JPH04201435A - Preparation of molded item made of polyimide resin - Google Patents
Preparation of molded item made of polyimide resinInfo
- Publication number
- JPH04201435A JPH04201435A JP33463790A JP33463790A JPH04201435A JP H04201435 A JPH04201435 A JP H04201435A JP 33463790 A JP33463790 A JP 33463790A JP 33463790 A JP33463790 A JP 33463790A JP H04201435 A JPH04201435 A JP H04201435A
- Authority
- JP
- Japan
- Prior art keywords
- polyimide resin
- vibration
- filler
- molded
- pref
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920001721 polyimide Polymers 0.000 title claims abstract description 36
- 239000009719 polyimide resin Substances 0.000 title claims abstract description 32
- 239000000945 filler Substances 0.000 claims abstract description 10
- 238000000748 compression moulding Methods 0.000 claims abstract description 5
- 238000010304 firing Methods 0.000 claims description 7
- 230000006835 compression Effects 0.000 claims description 6
- 238000007906 compression Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000000465 moulding Methods 0.000 abstract description 12
- 239000000843 powder Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 5
- 239000011347 resin Substances 0.000 abstract description 5
- 229920005989 resin Polymers 0.000 abstract description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 4
- 239000004642 Polyimide Substances 0.000 abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000010439 graphite Substances 0.000 abstract description 3
- 229910002804 graphite Inorganic materials 0.000 abstract description 3
- 239000005995 Aluminium silicate Substances 0.000 abstract description 2
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 2
- 235000012211 aluminium silicate Nutrition 0.000 abstract description 2
- 239000010425 asbestos Substances 0.000 abstract description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract description 2
- 239000004917 carbon fiber Substances 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 abstract description 2
- 239000002657 fibrous material Substances 0.000 abstract description 2
- 239000011521 glass Substances 0.000 abstract description 2
- 239000003365 glass fiber Substances 0.000 abstract description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 abstract description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 abstract description 2
- 229910052895 riebeckite Inorganic materials 0.000 abstract description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- 239000000454 talc Substances 0.000 abstract description 2
- 229910052623 talc Inorganic materials 0.000 abstract description 2
- 239000011324 bead Substances 0.000 abstract 1
- 239000010456 wollastonite Substances 0.000 abstract 1
- 229910052882 wollastonite Inorganic materials 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 4
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- -1 inorganic whiskers Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000010582 Pisum sativum Nutrition 0.000 description 1
- 240000004713 Pisum sativum Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は高強度で、かつ成形品に割れ、くびれ、歪等の
欠損が生じないポリイミド樹脂成形品の製造方法に関す
る。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for manufacturing a polyimide resin molded product that has high strength and does not suffer from defects such as cracks, constrictions, and distortions in the molded product.
ポリイミド樹脂は耐熱性に極めて優れた樹脂であるが、
その軟化点があまりにも高いために通常の溶融成形が不
可能である。Polyimide resin is a resin with extremely excellent heat resistance, but
Its softening point is so high that normal melt molding is impossible.
したがって、従来からポリイミド樹脂を成形するにはポ
リイミド樹脂の粉末、あるいはこれに無機充填剤を添加
した樹脂配合物を金型内に充填し、加圧装置、たとえば
油圧プレス、空圧プレス、メカプレスを用いて加圧する
ことにより圧粉体を成形し、その後、この圧粉体を４０
０°Ｃ程度の高温に加熱して焼成し、ポリイミド樹脂成
形品を得る圧縮焼成成形法が採用されている。Therefore, conventionally, to mold polyimide resin, a mold is filled with polyimide resin powder or a resin compound with an inorganic filler added thereto, and a pressurizing device such as a hydraulic press, pneumatic press, or mechanical press is used to mold the polyimide resin. A green compact is formed by applying pressure using a
A compression firing molding method is used in which a polyimide resin molded product is obtained by heating and firing at a high temperature of about 0°C.
ポリイミド樹脂を圧縮焼成して高強度の成形品を得るた
めには約３０００ｋｇ／ Ｃｌ１１２の圧力をかける必
要があり、圧力が高い程、強度の高い成形品が得られる
が、ある圧力以上に加圧すると圧粉体の表面、特に側面
にクランクが生じたり、焼成時にくびれを生じたり、歪
が発生し割れたりして商品価値がなくなる欠点があった
。In order to obtain a high-strength molded product by compressing and firing polyimide resin, it is necessary to apply a pressure of approximately 3000 kg/Cl112.The higher the pressure, the stronger the molded product can be obtained, but if the pressure is applied above a certain pressure. This has the disadvantage that cranks occur on the surface of the green compact, especially on the sides, that it becomes constricted during firing, or that it becomes distorted and cracked, resulting in loss of commercial value.
この成形品の欠損は圧縮の圧力を下げると発生しないが
、圧力が低いと成形品の強度が低下するという問題があ
った。This defect in the molded product does not occur if the compression pressure is lowered, but there is a problem in that the strength of the molded product decreases when the pressure is low.
欠損の原因としては圧縮の際に圧力むらが生しることが
考えられ、これを防止する方法として、粉体の流動性を
改良するグラファイト等を添加することが考えられるが
十分ではなかった。The cause of the defects is thought to be uneven pressure during compression, and one possible way to prevent this is to add graphite or the like to improve the fluidity of the powder, but this has not been sufficient.
本発明の目的はポリイミド樹脂あるいはポリイミド樹脂
と充填剤の配合物を圧縮焼成する際、高圧をかけても成
形品に割れ、くびれ、歪等の欠損が発生しない成形品を
製造する方法を提供することにある。An object of the present invention is to provide a method for producing a molded product that does not suffer from cracks, constrictions, distortions, or other defects even when high pressure is applied when polyimide resin or a blend of polyimide resin and filler is compressed and fired. There is a particular thing.
上記従来技術の問題点を解決するため、本発明は次の手
段をとるものである。In order to solve the problems of the prior art described above, the present invention takes the following measures.
即ち本発明のポリイミド樹脂成形品の製造方法は、ポリ
イミド樹脂またはポリイミド樹脂と充填剤からなるポリ
イミド樹脂配合物を金型内で圧縮成形し、その後、焼成
して成形品を製造するに際し、圧縮成形を加振装置によ
って加振下で行なうことを特徴とするものである。That is, the method for producing a polyimide resin molded article of the present invention involves compression molding a polyimide resin or a polyimide resin compound consisting of a polyimide resin and a filler in a mold, and then firing it to produce a molded article. The method is characterized in that it is carried out under vibration using a vibration device.
本発明に用いるポリイミド樹脂は主として下記のポリイ
ミド構造を有しているものが使用される。The polyimide resin used in the present invention mainly has the following polyimide structure.
二のポリイミド樹脂は、普通、ピロメリット酸無水物と
ジアミノジフェニルエーテルヲ反応させて作られるが、
酸成分またはジアミン成分の一部を他の酸又はジアミン
成分に置き替えた共重合物又は他の分子構造を有するポ
リイミド樹脂を一部混合してなる樹脂混合物も使用でき
るが、上記ポリイミド構造の樹脂が最適である。The second polyimide resin is usually made by reacting pyromellitic anhydride with diaminodiphenyl ether.
A copolymer in which a part of the acid component or diamine component is replaced with another acid or diamine component, or a resin mixture formed by partially mixing a polyimide resin with another molecular structure can also be used, but the resin with the above polyimide structure can also be used. is optimal.
一方、本発明のポリイミド樹脂には成形性、寸法安定性
、低吸水性等を付与する目的で種々の充填剤を添加する
ことができる。On the other hand, various fillers can be added to the polyimide resin of the present invention for the purpose of imparting moldability, dimensional stability, low water absorption, etc.
好ましい充填剤としてはガラス繊維、炭素繊維、アスベ
スト、無機ウィスカー等の繊維状物、タルク、シリカ、
アルミナ、カオリン、ワラステナイト、ガラスピーズ、
セラミック粉末、カーボンパウダー、グラファイト、二
硫化モリブデン、炭酸カルシウム等が挙げられ、これら
の添加量はポリイミド樹脂と充填剤の合計量に対して１
０〜６０重量％が好ましい。Preferred fillers include glass fiber, carbon fiber, asbestos, fibrous materials such as inorganic whiskers, talc, silica,
Alumina, kaolin, wollastenite, glass peas,
Examples include ceramic powder, carbon powder, graphite, molybdenum disulfide, calcium carbonate, etc., and the amount of these added is 1% to the total amount of polyimide resin and filler.
0 to 60% by weight is preferred.
また、充填剤の添加量が増すと成形品にクラックが発生
しやすくなるが、６０重量％以下であれば、圧縮時に加
振することによってクランク等の発生を防止することが
できる。Furthermore, as the amount of filler added increases, cracks are more likely to occur in the molded product, but if it is less than 60% by weight, it is possible to prevent the occurrence of cracks and the like by applying vibration during compression.
本発明において圧縮成形を加振する方法としては圧縮機
に別体の加振装置を取付けることも可能であるが、好ま
しくは振動成形機、たとえば多目的振動成形プレス （
アサヒエンジニアリング（株）製）等を用いることがで
きる。本発明において用いる振動数としては３ ＫＦｌ
ｚが好ましい。In the present invention, as a method of vibrating compression molding, it is possible to attach a separate vibration device to the compressor, but it is preferable to use a vibration molding machine, such as a multipurpose vibration molding press (
(manufactured by Asahi Engineering Co., Ltd.), etc. can be used. The frequency used in the present invention is 3 KFl
z is preferred.
本発明における成形方法はポリイミド樹脂粉末を加振し
ながら圧縮して圧粉体を成形し、次いでこれを加熱焼成
するが、圧粉体を作るための圧力は２０００〜５０００
ｋｇ／ｃｍ”が好ましく、また焼成温度は３７０〜４３
０°Ｃが好ましい。In the molding method of the present invention, polyimide resin powder is compressed while being vibrated to form a green compact, which is then heated and fired, but the pressure for making the green compact is 2000 to 5000.
kg/cm" is preferable, and the firing temperature is 370 to 43
0°C is preferred.
以下、実施例を挙げて本発明を具体的に説明する。 The present invention will be specifically described below with reference to Examples.
実施例１
内径５０ｍｍ、高さ３００ｍｍの金型の中にピロメリッ
ト酸無水物と４，４゛−ジアミノジフェニルエーテルを
反応させて製造したポリイミド樹脂（東しく株）製“Ｔ
ｌ−３０００”）の顆粒状粉末を１６０ｇ投入し、常温
下で６０ ｔｏｎの圧力をかけて直径５０ｍｍ、高さ６
０ＩＩＩｌの丸棒圧粉体を成形する。この時、圧粉体の
成形を、アサヒエンジニアリング（株）製の多目的振動
成形プレスを使用して、加振下に行なった。Example 1 "T" made of polyimide resin (Toshishiku Co., Ltd.) produced by reacting pyromellitic anhydride and 4,4'-diaminodiphenyl ether in a mold with an inner diameter of 50 mm and a height of 300 mm.
160g of granular powder (1-3000") was added, and a pressure of 60 tons was applied at room temperature to create a mold with a diameter of 50mm and a height of 6.
A round bar green compact of 0IIIl is molded. At this time, the compact was molded under vibration using a multi-purpose vibration molding press manufactured by Asahi Engineering Co., Ltd.
このプレスは高周波クロス振動作用を加えながら加圧す
る成形機であり、高周波クロス振動により、材料粒子が
流動配列し、均一充填密度の成形品が得られる。その後
、圧粉体を焼成したが圧粉体は割れることがなかった。This press is a molding machine that applies pressure while applying a high-frequency cross vibration effect, and the high-frequency cross vibration causes material particles to flow and align, resulting in a molded product with uniform packing density. Thereafter, the green compact was fired, but the green compact did not crack.
比較例１
実施例１と同じ金型、同じ材料を用いて同じように圧粉
体を成形する工程において、成形プレスとして東邦プレ
ス製プレスを使用し、加振することなく １００ｔｏｎ
の圧力で、直径５抛ｍ、高さ６０ｍｎ＋の丸棒圧粉体を
成形した。これを焼成炉に入れて焼成したところ、成形
品は中心部で割れを生した。Comparative Example 1 In the process of molding a green compact in the same way as in Example 1 using the same mold and the same material, a Toho Press press was used as the molding press, and 100 tons was produced without vibration.
A round bar green compact with a diameter of 5 mm and a height of 60 mm+ was molded at a pressure of . When this was placed in a kiln and fired, the molded product cracked in the center.
実施例２および比較例２
１００ｍＩｗ Ｘ １００ｍｍ Ｘ ３００ｍｍ金型の
中にポリイミド樹脂（東しく株）“Ｔｌ−３０００”）
の顆粒状粉末を７００ｇ投入し、１５０°Ｃに加熱後、
１００ｔｏｎの圧力をかけて、１００ｍｍ Ｘ １００
ｍｍ Ｘ ５０ｍｍの圧粉体を成形した。Example 2 and Comparative Example 2 Polyimide resin (Toshishiku Co., Ltd. “Tl-3000”) was placed in a 100mIw x 100mm x 300mm mold.
After adding 700g of granular powder and heating to 150°C,
Applying 100 tons of pressure, 100mm x 100
A green compact measuring 50 mm x 50 mm was molded.
この時プレスとして東邦プレス（株）製の１００ｔｏｎ
油圧プレスを使用した（比較例２）。At this time, a 100 ton press manufactured by Toho Press Co., Ltd.
A hydraulic press was used (Comparative Example 2).
一方、同様にしてプレスしとてアサヒエンジニアリング
（株）製の多目的振動成形プレスを使用し、７Ｑｔｏｎ
の圧力で加振下に成形した（実施例２）。On the other hand, a 7Qton was pressed in the same manner using a multipurpose vibration molding press manufactured by Asahi Engineering Co.
It was molded under vibration at a pressure of (Example 2).
これらの圧粉体を焼成炉に入れて焼成したが振動成形プ
レスを使用した実施例のものは割れることがなかったが
、無振動の油圧プレスで成形した（比較例２）ものは高
さ２５ｍｍのあたりで割れが住じた。These green compacts were placed in a kiln and fired, but the example using a vibration forming press did not crack, but the one formed using a non-vibrating hydraulic press (Comparative Example 2) had a height of 25 mm. There was a crack in the area.
本発明はポリイミドを圧縮成形する際、加振下に圧縮し
て圧粉体を得る方法であるため、粉体の圧力にむらが生
じることなく、成形品に割れやクランクが入ることを防
止する。In the present invention, when polyimide is compression molded, a compacted powder is obtained by compressing it under vibration, so there is no unevenness in the pressure of the powder, and cracks and cranks are prevented from forming in the molded product. .
代理人 弁理士 小 川 信 −Agent: Patent Attorney Nobuo Kogawa -
Claims (1)
ポリイミド樹脂配合物を金型内で圧縮成形し、その後、
焼成して成形品を製造するに際し、圧縮成形を加振装置
によって加振下で行なうことを特徴とするポリイミド樹
脂成形品の製造方法。A polyimide resin or a polyimide resin compound consisting of a polyimide resin and a filler is compression molded in a mold, and then
1. A method for producing a polyimide resin molded article, which comprises performing compression molding under vibration using a vibrator when producing the molded article by firing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33463790A JPH04201435A (en) | 1990-11-30 | 1990-11-30 | Preparation of molded item made of polyimide resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33463790A JPH04201435A (en) | 1990-11-30 | 1990-11-30 | Preparation of molded item made of polyimide resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04201435A true JPH04201435A (en) | 1992-07-22 |
Family
ID=18279604
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33463790A Pending JPH04201435A (en) | 1990-11-30 | 1990-11-30 | Preparation of molded item made of polyimide resin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04201435A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996014977A1 (en) * | 1994-11-09 | 1996-05-23 | Kanegafuchi Kagaku Kogyo Kabushiki Kaisha | Process for molding aromatic polyimide resin |
| CN111253602A (en) * | 2020-03-25 | 2020-06-09 | 太湖方舟新材料科技有限公司 | Polyimide film and preparation method thereof |
-
1990
- 1990-11-30 JP JP33463790A patent/JPH04201435A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996014977A1 (en) * | 1994-11-09 | 1996-05-23 | Kanegafuchi Kagaku Kogyo Kabushiki Kaisha | Process for molding aromatic polyimide resin |
| US5718855A (en) * | 1994-11-09 | 1998-02-17 | Kaneka Corporation | Method of molding aromatic polyimide resin |
| CN111253602A (en) * | 2020-03-25 | 2020-06-09 | 太湖方舟新材料科技有限公司 | Polyimide film and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1046306A (en) | Acid-resistant concrete products, especially sulfur concrete pipes, and methods for their manufacture | |
| CN113336471A (en) | Epoxy resin-based mineral casting and preparation method thereof | |
| JPH02267170A (en) | Fire resistant substrate and preparation thereof | |
| JPH04201435A (en) | Preparation of molded item made of polyimide resin | |
| CN106336164A (en) | Preparation method of insulating baking-free brick | |
| JP4349775B2 (en) | Molded body of thermoplastic hydraulic composition and method for producing the molded body | |
| JPH04201433A (en) | Preparation of molded item made of polyimide resin | |
| KR101567530B1 (en) | Manufacturing method for Resin Coated Sand Using the Recycled silica sand | |
| JP2000281425A (en) | Method for producing molded article of sulfur composition | |
| RU2036136C1 (en) | Method for manufacture of blanks used for production of graphite material | |
| JP4275921B2 (en) | Manufacturing method of inorganic board | |
| RU2161142C1 (en) | Method of heat-insulating structural material production based on swollen vermiculite | |
| SU1680677A1 (en) | Method for manufacturing articles of heat-resistant concrete | |
| SU1109963A1 (en) | Process for manufacturing carbonaceous paste for self-baking electrode | |
| JPH0567581B2 (en) | ||
| KR20020030840A (en) | Economic manufacture and product of High strength whangtoh Block | |
| US3253067A (en) | Process for the production of ladle bricks | |
| JPH03268862A (en) | Method for forming nozzle for continuous casting | |
| JP2768492B2 (en) | Method for producing calcium silicate molding | |
| JPH09286643A (en) | Production of inorganic board | |
| JPH03131554A (en) | Inorganic formed article and production thereof | |
| JP4217807B2 (en) | Low-cost shirasu pressure-molded body and method for producing the same | |
| JPH0442849A (en) | Production of inorganic article | |
| JPH02206506A (en) | Centrifugal manufacture of resin concrete pipe | |
| JP4198889B2 (en) | Manufacturing method of wood cement board |