JPS59232146A - Silicone resin composition for transfer molding - Google Patents

Silicone resin composition for transfer molding

Info

Publication number
JPS59232146A
JPS59232146A JP10823783A JP10823783A JPS59232146A JP S59232146 A JPS59232146 A JP S59232146A JP 10823783 A JP10823783 A JP 10823783A JP 10823783 A JP10823783 A JP 10823783A JP S59232146 A JPS59232146 A JP S59232146A
Authority
JP
Japan
Prior art keywords
silicone resin
parts
transfer molding
examples
10pts
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
JP10823783A
Other languages
Japanese (ja)
Inventor
Shiyunrokurou Shirahama
白浜 俊六郎
Yoshihiro Koyama
芳弘 小山
Toshio Miyamoto
敏男 宮本
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.)
Shin Etsu Chemical Co Ltd
Original Assignee
Shin Etsu Chemical 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 Shin Etsu Chemical Co Ltd filed Critical Shin Etsu Chemical Co Ltd
Priority to JP10823783A priority Critical patent/JPS59232146A/en
Publication of JPS59232146A publication Critical patent/JPS59232146A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To obtain a silicone resin for transfer molding, which has excellent workability and is harmless to the human body, by adding a filler and zinc benzoate to a silicone resin. CONSTITUTION:50-500pts.wt. filler and 0.5-10pts.wt. zinc benzoate are kneaded with 100pts.wt. silicone resin. If desired, additives such as pigment or partint agent may be added. Examples of the pigments are iron oxide, carbon black and titanium dioxide. Examples of the parting agents are zinc stearate and calcium stearate. Examples of the fillers are dry-process silica, wet-process silica and calcium silicate. When the quantity of zinc benzoate is less than 0.5-pts.wt., no satisfactory catalytic effect can be obtd., while, when it exceeds 10pts.wt., a problem in flow characteristics required for transfer molding is caused, so that the quantity ranging from 0.5 to 10pts.wt. is preferred.

Description

【発明の詳細な説明】 不発明は圧送成形用シリコーン樹脂組成物、特には衛生
上無害とされる圧送成形用のシリコーン樹脂組成物に関
するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a silicone resin composition for pressure-feed molding, and particularly to a silicone resin composition for pressure-feed molding that is considered to be harmless from a sanitary standpoint.

圧送成形用のシリコーン樹脂組成物がシリコーン樹脂に
充填剤と触媒を添加したものであることはよく知られた
ところであり、この製造に当ってはシリコーン樹脂が一
般にもろい固体であることから、これを予じめ80〜1
00℃に加熱して溶融し、ついでこれに充填剤、鴫媒を
添加してこれらを均一に混合するという方法をとること
が必要とされているが、シリコーン樹脂が熱り更化性樹
脂であり、硬化触媒の共存下で加熱されると徐々に樹脂
が硬化し始め、最終的には流れ特性のわるい成形材料に
なってしまうというおそれがある。しかし、この圧送成
形用樹脂には、圧縮成形、移送成形あるいは射出成形用
の金型に入れたと氷に、150〜200℃に加熱されて
いる金型内で溶融してゲル化するまでにそれが金型のす
みずみにまで流れ込まなければならず、さらにはできる
だけ速やか(−ゲル化反応を起して成形品としての必要
特性をもつ硬化物にならなければならないという矛盾し
た特性が要求されている。
It is well known that silicone resin compositions for pressure molding are made by adding fillers and catalysts to silicone resin. 80-1 in advance
It is necessary to heat the silicone resin to 00°C to melt it, then add the filler and the solvent and mix them uniformly. However, when heated in the presence of a curing catalyst, the resin gradually begins to harden, and there is a risk that the resin will eventually become a molding material with poor flow characteristics. However, when this pressure molding resin is put into a mold for compression molding, transfer molding, or injection molding, it melts and gels in the mold heated to 150 to 200 degrees Celsius. It must flow into every corner of the mold, and it must also undergo a gelation reaction as quickly as possible to form a cured product with the necessary properties as a molded product. There is.

そのため、この圧送成形用シリコーン樹脂を構成するシ
リコーン樹脂、硬化触媒(二ついては、流れ特性を犠牲
にすることなく、しかもすぐれた硬化特性な示すものを
選択する必要があり、この触媒としては一酸化鉛、炭酸
鉛などの鉛化合物、またはカドミウムなどの重金属化合
物の使用が効果的であり、実用化されてきているけれど
も、この種の重金属化合物は衛生上有害であるといつこ
とから、この代わりC:各種のアミン、ある種のヱポキ
シ化合物、ヘテロポリ酸、有機カルボン酸塩などを使用
することも提案されているが、これらはいずれも圧送成
形用組成物として満足丁べき結果を与えるものではない
Therefore, it is necessary to select a silicone resin and a curing catalyst that make up this silicone resin for pressure-feed molding, and a curing catalyst that exhibits excellent curing properties without sacrificing flow properties. Although the use of lead, lead compounds such as lead carbonate, or heavy metal compounds such as cadmium is effective and has been put into practical use, since these types of heavy metal compounds are hazardous to hygiene, C. Although it has been proposed to use various amines, certain epixy compounds, heteropolyacids, organic carboxylic acid salts, etc., none of these gives satisfactory results as a pressure molding composition.

本発明はこれらの不利を解決した圧送成形用シリコーン
樹脂組成物に関するものであり、これはシリコーン樹脂
100重量部に対し充填剤50〜500重量部および安
息香酸亜鉛0.5〜10重量部を添加してなることを特
徴とするものである。
The present invention relates to a silicone resin composition for pressure-feed molding which solves these disadvantages, and which contains 50 to 500 parts by weight of filler and 0.5 to 10 parts by weight of zinc benzoate to 100 parts by weight of silicone resin. It is characterized by:

これを説明すると、本発明者らはこの圧送成形)   
   用シリコーン樹脂の無毒化に注目し、種々検討し
た結果、シリコーン樹脂と充填剤とからなる配合物C=
安息香酸亜鉛を添加テれば、人体に無害な圧送成形用シ
リコーン樹脂を得ることができることを見出すと共(二
、この安息香酸亜鉛が150〜280℃でシリコーン樹
脂に対し有効な硬化触媒として作動し、この温度で成形
加工丁れば容易(1硬化した成形品を得ることができる
が、これは50〜100℃では殆んど触媒効果を示さな
いので、この圧送成形用組成物がその製造工程における
事前の混練などの作業性に丁ぐれていること、これによ
れば特性のよい組成物を容易に得ることができること、
またこの組成物が毒性面では全く心配する必要がないと
いうことを確認して本発明を完成させた。
To explain this, the inventors have developed this pressure-feed molding)
As a result of various studies focusing on the detoxification of silicone resin for use in commercial use, we found a compound C= consisting of silicone resin and filler.
They discovered that by adding zinc benzoate, it was possible to obtain a silicone resin for pressure molding that was harmless to the human body. However, it is easy to obtain a cured molded product by molding at this temperature, but since it exhibits almost no catalytic effect at 50 to 100°C, this pressure molding composition is suitable for its production. It has excellent workability such as prior kneading in the process, and it is possible to easily obtain a composition with good characteristics.
Furthermore, the present invention was completed after confirming that there is no need to worry about the toxicity of this composition.

本発明の組成物を構成する主剤としてのシリコーン樹脂
は公知であり、これは  06H,5i03,2゜(0
,H5)2Sin、 0H3SiOp 、 (OH3)
2Sin。
The silicone resin as the main ingredient constituting the composition of the present invention is known, and is 06H,5i03,2°(0
,H5)2Sin, 0H3SiOp, (OH3)
2Sin.

キチン樹脂、メチルフェニルシロキサン樹脂などが例示
されるが、これについてはメチルフェニルシロキサン樹
脂とし、その分子中(二けい素原子に結合する水酸基を
少なくとも0.1重量%含有するものとすることが好ま
しい。
Examples include chitin resin, methylphenylsiloxane resin, etc., but it is preferable that the resin be methylphenylsiloxane resin and contain at least 0.1% by weight of hydroxyl groups bonded to disilicon atoms in the molecule. .

また、このシリコーン樹脂に配合される充填剤も公知の
ものでよく、これにはヒユームドシリカなどの乾式シリ
カ、湿式シリカ、石英粉、けい酸カルシウム、けい酸ジ
ルコニウム、けい酸マグネシウム、けい酸リチウム、け
い酸アルミニウムなどのけい酸塩、ガラス、けい藻土な
どが例示されるが、これは前記したシリコーン樹脂10
0重量部に対し、50〜500重量部の範囲で添加すれ
ばよい。
In addition, the filler compounded in this silicone resin may be a known filler, and includes dry silica such as fumed silica, wet silica, quartz powder, calcium silicate, zirconium silicate, magnesium silicate, lithium silicate, Examples include silicates such as aluminum acid, glass, diatomaceous earth, etc., which are similar to silicone resin 10 described above.
It may be added in an amount of 50 to 500 parts by weight relative to 0 parts by weight.

本発明の組成物はこのシリコーン樹脂と充填剤とからな
るシリコーンコンパウンドに硬化用触媒として安息香酸
亜鉛を添加するものであるが、その添加量をシリコーン
樹脂100重量部に対し0.5重量部以下とするとその
触媒効果が弱く、これを10重量部以上とすると圧送成
形に必要とされる流れ特性などC二問題が生じるので、
これはシリコーン樹脂100重櫃部に対し0.5〜10
重量部とすることがよい。
In the composition of the present invention, zinc benzoate is added as a curing catalyst to a silicone compound consisting of a silicone resin and a filler, and the amount of zinc benzoate added is 0.5 parts by weight or less per 100 parts by weight of silicone resin. If it is, the catalytic effect will be weak, and if it exceeds 10 parts by weight, C2 problem will occur, such as the flow characteristics required for pressure molding.
This is 0.5 to 10 parts per 100 parts of silicone resin.
It is preferable to use parts by weight.

なお、本発明の組成物は上記した各成分のほか、適宜の
顔料、離型剤を添加してもよく、この顔料としては酸化
鉄、カーボンブラック、二酸化チタンなどが例示され、
離型剤としてはステアリン酸亜鉛、ステアリン酸カルシ
ウムなどが例示される。
In addition to the above-mentioned components, the composition of the present invention may also contain appropriate pigments and release agents, such as iron oxide, carbon black, titanium dioxide, etc.
Examples of the mold release agent include zinc stearate and calcium stearate.

本発明の組゛成物は上記した各成分を混合することによ
って得ることができるが、これらは同時に混合しても順
次に配合してもよく、この混合は公知の方法である二本
ロール、押出機、加圧ニーダ−などを用いて行なえばよ
い。
The composition of the present invention can be obtained by mixing the above-mentioned components, which may be mixed simultaneously or sequentially. This may be carried out using an extruder, a pressure kneader, or the like.

本発明の組成物は上記したように安息香酸亜鉛を硬化触
媒とするものであることから、この組成物はその混合時
に何ら硬化することがなく、金型に対する圧送中におけ
るスパイラルフロー値も30ぼ以上と良好なもので金型
の丁みすみにまで容易に流れるし、加熱処理後は速か(
1硬化するので、圧送成形用として有用なものとされ、
例えば1、 O,、ダイオード、整流器、サイリスタ、
抵抗素子、コイルなどのように耐熱性と高電気特性を要
求される各種電子、電気分野に好適とされるほか、全く
無毒であるということから各種厨房器具部品用として最
適とされる。
Since the composition of the present invention uses zinc benzoate as a curing catalyst as described above, this composition does not harden at all during mixing, and its spiral flow value during pressure feeding to a mold is approximately 30. With the above-mentioned good properties, it flows easily to the nooks and crannies of the mold, and it is fast after heat treatment (
1 cures, so it is considered useful for pressure molding.
For example, 1, O, diode, rectifier, thyristor,
It is suitable for various electronic and electrical fields that require heat resistance and high electrical properties, such as resistive elements and coils, and is completely non-toxic, making it ideal for various kitchen appliance parts.

つぎ(二本発明の実施例をあげるが、例中における部は
重量部、粘度は25℃における測定値を示したものであ
る。
Two examples of the present invention are given below, in which parts are parts by weight and viscosity is a value measured at 25°C.

実施例1゜ 0.25%量のけい素原子に結合した水酸基を有する。Example 1゜ It has 0.25% amount of hydroxyl groups bonded to silicon atoms.

50%トルエン溶液の粘度が9oSであるメチルフェニ
ルシロキチン樹脂〔メチル基/フェニル基=1(モル比
))100部に石英粉200部、黒色顔料5部およびス
テアリン酸亜鉛2部を乾式混合してから、約100℃の
ロールと50℃のロールを組合せた二本ロールで4分間
混練し、ついでここに第1表に示したような種々の触媒
を添加して4分間混練りして組成物を作った。
200 parts of quartz powder, 5 parts of black pigment, and 2 parts of zinc stearate were dry mixed with 100 parts of methylphenylsilochitin resin [methyl group/phenyl group = 1 (molar ratio)] whose viscosity was 9oS in a 50% toluene solution. After that, the mixture was kneaded for 4 minutes using two rolls, one at about 100°C and the other at 50°C, and then various catalysts as shown in Table 1 were added and kneaded for 4 minutes to obtain the composition. made things.

つぎに、これらの組成物20.Pを42に9/、!(6
00psi )で金型に圧送し、175℃、56KP/
crIで成形したところ、そのときのスパイラルフロー
値は第1表に併記したとおりであり、これらの試験結果
は下記に示したとおりであった。
Next, these compositions 20. P to 42 9/,! (6
00psi) into the mold, 175℃, 56KP/
When molded with crI, the spiral flow values at that time were as listed in Table 1, and the test results were as shown below.

なお、本例のaxdは鉛系化合物を触媒として使用して
いないので、鉛系化合物を使用する従来品が鉛、カドミ
ウムなど人体に有害な物質を数千ppm含むものであっ
たのに対し、いずれもこれらの有害物質を殆んど含まな
いものであったが、このa−dでは下記のようにaだけ
が圧送成形用シリコーン樹脂として満μ丁べき結果を与
えた。
In addition, since the AXD of this example does not use lead-based compounds as a catalyst, conventional products that use lead-based compounds contain several thousand ppm of substances harmful to the human body such as lead and cadmium. All of them contained almost no of these harmful substances, but among these a to d, only a gave satisfactory results as a silicone resin for pressure-feed molding, as shown below.

第1表 試料a・・・圧送成形用樹脂として満足丁べき結果が得
られた。
Table 1 Sample a: Satisfactory results were obtained as a pressure-feed molding resin.

試料b・・・高温(150〜200℃)での硬化が非常
C二連く、実用には到らなかった。
Sample b: curing at high temperatures (150 to 200°C) was extremely severe twice, and could not be put to practical use.

試料0・・・圧送成形用樹脂としては満足すべき結果乞
得たが、硬化物に酢酸臭があり実用には適さなかった。
Sample 0: Satisfactory results were obtained as a pressure molding resin, but the cured product had an acetic acid odor and was not suitable for practical use.

試料d・・・高温時の硬化が非常に遅く、実用には到ら
なかった。
Sample d: Curing at high temperatures was extremely slow and could not be put to practical use.

実施例2゜ 実施例1で使用したメチルフェニルシロキサン樹脂10
0部に、石英粉200部、ガラス短繊維50部、黒色顔
料5部およびステアリン酸亜鉛2部を乾式混合してから
約100℃のロールと50℃のロールを組合わせた2本
ロールで約4分間混練りし、ついでこれに安息香酸亜鉛
2.5部を添加して約4分間混練りして組成物をつくっ
た。
Example 2゜Methylphenylsiloxane resin 10 used in Example 1
0 parts, 200 parts of quartz powder, 50 parts of short glass fibers, 5 parts of black pigment, and 2 parts of zinc stearate are dry-mixed, and then mixed with two rolls (a combination of rolls at about 100°C and rolls at 50°C). The mixture was kneaded for 4 minutes, and then 2.5 parts of zinc benzoate was added thereto and kneaded for about 4 minutes to prepare a composition.

つぎに、この組成物を前例と同様にして圧送成形し、得
られた成形品についての物性を測定したところ、つぎの
第2表に示すとおりの結果が得られた。
Next, this composition was pressure molded in the same manner as in the previous example, and the physical properties of the resulting molded product were measured, and the results shown in Table 2 below were obtained.

第2表 特許出願人 信越化学工業株式会社  11−Table 2 Patent applicant: Shin-Etsu Chemical Co., Ltd. 11-

Claims (1)

【特許請求の範囲】[Claims] 1、 シリコーン樹脂100重量部に充填剤50〜50
0重量部および安息香酸亜鉛0.5〜10重量部を添加
してなることを特徴とする圧送成形用シリコーン樹脂組
成物
1. 50-50 parts by weight of filler in 100 parts by weight of silicone resin
0 parts by weight and 0.5 to 10 parts by weight of zinc benzoate.
JP10823783A 1983-06-16 1983-06-16 Silicone resin composition for transfer molding Pending JPS59232146A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10823783A JPS59232146A (en) 1983-06-16 1983-06-16 Silicone resin composition for transfer molding

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP10823783A JPS59232146A (en) 1983-06-16 1983-06-16 Silicone resin composition for transfer molding

Publications (1)

Publication Number Publication Date
JPS59232146A true JPS59232146A (en) 1984-12-26

Family

ID=14479539

Family Applications (1)

Application Number Title Priority Date Filing Date
JP10823783A Pending JPS59232146A (en) 1983-06-16 1983-06-16 Silicone resin composition for transfer molding

Country Status (1)

Country Link
JP (1) JPS59232146A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2075280A1 (en) * 2007-12-26 2009-07-01 Shin-Etsu Chemical Co., Ltd. White heat-curable silicone resin composition, optoelectric part case, and molding method
US8012381B2 (en) 2008-06-09 2011-09-06 Shin-Etsu Chemical Co., Ltd. White heat-curable silicone resin composition and optoelectronic part case
US8173053B2 (en) 2008-06-09 2012-05-08 Shin-Etsu Chemical Co., Ltd. White heat-curable silicone resin composition and optoelectronic part case
US11091636B2 (en) 2017-06-19 2021-08-17 Dow Silicones Corporation Liquid silicone composition for transfer- or injection-molding optical parts, optical parts made therefrom, and a method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2075280A1 (en) * 2007-12-26 2009-07-01 Shin-Etsu Chemical Co., Ltd. White heat-curable silicone resin composition, optoelectric part case, and molding method
JP2009155415A (en) * 2007-12-26 2009-07-16 Shin Etsu Chem Co Ltd White thermosetting silicone resin composition for optical semiconductor case, optical semiconductor case, and molding method therefor
JP4623322B2 (en) * 2007-12-26 2011-02-02 信越化学工業株式会社 White thermosetting silicone resin composition for forming optical semiconductor case, optical semiconductor case and molding method thereof
US8013056B2 (en) 2007-12-26 2011-09-06 Shin-Etsu Chemical Co., Ltd. White heat-curable silicone resin composition, optoelectronic part case, and molding method
US8012381B2 (en) 2008-06-09 2011-09-06 Shin-Etsu Chemical Co., Ltd. White heat-curable silicone resin composition and optoelectronic part case
US8173053B2 (en) 2008-06-09 2012-05-08 Shin-Etsu Chemical Co., Ltd. White heat-curable silicone resin composition and optoelectronic part case
US11091636B2 (en) 2017-06-19 2021-08-17 Dow Silicones Corporation Liquid silicone composition for transfer- or injection-molding optical parts, optical parts made therefrom, and a method thereof

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