JPS621618B2 - - Google Patents
Info
- Publication number
- JPS621618B2 JPS621618B2 JP3222081A JP3222081A JPS621618B2 JP S621618 B2 JPS621618 B2 JP S621618B2 JP 3222081 A JP3222081 A JP 3222081A JP 3222081 A JP3222081 A JP 3222081A JP S621618 B2 JPS621618 B2 JP S621618B2
- Authority
- JP
- Japan
- Prior art keywords
- organic solvent
- water
- polystyrene
- boiling point
- amount
- 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.)
- Expired
Links
- 239000003960 organic solvent Substances 0.000 claims description 36
- 239000004793 Polystyrene Substances 0.000 claims description 28
- 229920002223 polystyrene Polymers 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000009835 boiling Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 239000005909 Kieselgur Substances 0.000 claims description 3
- 229910021536 Zeolite Inorganic materials 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004576 sand Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000010457 zeolite Substances 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 229920002472 Starch Polymers 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000008107 starch Substances 0.000 description 6
- 235000019698 starch Nutrition 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 5
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000011324 bead Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical group ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- -1 aliphatic halogen compounds Chemical class 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000001577 simple distillation Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 239000003799 water insoluble solvent Substances 0.000 description 1
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Description
【発明の詳細な説明】
本発明は有機溶媒の回収法に関するものであ
る。ポーラス状のジビニルベンゼン−スチレン共
重合体よりなる粒状ポリマーを製造する場合、ジ
ビニルベンゼン及びスチレンをポリスチレンの存
在下で懸濁重合し、次いで、得られた粒状ポリマ
ーを、ポリスチレンのみを溶解する有機溶媒例え
ばトルエン、ベンゼンなどで処理してポリマー粒
子中のポリスチレンのみを選択的に抽出除去する
ことによりポーラス状の粒状ポリマーを得る方法
が知られている。この方法では、抽出処理後ポリ
スチレンを溶存している有機溶媒を処理して純粋
な有機溶媒を回収する必要があるので通常、抽出
処理後の有機溶媒を水と混合して加熱することに
より、有機溶媒を留出させる方法が採られてい
る。
しかしながら、この処理法では有機溶媒の留出
量を上げて行くと、容器中にポリスチレンが水飴
状で析出し、装置内壁及び撹拌翼に粘着し、更に
は、有機溶媒がかなり残存していても全体の粘度
が上昇し撹拌が不能となることもある。ポリスチ
レンが水飴状となつた場合には、後の装置の洗浄
操作が大変であるため、有機溶媒の留出量を抑え
てかま残中に相当量の有機溶媒を残存させる必要
があり、有機溶媒の回収率を上げることはできな
かつた。
本発明者等は上記実情に鑑み、かま残中のポリ
スチレンが水飴状となるのを防止しながら有機溶
媒の回収率を上げる方法につき種々検討した結
果、有機溶媒留去の際、液中にある特定の粉粒体
を存在させることにより、ポリスチレンが粉粒体
とともにビーズ状となり、有機溶媒の回収率を上
昇させても、水飴状にならないことを見い出し本
発明を完成した。
すわち、本発明の要旨は、ポリスチレンが溶解
されている水不溶性で、しかも、沸点が水の沸点
よりも低いか又は水との共沸点が水の沸点よりも
低い有機溶媒を、該有機溶媒に対して、0.1重量
倍以上の水と混合し、次いで、この混合物を加熱
して有機溶媒を留出することによりポリスチレン
を水中に析出させて回収する方法において、前記
混合物中にポリスチレンに対して、0.6重量倍以
上の炭酸カルシウム、ゼオライト、カオリン、ケ
イ砂、ケイソウ土、ベントナイト、活性炭及びお
が屑から選ばれた少なくとも一種の粉粒体を存在
させて有機溶媒留去を行うことを特徴とする有機
溶媒の回収法に存する。
以下、本発明を詳細に説明する。
本発明で対象となる有機溶媒はポリスチレンを
溶解することのできる水不溶性のもので、しか
も、沸点が水の沸点よりも低いか又は水の共沸点
が水の沸点よりも低いものであり、例えば、ベン
ゼン、トルエン、ｍ−キシレン、ニトロベンゼン
などの芳香族化合物、又は塩化メチレン、ジクロ
ルエタン、ジクロルエチレンなどの脂肪族ハロゲ
ン化合物が挙げられる。有機溶媒中に溶解されて
いるポリスチレンの量はいくらでも差し支えない
が、通常、１〜30重量％程度である。このような
ポリスチレンを含有する有機溶媒はどのような工
程から排出されるものでもよく特に限定されない
が、例えば、ポーラス状のジビニルベンゼン−ス
チレン共重合体よりなる粒状ポリマーを製造する
際に、ポリスチレンの存在下でジビニルベンゼン
とスチレンとを懸濁重合して得た粒状ポリマーを
上述のような有機溶媒で処理した後のポリスチレ
ンが溶解された有機溶媒が挙げられる。
本発明では有機溶媒を水と混合するが、この際
の水の使用量は有機溶媒に対して、0.1重量倍以
上、好ましくは１〜５重量倍である。水の使用量
はあまり少ないと、ポリスチレンを良好に水中に
分散することができず、また、あまり多くても効
果に変りはなく加熱が大変となるので好ましくな
い。
加熱処理は通常、上部に蒸気抜出口とコンデン
サーを有する密閉型撹拌槽などの単蒸留装置を用
いて実施される。加熱温度は水の沸点よりも低
く、有機溶媒の沸点以上又は有機溶媒と水との共
沸点以上の温度である。この処理により有機溶媒
は上部より留出し回収され、また、ポリスチレン
はかま残の水中に析出される。
本発明では上記の加熱処理の際に、炭酸カルシ
ウム、ゼオライト、カオリン、ケイ砂、ケイソウ
土、ベントナイト、活性炭及びおが屑から選ばれ
た少なくとも一種の粉粒体を存在させることを必
須の要件とするものである。これらの粉粒体を存
在させることにより、有機溶媒の留出とともに析
出するポリスチレンが水飴状にならず、装置内壁
及び撹拌翼などに粘着することなく、ビーズ状で
水中に分散されるのである。これらの粉粒体の使
用量はポリスチレンに対して、0.6重量倍以上、
好ましくは１〜３重量倍であり、この使用量があ
まり少ない場合には、水中にポリスチレンを良好
に分散させることができず、逆に、あまり多い場
合には、効果に差異はないので経済的でない。粉
粒体の粒径は通常、10〜300μ、好ましくは50〜
120μ程度であり、極端に大きくても、また、小
さくてもポリスチレンがビーズ状にならない。粉
粒体は通常、加熱処理の最初から水と有機溶媒の
混合物中に添加し、加熱処理中は均一に分散する
ように撹拌される。
有機溶媒の留出を終えたかま残は水中にポリス
チレンを含有するビーズが分散されているので、
常法により過することにより容易にポリスチレ
ンを分離することができる。
以上、本発明によれば、有機溶媒の留出量を上
げても、かま残中に水飴状のポリスチレンが生成
しないので、有機溶媒の回収率を上昇させること
ができる。また、かま残中のポリスチレンもビー
ズ状で得られるため、後の過も容易であり好ま
しい。
次に、本発明を実施例により更に詳細に説明す
るが、本発明はその要旨を超えない限り以下の実
施例に限定されるものではない。
実施例及び比較例
加熱装置、撹拌機及び上部に有機溶媒を回収す
るための抜出口とコンデンサーを備えた１の密
閉ガラス容器に、水500ｇ、16.7％のポリスチレ
ンを溶解した第１表に示す有機溶媒及び第１表に
示す各種粉粒体（粒径50〜150μ）を仕込み、撹
拌下、加熱を行ない、有機溶媒の95％が留出する
まで加熱処理を行なつた。
このような有機溶媒の回収操作を行なつたの
ち、かま残の状態を観察したところ、第１表に示
す通りであつた。
【表】DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for recovering organic solvents. When producing a granular polymer consisting of a porous divinylbenzene-styrene copolymer, divinylbenzene and styrene are suspension polymerized in the presence of polystyrene, and then the resulting granular polymer is mixed with an organic solvent that dissolves only the polystyrene. For example, a method is known in which porous particulate polymers are obtained by selectively extracting and removing only polystyrene in polymer particles by treatment with toluene, benzene, or the like. In this method, it is necessary to recover the pure organic solvent by treating the organic solvent in which polystyrene is dissolved after the extraction process. A method is adopted in which the solvent is distilled off. However, with this treatment method, as the amount of organic solvent distilled is increased, polystyrene precipitates in the container in the form of starch syrup and sticks to the inner wall of the device and stirring blades, and even if a considerable amount of organic solvent remains. The overall viscosity may increase and stirring may become impossible. When polystyrene becomes starch syrup-like, it is difficult to clean the equipment afterwards, so it is necessary to reduce the amount of organic solvent distilled out and leave a considerable amount of organic solvent in the kettle. It was not possible to increase the recovery rate. In view of the above circumstances, the present inventors have investigated various ways to increase the recovery rate of organic solvent while preventing the polystyrene in the pot residue from becoming starch syrup-like. The present invention was completed by discovering that by allowing a specific powder or granule to exist, polystyrene becomes bead-like together with the powder and does not become starch syrup-like even if the recovery rate of the organic solvent is increased. In other words, the gist of the present invention is to use an organic solvent in which polystyrene is dissolved that is water-insoluble and has a boiling point lower than the boiling point of water or an azeotropic point with water lower than the boiling point of water. In this method, polystyrene is precipitated in water and recovered by mixing it with 0.1 times or more of water by weight, and then heating this mixture to distill off the organic solvent. , 0.6 times by weight or more of calcium carbonate, zeolite, kaolin, silica sand, diatomaceous earth, bentonite, activated carbon, and sawdust. It consists in the method of recovering the solvent. The present invention will be explained in detail below. The organic solvent targeted by the present invention is a water-insoluble solvent that can dissolve polystyrene and has a boiling point lower than the boiling point of water or an azeotropic point of water lower than the boiling point of water, such as , aromatic compounds such as benzene, toluene, m-xylene, and nitrobenzene, and aliphatic halogen compounds such as methylene chloride, dichloroethane, and dichloroethylene. The amount of polystyrene dissolved in the organic solvent may be any amount, but is usually about 1 to 30% by weight. Such polystyrene-containing organic solvents may be discharged from any process and are not particularly limited. Examples include organic solvents in which polystyrene is dissolved after a particulate polymer obtained by suspension polymerization of divinylbenzene and styrene is treated with an organic solvent as described above. In the present invention, an organic solvent is mixed with water, and the amount of water used at this time is 0.1 times or more, preferably 1 to 5 times the weight of the organic solvent. If the amount of water used is too small, the polystyrene cannot be well dispersed in water, and if it is too large, the effect will not change and heating will become difficult, which is not preferable. The heat treatment is usually carried out using a simple distillation apparatus such as a closed stirred tank having a steam outlet and a condenser at the top. The heating temperature is lower than the boiling point of water and higher than the boiling point of the organic solvent or higher than the azeotropic point of the organic solvent and water. Through this treatment, the organic solvent is distilled and recovered from the upper part, and polystyrene is precipitated in the water remaining in the kettle. In the present invention, it is an essential requirement that at least one kind of granular material selected from calcium carbonate, zeolite, kaolin, silica sand, diatomaceous earth, bentonite, activated carbon, and sawdust be present during the above heat treatment. It is. Due to the presence of these powders, the polystyrene that precipitates with the distillation of the organic solvent does not become starch syrup-like and is dispersed in the water in the form of beads without sticking to the inner walls of the device, stirring blades, etc. The amount of these powders used is at least 0.6 times the weight of polystyrene.
Preferably, it is 1 to 3 times the weight. If the amount used is too small, polystyrene cannot be well dispersed in water, and if it is too large, there will be no difference in the effect, so it is not economical. Not. The particle size of the powder is usually 10 to 300μ, preferably 50 to 300μ.
The diameter is approximately 120μ, so polystyrene will not form beads even if it is extremely large or small. The granular material is usually added to a mixture of water and an organic solvent from the beginning of the heat treatment, and is stirred during the heat treatment so as to be uniformly dispersed. The residue after distilling off the organic solvent contains beads containing polystyrene dispersed in water.
Polystyrene can be easily separated by filtration using a conventional method. As described above, according to the present invention, even if the distillation amount of the organic solvent is increased, starch syrup-like polystyrene is not generated in the pot residue, so that the recovery rate of the organic solvent can be increased. In addition, since the polystyrene in the pot residue is also obtained in the form of beads, subsequent filtration is easy, which is preferable. Next, the present invention will be explained in more detail with reference to examples, but the present invention is not limited to the following examples unless it exceeds the gist thereof. Examples and Comparative Examples The organic solvent shown in Table 1 was prepared by dissolving 500 g of water and 16.7% polystyrene in a sealed glass container 1 equipped with a heating device, a stirrer, and an outlet and a condenser at the top for recovering the organic solvent. A solvent and various powders (particle size 50 to 150 μm) shown in Table 1 were charged and heated while stirring until 95% of the organic solvent was distilled off. After carrying out such an operation for recovering the organic solvent, the condition of the residue in the pot was observed, and the condition was as shown in Table 1. 【table】
Claims (1)
しかも、沸点が水の沸点よりも低いか又は水との
共沸点が水の沸点よりも低い有機溶媒を、該有機
溶媒に対して、0.1重量倍以上の水と混合し、次
いで、この混合物を加熱して有機溶媒を留去する
ことによりポリスチレンを水中に析出させて回収
する方法において、前記混合物中にポリスチレン
に対して、0.6重量倍以上の炭酸カルシウム、ゼ
オライト、カオリン、ケイ砂、ケイソウ土、ベン
トナイト、活性炭及びおが屑から選ばれた少なく
とも一種の粉粒体を存在させて有機溶媒留去を行
うことを特徴とする有機溶媒の回収法。1 Water-insoluble in which polystyrene is dissolved,
Moreover, an organic solvent whose boiling point is lower than the boiling point of water or whose azeotropic point with water is lower than the boiling point of water is mixed with water at least 0.1 times the weight of the organic solvent, and then this mixture is In a method of precipitating and recovering polystyrene in water by heating and distilling off an organic solvent, the mixture contains calcium carbonate, zeolite, kaolin, silica sand, diatomaceous earth, in an amount of 0.6 times or more by weight relative to polystyrene. 1. A method for recovering an organic solvent, which comprises distilling off an organic solvent in the presence of at least one kind of powder selected from bentonite, activated carbon, and sawdust.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3222081A JPS57147530A (en) | 1981-03-06 | 1981-03-06 | Recovering method of organic solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3222081A JPS57147530A (en) | 1981-03-06 | 1981-03-06 | Recovering method of organic solvent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57147530A JPS57147530A (en) | 1982-09-11 |
| JPS621618B2 true JPS621618B2 (en) | 1987-01-14 |
Family
ID=12352851
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3222081A Granted JPS57147530A (en) | 1981-03-06 | 1981-03-06 | Recovering method of organic solvent |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS57147530A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60161440A (en) * | 1984-01-31 | 1985-08-23 | Human Ind Corp | Method for reclaiming resin |
| JPH0784504B2 (en) * | 1987-10-13 | 1995-09-13 | 株式会社トクヤマ | Method for producing polystyrene sulfonic acid or derivative thereof |
| JP4673345B2 (en) * | 2007-06-18 | 2011-04-20 | 株式会社前川製作所 | Solvent separation and recovery method and apparatus |
-
1981
- 1981-03-06 JP JP3222081A patent/JPS57147530A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57147530A (en) | 1982-09-11 |
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