TW202039404A - 有機溶劑的製造方法 - Google Patents
有機溶劑的製造方法 Download PDFInfo
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- TW202039404A TW202039404A TW109106862A TW109106862A TW202039404A TW 202039404 A TW202039404 A TW 202039404A TW 109106862 A TW109106862 A TW 109106862A TW 109106862 A TW109106862 A TW 109106862A TW 202039404 A TW202039404 A TW 202039404A
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- 239000003960 organic solvent Substances 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 69
- 239000002184 metal Substances 0.000 claims abstract description 69
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 48
- 239000000835 fiber Substances 0.000 claims abstract description 39
- 229920000098 polyolefin Polymers 0.000 claims abstract description 32
- 238000001179 sorption measurement Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical group OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 125000003277 amino group Chemical group 0.000 claims abstract description 9
- SFZULDYEOVSIKM-UHFFFAOYSA-N chembl321317 Chemical group C1=CC(C(=N)NO)=CC=C1C1=CC=C(C=2C=CC(=CC=2)C(=N)NO)O1 SFZULDYEOVSIKM-UHFFFAOYSA-N 0.000 claims abstract description 9
- OUDSFQBUEBFSPS-UHFFFAOYSA-N ethylenediaminetriacetic acid Chemical group OC(=O)CNCCN(CC(O)=O)CC(O)=O OUDSFQBUEBFSPS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 150000002739 metals Chemical class 0.000 claims abstract description 6
- 239000004744 fabric Substances 0.000 claims description 27
- -1 imino diacetoxy groups Chemical group 0.000 claims description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 125000000542 sulfonic acid group Chemical group 0.000 claims description 9
- OBSLWIKITOYASJ-YDEIVXIUSA-N (3r,4r,5s,6r)-6-(hydroxymethyl)-3-(methylamino)oxane-2,4,5-triol Chemical group CN[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O OBSLWIKITOYASJ-YDEIVXIUSA-N 0.000 claims description 8
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 8
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 claims description 8
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical group COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 6
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 125000002843 carboxylic acid group Chemical group 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- JOLQKTGDSGKSKJ-UHFFFAOYSA-N 1-ethoxypropan-2-ol Chemical compound CCOCC(C)O JOLQKTGDSGKSKJ-UHFFFAOYSA-N 0.000 claims description 5
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- MRABAEUHTLLEML-UHFFFAOYSA-N Butyl lactate Chemical compound CCCCOC(=O)C(C)O MRABAEUHTLLEML-UHFFFAOYSA-N 0.000 claims description 4
- 239000001191 butyl (2R)-2-hydroxypropanoate Substances 0.000 claims description 4
- 229940116333 ethyl lactate Drugs 0.000 claims description 4
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- 239000000463 material Substances 0.000 claims description 3
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- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical group OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 abstract description 5
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- MBBZMMPHUWSWHV-BDVNFPICSA-N N-methylglucamine Chemical group CNC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO MBBZMMPHUWSWHV-BDVNFPICSA-N 0.000 abstract 1
- 150000007942 carboxylates Chemical group 0.000 abstract 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 abstract 1
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
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- 229910052799 carbon Inorganic materials 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- CGZZMOTZOONQIA-UHFFFAOYSA-N cycloheptanone Chemical compound O=C1CCCCCC1 CGZZMOTZOONQIA-UHFFFAOYSA-N 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
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- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- GFUIDHWFLMPAGY-UHFFFAOYSA-N ethyl 2-hydroxy-2-methylpropanoate Chemical compound CCOC(=O)C(C)(C)O GFUIDHWFLMPAGY-UHFFFAOYSA-N 0.000 description 1
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- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
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- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
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- B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
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- B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
- B01D39/163—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin sintered or bonded
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- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
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- B01D25/02—Filters formed by clamping together several filtering elements or parts of such elements in which the elements are pre-formed independent filtering units, e.g. modular systems
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D29/11—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with bag, cage, hose, tube, sleeve or like filtering elements
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
- B01D35/02—Filters adapted for location in special places, e.g. pipe-lines, pumps, stop-cocks
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B63/00—Purification; Separation; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/36—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C43/00—Ethers; Compounds having groups, groups or groups
- C07C43/02—Ethers
- C07C43/03—Ethers having all ether-oxygen atoms bound to acyclic carbon atoms
- C07C43/04—Saturated ethers
- C07C43/13—Saturated ethers containing hydroxy or O-metal groups
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/66—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety
- C07C69/67—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of saturated acids
- C07C69/708—Ethers
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- G—PHYSICS
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- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
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- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
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Abstract
本發明為提供一種在半導體裝置製造之微影步驟,減低成為晶圓上之微小缺陷的原因之金屬雜質的有機溶劑的製造方法,或被純化有機溶劑的金屬減低方法。
本發明為一種有機溶劑的製造方法,其係包含通液在過濾器濾芯之步驟之有機溶劑的製造方法,前述過濾器濾芯的特徵為將複數種類之過濾用基布層合或纏繞在中空狀內筒之過濾器濾芯,
前述過濾用基布係於聚烯烴纖維化學鍵結金屬吸附基之不織布,
前述過濾用基布包含不織布層A及不織布層B,
前述不織布層A係以化學鍵結磺酸基作為金屬吸附基的聚烯烴纖維構成,
前述不織布層B係以化學鍵結選自由胺基、N-甲基-D-葡萄糖胺基、亞胺基二乙酸基、亞胺基二乙醇基、醯胺肟基、磷酸基、羧酸基及乙二胺三乙酸基所成之群組中之至少一種作為金屬吸附基的聚烯烴纖維構成。
Description
本發明係關於在半導體裝置製造之微影步驟,減低成為缺陷的原因之金屬雜質的有機溶劑的製造方法。
在半導體裝置製造之微影步驟中所使用之有機溶劑,尋求有成為晶圓上之微小缺陷(例如1~100nm左右,被稱為瑕疵(Defect)等)之原因的金屬雜質的減低。專利文獻1中揭示有金屬之吸附去除效率高的過濾器。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開2018-167223號公報
[發明欲解決之課題]
本發明為提供一種在半導體裝置製造之微影步驟,減低成為晶圓上之微小缺陷的原因之金屬雜質的有機溶劑的製造方法及有機溶劑的金屬減低方法。
[用以解決課題之手段]
本發明係包含以下。
[1] 一種有機溶劑的製造方法,其係包含通液在金屬去除用過濾器濾芯之步驟之有機溶劑的製造方法,前述金屬去除用過濾器濾芯的特徵為將複數種類之過濾用基布層合或纏繞在中空狀內筒之過濾器濾芯,
前述過濾用基布係於聚烯烴纖維化學鍵結金屬吸附基之不織布,
前述過濾用基布包含不織布層A及不織布層B,
前述不織布層A係以化學鍵結磺酸基作為金屬吸附基的聚烯烴纖維構成,
前述不織布層B係以化學鍵結選自由胺基、N-甲基-D-葡萄糖胺基、亞胺基二乙酸基、亞胺基二乙醇基、醯胺肟基、磷酸基、羧酸基及乙二胺三乙酸基所成之群組中之至少一種作為金屬吸附基的聚烯烴纖維構成。
[2] 如[1]所記載之有機溶劑的製造方法,其係進一步包含通液在微粒子去除用過濾器濾芯之步驟。
[3] 如[2]所記載之有機溶劑的製造方法,其中,上述微粒子去除用過濾器的材質係選自由聚乙烯及尼龍所成之群組中之至少一種。
[4] 如[1]~[3]中任一項所記載之有機溶劑的製造方法,其中,上述有機溶劑係作為阻劑下層膜形成用使用之有機溶劑。
[5] 如[4]所記載之有機溶劑的製造方法,其中,上述有機溶劑為選自由丙二醇單甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚、γ-丁內酯、乳酸乙酯、乳酸丁酯及環己酮所成之群組中之至少一種。
[6] 一種被純化有機溶劑的金屬減低方法,其係將被純化有機溶劑通液在金屬去除用濾芯過濾器,減低金屬之方法,前述過濾器濾芯的特徵為將複數種類之過濾用基布層合或纏繞在中空狀內筒,
前述過濾用基布係於聚烯烴纖維化學鍵結金屬吸附基之不織布,
前述過濾用基布包含不織布層A及不織布層B,
前述不織布層A係以化學鍵結磺酸基作為金屬吸附基的聚烯烴纖維構成,
前述不織布層B係以化學鍵結選自由胺基、N-甲基-D-葡萄糖胺基、亞胺基二乙酸基、亞胺基二乙醇基、醯胺肟基、磷酸基、羧酸基及乙二胺三乙酸基所成之群組中之至少一種作為金屬吸附基的聚烯烴纖維構成。
[發明效果]
藉由使用本發明所記載之過濾器濾芯,進行有機溶劑的製造,可製造大幅減低金屬雜質之有機溶劑。藉由使用該有機溶劑,可減低在半導體製造步驟之微影步驟中的各種微小缺陷(瑕疵(Defect))。
<有機溶劑的製造方法>
本發明之有機溶劑的製造方法,係包含將於常溫為溶液狀之被純化有機溶劑通液在下述所詳述之金屬去除用過濾器濾芯之步驟。
上述通液步驟可藉由例如可將被純化有機溶劑作為市售品取得,通液在與使用該有機溶劑之製造設備(製造用容器)直接聯結(入口與出口之2處)之金屬去除用過濾器濾芯來進行。上述通液步驟可為1次或2次以上。上述通液步驟較佳為使用泵之循環過濾。較佳為除了本案的金屬去除用過濾器濾芯之外,並於以直列連結之微粒子去除用過濾器濾芯雙方通液有機溶劑使其循環。循環所需要的時間例如為3~144小時。過濾流量例如為1~1000L/小時。
<被純化有機溶劑>
於本案使用之被純化有機溶劑,雖推薦例如於下述所記載之微影步驟一般所使用之有機溶劑,但並非被限定於此等。
作為前述被純化有機溶劑,例如可列舉乙二醇單甲基醚、乙二醇單乙基醚、甲基溶纖劑乙酸酯、乙基溶纖劑乙酸酯、二乙二醇單甲基醚、二乙二醇單乙基醚、丙二醇、丙二醇單甲基醚、丙二醇單乙基醚、丙二醇單甲基醚乙酸酯、丙二醇丙基醚乙酸酯、甲苯、二甲苯、甲基乙基酮、甲基異丁基酮、環戊酮、環己酮、環庚酮、4-甲基-2-戊醇、2-羥基異丁酸甲酯、2-羥基異丁酸乙酯、乙氧基乙酸乙酯、乙酸2-羥基乙基、3-甲氧基丙酸甲酯、3-甲氧基丙酸乙酯、3-乙氧基丙酸乙酯、3-乙氧基丙酸甲酯、丙酮酸甲酯、丙酮酸乙酯、乙酸乙酯、乙酸丁酯、乳酸乙酯、乳酸丁酯、2-庚酮、甲氧基環戊烷、苯甲醚、γ-丁內酯、N-甲基吡咯烷酮、N,N-二甲基甲醯胺及N,N-二甲基乙醯胺。此等之溶劑可單獨或組合2種以上使用。
此等之溶劑當中,較佳為丙二醇單甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚、γ-丁內酯、乳酸乙酯、乳酸丁酯及環己酮等。特佳為丙二醇單甲基醚、丙二醇單甲基醚乙酸酯及丙二醇單乙基醚。
<過濾器濾芯>
作為本案之過濾器濾芯,較佳為日本特開2018-167223號公報所記載者。
本發明之過濾器濾芯,其係將複數種類之過濾用基布層合或纏繞在中空狀內筒之過濾器濾芯,其特徵為前述過濾用基布係於聚烯烴纖維化學鍵結金屬吸附基之不織布,前述過濾用基布包含不織布層A及不織布層B,前述不織布層A係以化學鍵結磺酸基作為金屬吸附基的聚烯烴纖維構成,前述不織布層B係以化學鍵結選自由胺基、N-甲基-D-葡萄糖胺基、亞胺基二乙酸基(亞胺基二乙酸基)、亞胺基二乙醇基、醯胺肟基、磷酸基、羧酸基及乙二胺三乙酸基所成之群組中之至少一種作為金屬吸附基的聚烯烴纖維構成。
本發明,其係將複數種類之過濾用基布層合或纏繞在中空狀內筒之過濾器濾芯,前述過濾用基布係於聚烯烴纖維化學鍵結金屬吸附基之不織布,前述過濾用基布包含不織布層A及不織布層B。而且,前述不織布層A係以化學鍵結碸基作為金屬吸附基的聚烯烴纖維構成,前述不織布層B係以化學鍵結選自由胺基、N-甲基-D-葡萄糖胺基、亞胺基二乙酸基(亞胺基二乙酸基)、亞胺基二乙醇基、醯胺肟基、磷酸基、羧酸基及乙二胺三乙酸基所成之群組中之至少一種作為金屬吸附基的聚烯烴纖維構成。藉此可效率良好地去除金屬。尚,結合不同種類之過濾用基布,成為1枚之過濾用基布者,亦包含在複數種類之過濾用基布。
在本發明,特佳為不織布層B係以化學鍵結亞胺基二乙醇基的聚烯烴纖維構成。係因為金屬之去除效率高。針對可吸附之金屬,磺酸基主要是吸附Na、Cu、K,亞胺基二乙醇基主要是吸附Cr、Al、Fe。
構成不織布A及B之聚烯烴纖維較佳為長纖維。這是因為長纖維不織布難以產生纖維屑,過濾器性能高。其中較佳為,每一面積的質量(每單位面積重量)為10~100g/m2
之熔噴(Meltblown)長纖維不織布。
構成前述不織布A及B之聚烯烴纖維的單纖維平均直徑較佳為0.2~10μm。若為前述的範圍,期待過濾器性能高。此外,由於可增大表面積(比表面積),亦增加接枝聚合反應的基材表面,故亦可期待提高接枝率。
聚烯烴纖維較佳為選自由聚丙烯、丙烯與乙烯之共聚物、聚乙烯及乙烯與碳數4以上之其他α-烯烴的共聚物所成之群組中之至少一種,特佳為高密度聚乙烯。此等之聚合物為惰性,對藥液安定,可以接枝聚合。
前述過濾器濾芯較佳為包含中空狀內筒及過濾用基布之過濾器濾芯,前述過濾用基布係於聚烯烴纖維化學鍵結金屬吸附基之不織布,前述過濾用基布係藉由纏繞在前述中空狀內筒,而形成層合構造而成之過濾器濾芯。
本發明之過濾器係組裝前述過濾器濾芯之過濾器。例如過濾器濾芯係於內筒纏繞過濾用基布,並收納在容器。將過濾器濾芯組裝在過濾器的容器時,例如以於容器收納過濾器濾芯的狀態組裝在過濾器。尚,為濾芯型過濾器時,藉由僅交換過濾器濾芯,可再生過濾器機能。如交換每個過濾器的容器般,例如如膠囊型過濾器的情況亦包含在本發明。如膠囊型過濾器的情況,相當於過濾器濾芯的部分成為過濾部。
其次,說明於聚烯烴纖維化學鍵結各種官能基之方法。作為該方法,例如有於聚烯烴纖維照射電子束、γ線等之放射線後,與包含GMA等之反應性單體的乳膠液接觸之方法、使聚烯烴纖維與包含反應性單體的乳膠液接觸後,照射電子束、γ線等之放射線,並使反應性單體接枝聚合在聚烯烴纖維之方法等。照射電子束時,若達成通常為1~200kGy,較佳為5~100kGy,更佳為10~50kGy的照射量即可。照射較佳為於氮環境下進行。作為電子束照射裝置,可使用市售者,例如可使用EC250/15/180L(岩崎電氣(股)公司製)、EC300/165/800(岩崎電氣(股)公司製)、EPS300((股)NHVCorporation製)等作為區域光束(Area beam)型電子束照射裝置。
作為前述接枝聚合法,具體而言,例如可列舉液相接枝聚合法,將不織布藉由γ線或電子束等之放射線照射活性化後,浸漬在包含水、界面活性劑及反應性單體的乳膠,並於前述之不織布基材完成接枝聚合。其次,於前述基材所形成之接枝鏈,導入磺酸基、胺基、N-甲基-D-葡萄糖胺基或亞胺基二乙酸基(亞胺基二乙酸基)、亞胺基二乙醇基、醯胺肟基、磷酸基、羧酸基、乙二胺三乙酸基等之機能性官能基,亦即離子交換基及/或螯合基。在本發明,特別是並未限定在液相接枝聚合法,亦可使用於單體之蒸氣接觸基材,進行聚合之氣相接枝聚合法、將基材浸漬在單體溶液後,從單體溶液取出,並於氣相中進行反應之含浸氣相接枝聚合法等。作為代表性機能性官能基之化學式,於(化1)表示磺酸基(SC基),於(化2)表示亞胺基二乙醇基(IDE基),於(化3)表示亞胺基二乙酸基(IDA基),於(化4)表示N-甲基-D-葡萄糖胺基(NMDG基)。
惟,在(化1)~(化3)之R為下述之聚乙烯(PE)+GMA(化5)或聚丙烯(PP)+GMA(化6)。在(化4)之R為甲基。
惟,在前述(化5)~(化6)之n、m為1以上之整數。
<微粒子去除用過濾器>
本發明之有機溶劑的製造方法,較佳為將上述被純化有機溶劑通液在上述過濾器濾芯後,進而通液微粒子去除用過濾器。微粒子去除用過濾器可使用本身公知者。作為微粒子去除用過濾器的材質,較佳為選自由聚乙烯及尼龍所成之群組中之至少一種。
微粒子去除用過濾器的孔徑通常為30nm以下,較佳為例如為0.1nm~30nm,例如為0.1nm~20nm,或例如為1nm~10nm。
<金屬減低方法>
本案之金屬減低方法,為一種被純化有機溶劑的金屬減低方法,其係將被純化有機溶劑通液在金屬去除用濾芯過濾器,減低金屬之方法,前述過濾器濾芯的特徵為將複數種類之過濾用基布層合或纏繞在中空狀內筒,
前述過濾用基布係於聚烯烴纖維化學鍵結金屬吸附基之不織布,
前述過濾用基布包含不織布層A及不織布層B,
前述不織布層A係以化學鍵結磺酸基作為金屬吸附基的聚烯烴纖維構成,
前述不織布層B係以化學鍵結選自由胺基、N-甲基-D-葡萄糖胺基、亞胺基二乙酸基、亞胺基二乙醇基、醯胺肟基、磷酸基、羧酸基及乙二胺三乙酸基所成之群組中之至少一種作為金屬吸附基的聚烯烴纖維構成。
藉由經由此步驟,可減低源自被純化有機溶劑所包含之原料或溶劑的金屬雜質,並減少於微影步驟之缺陷。
各種金屬雜質(例如Na、Cu、Cr、Al、Fe等)藉由上述金屬減低方法,可減低至例如0.5ppb以下、例如0.4ppb以下。
上述金屬雜質含量係以例如實施例所記載之方法求出。
[實施例]
於以下雖參照實施例等更加詳細說明本發明,但本發明並非因以下之實施例等而受到任何限制者。
<實施例1>
作為被純化有機溶劑,將丙二醇單甲基醚(PM-P:KH Neochem股份有限公司製)20L使用日本特開2018-167223所記載之濾芯過濾器(10inch)1個(倉敷纖維加工股份有限公司製),以每分鐘3L的流量實施100分鐘過濾。將過濾後之有機溶劑的金屬含量以ICP-MS(Agilent8800:Agilent Technologies股份有限公司製)測定。
<比較例1>
並未過濾實施例1所使用之被純化有機溶劑,而是以同樣的方法測定金屬含量。
<比較例2>
除了將實施例1之濾芯過濾器變更為濾芯過濾器(尼龍過濾器ABD1ANM3EH1(20nm尼龍過濾器):日本Pall股份有限公司製)之外,其他以與實施例1相同的方法實施過濾,並以同樣的方法測定金屬含量。
<比較例3>
除了將實施例1之濾芯過濾器變更為強酸性離子交換樹脂(XSC-1115-H:室町Chemicals股份有限公司製)20kg,進行4小時離子交換之外,其他以與實施例1相同的方法實施過濾,並以同樣的方法測定金屬含量。
<有機溶劑中的金屬濃度>
將測定實施實施例1之處理方法後的金屬濃度的結果示於表1。
由表1之結果,實施例1顯示有效果地減低金屬濃度。
<實施例2>
作為被純化有機溶劑,將丙二醇單甲基醚乙酸酯(EL-PGMEA:東洋合成工業股份有限公司製)20L使用日本特開2018-167223所記載之濾芯過濾器(10inch)1個(倉敷纖維加工股份有限公司製),以每分鐘2L的流量實施50分鐘過濾。將過濾後之有機溶劑的金屬含量以ICP-MS(Agilent8800:Agilent Technologies股份有限公司製)測定。
<比較例4>
並未過濾實施例1所使用之被純化有機溶劑,而是以同樣的方法測定金屬含量。
由表2之結果,實施例2顯示有效果地減低金屬濃度。
[產業上之可利用性]
根據本發明,可提供特別是減低金屬雜質的量之有機溶劑。
Claims (6)
- 一種有機溶劑的製造方法,其係包含通液在金屬去除用過濾器濾芯之步驟之有機溶劑的製造方法,前述金屬去除用過濾器濾芯的特徵為將複數種類之過濾用基布層合或纏繞在中空狀內筒之過濾器濾芯, 前述過濾用基布係於聚烯烴纖維化學鍵結金屬吸附基之不織布, 前述過濾用基布包含不織布層A及不織布層B, 前述不織布層A係以化學鍵結磺酸基作為金屬吸附基的聚烯烴纖維構成, 前述不織布層B係以化學鍵結選自由胺基、N-甲基-D-葡萄糖胺基、亞胺基二乙酸基、亞胺基二乙醇基、醯胺肟基、磷酸基、羧酸基及乙二胺三乙酸基所成之群組中之至少一種作為金屬吸附基的聚烯烴纖維構成。
- 如請求項1所記載之有機溶劑的製造方法,其係進一步包含通液在微粒子去除用過濾器濾芯之步驟。
- 如請求項2所記載之有機溶劑的製造方法,其中,上述微粒子去除用過濾器的材質係選自由聚乙烯及尼龍所成之群組中之至少一種。
- 如請求項1~3中任一項所記載之有機溶劑的製造方法,其中,上述有機溶劑係作為阻劑下層膜形成用使用之有機溶劑。
- 如請求項4所記載之有機溶劑的製造方法,其中,上述有機溶劑為選自由丙二醇單甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚、γ-丁內酯、乳酸乙酯、乳酸丁酯及環己酮所成之群組中之至少一種。
- 一種被純化有機溶劑的金屬減低方法,其係將被純化有機溶劑通液在金屬去除用濾芯過濾器,減低金屬之方法,前述過濾器濾芯的特徵為將複數種類之過濾用基布層合或纏繞在中空狀內筒, 前述過濾用基布係於聚烯烴纖維化學鍵結金屬吸附基之不織布, 前述過濾用基布包含不織布層A及不織布層B, 前述不織布層A係以化學鍵結磺酸基作為金屬吸附基的聚烯烴纖維構成, 前述不織布層B係以化學鍵結選自由胺基、N-甲基-D-葡萄糖胺基、亞胺基二乙酸基、亞胺基二乙醇基、醯胺肟基、磷酸基、羧酸基及乙二胺三乙酸基所成之群組中之至少一種作為金屬吸附基的聚烯烴纖維構成。
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