の硫酸塩;その他にシリカ、タルク
、クレー、マイカ、ガラス繊維、金属繊維、木粉、セル
リースなどの各種物質がある。
The filler used in the present invention is not particularly limited, and includes carbonates such as 0aOO, I Mg0O1, and BaOOB;
OaO, MgO, Bad, All0. , Ti
on, oxides such as ZnO; 0a(OH)1. Mg
(OH), , mu1(OH'), e ”a(01
Hydroxide such as 10m; 0a804, Mg80.
, sulfates such as Ba804; and various other substances such as silica, talc, clay, mica, glass fiber, metal fiber, wood powder, and cellulose.

これらは単独で用いてもよく、2以上を組合せて混合物
として用いてもよい。また、これら充填剤は通常、α1
〜10μ程度のサイズのものを用いる。
These may be used alone, or two or more may be used in combination as a mixture. In addition, these fillers are usually α1
A size of about 10 μm is used.

充填剤の表面に被膜を形成するために用いるヒドロキシ
ル基を有するカルボン酸エステルとじてt、i 、不飽
和カルボン酸のヒドロキシ低級アルキルエステルが好ま
しい。このエステルの具体例としては、2−ヒドロキシ
エチルアクリレート、2−ヒドロキシエチルメタクリレ
ート、2−ヒドロキシプロピルアクリレートなどがある
。これらの中では2−ヒドロキシエチルメタクリレ−F
が特に好ましい。このヒドロキシル基を有するカルボン
酸エステルは単独で用いてもよく、あるいは不飽和カル
ボン酸と混合して用いてもよい。ここで用イル不飽和カ
ルボン酸を例示するとアクリル酸。
The carboxylic acid ester having a hydroxyl group used to form a film on the surface of the filler is preferably a hydroxy lower alkyl ester of an unsaturated carboxylic acid. Specific examples of this ester include 2-hydroxyethyl acrylate, 2-hydroxyethyl methacrylate, and 2-hydroxypropyl acrylate. Among these, 2-hydroxyethyl methacrylate-F
is particularly preferred. This carboxylic acid ester having a hydroxyl group may be used alone or in combination with an unsaturated carboxylic acid. An example of the unsaturated carboxylic acid used here is acrylic acid.

メタクリル酸などをあげることができる。不飽和カルボ
ン酸を組合せて用いる場合、前記エステル100重量部
あたυ50重量部までの範囲で混合することができ、通
常は該エステル1Do重量部あたり10〜50重量部の
調合で用いる。不飽和カルボン酸の配合−が50重量部
を超えると、得られる表向処理充填剤をポリオレフィン
などの合成樹8ぽに配合した場合、白色度、成形性が劣
る場合がある。なお、上記範囲内で不飽和カルボン酸を
用いると、何らかの脱水反応が生起するものと!#測さ
れ、非常に良好な表面処理充填剤が得られる。
Examples include methacrylic acid. When unsaturated carboxylic acids are used in combination, they can be mixed in an amount of up to 50 parts by weight per 100 parts by weight of the ester, and usually 10 to 50 parts by weight per 1 part by weight of the ester. If the amount of unsaturated carboxylic acid exceeds 50 parts by weight, the whiteness and moldability may be poor when the resulting surface-treated filler is blended with a synthetic resin such as polyolefin. Note that if an unsaturated carboxylic acid is used within the above range, some dehydration reaction will occur! A very good surface treated filler is obtained.

この表面処理充填剤をポリオレフィンなどの合成樹脂に
配合すると、上記のようなトラブルがなく、W脂組成物
の成形性が向上し、かつ成形品の機械的強度が改良され
る。
When this surface-treated filler is blended with a synthetic resin such as polyolefin, the above-mentioned troubles are not caused, the moldability of the W resin composition is improved, and the mechanical strength of the molded article is improved.

充填剤に上記のカルボン酸エステルなど)被膜を形成せ
しめるには種々の方法を適用することができるか、たと
えば加熱型混練機に両者の所定臘を入れ、100〜15
0℃で5〜15分間混合する方法か好ましい。この場合
、必要に応じて他の成分、たとえば滑剤、ラジカル発生
剤(有機パーオキサイドなど)1m料、帯電防止剤、熱
安定剤などを適宜IJuえることができる。
Various methods can be used to form a coating (such as the above-mentioned carboxylic acid ester) on the filler.
A method of mixing at 0° C. for 5 to 15 minutes is preferred. In this case, other components such as a lubricant, a radical generator (organic peroxide, etc.), an antistatic agent, a heat stabilizer, etc. can be added as necessary.

充填剤の表面処理は上記カルボン酸ニス−y−hなどの
表向処理剤が単分子層を形成する程度に被覆すればよく
、具体的には充填剤100重量部あたり表向処理剤をα
5〜5重量部、好ましくはα5〜5重一部の割合で用い
ることが適当である。
For surface treatment of the filler, it is sufficient to coat the surface treatment agent such as the above-mentioned carboxylic acid varnish-yh to such an extent that a monomolecular layer is formed.
It is appropriate to use it in a proportion of 5 to 5 parts by weight, preferably 5 to 5 parts by weight.

本発明により表向処理した充填剤をポリオレフィンなど
の合成樹脂に配合する場合、合成樹脂に対し10〜90
重量%の範囲で配合することができる。本発明の表面処
理充填剤を合成樹脂に配合することにより、表向処理を
しない、あるいは既知の方法で表[i[iIJ!!1理
した充填剤の場合と同様に機械的性質や熱的性質を向上
させることができる。
When blending the surface-treated filler according to the present invention into synthetic resin such as polyolefin, the
It can be blended within a range of weight %. By blending the surface-treated filler of the present invention into a synthetic resin, surface treatment can be performed without surface treatment or by a known method. ! Mechanical properties and thermal properties can be improved in the same way as in the case of treated fillers.

しかも、得られる樹脂組成物の成形性が向上し、特に温
度依存性が小さく、金型内での流れが均一化する。した
がって、成形品の変形やソリが小さい。さらに、得られ
る成形品には70−マークが発生せず、変色もしない。
Moreover, the moldability of the resulting resin composition is improved, particularly the temperature dependence is small, and the flow within the mold becomes uniform. Therefore, deformation and warpage of the molded product are small. Furthermore, the resulting molded product does not have 70-marks or discoloration.

その上、成形品の塗装性も良好である。それ故、かかる
成形品は自動車部品、電機部品などの工業用材料として
有用である。本発明の表面処理充填剤は合成樹脂の改質
のほか、ゴム類の改智剤として有用である。また、充填
剤のうち炭酸カルシウムやクレーなどはさらに紙のコー
ティング剤、塗料やインキの体質顔料などとして用いる
ことができる。
Moreover, the paintability of the molded product is also good. Therefore, such molded products are useful as industrial materials for automobile parts, electrical equipment parts, and the like. The surface-treated filler of the present invention is useful not only for modifying synthetic resins but also as a plasticizer for rubbers. Further, among the fillers, calcium carbonate, clay, and the like can be further used as coating agents for paper, extender pigments for paints and inks, and the like.

次に本発明の実施例を示す。Next, examples of the present invention will be shown.

実施例1〜8 平均粒子径t7μ、比表面@ 1500cd/lの重質
炭酸カルシウム100重置部をヘンシェルミキサー中に
入れ、150℃に加温して攪拌しながら分装置150の
2−ヒドロキシエチルメタクリレート単独またはアクリ
ル酸との混合液を第1表に記載の割合でスプレー装置に
て霧状に添加し、常圧で15分間混合して表面を処理し
た充填剤(以下、表面処理充填剤という。)を得た。
Examples 1 to 8 100 overlapping parts of heavy calcium carbonate with an average particle diameter of t7μ and a specific surface of 1500 cd/l were placed in a Henschel mixer, heated to 150°C, and while stirring, 2-hydroxyethyl was added to the separation device 150. A filler whose surface has been treated by adding methacrylate alone or a mixture with acrylic acid in the proportions shown in Table 1 in the form of a mist using a spray device and mixing at normal pressure for 15 minutes (hereinafter referred to as surface-treated filler) ) was obtained.

表向処理充填剤をエチレン−プロピレンブロック共重合
体(メルトインデックス(iJ12t6ay。
The surface-treated filler is an ethylene-propylene block copolymer (melt index (iJ12t6ay).

温度250°C)8p710分、密度αq floi 
、商品名:J750H,出光石油化学■製)と第1表に
記載した割合で配合した。この配合物100重W部に対
してジクミルパーオキサイド102重量s、  ステア
リン酸モノグリセリド12重一部を加え、ヘンシェルミ
キサーにて常温で10分間攪拌、混合し。
Temperature 250°C) 8p710min, density αq floi
, trade name: J750H, manufactured by Idemitsu Petrochemical Co., Ltd.) in the proportions shown in Table 1. To 100 parts by weight of this mixture, 102 parts by weight of dicumyl peroxide and 12 parts by weight of stearic acid monoglyceride were added, and the mixture was stirred and mixed for 10 minutes at room temperature using a Henschel mixer.

た。次いで、この混合物の所定量をバンパIJ  ミキ
サーで樹脂温度230℃にて5分関湿練し、しかる後ロ
ールでシート化し、シートヘレタイザーでペレット化し
た。
Ta. Next, a predetermined amount of this mixture was wet kneaded for 5 minutes at a resin temperature of 230° C. using a bumper IJ mixer, and then formed into a sheet using a roll and pelletized using a sheet heretizer.

このようにして得られた樹脂組成物を用い射出成形+I
A(新潟鉄工所製、811(So )にて樹脂温度21
0°C2金型温度50℃の条件で成形してASTM規格
試験片を作製した。この試験片の物性を測定1、た結果
を第1表に示す。なお、各項目の測定力r人は以Fのと
おりである。
Injection molding +I using the resin composition thus obtained
A (manufactured by Niigata Iron Works, resin temperature 21 at 811 (So)
An ASTM standard test piece was prepared by molding at a temperature of 0°C and a mold temperature of 50°C. The physical properties of this test piece were measured 1 and the results are shown in Table 1. The measurement ability of each item is as follows.

引張特性:A8テM D−658による曲げ特性: h
BTM D−790によるアイゾツト−撃性: A8T
M D−256による表面光沢度:ム8〒M D−52
5による白色度:標準体(Mgo )を100%とした
比較法によシケット科研光電比色、計C− 1型プルーフイルターを用いて測定 した。
Tensile properties: A8 TeM Bending properties by D-658: h
Izot impact performance with BTM D-790: A8T
Surface gloss according to MD-256: 8〒MD-52
Whiteness according to No. 5: Measured using a comparative method using a standard (Mgo) as 100% using a Thickett Kaken photoelectric colorimeter and a C-1 type proof filter.

成形性:飯150■、横200■、深さ4o■、肉厚2
■の釉を各成形温度、金型温度 で成形したときの最小光てん圧力の 圧力差(△P)を測定して判定した。
Formability: Rice 150■, Width 200■, Depth 4o■, Wall thickness 2
The determination was made by measuring the pressure difference (△P) of the minimum light pressure when molding the glaze (2) at each molding temperature and mold temperature.

○・・・ΔPが小さい △・・・△Pがやや大きい ×・・・△Pが大きい フト→−ン:縦76so*、横76■、肉厚5IIll
Iのプレートを成形したときの樹脂組成物の流 れ状態を観察して判定した。なお、 70−パターンは第1図のような均 一なフローをパターンAとし、第2 図のような不均一なフローをパター ンBとした。
○... ΔP is small △... △P is slightly large ×... △P is large Foot→-N: Height 76so*, width 76■, wall thickness 5IIll
The determination was made by observing the flow state of the resin composition when molding the plate I. As for the 70-pattern, a uniform flow as shown in FIG. 1 was designated as pattern A, and a non-uniform flow as shown in FIG. 2 was designated as pattern B.

成形品のソlJ:  縦150■、横200諺、深さ4
0■、肉厚2■の箱を成形したときの内シリ の程度を観察して判定した。
Molded product size: 150mm long, 200mm wide, 4 deep
It was determined by observing the degree of internal sillage when a box with a wall thickness of 0.0 cm and a wall thickness of 2.0 cm was molded.

塗装性:ポリウレタン樹脂塗料を塗布後、120℃で5
0分乾燥して塗布面に1■平方のゴパン目を100個鋭
い刃先で 傷を入れ、セロハンテープを用いて 剥離した。表中のA/100のムはゴバン目塗膜の残数
を示す。
Paintability: 5 at 120℃ after applying polyurethane resin paint.
After drying for 0 minutes, 100 1 square goblets were scratched on the coated surface with a sharp knife edge and peeled off using cellophane tape. In the table, A/100 indicates the number of remaining rough coating films.

比較例1〜5 表面処理をしない充填剤もしくは本発明に用いる表ll
11処理剤以外のもので表面処理をした充填剤を使用1
.7たこと以外は実施例1と同様に行なった。
Comparative Examples 1 to 5 Fillers without surface treatment or Table II used in the present invention
11 Using a filler whose surface has been treated with something other than a treatment agent 1
.. The same procedure as in Example 1 was carried out except for the following.

結果を第1表に示す。The results are shown in Table 1.

11較例 1表11 comparative examples 1 table

【図面の簡単な説明】[Brief explanation of the drawing]

第1図および第2図Fi樹脂組成物の成形時のローパタ
ーンを示すものである。 1−・ Tダイ 、  2・−金型 特許出願人  カルプ工業株式会社
FIGS. 1 and 2 show row patterns during molding of the Fi resin composition. 1-・T-die, 2--Mold patent applicant Calp Industries Co., Ltd.

Claims (1)

【特許請求の範囲】 (II  ヒドロキシル基を有するカルメン酸エステル
の被膜を表面に形成してなる表面処理充填剤。 (2)  ヒドロキシル基を有するカルビン酸エステル
が不飽和カルホ゛ン酸のヒドロキシ低級アルキルエステ
ルである特許請求の範囲第1項記載の表面処理充填剤。 (3)  ヒドロキシル基を有するカルビン酸エステル
および不飽和カルメン酸の被膜を表面に形成してなる表
面処理充填剤。 (4)  ヒドロキシル基を有するカルビン酸エステル
が不飽和カルボン酸のとドロキシ低級アルキルエステル
である特許請求の範囲第3項記載の表面処理充填剤。
[Scope of Claims] (II) A surface-treated filler formed by forming a film of a carmenic acid ester having a hydroxyl group on its surface. (2) The carbic acid ester having a hydroxyl group is a hydroxy lower alkyl ester of an unsaturated carbonic acid. A surface-treated filler according to claim 1. (3) A surface-treated filler formed by forming a film of carbic acid ester and unsaturated carmenic acid having hydroxyl groups on the surface. (4) A filler having hydroxyl groups. 4. The surface-treated filler according to claim 3, wherein the carbic acid ester is a droxy lower alkyl ester of an unsaturated carboxylic acid.
JP6546082A 1982-04-21 1982-04-21 Surface-treated filler Granted JPS58183737A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP6546082A JPS58183737A (en) 1982-04-21 1982-04-21 Surface-treated filler

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP6546082A JPS58183737A (en) 1982-04-21 1982-04-21 Surface-treated filler

Publications (2)

Publication Number Publication Date
JPS58183737A true JPS58183737A (en) 1983-10-27
JPS6313450B2 JPS6313450B2 (en) 1988-03-25

Family

ID=13287754

Family Applications (1)

Application Number Title Priority Date Filing Date
JP6546082A Granted JPS58183737A (en) 1982-04-21 1982-04-21 Surface-treated filler

Country Status (1)

Country Link
JP (1) JPS58183737A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6375055A (en) * 1986-09-19 1988-04-05 Mitsui Toatsu Chem Inc Polypropylene resin composition
JPH028265A (en) * 1988-01-21 1990-01-11 Deutsche Solvay Werke Gmbh Under floor surface protective composition for car and production thereof and control of rheology of said composition

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS50129496A (en) * 1974-02-09 1975-10-13
JPS5141039A (en) * 1974-10-02 1976-04-06 Sumitomo Chemical Co HOKYO SEIJUTENZAI
JPS5238581A (en) * 1975-09-23 1977-03-25 Nippon Kokan Kk Method of inhibiting corrosion for deformed pipes
JPS5272739A (en) * 1975-12-13 1977-06-17 Maruo Calcium Process for manufacturing reinforcing calcium carbonate for thermosetting resin
JPS5349049A (en) * 1976-10-18 1978-05-04 Asahi Chem Ind Co Ltd Polyolefin composition
JPS5538874A (en) * 1978-09-11 1980-03-18 Nl Industries Inc Coupling agent for thermoplastic composite

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS50129496A (en) * 1974-02-09 1975-10-13
JPS5141039A (en) * 1974-10-02 1976-04-06 Sumitomo Chemical Co HOKYO SEIJUTENZAI
JPS5238581A (en) * 1975-09-23 1977-03-25 Nippon Kokan Kk Method of inhibiting corrosion for deformed pipes
JPS5272739A (en) * 1975-12-13 1977-06-17 Maruo Calcium Process for manufacturing reinforcing calcium carbonate for thermosetting resin
JPS5349049A (en) * 1976-10-18 1978-05-04 Asahi Chem Ind Co Ltd Polyolefin composition
JPS5538874A (en) * 1978-09-11 1980-03-18 Nl Industries Inc Coupling agent for thermoplastic composite

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6375055A (en) * 1986-09-19 1988-04-05 Mitsui Toatsu Chem Inc Polypropylene resin composition
JPH028265A (en) * 1988-01-21 1990-01-11 Deutsche Solvay Werke Gmbh Under floor surface protective composition for car and production thereof and control of rheology of said composition

Also Published As

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JPS6313450B2 (en) 1988-03-25

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