JPH0365505A - Low density swollen graphite molded product and preparation thereof - Google Patents
Low density swollen graphite molded product and preparation thereofInfo
- Publication number
- JPH0365505A JPH0365505A JP1202202A JP20220289A JPH0365505A JP H0365505 A JPH0365505 A JP H0365505A JP 1202202 A JP1202202 A JP 1202202A JP 20220289 A JP20220289 A JP 20220289A JP H0365505 A JPH0365505 A JP H0365505A
- Authority
- JP
- Japan
- Prior art keywords
- resin
- expanded graphite
- molded product
- density
- molded body
- 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 52
- 239000010439 graphite Substances 0.000 title claims abstract description 52
- 229920005989 resin Polymers 0.000 claims abstract description 38
- 239000011347 resin Substances 0.000 claims abstract description 38
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 6
- 238000005087 graphitization Methods 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 abstract description 11
- 239000005011 phenolic resin Substances 0.000 abstract description 4
- 239000007849 furan resin Substances 0.000 abstract description 3
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011810 insulating material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- ZFLRDGZJSCQDSR-KLSJZZFUSA-N (ne)-n-[1-(propan-2-ylamino)-3-(2-prop-2-enylphenoxy)propan-2-ylidene]hydroxylamine;hydrochloride Chemical compound Cl.CC(C)NC\C(=N/O)COC1=CC=CC=C1CC=C ZFLRDGZJSCQDSR-KLSJZZFUSA-N 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 235000011835 quiches Nutrition 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
(産業上の利用分野)
本発明は、樹脂で補強した低密度膨張黒鉛成形体及びそ
の製造法に関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a resin-reinforced low-density expanded graphite molded body and a method for producing the same.
(従来の技術)
膨張黒鉛成形体は、特公昭54−33799号公報に示
されるように、天然黒鉛、キッシュ黒鉛。(Prior Art) The expanded graphite molded body is natural graphite or quiche graphite, as shown in Japanese Patent Publication No. 54-33799.
熱分解黒鉛など高度に結晶構造の発達した黒鉛を。Graphite with a highly developed crystal structure, such as pyrolytic graphite.
濃硫酸と硝酸、!I硫酸と過マンガン酸カリウム溶液な
どの強酸化性の混液で酸処理して熱鏡層間化合物を生成
させ2次いで該層間化合物を水洗してから急速加熱し、
黒鉛結晶のC軸方向に膨張処理した真状形で圧縮復元性
を有する膨張黒鉛粒子とし、該膨張黒鉛粒子を圧縮加工
して得られる。Concentrated sulfuric acid and nitric acid! Acid treatment with a strong oxidizing mixture such as I sulfuric acid and potassium permanganate solution to generate a thermal mirror intercalation compound, followed by washing the intercalation compound with water and rapid heating,
Expanded graphite particles are obtained by expanding graphite crystals in the C-axis direction to obtain true-shaped expanded graphite particles that have compression recovery properties, and are obtained by compression processing the expanded graphite particles.
この膨張黒鉛成形体は、低密度のものは、断熱材、均熱
材などに使用され、高密度のものはシール性に優れるの
でバッキング、ガスケットなどに使用される。Low-density expanded graphite molded bodies are used for heat insulating materials, heat-uniforming materials, etc., while high-density ones have excellent sealing properties and are used for backings, gaskets, etc.
(発明が解決しようとする課題)
膨張黒鉛粒子を冷間圧縮加工して得られる低密度膨張黒
鉛成形体は9強度が極めて弱いために大型のものや複雑
な形状のものは製作が困難であるほか装置への組付は時
に取扱いにくい等の問題がある。また、*m昭63−2
40524号に示される低密度黒鉛成形体では9機械的
強度が改善されるが、加工が難かしい等の問題がある。(Problems to be Solved by the Invention) Low-density expanded graphite molded bodies obtained by cold compression processing of expanded graphite particles have extremely low strength, so it is difficult to manufacture large-sized ones or ones with complicated shapes. In addition, there are other problems such as difficulty in assembling it into equipment. Also, *m Showa 63-2
Although the low-density graphite molded body shown in No. 40524 has improved mechanical strength, it has problems such as difficulty in processing.
本発明は上記した問題を解消する低密度膨張黒鉛成形体
を提供することを目的とする。An object of the present invention is to provide a low-density expanded graphite molded body that solves the above-mentioned problems.
(!!題を解決するための手段)
本発明は、樹脂、樹脂の炭化物又は樹脂の黒鉛化物を含
有してなる低密度膨張黒鉛成形体及びその製造法に関す
る。(!!Means for solving the problem) The present invention relates to a low-density expanded graphite molded body containing a resin, a carbide of a resin, or a graphitized product of a resin, and a method for producing the same.
本発明において、低密度膨張黒鉛成形体用の膨張黒鉛粒
子は公知の製造法で得られたものでよいが、かさ密度は
0.001〜0.01 g/an”が好ましい。かさ密
度が小さすぎると、膨張黒鉛のかさが荒く、取扱す性が
低下する。かさ密度が大きすぎると2機械的強度が弱く
、取扱いが困難となる。In the present invention, the expanded graphite particles for the low-density expanded graphite molded body may be obtained by a known manufacturing method, but the bulk density is preferably 0.001 to 0.01 g/an''.The bulk density is small. If the bulk density is too high, the bulk of the expanded graphite will be rough, resulting in poor handling.If the bulk density is too high, the mechanical strength will be weak, making handling difficult.
膨張黒鉛粒子はプレス又はロール掛けにより低密度の成
形体とされる。成形体の密度は0.05〜0、3 g
/cm”が好ましい。密度が低すぎると機械的強度が弱
く、取扱いが困難となる。密度が高すぎると熱伝導率が
大きくなり、断熱材として好1しくなくなる。The expanded graphite particles are formed into a low-density compact by pressing or rolling. The density of the molded body is 0.05-0.3 g
/cm" is preferable. If the density is too low, the mechanical strength will be weak and handling will be difficult. If the density is too high, the thermal conductivity will be high, making it undesirable as a heat insulating material.
樹脂を複合するには、樹脂粉末と膨張黒鉛粒子との混合
物を成形してもよいが、前記の膨張黒鉛成形体に樹脂溶
液を塗布又は含浸するのが作業が簡単でかつ均一なもの
ができるので好ましい。含浸に使う樹脂は熱硬化性樹脂
又は熱可塑性樹脂のいずれでもよいが、熱可塑性樹脂は
その溶液を膨張黒鉛成形体に塗布又は含浸後乾燥して溶
剤を除去するだけであるのに対し、熱硬化性樹脂は更に
熱処理によシ樹脂を硬化させるので、得られる低密度膨
張黒鉛成形体の耐熱性がよく1機械的強度も大きいので
熱硬化性樹脂の方が好捷しい。熱硬化性樹脂としては、
フェノール樹脂、フラン樹脂。To composite the resin, a mixture of resin powder and expanded graphite particles may be molded, but it is easier to work and a uniform product can be obtained by coating or impregnating the expanded graphite molded body with a resin solution. Therefore, it is preferable. The resin used for impregnation may be either a thermosetting resin or a thermoplastic resin, but with thermoplastic resins, the solution is simply applied to the expanded graphite molded body or dried after impregnation to remove the solvent. Since the curable resin is further cured by heat treatment, the resulting low-density expanded graphite molded product has good heat resistance and high mechanical strength, so thermosetting resins are preferable. As a thermosetting resin,
Phenolic resin, furan resin.
エポキシ樹脂、尿素樹脂、メラミン樹脂、不飽和ポリエ
ステル樹脂等が用いられる。熱可塑性樹脂としては、ポ
リ酢酸ビニル樹脂、ポリビニルアルコール樹脂、ポリ塩
化ビニル樹脂、アクリル樹脂等が用いられる。Epoxy resins, urea resins, melamine resins, unsaturated polyester resins, etc. are used. As the thermoplastic resin, polyvinyl acetate resin, polyvinyl alcohol resin, polyvinyl chloride resin, acrylic resin, etc. are used.
低密度膨張黒鉛成形体の使用温度が500℃付近の場合
は、膨張黒鉛成形体に炭化収率の高いフラン樹脂、フェ
ノール樹脂等の溶液を塗布又は含浸し、加熱して樹脂を
硬化させ1次いで焼成して樹脂を炭化させたものを用い
る。更に高い温度で使用する場合は、上記炭化物含有成
形体を黒鉛化処理した低密度膨張黒鉛成形体を用いる。When the operating temperature of the low-density expanded graphite molded body is around 500°C, the expanded graphite molded body is coated with or impregnated with a solution of furan resin, phenol resin, etc. that has a high carbonization yield, and heated to harden the resin. The resin is carbonized by firing. When used at a higher temperature, a low-density expanded graphite molded body obtained by graphitizing the carbide-containing molded body is used.
膨張黒鉛成形体に塗布又は含浸する場合の樹脂の含浸f
iE#″i重量で5〜15%が好ましい。含浸量が少な
いと機械的強度改善の効果がなく、多すぎると樹脂を硬
化、炭化又は黒鉛化させた場合の成形体の変形が大きく
なったり、また成形体に亀裂が入るなどの不具合が起り
易い。Impregnation f of resin when coating or impregnating expanded graphite molded body
iE#'' i is preferably 5 to 15% by weight. If the amount of impregnation is too small, there will be no effect of improving mechanical strength, and if it is too large, the molded product will be greatly deformed when the resin is hardened, carbonized, or graphitized. In addition, problems such as cracks in the molded body are likely to occur.
樹脂溶液の塗布又は含浸及び含浸後の溶剤の除去は公知
の方法による。樹脂の加熱硬化は公知の方法でよく、硬
化温度は樹脂の種類にもよるが。Application or impregnation of the resin solution and removal of the solvent after impregnation are performed by known methods. The resin may be cured by heating using a known method, and the curing temperature depends on the type of resin.
通常100〜250℃である。焼成による樹脂の炭化処
理、黒鉛化処理も公知の方法により、焼成温度は通常8
00〜1000℃、黒鉛化温度は2500〜3000℃
とされる。It is usually 100-250°C. Carbonization and graphitization of the resin by firing are also carried out using known methods, and the firing temperature is usually 8.
00~1000℃, graphitization temperature 2500~3000℃
It is said that
(実施例) 次に本発明の詳細な説明する。(Example) Next, the present invention will be explained in detail.
実施例1
かさ密度0.02 ta /cm3の膨張黒鉛粒子(日
立化成工業■製、HGP−5)を金型に入れて加圧成形
し、厚さ20−2かさ密度0.19/■1の膨張黒鉛成
形体を得た。一方、昭和高分子■製のフェノール樹脂B
R240の100重量部及びFRH−30の20重量部
をメタノール5001i量部に溶解して樹脂溶液を準備
した。この樹脂溶液を前記成形体に塗布し風乾後、10
0℃次いで160℃で各1時間加熱し、溶剤を除去する
と共に樹脂を硬化させ、低密度膨張黒鉛成形体を得た。Example 1 Expanded graphite particles (manufactured by Hitachi Chemical Co., Ltd., HGP-5) with a bulk density of 0.02 ta/cm3 were placed in a mold and pressure-molded to a thickness of 20-2 and a bulk density of 0.19/cm3. An expanded graphite molded body was obtained. On the other hand, phenolic resin B manufactured by Showa Kobunshi ■
A resin solution was prepared by dissolving 100 parts by weight of R240 and 20 parts by weight of FRH-30 in 5001 parts by weight of methanol. This resin solution was applied to the molded body, and after air drying,
The mixture was heated at 0° C. and then at 160° C. for 1 hour each to remove the solvent and harden the resin, thereby obtaining a low-density expanded graphite molded body.
なお。In addition.
樹脂の含有量は固形分で5i量多であり、かさ密度及び
厚さは当初の成形体と変らない。The solid content of the resin was 5i high, and the bulk density and thickness were the same as the original molded product.
実施例2 実施例1で得られた低密度膨張黒鉛成形体を。Example 2 The low density expanded graphite molded body obtained in Example 1.
250℃で24時間加熱処理後、窒素雰囲気中で900
℃筐で毎時3℃の速度で昇温し、900℃で1時間保持
焼成し9次いで徐冷して樹脂を炭化させた低密度膨張黒
鉛成形体を得た。After heat treatment at 250℃ for 24 hours, 900℃ in nitrogen atmosphere
The temperature was raised at a rate of 3° C. per hour in a 900° C. cabinet, and the mixture was held and fired at 900° C. for 1 hour, followed by slow cooling to carbonize the resin to obtain a low-density expanded graphite molded body.
実施例3
実施例2で得られた低密度黒鉛成形体を電気抵抗炉に入
れ窒素雰囲気でa、ooo℃壕で毎時3℃の速度で昇温
し、a、ooo℃で24時間保持後徐冷し、樹脂を黒鉛
化した低密度膨張黒鉛成形体を得た。Example 3 The low-density graphite molded body obtained in Example 2 was placed in an electric resistance furnace and heated at a rate of 3°C per hour in a nitrogen atmosphere at a,ooo°C, and after being held at a,ooo°C for 24 hours, it was gradually heated. The resin was cooled and the resin was graphitized to obtain a low-density expanded graphite molded body.
比較例1
実施例1で用いたかさ密度0.02 g/cm3の膨張
黒鉛粒子を金型に入れて加圧成形し、厚さ20mm。Comparative Example 1 Expanded graphite particles with a bulk density of 0.02 g/cm3 used in Example 1 were placed in a mold and pressure-molded to a thickness of 20 mm.
かさ密度0.1 g 70m3の膨張黒鉛成形体を得た
。An expanded graphite molded body having a bulk density of 0.1 g and 70 m3 was obtained.
比較例2
実施例1で用いたかさ密度0.02 g 70m3の膨
張黒鉛粒子を金型に入れて加圧成形し、厚さ5鴫。Comparative Example 2 Expanded graphite particles with a bulk density of 0.02 g and 70 m3 used in Example 1 were placed in a mold and pressure-molded to a thickness of 5 mm.
かさ密度1.5 g/am’の膨張黒鉛成形体を得た。An expanded graphite molded body having a bulk density of 1.5 g/am' was obtained.
実施例及び比較例で得られた膨張黒鉛成形体について基
礎物性を測定したところ第1表の結果が得られた。When the basic physical properties of the expanded graphite molded bodies obtained in the Examples and Comparative Examples were measured, the results shown in Table 1 were obtained.
第1表
第1表の結果から明らかな様に、実施例の低密度膨張黒
鉛成形体は、比較例1の成形体に比べ樹脂を含浸するこ
とで曲げ強度の改善が認められた。As is clear from the results in Table 1, the bending strength of the low-density expanded graphite molded bodies of Examples was improved compared to the molded bodies of Comparative Example 1 by impregnation with resin.
また、比較例2の成形体は、密度が高い為に曲げ強度は
優れるが、熱伝導率も高くなり断熱材としては適さない
。!た取扱い性は実施例のものが破損せず良好であるこ
とが確認された。Further, the molded product of Comparative Example 2 has a high density and therefore has excellent bending strength, but its thermal conductivity is also high and it is not suitable as a heat insulating material. ! It was confirmed that the handling properties of the examples were good with no breakage.
(発明の効果)
本発明によれば1機械的強度が向上し、取扱い性がよく
、断熱性の優れた低密度膨張黒鉛成形体が得られ、製造
法も容易である。また、焼成処理したもの又は黒鉛化処
理したものは高温炉の断熱材として好適である。(Effects of the Invention) According to the present invention, a low-density expanded graphite molded body with improved mechanical strength, good handling properties, and excellent heat insulation properties can be obtained, and the manufacturing method is easy. Furthermore, those subjected to firing treatment or graphitization treatment are suitable as heat insulating materials for high-temperature furnaces.
Claims (1)
なる低密度膨張黒鉛成形体。 2、膨張黒鉛成形体に熱硬化性樹脂の溶液を塗布又は含
浸した後、樹脂の硬化温度で加熱することを特徴とする
低密度膨張黒鉛成形体の製造法。 3、請求項2における加熱後の膨張黒鉛成形体を焼成し
、更には必要に応じて黒鉛化処理することを特徴とする
低密度膨張黒鉛成形体の製造法。[Claims] 1. A low-density expanded graphite molded body containing a resin, a carbide of the resin, or a graphitized product of the resin. 2. A method for producing a low-density expanded graphite molded body, which comprises coating or impregnating the expanded graphite molded body with a solution of a thermosetting resin and then heating it at the curing temperature of the resin. 3. A method for producing a low-density expanded graphite molded body according to claim 2, which comprises firing the heated expanded graphite molded body and further subjecting it to graphitization treatment as required.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1202202A JPH0365505A (en) | 1989-08-03 | 1989-08-03 | Low density swollen graphite molded product and preparation thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1202202A JPH0365505A (en) | 1989-08-03 | 1989-08-03 | Low density swollen graphite molded product and preparation thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH0365505A true JPH0365505A (en) | 1991-03-20 |
Family
ID=16453657
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP1202202A Pending JPH0365505A (en) | 1989-08-03 | 1989-08-03 | Low density swollen graphite molded product and preparation thereof |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH0365505A (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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US5247005A (en) * | 1991-05-25 | 1993-09-21 | Bayer Aktiengesellschaft | Process for the production of mouldings |
JP2002106081A (en) * | 2000-09-28 | 2002-04-10 | Achilles Corp | Heat insulative structure of roof |
JP2007191180A (en) * | 2006-01-18 | 2007-08-02 | Tokan Kogyo Co Ltd | Composite container |
JP2013047607A (en) * | 2012-11-30 | 2013-03-07 | Sgl Carbon Se | Heat conductive plate formed of expanded graphite and production method therefor |
CN107008213A (en) * | 2017-04-20 | 2017-08-04 | 南通理工学院 | The heat curing process and its equipment of furane resins impregnated graphite materials |
US10538691B2 (en) | 2004-08-27 | 2020-01-21 | Toyo Tanso Co., Ltd. | Expanded-graphite sheet |
-
1989
- 1989-08-03 JP JP1202202A patent/JPH0365505A/en active Pending
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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JP4676053B2 (en) * | 2000-09-28 | 2011-04-27 | アキレス株式会社 | Insulation structure of roof |
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JP2013047607A (en) * | 2012-11-30 | 2013-03-07 | Sgl Carbon Se | Heat conductive plate formed of expanded graphite and production method therefor |
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