JPH01111708A - Production of activated carbon molded body - Google Patents
Production of activated carbon molded bodyInfo
- Publication number
- JPH01111708A JPH01111708A JP62269992A JP26999287A JPH01111708A JP H01111708 A JPH01111708 A JP H01111708A JP 62269992 A JP62269992 A JP 62269992A JP 26999287 A JP26999287 A JP 26999287A JP H01111708 A JPH01111708 A JP H01111708A
- Authority
- JP
- Japan
- Prior art keywords
- activated carbon
- heat treatment
- polyvinylidene chloride
- chloride resin
- 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 55
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 229920001328 Polyvinylidene chloride Polymers 0.000 claims abstract description 18
- 239000005033 polyvinylidene chloride Substances 0.000 claims abstract description 18
- 239000012298 atmosphere Substances 0.000 claims abstract description 17
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000007033 dehydrochlorination reaction Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- 230000035699 permeability Effects 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- LGXVIGDEPROXKC-UHFFFAOYSA-N 1,1-dichloroethene Chemical group ClC(Cl)=C LGXVIGDEPROXKC-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 that is Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/384—Granulation
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） 活性炭機能や気体透過能などが要求される。[Detailed description of the invention] (Industrial application field) Activated carbon function and gas permeability are required.
例えば、フィルター、触媒担体、空気電池の電極などに
使用される活性炭成形物の製造方法に関する。詳しくは
、ポリ塩化ビニリデン系樹脂と活性炭とを少なくとも主
材とする混線物に。For example, the present invention relates to a method for manufacturing activated carbon molded products used for filters, catalyst carriers, electrodes of air batteries, etc. Specifically, it is a mixed material whose main ingredients are at least polyvinylidene chloride resin and activated carbon.
前記ポリ塩化ビニリデン系樹脂の脱塩酸反応が完全に終
了するよう５００ ”Ｃ以上の熱処理を施すものにして
活性炭成形物を製造する方法に関する。The present invention relates to a method for producing an activated carbon molded article by subjecting the polyvinylidene chloride resin to heat treatment at a temperature of 500''C or higher to completely complete the dehydrochlorination reaction.
（従来の技術）
ポリ塩化ビニリデンが脱塩酸反応後、活性炭化すること
は知られている。−例として、特開昭５２’−７５６９
１号公報には、「ポリ塩化ビニリデン及び塩化ビニリデ
ンを６５％以上含む塩化ビニリデン共重合体を脱塩酸し
て活性炭を製造するにあたり、酸化性物質を共存させる
か、あるいは導入しながら脱塩酸を行なうことを特徴と
する高性能活性炭の製造方法」について開示がある。(Prior Art) It is known that polyvinylidene chloride is activated carbonized after dehydrochlorination reaction. -For example, JP-A-52'-7569
Publication No. 1 states, ``When producing activated carbon by dehydrochlorinating polyvinylidene chloride and a vinylidene chloride copolymer containing 65% or more of vinylidene chloride, dehydrochlorination is carried out while coexisting or introducing an oxidizing substance. A method for producing high-performance activated carbon characterized by the following is disclosed.
（発明が解決しようとする問題点）
ポリ塩化ビニリデン系樹脂を単独で活性炭化させる場合
には、前述公報開示のように酸化性雰囲気で熱処理を施
すのが高性能の活性炭を得る方法であるとしても、ポリ
塩化ビニリデンを他のもの、特に活性炭とともに併用し
て混線物とし、その全体物の活性炭性能を良好ならしめ
る場合には、必ずしも、酸化性雰囲気が最善であるとは
言えない。(Problems to be Solved by the Invention) When polyvinylidene chloride resin is activated carbonized alone, heat treatment in an oxidizing atmosphere as disclosed in the above-mentioned publication is a method for obtaining high-performance activated carbon. However, when polyvinylidene chloride is used in combination with other substances, especially activated carbon, to form a crosstalk material and the activated carbon performance of the whole is improved, an oxidizing atmosphere is not necessarily the best.
（問題点を解決するための手段）
本発明は、ポリ塩化ビニリデン系樹脂と活性炭とを少な
くとも主材とする混練物に、前記ポリ塩化ビニリデン系
樹脂の脱塩酸反応が完全に終了するよう５００℃以上の
熱処理を施して活性炭成形物を製造する方法であって、
前記熱処理として、まず、真空雰囲気において処理を施
した後、窒素雰囲気で処理を施すことを特徴とする活性
炭成形物の製造方法を要旨とする。(Means for Solving the Problems) The present invention provides a kneaded material containing at least a polyvinylidene chloride resin and activated carbon at a temperature of 500° C. so that the dehydrochloric acid reaction of the polyvinylidene chloride resin is completely completed. A method for producing an activated carbon molded article by performing the above heat treatment,
The gist of the present invention is a method for manufacturing an activated carbon molded article, which is characterized in that the heat treatment is first performed in a vacuum atmosphere and then treated in a nitrogen atmosphere.
以下、詳述する。The details will be explained below.
ポリ塩化ビニリデン系樹脂、即ち、ポリ塩化ビニリデン
そのもの、あるいは塩化ビニリデン部分を成分の一つと
する共重合物は、本発明においては活性炭成形物の骨格
形成材、従って、バインダーとして使用される。１種も
しくは適宜２種以上併用されてよく、また、ポリ塩化ビ
ニル等、他のものを成形性の向上等の目的でバインダー
として併用することもできる。A polyvinylidene chloride resin, that is, polyvinylidene chloride itself or a copolymer containing a vinylidene chloride moiety as one of its components, is used in the present invention as a skeleton forming material for an activated carbon molded product, and therefore as a binder. They may be used alone or in combination of two or more, and other materials such as polyvinyl chloride may also be used as a binder for the purpose of improving moldability.
また、活性炭は、原材料や製法等によらず適宜使用でき
、粒径も特に限定されないが、望ましくは１５０μｍ以
下のものを使用する。混練物を得る際、十分に粉砕され
ればよいが、あまりに粒径が大きいまま混練物中に存在
すると、活性炭成形物としての強度低下を招く一因にな
るからである。Furthermore, activated carbon can be used as appropriate regardless of the raw material, manufacturing method, etc., and the particle size is not particularly limited, but preferably 150 μm or less is used. When obtaining a kneaded product, it is sufficient if the particles are sufficiently pulverized, but if the particles are present in the kneaded product with too large a particle size, this will be a contributing factor to a decrease in the strength of the activated carbon molded product.
これら両者、及び、可塑剤、安定剤、溶剤といった成形
助剤、それに黒鉛など活性炭成形物の使用目的に応じて
使用されるものを、必要に応じて適宜選択して使用し、
ニーダ−１３本ロール等で混練し、板状、円筒状、ハニ
カム状など所望形状としたものに熱処理を施す。熱処理
の最高温度は前述したようにポリ塩化ビニリデン系樹脂
の脱塩酸反応が完全に進行するように５００℃以上、望
ましくは、６００〜１０００℃とする。そして、このと
き、まず真空雰囲気で熱処理を施した後、窒素雰囲気で
熱処理を施す。真空雰囲気における真空度は高い方が望
ましく、例えば、１ ／ ｌ Ｏ”Ｔｏｒｒ以下とする
のがよい。同様に、窒素雰囲気における窒素濃度も高い
方がよい。また、窒素雰囲気における熱処理はできれば
真空雰囲気における熱処理と同等もしくは高温まで施す
。更にまた、真空雰囲気における熱処理の前に、例えば
３００〜３５０℃まで程度といった比較的低温領域の熱
処理として、空気雰囲気等の酸化性雰囲気で処理するこ
ともでき、これによって、得られる活性炭成形物の品質
が往々にしてより高くなる。尚、これら熱処理は、それ
ぞれ独立に低温領域から施してもよいし、また、例えば
、真空雰囲気における熱処理を施している過程で窒素ガ
スを導入して窒素雰囲気での熱処理にするといったよう
に、継続的に施したりすることもできる。Both of these, as well as molding aids such as plasticizers, stabilizers, and solvents, as well as those used depending on the purpose of use of the activated carbon molded product, such as graphite, are appropriately selected and used as necessary.
The mixture is kneaded using a kneader with 13 rolls, etc., and then heat-treated into a desired shape such as a plate, cylinder, or honeycomb. As mentioned above, the maximum temperature of the heat treatment is set to 500° C. or higher, preferably 600 to 1000° C., so that the dehydrochloric acid reaction of the polyvinylidene chloride resin proceeds completely. At this time, heat treatment is first performed in a vacuum atmosphere, and then heat treatment is performed in a nitrogen atmosphere. It is desirable that the degree of vacuum in the vacuum atmosphere is high, for example, 1/l O" Torr or less. Similarly, the nitrogen concentration in the nitrogen atmosphere is also preferably high. Also, heat treatment in the nitrogen atmosphere should preferably be performed in a vacuum atmosphere. Furthermore, before the heat treatment in a vacuum atmosphere, it is possible to perform heat treatment in an oxidizing atmosphere such as an air atmosphere as a heat treatment in a relatively low temperature range of about 300 to 350 ° C. As a result, the quality of the obtained activated carbon molded product is often higher.These heat treatments may be performed independently from a low temperature region, or, for example, during the heat treatment in a vacuum atmosphere. Heat treatment can also be performed continuously, such as by introducing nitrogen gas and performing heat treatment in a nitrogen atmosphere.
（実施例） 以下、単に部とあるのは重量部を示す。(Example) Hereinafter, parts simply refer to parts by weight.
〈実施例１〉
ポリ塩化ビニリデン ５０部活性炭（ダ
イアソープＦ１００Ｄ；
三菱化成■製；１００メツシユ以下） ６０部
フタル酸ジオクチル ２５部ステアリン
酸塩（安定剤） ２部メチルエチルケトン
（溶剤） ３０部上記上記物をニーダ−で１５分
間混棟後、押出成形して直径約５ｍの棒状成形物を得た
。これに、真空雰囲気（１／ １０’Ｔｏｒｒ ）で最
高温度８５０℃に１時間保持する熱処理を施し、いった
ん冷却した後、窒素雰囲気（窒素濃度９５％以上）で最
高温度８５０℃に１時間保持する熱処理を施した。<Example 1> Polyvinylidene chloride 50 parts Activated carbon (Diasoap F100D; manufactured by Mitsubishi Kasei ■; 100 mesh or less) 60 parts Dioctyl phthalate 25 parts Stearate (stabilizer) 2 parts Methyl ethyl ketone (solvent) 30 parts Above mentioned above The mixture was mixed in a kneader for 15 minutes and then extruded to obtain a rod-shaped molded product with a diameter of about 5 m. This is heat-treated by holding it at a maximum temperature of 850°C for 1 hour in a vacuum atmosphere (1/10' Torr), and once cooled, it is held at a maximum temperature of 850°C for 1 hour in a nitrogen atmosphere (nitrogen concentration of 95% or more). Heat treatment was performed.
〈実施例２〉
実施例１において、ポリ塩化ビニリデンの使用量を５０
部から４０部に変え、また、ポリ塩化ビニル１０部を併
用した以外は、すべて実施例１と同様にした。<Example 2> In Example 1, the amount of polyvinylidene chloride used was reduced to 50
The procedure was the same as in Example 1 except that the amount was changed from 1 part to 40 parts, and 10 parts of polyvinyl chloride was also used.
〈実施例３〉
実施例１において、真空雰囲気における熱処理を施す前
に、空気雰囲気で室温から３００’Ｃまで毎分２℃程度
で昇温させる熱処理を施す工程を付加した以外は、すべ
て実施例１と同様にした。<Example 3> All the same as in Example 1 except that a step of performing heat treatment in which the temperature was raised from room temperature to 300'C at a rate of about 2 °C per minute in an air atmosphere was added before performing heat treatment in a vacuum atmosphere. Same as 1.
〈比較例１〉
実施例１において、窒素雰囲気における熱処理を施さな
かった以外は、すべて実施例１と同様にした。<Comparative Example 1> Everything was the same as in Example 1 except that the heat treatment in a nitrogen atmosphere was not performed.
く比較例２〉
実施例１において、真空雰囲気における熱処理を施さな
かった以外は、すべて実施例１と同様にした。Comparative Example 2> All the same procedures as in Example 1 were carried out except that the heat treatment in a vacuum atmosphere was not performed.
〈比較例３〉
実施例１において、真空雰囲気における熱処理と窒素雰
囲気における熱処理の、処理を施す順番を逆にした以外
は、すべて実施例１と同様にした。<Comparative Example 3> Everything was the same as in Example 1 except that the order of heat treatment in a vacuum atmosphere and heat treatment in a nitrogen atmosphere was reversed.
（発明の効果）
上記各側で得たものについて、比表面積と吸着能を測定
した結果を表−１に示す。尚、比表面積はＢＥＴ法によ
り、また、吸着能はメチレンブルー脱色能をＪＩＳＫ
１４７０に準じて測定した。(Effects of the Invention) Table 1 shows the results of measuring the specific surface area and adsorption capacity of the samples obtained on each side. In addition, the specific surface area is determined by the BET method, and the adsorption capacity is determined by the methylene blue decolorizing ability by JISK.
Measured according to 1470.
表−１
表−１より判るように、本発明によれば、活性炭機能に
優れた活性炭成形物を得ることができる。Table 1 As can be seen from Table 1, according to the present invention, it is possible to obtain an activated carbon molded article with excellent activated carbon functionality.
特許出願人 ぺんてる株式会社Patent applicant: Pentel Co., Ltd.
Claims (1)
材とする混練物に、前記ポリ塩化ビニリデン系樹脂の脱
塩酸反応が完全に終了するよう５００℃以上の熱処理を
施して活性炭成形物を製造する方法であって、前記熱処
理として、まず、真空雰囲気において処理を施した後、
窒素雰囲気で処理を施すことを特徴とする活性炭成形物
の製造方法。A method of producing an activated carbon molded product by heat-treating a kneaded material containing at least a polyvinylidene chloride resin and activated carbon as main materials at 500°C or higher so that the dehydrochloric acid reaction of the polyvinylidene chloride resin is completely completed. As the heat treatment, first, after performing treatment in a vacuum atmosphere,
A method for producing an activated carbon molded article, characterized by performing treatment in a nitrogen atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62269992A JPH01111708A (en) | 1987-10-26 | 1987-10-26 | Production of activated carbon molded body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62269992A JPH01111708A (en) | 1987-10-26 | 1987-10-26 | Production of activated carbon molded body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01111708A true JPH01111708A (en) | 1989-04-28 |
Family
ID=17480055
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62269992A Pending JPH01111708A (en) | 1987-10-26 | 1987-10-26 | Production of activated carbon molded body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01111708A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07249551A (en) * | 1994-03-11 | 1995-09-26 | Isuzu Motors Ltd | Method of manufacturing electrode for electric double layer capacitor |
| JPH08236406A (en) * | 1994-12-29 | 1996-09-13 | Isuzu Motors Ltd | Electrode for electric double layer capacitor and manufacture thereof |
| EP0727233A3 (en) * | 1995-02-02 | 1997-05-28 | Rainer H Frey | Biocompatible material and method of manufacture and use thereof |
| EP0724905A3 (en) * | 1995-02-02 | 1997-05-28 | Rainer H Frey | Biocompatible porous hollow fiber and method of manufacture and use thereof |
| JPH09213589A (en) * | 1996-02-02 | 1997-08-15 | Takeda Chem Ind Ltd | Activated carbon for electric double-layer capacitor and manufacture thereof |
-
1987
- 1987-10-26 JP JP62269992A patent/JPH01111708A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07249551A (en) * | 1994-03-11 | 1995-09-26 | Isuzu Motors Ltd | Method of manufacturing electrode for electric double layer capacitor |
| JPH08236406A (en) * | 1994-12-29 | 1996-09-13 | Isuzu Motors Ltd | Electrode for electric double layer capacitor and manufacture thereof |
| EP0727233A3 (en) * | 1995-02-02 | 1997-05-28 | Rainer H Frey | Biocompatible material and method of manufacture and use thereof |
| EP0724905A3 (en) * | 1995-02-02 | 1997-05-28 | Rainer H Frey | Biocompatible porous hollow fiber and method of manufacture and use thereof |
| US5863654A (en) * | 1995-02-02 | 1999-01-26 | Rainer H. Frey | Biocompatible porous hollow fiber and method of manufacture and use thereof |
| US5998024A (en) * | 1995-02-02 | 1999-12-07 | Rainer H. Frey | Biocompatible material and method of manufacture and use thereof |
| JPH09213589A (en) * | 1996-02-02 | 1997-08-15 | Takeda Chem Ind Ltd | Activated carbon for electric double-layer capacitor and manufacture thereof |
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