JP2001261883A - Method of reclaiming vulcanized rubber - Google Patents
Method of reclaiming vulcanized rubberInfo
- Publication number
- JP2001261883A JP2001261883A JP2000082757A JP2000082757A JP2001261883A JP 2001261883 A JP2001261883 A JP 2001261883A JP 2000082757 A JP2000082757 A JP 2000082757A JP 2000082757 A JP2000082757 A JP 2000082757A JP 2001261883 A JP2001261883 A JP 2001261883A
- Authority
- JP
- Japan
- Prior art keywords
- rubber
- ozone
- vulcanized
- vulcanized rubber
- plasticized
- 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
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、使用済み又は工場
排出加硫ゴムを再生処理により、ゴム原材料として再利
用する、加硫ゴムの再生方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for regenerating vulcanized rubber, in which used or factory-discharged vulcanized rubber is reused as a rubber raw material by a regenerating process.
【０００２】[0002]
【従来の技術】従来から、廃タイヤ等の使用済みゴム製
品やゴム製品の製造工場から排出される端材、バリ、不
良品等を脱硫・解重合して可塑化し、再生ゴムとして再
利用することが行われている。再利用には、再生ゴムを
100％用いて再加硫し製品とする場合と、原料生ゴムの
代替材料として、生ゴムに所定量混合して加硫し、製品
とする場合がある。2. Description of the Related Art Conventionally, used rubber products such as waste tires and scraps, burrs, and defective products discharged from a rubber product manufacturing plant are desulfurized, depolymerized, plasticized, and reused as recycled rubber. That is being done. For reuse, use recycled rubber
There are cases where the product is re-vulcanized using 100% to obtain a product, and as an alternative material to raw rubber, a predetermined amount is mixed with the raw rubber and vulcanized to obtain a product.
【０００３】再生処理方法としては、(1)粉砕されたゴ
ム粉末に軟化剤、脂肪族又は芳香族ジスルフィドなどし
ゃく解剤と呼ばれる化合物などを混合し、オートクレー
ブ中で、例えば水蒸気圧1.4ＭPa程度(200℃程度)で４〜
５時間処理するオイルパン法、(2)分解剤にアルカリ水
溶液を用い、オートクレーブ中で加熱処理するアルカリ
蒸解法、(3)リクリメーターと呼ばれる特殊な押出機と
薬剤を用いるリクリメーター法、(4)加硫ゴムに熱とせ
ん断力を加えるせん断流動場反応法(特開平09-227724
号)などがある。[0003] As a regeneration treatment method, (1) a softening agent, a compound called a peptizer such as aliphatic or aromatic disulfide, or the like is mixed with the ground rubber powder, and the mixture is subjected to, for example, a steam pressure of about 1.4 MPa in an autoclave. About 200 ℃)
5 hours oil pan method, (2) alkali digestion method using an aqueous alkali solution as a decomposing agent and heat treatment in an autoclave, (3) liquometer method using a special extruder and chemicals called riclimeter, (4 ) A shear flow field reaction method in which heat and shear force are applied to vulcanized rubber (JP-A-09-227724)
No.).
【０００４】[0004]
【発明が解決しようとする課題】従来のいずれの方法も
高温下で加熱する方法であり、多大なエネルギーを要す
る上に、高温下での処理のために、硫黄及び添加する薬
剤が主な原因と思われる悪臭を発生する化合物の生成が
避けられず、２次的な環境汚染の原因となる。また再生
された材料にも悪臭が残留するため、用途が限定され
る。更に安全性に欠ける薬剤を用いる問題点もある。そ
こで、エネルギーをあまり必要とせず、しゃく解剤等の
安全性に問題のある薬剤を用いず、室温近辺で常圧下で
実施でき、悪臭を発生しない環境負荷の少ない方法を開
発する必要がある。All of the conventional methods are methods of heating at a high temperature, requiring a large amount of energy, and are mainly caused by sulfur and added chemicals for the treatment at a high temperature. The generation of a compound that generates a foul odor, which is considered to be inevitable, is inevitable and causes secondary environmental pollution. Further, since the odor remains in the regenerated material, its use is limited. There is also a problem of using drugs that lack safety. Therefore, it is necessary to develop a method that does not require much energy, does not use a chemical having a problem in safety such as a peptizing agent, can be carried out at about room temperature under normal pressure, and has a low environmental load that does not generate odor.
【０００５】[0005]
【課題を解決するための手段】本発明に係る加硫ゴムの
再生方法は、加硫ゴム粉砕物品を撹拌しながら、温度５
〜40℃、好ましくは10〜30℃、常圧下でオゾンを吹き込
み、オゾンの酸化作用を利用してゴム成分を解重合する
ことを特徴とする。短時間処理で材料として再利用する
ことが可能で、エネルギーを多く必要とせず、悪臭の発
生が少なく、薬剤も用いない簡易な処理方法である。According to the present invention, there is provided a method for regenerating a vulcanized rubber according to the present invention.
Ozone is blown under normal pressure at a temperature of -40 ° C, preferably 10-30 ° C, and the rubber component is depolymerized by utilizing the oxidizing action of ozone. This is a simple processing method that can be reused as a material in a short time, does not require much energy, generates little odor, and does not use chemicals.
【０００６】すなわち、オゾンが漏れないように密閉し
た撹拌機付き容器内に、粉砕したゴムを入れ、オゾン発
生装置からオゾンを容器内に導入し、温度５〜40℃、好
ましくは10〜30℃、常圧下でゴムとオゾンを反応させ
る。対象とするゴムの種類によって反応条件(反応時
間、オゾン濃度、圧力、温度)が選択される。容器内を
通過した未反応オゾンは活性炭充填塔で分解する。That is, pulverized rubber is placed in a container equipped with a stirrer that is sealed so as not to leak ozone, and ozone is introduced into the container from an ozone generator, and the temperature is 5 to 40 ° C., preferably 10 to 30 ° C. The rubber and ozone are reacted under normal pressure. The reaction conditions (reaction time, ozone concentration, pressure, temperature) are selected depending on the type of rubber to be used. Unreacted ozone that has passed through the vessel is decomposed in the activated carbon packed tower.
【０００７】用いるオゾンの原料に純酸素を用いた場
合、多量のオゾニドが発生し、爆発的に反応する危険が
あるため、空気を原料に用いるのが好ましい。When pure oxygen is used as a raw material of ozone, a large amount of ozonide is generated and there is a risk of explosive reaction. Therefore, it is preferable to use air as a raw material.
【０００８】オゾン濃度は、0.1％以下の低濃度では反
応が非常に遅く、実用的ではない。したがって、0.1％
以上とする必要があるが、効率よく処理するためには、
１％程度以上の10％までの濃度範囲が好ましい。[0008] When the ozone concentration is as low as 0.1% or less, the reaction is very slow and is not practical. Therefore, 0.1%
It is necessary to make it above, but in order to process efficiently,
A concentration range of about 1% to 10% is preferred.
【０００９】ゴムとオゾンとの気固反応であるので、オ
ゾンとの接触面積が大きいほど望ましく、したがって、
ゴム粉砕物の粒子径は小さいほど好ましいが、１mm程度
でも十分適用できる。Since the gas-solid reaction between rubber and ozone is desirable, the larger the contact area with ozone, the better.
The smaller the particle size of the rubber pulverized material is, the more preferable it is. However, about 1 mm can be sufficiently applied.
【００１０】再生可能な加硫ゴムの例は、主鎖か又は側
鎖に二重結合を有する天然ゴム、イソプレンゴム、スチ
レンブタジエンゴム、ブタジエンゴム、アクリロニトリ
ルブタジエンゴム、ブチルゴム、エチレンプロピレンゴ
ムを硫黄又は過酸化物で加硫したものである。Examples of the renewable vulcanized rubber include natural rubber having a double bond in a main chain or a side chain, isoprene rubber, styrene butadiene rubber, butadiene rubber, acrylonitrile butadiene rubber, butyl rubber, and ethylene propylene rubber. It is vulcanized with peroxide.
【００１１】再生加硫ゴム及び再生ゴムを混合した加硫
ゴムの製造に用いる配合薬品は、一般的に使用される架
橋剤、加硫促進剤、老化防止剤、加工助剤である。架橋
剤は硫黄又は過酸化物のいずれでもよい。The compounding chemicals used in the production of reclaimed vulcanized rubber and vulcanized rubber mixed with reclaimed rubber are generally used crosslinking agents, vulcanization accelerators, antioxidants and processing aids. The crosslinker may be either sulfur or peroxide.
【００１２】[0012]
【発明の実施の形態】実施例１ 工場から排出された天然ゴム加硫物を粉砕したもの(平
均粒子径１mm)100ｇをガス導入及び排出管、撹拌装置を
装着した円筒状ガラス容器に入れ、無声放電式発生装置
からのオゾン発生量を20ｇ/Nm3に設定し、ガス流量0.2N
m3/minで導入管より吹き込み、所定時間反応させた。図
１には、処理時間と解重合量の関係を示す。解重合量は
クロロフォルム抽出量で評価する。処理初期、解重合量
は急速に増加するが、時間が長くなるほど増加率は低下
しており、これは表面近傍のみで解重合が進行している
ことを示している。15分以上の反応時間で、ゴムはロー
ル加工可能な可塑性を示したので、そのままロール機を
用いて硫黄、加硫促進剤を混練して、加硫・成形した。
表１にはその物性値を示した。DESCRIPTION OF THE PREFERRED EMBODIMENTS Example 1 100 g of a pulverized natural rubber vulcanizate (average particle diameter: 1 mm) discharged from a factory is put into a cylindrical glass container equipped with a gas introduction / discharge tube and a stirrer. the amount of ozone generated from the silent discharge type generator set to 20 g / Nm 3, the gas flow rate 0.2N
Blowing was performed from the introduction tube at m 3 / min, and the reaction was performed for a predetermined time. FIG. 1 shows the relationship between the treatment time and the amount of depolymerization. The amount of depolymerization is evaluated based on the amount of chloroform extracted. At the beginning of the treatment, the amount of depolymerization increases rapidly, but the rate of increase decreases as the time becomes longer, indicating that depolymerization proceeds only near the surface. After a reaction time of 15 minutes or more, the rubber exhibited plasticity that could be roll-processed. Therefore, the rubber and the vulcanization accelerator were kneaded using a roll machine and vulcanized and molded.
Table 1 shows the physical property values.
【００１３】[0013]
【表１】 [Table 1]
【００１４】新ゴム(０分)と比較して伸張モジュラス以
外の諸性質は1/2程度に低下しているが、ゴム製マット
のような用途には十分使用可能である。また、新ゴム代
替材料としての効果を調べるために、天然ゴム生ゴム10
0部に対して25部混合し、硫黄、加硫促進剤等を混練し
て加硫、成形し、その物性を調べた。結果は表２に示
す。表２は、オゾン処理によってムーニー粘度で示され
る未加硫ゴム粘度が低下して加工性が改善されて、加硫
ゴム物性はほとんど低下せず、また、耐熱老化性が向上
していることを示している。Various properties other than the elongation modulus are reduced to about 1/2 as compared with the new rubber (0 minute), but it can be sufficiently used for applications such as rubber mats. In addition, in order to investigate the effect as a new rubber substitute material, natural rubber raw rubber 10
0 parts was mixed with 25 parts, sulfur, a vulcanization accelerator and the like were kneaded, vulcanized and molded, and the physical properties were examined. The results are shown in Table 2. Table 2 shows that the unvulcanized rubber viscosity represented by Mooney viscosity is reduced by the ozone treatment, the processability is improved, the physical properties of the vulcanized rubber are hardly reduced, and the heat aging resistance is improved. Is shown.
【００１５】[0015]
【表２】 [Table 2]
【００１６】実施例２ 工場から排出されたエチレンプロピレンゴム加硫物を粉
砕したものを、実施例１と同様な方法で処理した。図２
に処理時間と解重合量の関係を示す。解重合量はシクロ
ヘキサン抽出量で評価するが、天然ゴム同様の傾向を示
している。エチレンプロピレンゴムでは15分以上の処理
時間でロール加工可能な可塑性を示したので、そのまま
ロール機を用いて硫黄、加硫促進剤等を混練して、加硫
・成形し、引張試験を実施した。結果は表３に示す。Example 2 A vulcanized ethylene propylene rubber discharged from a factory was ground and treated in the same manner as in Example 1. FIG.
Shows the relationship between the treatment time and the amount of depolymerization. The amount of depolymerization is evaluated by the amount of cyclohexane extracted, and shows the same tendency as natural rubber. Ethylene propylene rubber showed plasticity that could be rolled in a processing time of 15 minutes or more, so sulfur, a vulcanization accelerator, etc. were kneaded using a roll machine as it was, and vulcanized and molded, and a tensile test was performed. . The results are shown in Table 3.
【００１７】[0017]
【表３】 [Table 3]
【００１８】表４にはエチレンプロピレンゴム生ゴム10
0部に対して50部混合し、硫黄、加硫促進剤等を混練し
て加硫、成形した加硫ゴムの引張試験結果である。Table 4 shows ethylene propylene rubber raw rubber 10
5 shows the results of a tensile test of vulcanized rubber obtained by mixing 50 parts with respect to 0 part, kneading sulfur, a vulcanization accelerator, and the like, vulcanizing and molding.
【００１９】[0019]
【表４】 [Table 4]
【００２０】[0020]
【発明の効果】本発明のオゾンを用いた使用済み又は工
場排出ゴムの再生方法は、室温近辺で常圧下で実施可能
なためにエネルギー消費が少なく、従来の再生方法で発
生する悪臭がほどんど発生せず、また安全性の疑われる
薬剤を必要としないため、排ガス、排水等の処理を全く
必要としない環境負荷の少ない方法である。The method for regenerating used or factory-discharged rubber using ozone according to the present invention can be carried out at around room temperature under normal pressure, so that it consumes little energy and has almost no odor generated by the conventional regenerating method. Since this method does not generate and does not require a chemical suspected to be safe, it is a method with a low environmental load that does not require any treatment of exhaust gas, wastewater and the like.
【００２１】処理後のゴムの再加硫物も用途によっては
十分な物性を示し、原料生ゴムの代替材料として用いる
ことにより新ゴム量を節約できる。また、この場合、未
加硫ゴムの加工性を改善することができる。このように
本発明は、ゴム製品製造業における循環型生産システム
の確立に寄与するものである。The re-vulcanized product of the treated rubber also exhibits sufficient physical properties depending on the application, and the amount of new rubber can be saved by using it as a substitute for raw rubber. In this case, the processability of the unvulcanized rubber can be improved. Thus, the present invention contributes to the establishment of a recycling-type production system in the rubber product manufacturing industry.
【図面の簡単な説明】[Brief description of the drawings]
【図１】天然ゴムの場合のオゾンとゴムとの反応時間と
ゴムの解重合量の関係のグラフである。FIG. 1 is a graph showing the relationship between the reaction time of ozone and rubber and the amount of depolymerization of rubber in the case of natural rubber.
【図２】エチレンプロピレンゴムの場合のオゾンとゴム
との反応時間とゴムの解重合量の関係のグラフである。FIG. 2 is a graph showing the relationship between the reaction time of ozone and rubber and the amount of depolymerization of rubber in the case of ethylene propylene rubber.
───────────────────────────────────────────────────── フロントページの続き (71)出願人 000157278 丸五ゴム工業株式会社 岡山県倉敷市上富井58番地 (71)出願人 000225359 内山工業株式会社 岡山県岡山市江並338番地 (71)出願人 595109719 岡山県新技術振興財団 岡山県岡山市芳賀5301番地 (72)発明者 児玉 総治 岡山県岡山市芳賀5301 岡山県工業技術セ ンター内 (72)発明者 阪田 祐作 岡山県岡山市学南町２丁目３−26 (72)発明者 遠藤 正幸 岡山県邑久郡邑久町下笠加488 多田電機 株式会社岡山工場内 (72)発明者 植木 清介 岡山県倉敷市連島町矢柄４−4630 倉敷化 工株式会社内 (72)発明者 歳森 康弘 岡山県倉敷市上富井58番地 丸五ゴム工業 株式会社内 (72)発明者 平田 正勝 岡山県赤磐郡赤坂町大苅田1160−11 内山 工業株式会社内 (72)発明者 稲村 實 岡山県岡山市芳賀5301 岡山県新技術振興 財団内 Ｆターム(参考） 4F301 AA04 AA06 AA07 AB03 CA09 CA23 CA72 CA73 CA74 4J100 AA02P AA03Q AA06P AB02P AM02P AS02Q AS03P CA01 CA04 HA51 HB08 ──────────────────────────────────────────────────続 き Continuing from the front page (71) Applicant 000157278 Marugo Rubber Industry Co., Ltd. 58, Kamitomii, Kurashiki City, Okayama Prefecture (71) Applicant 000225359 Uchiyama Industry Co., Ltd. 338, Enami, Okayama City, Okayama Prefecture (71) Applicant 595109719 Okayama Prefectural New Technology Promotion Foundation 5301 Haga, Okayama-shi, Okayama Pref. 3-26 (72) Inventor Masayuki Endo 488 Shimogasaka, Oku-cho, Oku-gun, Okayama Prefecture Inside Tada Electric Co., Ltd.Okayama Plant (72) Inventor Seisuke Ueki 4-4630, Yagura, Renshima-cho, Kurashiki-shi, Okayama Prefecture Inside Kurashiki Chemical Co., Ltd. 72) Inventor Yasuhiro Toshimori 58 Kamitomii, Kurashiki-shi, Okayama Marugo Rubber Industry Co., Ltd. (72) Inventor Masakatsu Hirata 116 Okanda, Akasaka-cho, Akaiwa-gun, Okayama Prefecture 0-11 Uchiyama Kogyo Co., Ltd. AS03P CA01 CA04 HA51 HB08
Claims (2)
ン処理により解重合し、可塑性を付与して再生ゴム原料
にすることを特徴とする加硫ゴムの再生方法。1. A method for regenerating vulcanized rubber, comprising depolymerizing a used or factory-discharged vulcanized rubber by ozone treatment to impart plasticity to a recycled rubber raw material.
オゾン生成能力を有するオゾン発生装置を用い、温度５
〜40℃、常圧下で再生処理する請求項１記載の加硫ゴム
の再生方法。2. The ozone treatment is carried out using an ozone generator having an ozone generating capacity of 2 g / Nm 3 (0.1%) or more, at a temperature of 5 g / Nm 3 (0.1%).
The method for regenerating a vulcanized rubber according to claim 1, wherein the regenerating treatment is carried out at a temperature of from 40 to 40 ° C under normal pressure.
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|---|---|---|---|
| JP2000082757A JP2001261883A (en) | 2000-03-23 | 2000-03-23 | Method of reclaiming vulcanized rubber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000082757A JP2001261883A (en) | 2000-03-23 | 2000-03-23 | Method of reclaiming vulcanized rubber |
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| Publication Number | Publication Date |
|---|---|
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Family
ID=18599513
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Cited By (5)
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|---|---|---|---|---|
| JP2005212174A (en) * | 2004-01-28 | 2005-08-11 | Nok Corp | Vulcanized scrap rubber regenerating method |
| CN101791831A (en) * | 2010-03-24 | 2010-08-04 | 际华三五一七橡胶制品有限公司 | Novel method for improving plasticity of regenerated crepe rubber |
| WO2018061404A1 (en) * | 2016-09-29 | 2018-04-05 | 太平洋セメント株式会社 | Method for treating carbon-containing waste |
| JP2018134574A (en) * | 2017-02-21 | 2018-08-30 | 太平洋セメント株式会社 | Carbon-containing waste disposal method |
| CN109790979A (en) * | 2016-09-29 | 2019-05-21 | 太平洋水泥株式会社 | The processing method of carbonaceous refuse |
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| JPH0518654U (en) * | 1991-08-19 | 1993-03-09 | ホクセイ機装株式会社 | Rubber waste treatment equipment |
| JPH07502552A (en) * | 1991-12-23 | 1995-03-16 | アントルプリス“マレ” | How to treat crosslinked polymers |
| JP2001261707A (en) * | 2000-03-23 | 2001-09-26 | Okayama Prefecture | Method of depolymerizing natural rubber |
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| JP2005212174A (en) * | 2004-01-28 | 2005-08-11 | Nok Corp | Vulcanized scrap rubber regenerating method |
| CN101791831A (en) * | 2010-03-24 | 2010-08-04 | 际华三五一七橡胶制品有限公司 | Novel method for improving plasticity of regenerated crepe rubber |
| WO2018061404A1 (en) * | 2016-09-29 | 2018-04-05 | 太平洋セメント株式会社 | Method for treating carbon-containing waste |
| CN109790979A (en) * | 2016-09-29 | 2019-05-21 | 太平洋水泥株式会社 | The processing method of carbonaceous refuse |
| JP2018134574A (en) * | 2017-02-21 | 2018-08-30 | 太平洋セメント株式会社 | Carbon-containing waste disposal method |
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