JPH0332565B2 - - Google Patents
Info
- Publication number
- JPH0332565B2 JPH0332565B2 JP14137781A JP14137781A JPH0332565B2 JP H0332565 B2 JPH0332565 B2 JP H0332565B2 JP 14137781 A JP14137781 A JP 14137781A JP 14137781 A JP14137781 A JP 14137781A JP H0332565 B2 JPH0332565 B2 JP H0332565B2
- Authority
- JP
- Japan
- Prior art keywords
- solvent
- molecular weight
- low molecular
- weight polyolefin
- waste
- 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
- 239000010887 waste solvent Substances 0.000 claims description 46
- 229920000098 polyolefin Polymers 0.000 claims description 42
- 239000002904 solvent Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 30
- 239000012528 membrane Substances 0.000 claims description 26
- 238000000108 ultra-filtration Methods 0.000 claims description 21
- 239000003960 organic solvent Substances 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000010409 thin film Substances 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 2
- -1 polyethylene Polymers 0.000 description 21
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 12
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 10
- 239000004743 Polypropylene Substances 0.000 description 9
- 229930195733 hydrocarbon Natural products 0.000 description 9
- 238000006116 polymerization reaction Methods 0.000 description 9
- 229920001155 polypropylene Polymers 0.000 description 9
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 150000002430 hydrocarbons Chemical class 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 5
- 239000005977 Ethylene Substances 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 4
- 238000001256 steam distillation Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 125000003710 aryl alkyl group Chemical group 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000012466 permeate Substances 0.000 description 3
- 229920001748 polybutylene Polymers 0.000 description 3
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001282 iso-butane Substances 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 229920001684 low density polyethylene Polymers 0.000 description 2
- 239000004702 low-density polyethylene Substances 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methylcyclopentane Chemical compound CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 229920002492 poly(sulfone) Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 229920005604 random copolymer Polymers 0.000 description 2
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 1
- JLBJTVDPSNHSKJ-UHFFFAOYSA-N 4-Methylstyrene Chemical compound CC1=CC=C(C=C)C=C1 JLBJTVDPSNHSKJ-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 1
- 229920006370 Kynar Polymers 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000012685 gas phase polymerization Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 229940035429 isobutyl alcohol Drugs 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 235000014594 pastries Nutrition 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920005606 polypropylene copolymer Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000004094 preconcentration Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 235000015096 spirit Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Description
本発明はポリオレフイン製造工程で得られる低
分子量ポリオレフインを含む廃溶媒から低分子量
ポリオレフインと有機溶媒とを分離する方法に関
する。
中低圧法高密度ないし低密度ポリエチレンまた
はポリプロピレンなどの製造工程から排出される
低分子量のポリエチレンワツクスまたは低分子量
低結晶性ポリプロピレン（いわゆるアタクチツク
ポリプロピレン）（以下これらを低分子量ポリオ
レフインという）などを含有している炭化水素、
あるいはアルコールなどの廃溶媒（以下これらを
単に廃溶媒という）を処理して低分子量ポリオレ
フインと炭化水素あるいはアルコールなどの溶媒
（以下溶媒という）を分離する方法として、水蒸
気蒸留法、溶剤置換法、遠心薄膜蒸発法が知られ
ている。
水蒸気蒸留法は、廃溶媒を水蒸気蒸留釡に入
れ、これに水蒸気を吹込んで溶媒を水蒸気ととも
に留出させ、一方低分子量ポリオレフインは水に
浮いて釡内に残留するので一定量たまつたならば
とりだす方法である。溶剤置換法は、廃溶媒中の
溶媒を低分子量ポリオレフインの融点以上の沸点
をもつ第２の溶媒たとえば、灯油、軽油、重油、
およびミネラルスピリツトのような高沸点不活性
液体に置換する方法がある。この方法は溶媒は回
収されるが、第２溶剤と低分子量ポリオレフイン
は通常焼却処理される。それ故低分子量ポリオレ
フインを分離したい場合適当な方法ではない。遠
心薄膜蒸発法は、廃溶媒を予備濃縮後、加圧下、
高温で加熱し、大気圧下の遠心薄膜蒸発器内にフ
ラツシユさせ、析出した低分子量ポリオレフイン
の再溶融と残留する溶媒の蒸発を遠心薄膜蒸発器
で行なわせるものである。しかし、有機溶媒がプ
ロピレン、イソブタンなどの常温以下の低沸点の
場合、液化のために再圧縮するエネルギーが必要
なのが欠点である。
これらの方法は、溶媒の蒸発または再圧縮を基
本にしているためにかなりの熱または電気エネル
ギーを必要とする。近年、省エネルギー化は重要
な課題となつている。本発明者は、これらの問題
点を解決すべく検討の上、本発明に到つたもので
ある。
すなわち、本発明の目的は、ポリオレフインの
製造工程から排出される廃溶媒から低分子量ポリ
オレフインと溶媒とを分離するに際し省エネルギ
ー化された方法を提供することである。
本発明はポリオレフイン製造工程中で得られる
低分子量ポリオレフインを含む廃溶媒を加圧して
限外過膜を通して過することにより、濃縮さ
せることを特徴とする低分子量ポリオレフインを
含む廃溶媒から有機溶媒を分離する方法である。
本発明の方法における廃溶媒に加圧する圧力
は、１〜100Kg／cm2Ｇであり、限外過膜前後の
圧力差は１〜100Kg／cm2Ｇである。また、過温
度は限外過膜の材質によつて異なるが、該膜が
膨潤をおこさない低い温度で行なう必要がある。
反対に過温度を高くすることは、溶媒の限外
過膜の透過速度を速くするので好ましい。通常の
温度としては−20℃〜200℃、好ましくは０℃〜
150℃、より好ましくは20℃〜100℃である。
本発明に使用する限外過膜は、有機溶媒に膨
潤しにくい耐溶剤性がすぐれているものがよく、
芳香族ポリアミド系、ポリアミドイミド系、ポリ
イミド系、ポリふつ化ビニリデン系、ポリテトラ
フルオロエチレン系、ポリスルホン系などが用い
られる。本発明における限外過膜の適当な平均
孔径は10Å〜1000Å、好ましくは20Å〜200Å、
さらに好ましくは50Å〜150Åである。平均孔径
は低分子量ポリオレフインの分子量によつて選択
する。及び分割すべき分子量範囲から選択するこ
とが重要である。本発明における限外過膜は通
常モジユールにして使用する。膜モジユールの形
状は、中空繊維状、のりまき状、平板状、管状な
どであある。管状のモジユールは構造が簡単なた
め、廃溶媒に混入してくる有機溶媒に不溶性の低
分子量ポリオレフインのゲル又は粒子が膜モジユ
ールの目詰りが生じにくいばかりなく、膜面流速
を大きくすることができるので好ましい。また、
スポンジボール洗浄のような物理洗浄あるいは有
機溶媒による薬品洗浄ができるので好ましい。
本発明における低分子量ポリオレフインとは、
エチレンもしくはプロピレン、ブテン−１、ペン
テン−１、ヘキセン−１，４−メチルペンテン−
１などのα−オレフイン、またはスチレン、α−
メチルスチレンなどの芳香族スチレン系誘導体を
単量体とするホモ重合体もしくは共重合体であつ
て、有機溶媒に溶解する低分子量のものである。
その平均分子量は通常500，000以下のものであ
る。具体的な低分子量ポリオレフインとしては、
ポリエチレンワツクス、溶媒可溶のポリプロピレ
ンいわゆるアタクチツクポリプロピレン、ポリプ
ロピレンコポリマー（プロピレン／エチレン系、
プロピレン／ブテン−１系）、溶媒可溶のポリブ
テン−１いわゆるアタクチツクポリブテン−１、
ポリブテン−１コポリマー、溶媒可溶のエチレ
ン・プロピレンラバー、溶媒可溶なポリヘキセン
−１いわゆるアタクチツクポリヘキセン−１、ポ
リヘキセン−１コポリマー、溶媒可溶なポリ４−
メチルペンテン−１いわゆるアタクチツクポリ４
−メチルペンテン−１、ポリ４−メチルペンテン
−１コポリマー、溶媒可溶のポリスチレンななど
をあけることができる。
本発明の方法で廃溶媒から分離できる低分子量
ポリオレフインは、平均分子量が500以上であり、
500未満では分離が困難であり分離効率が低下す
る。分子量150未満のものは限外過膜を容易に
通過するので有機溶媒と分離することができな
い。
本発明の方法に供せられる廃溶媒とは、低分子
量ポリオレフインが有機溶媒に溶解している溶液
である。その濃度は30重量％以下、好ましくは10
重量％以下、より好ましくは３重量％以下であ
る。廃溶媒には、有機溶媒に不溶性の高分子量ポ
リオレフインの粒子もしくはゲルまたはその他の
無機化合物の微粒子（たとえば100μ以下）が含
有してもよく、その量は５重量％以下、好ましく
は１重量％以下、より好ましくは0.1重量％以下
である。また、水は相分離しない範囲内の量で含
有していてもよい。しかし、不溶性物質は限外
過膜に通過する前に別しておくのが好ましい。
本発明に供する廃溶媒の例としては、ポリエチ
レン−ノルマルヘキサン溶液、ポリエチレンノル
マルヘプタン溶液、ポリエチレン−液化イソブタ
ン溶液、ポリエチレン−シクロヘキサン溶液、ポ
リプロピレン−ノルマルヘキサン溶液、ポリプロ
ピレン−ノルマルヘキサン溶液、ポリプロピレン
−液化プロピレン溶液、ポリプロピレン−液化プ
ロパン溶液、ポリプロピレン−イソプロパノール
溶液、ポリプロピレン−プタノール（イソorノル
マル）溶液、ポリプロピレン−アセトン溶液、ポ
リプロピレン−酢酸メチル溶液、ポリエチレン−
イソプロパノール溶液、ポリエチレン−ブタノー
ル（イソorノルマル）溶液、ポリエチレン−アセ
トン溶液、ポリエチレン−酢酸メチル溶液、液化
ブテン−１−液化ブテン−１溶液などのを例示す
ることができる。
更に具体的に廃溶媒を例示すると、１）ノルマ
ルヘキサン、ノルマルヘプタンなどの不活性炭化
水素、有機溶媒を用いるエチレンもしくはプロピ
レンの低圧溶媒重合後、アルコール、水などで触
媒を脱活性化して得られたスラリーを遠心分離機
にかけて得られた廃溶媒、２）液化プロピレン自
身を重合溶媒とするプロピレンのバルブ液体プー
ル重合の後、アルコール、水などで触媒を脱活性
化して得たスラリーを高圧遠心分離あるいは液化
プロピレンによる向流洗浄後沈降分離などの処理
で得れれた廃溶媒、３）液化プロピレン自身を重
合溶媒とするバルク液体プール重合によつて得ら
れるポリプロピレンスラリーを減圧室に送り乾燥
されたポリプロピレン粉末をイソプロパノールな
どのアルコール類、アセトンなどのケトン類、も
しくはノルマルヘキサンななどの炭化水素類など
の有機溶媒で洗浄し、洗浄後のスラリーを遠心分
離などの処理で得られた廃溶媒、４）気相重合で
得られたポリオレフイン粉末を３）と同様に洗
浄、処理されて得られた廃溶媒、５）１）におい
てアルコール、水などで脱活性化せずして得られ
たスラリーを遠心分離機にかけて得られた廃溶
媒、６）２）においてアルコール、水などで脱活
性化せずして得られたスラリーを同様の処理をし
て得られた廃溶媒などがあげられる。
これらの廃溶媒を加圧下で限外過膜モジユー
ルを通して過し、有機溶媒が分離され、廃溶媒
は濃縮される。濃縮された廃溶媒の低分子量ポリ
オレフインの濃度は５〜60％となり、廃溶媒の初
期の濃度の２〜30倍となる。濃縮された廃溶媒中
の低分子量ポリオレフインの濃度が60％をこえる
と、透過（過）速度が著しく低下するので好ま
しくない。
濃縮された廃溶媒は、必要に応じて種々の方法
で処理され低分子量ポリオレフインを分離もしく
は回収することができる。たとえば、１）過を
くり返し更に濃縮する方法、２）水蒸気を吹き込
み低分子量ポリオレフインを水に浮かして回収す
る方法、３）濃縮された廃溶媒中の溶媒を低分子
量ポリオレフインの融点以上の沸点をもつ溶媒と
置換する方法、４）低分子量ポリオレフインの融
点以上の温度で加圧し、これを遠心薄膜蒸発器へ
フラツシユさせ低分子量ポリオレフインを回収す
る方法、５）液化プロピレンのような低沸点溶媒
を含むような場合、減圧下にフラツシユする方法
などがあげられる。
限外過膜モジユールを透過した有機溶媒は、
そのまま直接、もしくは吸着、脱水もしくは蒸留
操作などを行なつた後、重合工程もしくは洗浄工
程に再循環して使用される。
本発明の廃溶媒に係る有機溶媒としては、炭化
水素類、アルコール類、エーテル類、エステル
類、ケトン類などである。炭化水素類としては脂
肪族炭化水素、脂環式炭化水素、芳香族炭化水
素、脂肪族炭化水素として液化プロパン、液化ブ
タン（ノルマンあるいは／およびイソ）、イソペ
ンタン、ノルマン、ヘキサン、ノルマルヘプタ
ン、液化プロピレン、液化ブテン−１、ペンテン
−１、ヘキセン−１，４−メチルペンテン−１な
どが例示できる。脂環式炭化水素としてメチルシ
クロペンタン、シクロヘキサン、メチルシクロヘ
キサンなどが例示できる。芳香族炭化水素として
ベンゼン、トルエン、キシレン、スチレンなどが
例示できる。炭化水素類としてリグロイン、灯
油、軽油などもあげられる。アルコール類は１価
アルコールとして、メチルアルコール、エチルア
ルコール、イソプロピルアルコール、ノルマルブ
チルアルコール、イソブチルアルコール、ターシ
ヤリーブチルアルコール、イソアミルアルコー
ル、２−エチルヘキシルアルコールを例示でき
る。多価アルコールとしてエチレングリコール、
プロピレングリコール、グリセリンなどが例示で
きる。エーテル類は一般式R1−（OR2）o−OR3
（R1，R2，R3＝アルキル・アリル、アラルキル
基、ｎ＝０−５の整数）で表示されるもので、エ
チルエーテル、イソプロピルアルコール、エチレ
ングリコール、ジメチルエーテルなどが例示でき
る。エステル類は一般式R1COOR2（R1，R2＝ア
ルキル・アリル・アラルキル基）で表示されるも
ので、酢酸メチル、酢酸エチルなどが例示でき
る。ケトン類は一般式R1CO（R2CO）oR3（R1，R2，
R3＝アルキル・アリル・アラルキル基、ｎ＝０
−５整数）で表示されるもので、アセトン、メチ
ル、エチルケトン、アセチルアセトンが例示でき
る。これらの例示された有機溶媒は、単独もしく
は種々の混合物の状態であつてもよく、混合物の
場合は相分離の起らない範囲であればよい。
本発明の方法において、限外過膜を過する
ことによつて濃縮された廃溶媒の低分子量ポリオ
レフインの濃度は著しく高くなる。すなわち低分
子量ポリオレフインの濃度約１％の廃溶媒は、
過により５〜10％となり、過をくり返すことに
よつて60％程度までになる。そのため廃溶媒中の
大部分の溶媒は、本発明による過によつて分離
される。それ故、濃縮された廃溶媒中から低分子
量ポリオレフインを分離もしくは回収する場合、
従来の水蒸気蒸留法、溶剤置換法、遠心薄膜を使
用するとしてもスチームなどの熱エネルギーは著
しく軽減される。本発明の分離方法を中低圧法、
高密度ないし低密度ポリエチレン又はポリプロピ
レンなどの製造プロセスに直結することにより前
記ポリオレフインの製造コストを著しく低下する
ことができる。
本発明者は特願55−107487に提案したポリプロ
ピレン製造プロセス（特に炭化水素不溶性重合体
生成率が著しく高いコポリマー製造プロセス）に
本発明の分離方法を適用することにより重合溶媒
を精製することなく重合工程にリサイクルする重
合溶媒の完全循環プロセスを完成することができ
る。
以下、実施例を示す。
実施例１〜23
表示した限外過膜をモジユール化した装置に
表示条件下で、、表示した廃溶媒を連続的にフイ
ードし、限外過膜を透過した透過溶液と排出廃
溶媒に分離した。排出廃溶媒はモジユールに連続
リサイクルした。最終的にはフイードされた廃溶
媒は透過溶媒と排出濃縮溶媒に分離した。
実施例−１について説明するとポリマー濃度
1.2重量％の仕込み廃溶媒を限外過膜モジユー
ルに通し、著しくポリマー濃度の低い（0.04重量
％）透過溶媒と著しくポリマー濃度の高い（11.0
重量％）排出濃縮廃溶媒に分離した。したがつて
溶媒の濃縮率は
100×｛１−100−11／11×1.2／100−1.2｝＝99.1％
となる。一方従来の遠心薄膜蒸発法の前段階工程
である予備濃縮操作をスチーム加熱による従来法
と比較した場合、本発明の限外過膜を用いる方
法は、廃溶媒の加圧、循環用ポンプの動力用電気
をごく少量使用するだけでよいので、従来法に比
していちじるしいエネルギーの低下となつた。
表についての説明を下記する。
１ 限外過膜
ポリイミド系−日東電工社製
NTU−4200シリーズ
ポリイアミド系−Berghof社製
ポリフツ化ビニリデン系−Pennwalt社製
KYNAR
ポリ四フツ化エチレン系−住友電工社製
ポマフロン
ポリスルホン系−UCC社製
Udel Ｐ−1700
２ 廃溶媒中のポリマー種類
＊１）プロピレンエチレンランダム共重合体
（エチレン含量2.0〜5.5重量％）を製造する時
に副生した低分子量低結晶性共重合体。
＊２）プロピレンエチレンブロツク共重合体
（エチレン含量８〜19重量％）製造時副生した
低分子量低結晶性共重合体。
３ ポリマー濃度
試料の溶媒を蒸発乾固し、残存量より計算して
求めた。
４ 平均分子量
Water associaton社のGelPermeation
chromatographyにより求めた。
５ 操作条件
圧力−モジユール入口と出口の圧力の平均値温
度−仕込み廃溶媒の温度
６ 透過速度
限外過膜１m2当り、１時間当りの透過廃溶量
（）
７ 分割分子量
単分散ポリエチレングリコールの0.5％トルエ
ン溶液を限外過膜に通し、Delpermeation
chromatographyを用い95％溶質除去率を得る分
子量。
The present invention relates to a method for separating a low molecular weight polyolefin and an organic solvent from a waste solvent containing a low molecular weight polyolefin obtained in a polyolefin manufacturing process. Contains low-molecular-weight polyethylene wax or low-molecular-weight, low-crystalline polypropylene (so-called atactic polypropylene) (hereinafter referred to as low-molecular-weight polyolefin) discharged from the manufacturing process of medium-low pressure high-density to low-density polyethylene or polypropylene. hydrocarbons,
Alternatively, methods for treating waste solvents such as alcohol (hereinafter simply referred to as waste solvents) to separate low molecular weight polyolefins from hydrocarbons or solvents such as alcohols (hereinafter referred to as solvents) include steam distillation, solvent displacement, centrifugation, etc. Thin film evaporation methods are known. In the steam distillation method, the waste solvent is placed in a steam distillation pot and steam is blown into it to distill the solvent together with the steam.On the other hand, low molecular weight polyolefin floats on water and remains in the pot, so once a certain amount has accumulated. This is the way to take it out. In the solvent replacement method, the solvent in the waste solvent is replaced with a second solvent having a boiling point higher than the melting point of the low molecular weight polyolefin, such as kerosene, light oil, heavy oil,
and high boiling inert liquids such as mineral spirits. In this method, the solvent is recovered, but the second solvent and low molecular weight polyolefin are usually incinerated. Therefore, it is not a suitable method when it is desired to separate low molecular weight polyolefins. In the centrifugal thin film evaporation method, after preconcentrating the waste solvent, under pressure,
It is heated at high temperature and flashed in a centrifugal thin film evaporator under atmospheric pressure, and the precipitated low molecular weight polyolefin is remelted and the remaining solvent is evaporated in the centrifugal thin film evaporator. However, when the organic solvent has a low boiling point below room temperature, such as propylene or isobutane, the disadvantage is that energy is required to recompress it for liquefaction. These methods require considerable thermal or electrical energy because they are based on evaporation or recompression of the solvent. In recent years, energy conservation has become an important issue. The inventor of the present invention arrived at the present invention after conducting studies to solve these problems. That is, an object of the present invention is to provide an energy-saving method for separating a low molecular weight polyolefin and a solvent from waste solvent discharged from a polyolefin manufacturing process. The present invention is characterized in that the waste solvent containing low molecular weight polyolefin obtained during the polyolefin manufacturing process is concentrated by passing it through an ultrafiltration membrane under pressure.The organic solvent is separated from the waste solvent containing low molecular weight polyolefin. This is the way to do it. The pressure applied to the waste solvent in the method of the present invention is 1 to 100 Kg/cm 2 G, and the pressure difference before and after the ultrafiltration membrane is 1 to 100 Kg/cm 2 G. Further, although the overtemperature differs depending on the material of the ultrafiltration membrane, it is necessary to carry out the heating at a low temperature at which the membrane does not swell.
On the contrary, it is preferable to increase the supertemperature because it increases the permeation rate of the solvent through the ultrafiltration membrane. Normal temperature is -20℃~200℃, preferably 0℃~
The temperature is 150°C, more preferably 20°C to 100°C. The ultrafiltration membrane used in the present invention preferably has excellent solvent resistance and is resistant to swelling in organic solvents.
Aromatic polyamide, polyamideimide, polyimide, polyvinylidene fluoride, polytetrafluoroethylene, polysulfone, and the like are used. A suitable average pore diameter of the ultrafiltration membrane in the present invention is 10 Å to 1000 Å, preferably 20 Å to 200 Å,
More preferably, it is 50 Å to 150 Å. The average pore size is selected depending on the molecular weight of the low molecular weight polyolefin. It is important to select from among the molecular weight range and the molecular weight range to be divided. The ultrafiltration membrane in the present invention is usually used as a module. The shape of the membrane module may be hollow fiber, pastry, flat, tubular, or the like. Since the tubular module has a simple structure, the membrane module is less likely to be clogged by gel or particles of low molecular weight polyolefin that are insoluble in the organic solvent mixed into the waste solvent, and the membrane surface flow rate can be increased. Therefore, it is preferable. Also,
This is preferable because physical cleaning such as sponge ball cleaning or chemical cleaning using an organic solvent can be performed. The low molecular weight polyolefin in the present invention is
Ethylene or propylene, butene-1, pentene-1, hexene-1,4-methylpentene-
α-olefins such as 1, or styrene, α-
It is a homopolymer or copolymer containing an aromatic styrene derivative such as methylstyrene as a monomer, and has a low molecular weight that dissolves in an organic solvent.
Its average molecular weight is usually less than 500,000. Specific low molecular weight polyolefins include:
Polyethylene wax, solvent-soluble polypropylene, so-called atactic polypropylene, polypropylene copolymer (propylene/ethylene-based,
propylene/butene-1 system), solvent-soluble polybutene-1 so-called atactic polybutene-1,
Polybutene-1 copolymer, solvent-soluble ethylene-propylene rubber, solvent-soluble polyhexene-1, so-called atactic polyhexene-1, polyhexene-1 copolymer, solvent-soluble poly4-
Methylpentene-1 so-called atactic poly-4
-Methylpentene-1, poly-4-methylpentene-1 copolymer, solvent-soluble polystyrene, etc. can be used. The low molecular weight polyolefin that can be separated from waste solvent by the method of the present invention has an average molecular weight of 500 or more,
If it is less than 500, separation will be difficult and separation efficiency will decrease. Those with a molecular weight of less than 150 easily pass through an ultrafiltration membrane and cannot be separated from the organic solvent. The waste solvent used in the method of the present invention is a solution in which a low molecular weight polyolefin is dissolved in an organic solvent. Its concentration is less than 30% by weight, preferably 10
It is not more than 3% by weight, more preferably not more than 3% by weight. The waste solvent may contain particles or gels of high molecular weight polyolefin insoluble in organic solvents or fine particles (for example, 100μ or less) of other inorganic compounds, and the amount thereof is 5% by weight or less, preferably 1% by weight or less. , more preferably 0.1% by weight or less. Further, water may be contained in an amount within a range that does not cause phase separation. However, it is preferred that insoluble materials be separated before passing through the ultrafiltration membrane. Examples of waste solvents used in the present invention include polyethylene-normal hexane solution, polyethylene-normal heptane solution, polyethylene-liquefied isobutane solution, polyethylene-cyclohexane solution, polypropylene-normal hexane solution, polypropylene-normal hexane solution, and polypropylene-liquefied propylene solution. , polypropylene-liquefied propane solution, polypropylene-isopropanol solution, polypropylene-butanol (iso or normal) solution, polypropylene-acetone solution, polypropylene-methyl acetate solution, polyethylene-
Examples include isopropanol solution, polyethylene-butanol (iso or normal) solution, polyethylene-acetone solution, polyethylene-methyl acetate solution, and liquefied butene-1-liquefied butene-1 solution. More specific examples of waste solvents include: 1) Low-pressure solvent polymerization of ethylene or propylene using an inert hydrocarbon or organic solvent such as n-hexane or n-heptane, followed by deactivation of the catalyst with alcohol, water, etc. 2) Valve liquid pool of propylene using liquefied propylene itself as the polymerization solvent After polymerization, the slurry obtained by deactivating the catalyst with alcohol, water, etc. is subjected to high-pressure centrifugation. Alternatively, waste solvent obtained from a treatment such as countercurrent washing with liquefied propylene followed by sedimentation separation, 3) polypropylene slurry obtained by bulk liquid pool polymerization using liquefied propylene itself as a polymerization solvent, and dried polypropylene by sending it to a vacuum chamber. Waste solvent obtained by washing the powder with an organic solvent such as an alcohol such as isopropanol, a ketone such as acetone, or a hydrocarbon such as n-hexane, and then centrifuging the slurry after washing; 4) The polyolefin powder obtained by gas phase polymerization is washed and treated in the same manner as in 3), and the waste solvent obtained is 5) The slurry obtained without deactivating with alcohol, water, etc. in 1) is centrifuged. Examples include waste solvent obtained by subjecting the slurry obtained without deactivation with alcohol, water, etc. in 6) and 2) to the same treatment. These waste solvents are passed through an ultrafiltration membrane module under pressure to separate the organic solvents and concentrate the waste solvents. The concentration of low molecular weight polyolefin in the concentrated waste solvent is 5 to 60%, which is 2 to 30 times the initial concentration of the waste solvent. If the concentration of the low molecular weight polyolefin in the concentrated waste solvent exceeds 60%, the permeation rate will drop significantly, which is not preferable. The concentrated waste solvent can be treated by various methods as necessary to separate or recover the low molecular weight polyolefin. For example, 1) a method of further concentrating by repeating filtration, 2) a method of blowing steam to float the low molecular weight polyolefin on water, and 3) a method of recovering the solvent in the concentrated waste solvent with a boiling point higher than the melting point of the low molecular weight polyolefin. 4) A method of pressurizing the low molecular weight polyolefin at a temperature higher than its melting point and flashing it to a centrifugal thin film evaporator to recover the low molecular weight polyolefin; 5) A method of replacing the low molecular weight polyolefin with a low boiling point solvent such as liquefied propylene. In such cases, a method such as flashing under reduced pressure may be mentioned. The organic solvent that has passed through the ultrafiltration membrane module is
It can be used directly as it is, or after being subjected to adsorption, dehydration, or distillation operations, it can be recycled to the polymerization process or washing process. Organic solvents related to the waste solvent of the present invention include hydrocarbons, alcohols, ethers, esters, ketones, and the like. Hydrocarbons include aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons, and aliphatic hydrocarbons include liquefied propane, liquefied butane (Norman and/or iso), isopentane, Norman, hexane, normal heptane, and liquefied propylene. , liquefied butene-1, pentene-1, hexene-1,4-methylpentene-1, and the like. Examples of alicyclic hydrocarbons include methylcyclopentane, cyclohexane, and methylcyclohexane. Examples of aromatic hydrocarbons include benzene, toluene, xylene, and styrene. Examples of hydrocarbons include ligroin, kerosene, and light oil. Examples of alcohols include methyl alcohol, ethyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutyl alcohol, tert-butyl alcohol, isoamyl alcohol, and 2-ethylhexyl alcohol. Ethylene glycol as a polyhydric alcohol,
Examples include propylene glycol and glycerin. Ethers have the general formula R 1 −(OR 2 ) o −OR 3
(R 1 , R 2 , R 3 = alkyl/allyl, aralkyl group, n = an integer of 0-5), and examples include ethyl ether, isopropyl alcohol, ethylene glycol, and dimethyl ether. The esters are represented by the general formula R 1 COOR 2 (R 1 , R 2 = alkyl, allyl, aralkyl group), and examples include methyl acetate and ethyl acetate. Ketones have the general formula R 1 CO (R 2 CO) o R 3 (R 1 , R 2 ,
R 3 = alkyl/allyl/aralkyl group, n=0
-5 integer), and examples include acetone, methyl, ethyl ketone, and acetylacetone. These exemplified organic solvents may be used alone or in the form of various mixtures, and in the case of a mixture, it is sufficient as long as phase separation does not occur. In the method of the present invention, the concentration of low molecular weight polyolefin in the waste solvent concentrated by passing through the ultrafiltration membrane becomes significantly high. In other words, the waste solvent with a concentration of about 1% of low molecular weight polyolefin is
The rate increases to 5-10% depending on the condition, and increases to about 60% by repeating the condition. Therefore, most of the solvent in the waste solvent is separated by the filtration according to the present invention. Therefore, when separating or recovering low molecular weight polyolefin from concentrated waste solvent,
Even if conventional steam distillation methods, solvent replacement methods, and centrifugal thin membranes are used, the thermal energy of steam and the like can be significantly reduced. The separation method of the present invention is a medium-low pressure method,
By directly linking to the manufacturing process of high density to low density polyethylene or polypropylene, the manufacturing cost of the polyolefin can be significantly reduced. By applying the separation method of the present invention to the polypropylene production process proposed in Japanese Patent Application No. 55-107487 (particularly a copolymer production process with a significantly high production rate of hydrocarbon-insoluble polymers), the present inventor has achieved polymerization without purifying the polymerization solvent. A complete circulation process of polymerization solvent recycled to the process can be completed. Examples are shown below. Examples 1 to 23 The indicated waste solvent was continuously fed under the indicated conditions to a device in which the indicated ultrafiltration membrane was modularized, and was separated into the permeated solution that had passed through the ultrafiltration membrane and the discharged waste solvent. . The discharged waste solvent was continuously recycled into the module. Finally, the fed waste solvent was separated into a permeate solvent and a discharged concentrated solvent. To explain Example-1, polymer concentration
1.2% by weight of the charged waste solvent was passed through the ultrafiltration membrane module, with the permeate solvent having a significantly lower polymer concentration (0.04% by weight) and the permeate solvent having a significantly higher polymer concentration (11.0% by weight).
% by weight) was separated into discharge concentrated waste solvent. Therefore, the concentration rate of the solvent is 100 x {1-100-11/11 x 1.2/100-1.2} = 99.1%. On the other hand, when comparing the pre-concentration operation, which is a preliminary step in the conventional centrifugal thin film evaporation method, with the conventional method using steam heating, the method using the ultrafiltration membrane of the present invention has the advantage of pressurizing the waste solvent and powering the circulation pump. Since only a small amount of electricity is required, this is a significant reduction in energy consumption compared to conventional methods. An explanation of the table is given below. 1 Ultrafiltration membrane Polyimide system - manufactured by Nitto Denko Corporation NTU-4200 series Polyamide system - manufactured by Berghof Company Polyvinylidene fluoride system - manufactured by Pennwalt Company KYNAR Polytetrafluoroethylene system - manufactured by Sumitomo Electric Industries, Ltd. Pomaflon Polysulfone system - manufactured by UCC Company Ltd. P-1700 2 Types of polymers in waste solvent *1) Propylene ethylene random copolymer A low molecular weight, low crystalline copolymer produced as a by-product during the production of propylene ethylene random copolymer (ethylene content 2.0 to 5.5% by weight). *2) Propylene ethylene block copolymer (ethylene content: 8-19% by weight) A low-molecular-weight, low-crystalline copolymer produced as a by-product during production. 3 Polymer concentration This was determined by evaporating the solvent of the sample to dryness and calculating from the remaining amount. 4 Average molecular weight Water associaton GelPermeation
Obtained by chromatography. 5 Operating conditions Pressure - Average value of pressure at module inlet and outlet Temperature - Temperature of charged waste solvent 6 Permeation rate Amount of permeated waste solution per hour per 1 m 2 of ultrafiltration membrane ( ) 7 Molecular weight of monodisperse polyethylene glycol Delpermeation by passing 0.5% toluene solution through an ultrafiltration membrane
Molecular weight to obtain 95% solute removal rate using chromatography.
【表】【table】
Claims (1)
量ポリオレフインを含む廃溶媒を、加圧して限外
過膜を通して過することにより、濃縮させる
ことを特徴とする低分子量ポリオレフインを含む
廃溶媒から有機溶媒を分離する方法。 ２ 濃縮された廃溶媒を更に限外過膜を通して
過をくりかえし更に濃縮させる特許請求の範囲
第１項記載の方法。 ３ 濃縮された廃溶媒に水蒸気を吹き込み低分子
量ポリオレフインを分離させる特許請求の範囲第
１もしくは第２項記載の方法。 ４ 濃縮された廃溶媒中の溶媒を低分子量ポリオ
レフインの融点以上の沸点をもつ溶媒と置換して
低分子量ポリオレフインを分離させる特許請求の
範囲第１項もしくは第２項記載の方法。 ５ 濃縮された廃溶媒を低分子量ポリオレフイン
の融点以上の温度で加圧し遠心薄膜蒸発器へフラ
ツシユさせ低分子量ポリオレフインを分離させる
特許請求の範囲第１項もしくは第２項記載の方
法。[Scope of Claims] 1. A waste solvent containing a low molecular weight polyolefin obtained in a polyolefin manufacturing process, which is concentrated by passing it through an ultrafiltration membrane under pressure. A method of separating organic solvents from. 2. The method according to claim 1, wherein the concentrated waste solvent is further concentrated by repeatedly passing it through an ultrafiltration membrane. 3. The method according to claim 1 or 2, wherein the low molecular weight polyolefin is separated by blowing steam into the concentrated waste solvent. 4. The method according to claim 1 or 2, wherein the solvent in the concentrated waste solvent is replaced with a solvent having a boiling point higher than the melting point of the low molecular weight polyolefin to separate the low molecular weight polyolefin. 5. The method according to claim 1 or 2, wherein the concentrated waste solvent is pressurized at a temperature higher than the melting point of the low molecular weight polyolefin and flashed to a centrifugal thin film evaporator to separate the low molecular weight polyolefin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14137781A JPS5842605A (en) | 1981-09-08 | 1981-09-08 | Separation of organic solvent from waste solvent containing low-molecular weight polyolefin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14137781A JPS5842605A (en) | 1981-09-08 | 1981-09-08 | Separation of organic solvent from waste solvent containing low-molecular weight polyolefin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5842605A JPS5842605A (en) | 1983-03-12 |
| JPH0332565B2 true JPH0332565B2 (en) | 1991-05-13 |
Family
ID=15290576
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14137781A Granted JPS5842605A (en) | 1981-09-08 | 1981-09-08 | Separation of organic solvent from waste solvent containing low-molecular weight polyolefin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5842605A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6044540B2 (en) * | 1978-11-08 | 1985-10-04 | ダイキン工業株式会社 | DC operated solenoid valve |
| US4606903A (en) * | 1984-04-27 | 1986-08-19 | Exxon Research And Engineering Co. | Membrane separation of uncoverted carbon fiber precursors from flux solvent and/or anti-solvent |
| JPS60243105A (en) * | 1984-05-17 | 1985-12-03 | Osaka Soda Co Ltd | Preparation of diallyl phthalate based polymer |
| JPH0735409B2 (en) * | 1986-02-03 | 1995-04-19 | 三井東圧化学株式会社 | How to remove volatile substances |
-
1981
- 1981-09-08 JP JP14137781A patent/JPS5842605A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5842605A (en) | 1983-03-12 |
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