JP6458964B2 - Azeotropic cleaning agent and its regeneration method, cleaning method, and cleaning agent kit - Google Patents
Azeotropic cleaning agent and its regeneration method, cleaning method, and cleaning agent kit Download PDFInfo
- Publication number
- JP6458964B2 JP6458964B2 JP2017184329A JP2017184329A JP6458964B2 JP 6458964 B2 JP6458964 B2 JP 6458964B2 JP 2017184329 A JP2017184329 A JP 2017184329A JP 2017184329 A JP2017184329 A JP 2017184329A JP 6458964 B2 JP6458964 B2 JP 6458964B2
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- Prior art keywords
- azeotropic
- cleaning agent
- group
- cleaning
- carbon atoms
- Prior art date
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- 238000004140 cleaning Methods 0.000 title claims description 55
- 238000000034 method Methods 0.000 title claims description 23
- 238000011069 regeneration method Methods 0.000 title description 17
- 239000000203 mixture Substances 0.000 claims description 40
- 239000007788 liquid Substances 0.000 claims description 35
- 125000000217 alkyl group Chemical group 0.000 claims description 34
- 125000004432 carbon atom Chemical group C* 0.000 claims description 34
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 33
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- 239000003795 chemical substances by application Substances 0.000 claims description 23
- 239000000356 contaminant Substances 0.000 claims description 23
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 22
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 18
- 239000002738 chelating agent Substances 0.000 claims description 15
- 239000003921 oil Substances 0.000 claims description 15
- 239000003960 organic solvent Substances 0.000 claims description 13
- 150000001412 amines Chemical class 0.000 claims description 9
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 9
- 238000005476 soldering Methods 0.000 claims description 9
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 7
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- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 1
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 125000003538 pentan-3-yl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])C([H])([H])[H] 0.000 description 1
- GPCKFIWBUTWTDH-UHFFFAOYSA-N pentane-3,3-diamine Chemical compound CCC(N)(N)CC GPCKFIWBUTWTDH-UHFFFAOYSA-N 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- RGCLLPNLLBQHPF-HJWRWDBZSA-N phosphamidon Chemical compound CCN(CC)C(=O)C(\Cl)=C(/C)OP(=O)(OC)OC RGCLLPNLLBQHPF-HJWRWDBZSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 229920006350 polyacrylonitrile resin Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- CBPYOHALYYGNOE-UHFFFAOYSA-M potassium;3,5-dinitrobenzoate Chemical compound [K+].[O-]C(=O)C1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1 CBPYOHALYYGNOE-UHFFFAOYSA-M 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 150000003139 primary aliphatic amines Chemical class 0.000 description 1
- ZNZJJSYHZBXQSM-UHFFFAOYSA-N propane-2,2-diamine Chemical compound CC(C)(N)N ZNZJJSYHZBXQSM-UHFFFAOYSA-N 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002265 redox agent Substances 0.000 description 1
- 239000008237 rinsing water Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000002455 scale inhibitor Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 125000003548 sec-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000008234 soft water Substances 0.000 description 1
- 229940037312 stearamide Drugs 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229940095068 tetradecene Drugs 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229910001174 tin-lead alloy Inorganic materials 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
- 229940048102 triphosphoric acid Drugs 0.000 description 1
- JZNDMMGBXUYFNQ-UHFFFAOYSA-N tris(dodecylsulfanyl)phosphane Chemical compound CCCCCCCCCCCCSP(SCCCCCCCCCCCC)SCCCCCCCCCCCC JZNDMMGBXUYFNQ-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/263—Ethers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/10—Salts
- C11D7/12—Carbonates bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/265—Carboxylic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3227—Ethers thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5022—Organic solvents containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
- Cleaning By Liquid Or Steam (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Manufacturing Of Printed Wiring (AREA)
Description
本開示は、共沸洗浄剤及びその再生方法、洗浄方法、並びに洗浄剤キットに関する。 The present disclosure relates to an azeotropic cleaning agent, a regeneration method thereof, a cleaning method, and a cleaning agent kit.
ソルダペーストやヤニ入りはんだ等を用いてプリント配線基板の電極に電子部品を接合すると、フラックスが不可避的に生じるため、これを除去するべく、斯界では種々の洗浄剤が使用されている。 When an electronic component is joined to an electrode of a printed wiring board using solder paste, solder containing solder, or the like, flux is inevitably generated. Therefore, various cleaning agents are used in this field in order to remove the flux.
フラックス除去用洗浄剤としては、かつてはフロン系の洗浄剤が主流であったが、環境への悪影響が考慮された結果、近年では非フロン系の洗浄剤として例えば炭化水素系洗浄剤やグリコール系洗浄剤等が使用されている。 As a cleaning agent for removing flux, once a chlorofluorocarbon-based cleaning agent has been the mainstream. However, as a result of considering adverse environmental impacts, non-fluorocarbon-based cleaning agents such as hydrocarbon-based cleaning agents and glycol-based cleaning agents have recently been used. A cleaning agent is used.
非フロン系の洗浄剤のうちグリコール系洗浄剤は、各種グリコール系化合物と水とから構成されており、フラックスやイオン残渣の除去性に優れるだけでなく非危険物である点で炭化水素系洗浄剤に勝る(特許文献1〜3)。 Among non-fluorocarbon cleaners, glycol cleaners are composed of various glycol compounds and water, and are not only excellent in the removal of flux and ion residues, but are also non-hazardous hydrocarbon cleaners. Superior to agents (Patent Documents 1 to 3).
特定の炭化水素系溶剤の組み合わせからなる炭化水素系洗浄剤については、洗浄、及び濯ぎ(リンス)に使用した廃液を再生利用する目的でその共沸組成を限定し、蒸留再生を可能とする技術が幾つか提案されている(特許文献4〜6)。 For hydrocarbon cleaners consisting of a combination of specific hydrocarbon solvents, a technology that enables distillation regeneration by limiting the azeotropic composition for the purpose of recycling the waste liquid used for cleaning and rinsing. Have been proposed (Patent Documents 4 to 6).
グリコール系洗浄剤を用いると、洗浄の度にフラックス等の汚れを含む洗浄剤廃液や、洗浄剤をすすぐ(リンス)際に用いるリンス剤を含むリンス剤廃液(廃水等)が大量に生じてしまい、その処理のために相応の設備と費用が必要となる。そのため、洗浄の際に生じる洗浄剤廃液及び排水の量を削減することが求められていた。 When using a glycol-based cleaning agent, a large amount of cleaning agent waste fluid containing dirt such as flux and rinse agent waste fluid (rinsing water etc.) containing a rinsing agent used when rinsing the cleaning agent is rinsed. Therefore, appropriate equipment and cost are required for the processing. Therefore, it has been demanded to reduce the amount of cleaning agent waste liquid and waste water generated during cleaning.
本開示により解決される主たる課題は、グリコール系溶剤を含み、かつ再生利用可能である共沸洗浄剤、その再生方法及び洗浄方法を提供することである。 A main problem to be solved by the present disclosure is to provide an azeotropic cleaning agent that contains a glycol solvent and is recyclable, a regeneration method thereof, and a cleaning method.
本発明者らは鋭意検討の結果、特定のグリコールエーテルと水からなる洗浄剤の組成を共沸組成に限定することによって、蒸留再生が可能であり、尚且つ乾燥容易な共沸洗浄剤が得られることを見出した。 As a result of intensive studies, the inventors of the present invention obtained an azeotropic cleaning agent that can be regenerated by distillation and that can be easily dried by limiting the composition of a specific glycol ether and water to an azeotropic composition. I found out that
本開示により以下の項目が提供される。
(項目1)一般式(1):R−O−CH2−CHX−O−H
(式中、Xが水素原子を表すとき、Rは、メチル基、エチル基、n−プロピル基、iso−プロピル基、iso−ブチル基、sec−ブチル基、及びtert−ブチル基からなる群から選択される基を表し、
Xがメチル基を表すとき、Rは、メチル基、エチル基、n−プロピル基、iso−プロピル基、n−ブチル基、iso−ブチル基、sec−ブチル基、及びtert−ブチル基からなる群から選択される基を表す。)で表されるグリコールエーテル及び水を含む共沸混合物を含む、共沸洗浄剤。
(項目2)前記グリコールエーテルと水とからなる共沸混合物を含む、上記項目に記載の共沸洗浄剤。
(項目3)前記グリコールエーテルと
一般式(2):R1R2N−(CH2)n−NR3R4
(式中、R1〜R4はそれぞれ独立に炭素数1〜4のアルキル基を表し、nは1〜6の整数である)
で表されるジアミンと
水とからなる共沸混合物を含む、上記項目に記載の共沸洗浄剤。
(項目4)前記共沸洗浄剤が界面活性剤を含まない、上記項目のいずれか1項に記載の共沸洗浄剤。
(項目5)前記共沸洗浄剤が前記共沸混合物のみを含む、上記項目のいずれか1項に記載の共沸洗浄剤。
(項目6)前記共沸洗浄剤が曇点を有さない、上記項目のいずれか1項に記載の共沸洗浄剤。
(項目7)前記共沸洗浄剤がリンス剤である、上記項目のいずれか1項に記載の共沸洗浄剤。
(項目8)前記リンス剤がフラックス洗浄液用である、上記項目に記載の共沸洗浄剤。
(項目9)上記項目のいずれか1項に記載の共沸洗浄剤を含む液を蒸留し、前記共沸混合物を得る工程を含む、共沸洗浄剤の再生方法。
(項目10)上記項目のいずれか1項に記載の共沸洗浄剤を物品に付着している洗浄剤及び/又は汚染物質と接触させる工程を含むが、前記物品に付着している洗浄剤は、上記項目のいずれか1項に記載の共沸洗浄剤ではない、洗浄方法。
(項目11)一般式(A):RA1−O−(CH2−CHRA2−O)a−RA3
(式中、RA1は炭素数1〜6のアルキル基又はベンジル基を表し、RA2はメチル基又は水素原子を表し、RA3は炭素数1〜5のアルキル基又は水素原子を表し、aは2〜4の整数を表す。)
で表される有機溶剤(A)、
一般式(B):
で表されるアミン(B)、
及びアミノ基非含有キレート剤(C)を含む非共沸洗浄剤を
物品に付着している汚染物質と接触させる工程、並びに
上記項目のいずれか1項に記載の共沸洗浄剤を物品に付着している前記非共沸洗浄剤及び/又は汚染物質と接触させる工程を含む、上記項目に記載の洗浄方法。
(項目12)前記汚染物質がハンダ付け用フラックス、ソルダペースト、及び工業油からなる群の少なくとも1つを含む、上記項目のいずれか1項に記載の洗浄方法。
(項目13)
一般式(A):RA1−O−(CH2−CHRA2−O)a−RA3
(式中、RA1は炭素数1〜6のアルキル基又はベンジル基を表し、RA2はメチル基又は水素原子を表し、RA3は炭素数1〜5のアルキル基又は水素原子を表し、aは2〜4の整数を表す。)
で表される有機溶剤(A)、
一般式(B):
で表されるアミン(B)、
及びアミノ基非含有キレート剤(C)を含む非共沸洗浄剤
並びに上記項目のいずれか1項に記載の共沸洗浄剤を含む、洗浄剤キット。
The present disclosure provides the following items.
(Item 1) General formula (1): R—O—CH 2 —CHX—O—H
(In the formula, when X represents a hydrogen atom, R is selected from the group consisting of a methyl group, an ethyl group, an n-propyl group, an iso-propyl group, an iso-butyl group, a sec-butyl group, and a tert-butyl group. Represents the selected group,
When X represents a methyl group, R is a group consisting of a methyl group, an ethyl group, an n-propyl group, an iso-propyl group, an n-butyl group, an iso-butyl group, a sec-butyl group, and a tert-butyl group. Represents a group selected from: An azeotropic cleaning agent comprising an azeotropic mixture containing glycol ether and water represented by:
(Item 2) The azeotropic cleaning agent according to the above item, comprising an azeotropic mixture of the glycol ether and water.
(Item 3) The glycol ether and the general formula (2): R 1 R 2 N— (CH 2 ) n —NR 3 R 4
(Wherein R 1 to R 4 each independently represents an alkyl group having 1 to 4 carbon atoms, and n is an integer of 1 to 6)
The azeotropic cleaning agent according to the above item, comprising an azeotropic mixture comprising a diamine represented by
(Item 4) The azeotropic cleaning agent according to any one of the above items, wherein the azeotropic cleaning agent does not contain a surfactant.
(Item 5) The azeotropic cleaning agent according to any one of the above items, wherein the azeotropic cleaning agent includes only the azeotropic mixture.
(Item 6) The azeotropic cleaning agent according to any one of the above items, wherein the azeotropic cleaning agent does not have a cloud point.
(Item 7) The azeotropic cleaning agent according to any one of the above items, wherein the azeotropic cleaning agent is a rinse agent.
(Item 8) The azeotropic cleaning agent according to the above item, wherein the rinse agent is for a flux cleaning solution.
(Item 9) A method for regenerating an azeotropic cleaning agent, comprising a step of distilling a liquid containing the azeotropic cleaning agent according to any one of the above items to obtain the azeotropic mixture.
(Item 10) The method includes a step of bringing the azeotropic cleaning agent according to any one of the above items into contact with a cleaning agent and / or a contaminant adhering to an article. A cleaning method that is not an azeotropic cleaning agent according to any one of the above items.
(Item 11) General Formula (A): R A1 —O— (CH 2 —CHR A2 —O) a —R A3
(In the formula, R A1 represents an alkyl group having 1 to 6 carbon atoms or a benzyl group, R A2 represents a methyl group or a hydrogen atom, R A3 represents an alkyl group having 1 to 5 carbon atoms or a hydrogen atom, and a Represents an integer of 2 to 4.)
An organic solvent (A) represented by
Formula (B):
An amine (B) represented by
And a step of bringing a non-azeotropic cleaning agent containing an amino group-free chelating agent (C) into contact with a contaminant attached to the article, and attaching the azeotropic cleaning agent according to any one of the above items to the article The cleaning method according to the above item, which comprises a step of contacting the non-azeotropic cleaning agent and / or contaminants.
(Item 12) The cleaning method according to any one of the above items, wherein the contaminant includes at least one of the group consisting of soldering flux, solder paste, and industrial oil.
(Item 13)
Formula (A): R A1 —O— (CH 2 —CHR A2 —O) a —R A3
(In the formula, R A1 represents an alkyl group having 1 to 6 carbon atoms or a benzyl group, R A2 represents a methyl group or a hydrogen atom, R A3 represents an alkyl group having 1 to 5 carbon atoms or a hydrogen atom, and a Represents an integer of 2 to 4.)
An organic solvent (A) represented by
Formula (B):
An amine (B) represented by
And a non-azeotropic cleaning agent containing the amino group-free chelating agent (C) and the azeotropic cleaning agent according to any one of the above items.
本実施形態に係る共沸洗浄剤は、洗浄後の廃液にフラックスや本実施形態に係る共沸洗浄剤以外の洗浄剤を含んでいたとしても、蒸留操作により再生されることができる。再生後の共沸洗浄剤は、使用前の共沸洗浄剤と比べても組成比や洗浄力が殆ど変化しない。その結果、共沸洗浄剤を再生利用できるため、洗浄の際に生じる洗浄剤廃液を低減させることができる。また本実施形態に係る共沸洗浄剤は容易に乾燥する。その結果、被洗浄物の表面に残らないことからリンス剤及びリンス剤使用後に生じるリンス剤廃液の量を低減させることが可能となる。さらに、本実施形態に係る共沸洗浄剤は、良好なリンス性及び良好な乾燥性を有することから、リンス剤としても用いることが可能である。加えて、本実施形態に係る共沸洗浄剤をリンス剤として用いる場合、洗浄剤によっては、単蒸留であっても、安定して共沸洗浄剤溶液が再生できる。 The azeotropic cleaning agent according to this embodiment can be regenerated by distillation operation even if the waste liquid after cleaning contains a flux or a cleaning agent other than the azeotropic cleaning agent according to this embodiment. The composition ratio and the cleaning power of the azeotropic cleaning agent after regeneration hardly change even when compared with the azeotropic cleaning agent before use. As a result, since the azeotropic cleaning agent can be recycled, it is possible to reduce the cleaning agent waste liquid generated during cleaning. Moreover, the azeotropic cleaning agent according to this embodiment is easily dried. As a result, since it does not remain on the surface of the object to be cleaned, it is possible to reduce the amount of the rinse agent and the rinse agent waste liquid generated after using the rinse agent. Furthermore, since the azeotropic cleaning agent according to this embodiment has good rinsing properties and good drying properties, it can also be used as a rinsing agent. In addition, when the azeotropic cleaning agent according to this embodiment is used as a rinse agent, depending on the cleaning agent, an azeotropic cleaning agent solution can be stably regenerated even by simple distillation.
(1.共沸洗浄剤)
1つの局面において、本開示は、一般式(1):R−O−CH2−CHX−O−H
(式中、Xが水素原子を表すとき、Rは、メチル基、エチル基、n−プロピル基、iso−プロピル基、iso−ブチル基、sec−ブチル基、及びtert−ブチル基からなる群から選択される基を表し、
Xがメチル基を表すとき、Rは、メチル基、エチル基、n−プロピル基、iso−プロピル基、n−ブチル基、iso−ブチル基、sec−ブチル基、及びtert−ブチル基からなる群から選択される基を表す。)で表されるグリコールエーテル及び水を含む共沸混合物を含む、共沸洗浄剤を提供する。
(1. Azeotropic cleaning agent)
In one aspect, the present disclosure provides a general formula (1): R—O—CH 2 —CHX—O—H.
(In the formula, when X represents a hydrogen atom, R is selected from the group consisting of a methyl group, an ethyl group, an n-propyl group, an iso-propyl group, an iso-butyl group, a sec-butyl group, and a tert-butyl group. Represents the selected group,
When X represents a methyl group, R is a group consisting of a methyl group, an ethyl group, an n-propyl group, an iso-propyl group, an n-butyl group, an iso-butyl group, a sec-butyl group, and a tert-butyl group. Represents a group selected from: And an azeotropic mixture comprising water and a azeotropic detergent.
本開示において、「共沸混合物」は、気相と液相の組成が同じである混合物である。 In the present disclosure, an “azeotropic mixture” is a mixture having the same composition of the gas phase and the liquid phase.
本開示において、「共沸洗浄剤」は、共沸混合物を含む洗浄剤である。 In the present disclosure, an “azeotropic detergent” is a detergent comprising an azeotropic mixture.
(1.1.グリコールエーテルと水とからなる共沸混合物を含む共沸洗浄剤)
1つの実施形態において、上記共沸洗浄剤は、上記グリコールエーテルと水とからなる共沸混合物を含む。
(1.1. An azeotropic detergent containing an azeotropic mixture of glycol ether and water)
In one embodiment, the azeotropic detergent comprises an azeotropic mixture of the glycol ether and water.
(グリコールエーテル(以下(1)成分ともいう))
本実施形態に係る共沸洗浄剤を構成するグリコールエーテルは、常圧下の沸点が120〜180℃程度、好ましくは145〜165℃である。なお、「常圧」は標準大気圧を意味する。
(Glycol ether (hereinafter also referred to as component (1)))
The glycol ether constituting the azeotropic cleaning agent according to this embodiment has a boiling point of about 120 to 180 ° C, preferably 145 to 165 ° C under normal pressure. “Normal pressure” means standard atmospheric pressure.
また、(1)成分は、安全性の観点より本実施形態に係る共沸洗浄剤を非危険物とする目的から、引火点が30℃以上が好ましく、50〜60℃であるものがより好ましい。 In addition, from the viewpoint of safety, the component (1) has a flash point of preferably 30 ° C. or higher, more preferably 50 to 60 ° C. for the purpose of making the azeotropic cleaning agent according to the present embodiment non-hazardous. .
(1)成分の例は、エチレングリコールモノメチルエーテル、エチレングリコールモノエチルエーテル、エチレングリコールモノ−n−プロピルエーテル、エチレングリコールモノ−iso−プロピルエーテル、エチレングリコールモノ−iso−ブチルエーテル、エチレングリコールモノ−sec−ブチルエーテル、エチレングリコールモノ−tert−ブチルエーテル、プロピレングリコールモノメチルエーテル、プロピレングリコールモノエチルエーテル、プロピレングリコールモノ−n−プロピルエーテル、プロピレングリコールモノ−iso−プロピルエーテル、プロピレングリコールモノ−n−ブチルエーテル、プロピレングリコールモノ−iso−ブチルエーテル、プロピレングリコールモノ−sec−ブチルエーテル、プロピレングリコールモノ−tert−ブチルエーテル等が挙げられる。これらのグリコールエーテルは、2種以上を併用できる。 Examples of component (1) include ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol mono-n-propyl ether, ethylene glycol mono-iso-propyl ether, ethylene glycol mono-iso-butyl ether, ethylene glycol mono-sec. -Butyl ether, ethylene glycol mono-tert-butyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol mono-n-propyl ether, propylene glycol mono-iso-propyl ether, propylene glycol mono-n-butyl ether, propylene glycol Mono-iso-butyl ether, propylene glycol mono-sec-butyl ether, pro Glycol monobutyl -tert- butyl ether, and the like. Two or more of these glycol ethers can be used in combination.
(水)
本実施形態に係る共沸洗浄剤を構成する水としては、超純水、純水、蒸留水、イオン交換水、及び水道水等が挙げられる。上記水は軟水であっても硬水であってもよい。
(water)
Examples of the water constituting the azeotropic cleaning agent according to this embodiment include ultrapure water, pure water, distilled water, ion exchange water, and tap water. The water may be soft water or hard water.
(1.2.グリコールエーテルと水とジアミンとからなる共沸混合物を含む共沸洗浄剤)
1つの実施形態において、上記共沸洗浄剤は、上記グリコールエーテルと
一般式(2):R1R2N−(CH2)n−NR3R4
(式中、R1〜R4はそれぞれ独立に炭素数1〜4のアルキル基を表し、nは1〜6の整数である)
で表されるジアミンと
水とからなる共沸混合物を含む。
(1.2. An azeotropic detergent containing an azeotropic mixture of glycol ether, water and diamine)
In one embodiment, the azeotropic detergent comprises the glycol ether and the general formula (2): R 1 R 2 N— (CH 2 ) n —NR 3 R 4
(Wherein R 1 to R 4 each independently represents an alkyl group having 1 to 4 carbon atoms, and n is an integer of 1 to 6)
An azeotrope composed of diamine and water represented by
炭素数1〜4のアルキル基の例は、メチル基、エチル基、n−プロピル基、iso−プロピル基、n−ブチル基、iso−ブチル基、sec−ブチル基、及びtert−ブチル基が挙げられる。 Examples of the alkyl group having 1 to 4 carbon atoms include methyl group, ethyl group, n-propyl group, iso-propyl group, n-butyl group, iso-butyl group, sec-butyl group, and tert-butyl group. It is done.
(ジアミン(以下(2)成分ともいう))
上記一般式(2)で表わされるジアミンの例は、N,N,N’,N’−テトラメチルジアミノメタン等のジアミノメタン;
N,N,N’,N’−テトラメチルエチレンジアミン等のエチレンジアミン(ジアミノエタン);
N,N,N’,N’−テトラメチル−1,3−ジアミノプロパン等のジアミノプロパン;
N,N,N’,N’−テトラメチル−1,4−ジアミノブタン等のジアミノブタン;
N,N,N’,N’−テトラメチル−1,5−ジアミノペンタン等のジアミノペンタン;
N,N,N’,N’−テトラメチル−1,6−ジアミノヘキサン等のジアミノヘキサン等が挙げられる。
(Diamine (hereinafter also referred to as component (2)))
Examples of the diamine represented by the general formula (2) include diaminomethane such as N, N, N ′, N′-tetramethyldiaminomethane;
Ethylenediamine (diaminoethane) such as N, N, N ′, N′-tetramethylethylenediamine;
Diaminopropane such as N, N, N ′, N′-tetramethyl-1,3-diaminopropane;
Diaminobutane such as N, N, N ′, N′-tetramethyl-1,4-diaminobutane;
Diaminopentane such as N, N, N ′, N′-tetramethyl-1,5-diaminopentane;
Examples thereof include diaminohexane such as N, N, N ′, N′-tetramethyl-1,6-diaminohexane.
(1.3.共沸洗浄剤の物性等)
本実施形態に係る共沸洗浄剤は、常圧下の共沸点が好ましくは90〜100℃程度、より好ましくは95〜99℃程度である。
(1.3. Physical properties of azeotropic detergents)
The azeotropic cleaning agent according to this embodiment preferably has an azeotropic point under normal pressure of about 90 to 100 ° C, more preferably about 95 to 99 ° C.
上記共沸混合物は、上記共沸点を達成し、かつ容易に蒸留再生を行うために、[(1)成分/〔(1)成分+水〕]又は[〔(1)成分+(2)成分〕/〔(1)成分+(2)成分+水〕]で表される共沸組成比率が、好ましくは25〜45質量%程度であり、より好ましくは30〜40質量%程度である。 In order to achieve the above azeotropic point and perform distillation regeneration easily, the above azeotropic mixture is [(1) component / [(1) component + water]] or [[(1) component + (2) component]. ] / [(1) component + (2) component + water]] is preferably about 25 to 45% by mass, more preferably about 30 to 40% by mass.
1つの実施形態において、本実施形態に係る共沸洗浄剤は曇点を有さない。従来の洗浄剤は曇点を有するものが洗浄性に優れていることが知られていた。本発明者らは、鋭意検討した結果、驚くべきことに、曇点を有していない共沸洗浄剤であったとしても洗浄性やリンス性に優れていることを見出したものである。 In one embodiment, the azeotropic cleaning agent according to this embodiment does not have a cloud point. It has been known that a conventional cleaning agent having a cloud point has excellent cleaning properties. As a result of intensive studies, the present inventors have surprisingly found that even if an azeotropic cleaning agent does not have a cloud point, it has excellent cleaning properties and rinsing properties.
本開示において、「曇点」とは透明又は半透明な液体で温度変化によって相分離が起き、その結果不透明になる温度である。本実施形態に係る共沸洗浄剤の場合グリコールエーテルと水との間に形成される水素結合が切断され、水溶解度が急激に下がる温度をいう。 In the present disclosure, the “cloud point” is a temperature at which a phase separation occurs due to a temperature change in a transparent or translucent liquid, resulting in an opaqueness. In the case of the azeotropic cleaning agent according to this embodiment, it means a temperature at which the hydrogen bond formed between the glycol ether and water is cut and the water solubility rapidly decreases.
1つの実施形態において、本実施形態に係る共沸洗浄剤は引火点を有さない。その結果、本実施形態に係る共沸洗浄剤を非危険物として使用することができる。 In one embodiment, the azeotropic cleaning agent according to this embodiment does not have a flash point. As a result, the azeotropic cleaning agent according to this embodiment can be used as a non-hazardous material.
1つの実施形態において、本実施形態に係る共沸洗浄剤は界面活性剤を含まない。本実施形態に係る共沸洗浄剤は界面活性剤を含まない場合でも十分に洗浄性及びリンス性を有するものである。また、さらなる実施形態において、本実施形態に係る共沸洗浄剤は上記共沸混合物のみを含む。本実施形態に係る共沸洗浄剤は共沸混合物のみを含む場合でも十分に洗浄性及びリンス性を有するものである。 In one embodiment, the azeotropic cleaning agent according to this embodiment does not include a surfactant. The azeotropic cleaning agent according to this embodiment has sufficient cleaning and rinsing properties even when it does not contain a surfactant. In a further embodiment, the azeotropic cleaning agent according to this embodiment includes only the azeotropic mixture. The azeotropic cleaning agent according to the present embodiment has sufficient cleaning properties and rinsing properties even when it contains only an azeotropic mixture.
本開示において「界面活性剤」とは、溶液内において、臨界ミセル濃度以上でミセルのような会合体を形成する物質である。具体的には、陰イオン界面活性剤、陽イオン界面活性剤、両性界面活性剤、非イオン界面活性剤が挙げられる。例えば非イオン界面活性剤の例としては、アセチレンアルコール、アセチレングリコール、多価アルコール脂肪酸エステル、ポリオキシエチレンアルキルエーテル、ポリオキシエチレン多価アルコール脂肪酸エステル等が挙げられる。なお、一般式:R−O−CH2−CHX−O−H(式中、Rは炭素数1〜4のアルキル基を、Xは水素又はメチル基を表す。)で表されるグリコールエーテルは界面活性剤ではない。 In the present disclosure, the “surfactant” is a substance that forms an association like a micelle at a critical micelle concentration or higher in a solution. Specific examples include an anionic surfactant, a cationic surfactant, an amphoteric surfactant, and a nonionic surfactant. For example, examples of the nonionic surfactant include acetylene alcohol, acetylene glycol, polyhydric alcohol fatty acid ester, polyoxyethylene alkyl ether, polyoxyethylene polyhydric alcohol fatty acid ester, and the like. In addition, the glycol ether represented by the general formula: R—O—CH 2 —CHX—O—H (wherein R represents an alkyl group having 1 to 4 carbon atoms and X represents hydrogen or a methyl group) is It is not a surfactant.
1つの実施形態において、本実施形態に係る共沸洗浄剤は、表面張力低下剤(エチレングリコールモノヘキシルエーテル等)、スケール防止剤やキレート剤(グルコン酸ソーダ等)、防錆剤(炭酸アンモニウム等)、酸中和剤(テトラアルキルアンモニウムハイドライド、アンモニア等)、アルカリ中和剤(酢酸、ギ酸、塩酸等)、酸化還元剤(過酸化水素等)、酸化防止剤(ブチルヒドロトルエン等)を含み得る。 In one embodiment, the azeotropic cleaning agent according to this embodiment includes a surface tension reducing agent (such as ethylene glycol monohexyl ether), a scale inhibitor, a chelating agent (such as sodium gluconate), and a rust inhibitor (such as ammonium carbonate). ), Acid neutralizers (tetraalkylammonium hydride, ammonia, etc.), alkali neutralizers (acetic acid, formic acid, hydrochloric acid, etc.), redox agents (hydrogen peroxide, etc.), antioxidants (butylhydrotoluene, etc.) obtain.
1つの実施形態において、本実施形態に係る共沸洗浄剤はリンス剤である。本実施形態に係る共沸洗浄剤は乾燥性に優れている。したがって、水が被洗浄物に付着している場合であっても、リンス剤に用いることが可能である。本発明者らはさらなる検討の結果、水だけでなく、洗浄剤が被洗浄物に付着している場合であっても、リンス性に優れていることを見出した。好ましくは、上記リンス剤はフラックス洗浄液用である。 In one embodiment, the azeotropic cleaning agent according to this embodiment is a rinse agent. The azeotropic cleaning agent according to this embodiment is excellent in drying properties. Therefore, even when water adheres to the object to be cleaned, it can be used as a rinse agent. As a result of further studies, the present inventors have found that not only water but also a cleaning agent is excellent in rinsing properties even when the cleaning agent adheres to an object to be cleaned. Preferably, the rinse agent is for a flux cleaning solution.
本開示において「リンス剤」とは洗浄剤による洗浄後に被洗浄物に付着した水、洗浄剤、又は、水及び洗浄剤の両方を除去する剤である。 In the present disclosure, the “rinsing agent” is an agent that removes water, a cleaning agent, or both water and a cleaning agent attached to an object to be cleaned after cleaning with the cleaning agent.
(2.共沸洗浄剤の再生方法)
1つの局面において、本開示は、上記共沸洗浄剤を含む液を蒸留し、上記共沸混合物を得る工程を含む、共沸洗浄剤の再生方法を提供する。本実施形態に係る共沸洗浄剤は、洗浄後の廃液にフラックスや本実施形態に係る共沸洗浄剤以外の洗浄剤を含んでいたとしても、蒸留操作により再生されることができる。再生後の共沸洗浄剤は、使用前の共沸洗浄剤と比べても組成比や洗浄力が殆ど変化しない。その結果、共沸洗浄剤を再生利用できるため、洗浄の際に生じる洗浄剤廃液を低減させることができる。
(2. Regeneration method of azeotropic detergent)
In one aspect, the present disclosure provides a method for regenerating an azeotropic cleaning agent, which includes a step of distilling a liquid containing the azeotropic cleaning agent to obtain the azeotropic mixture. The azeotropic cleaning agent according to this embodiment can be regenerated by distillation operation even if the waste liquid after cleaning contains a flux or a cleaning agent other than the azeotropic cleaning agent according to this embodiment. The composition ratio and the cleaning power of the azeotropic cleaning agent after regeneration hardly change even when compared with the azeotropic cleaning agent before use. As a result, since the azeotropic cleaning agent can be recycled, it is possible to reduce the cleaning agent waste liquid generated during cleaning.
1つの実施形態において、上記再生方法は、ヒーターや熱媒等の熱源、及びコンデンサや熱交換器等の凝縮機構を備えた蒸留機によって廃液を気化する工程、濃縮する工程、得られた留出液を受器、若しくは洗浄機のタンクへ戻す工程、釜残渣として濃縮された汚染物質を除去する工程等を含む。尚、この蒸留機には、留出液の純度を上げる目的で必要に応じて、ラシヒリング、ディクソンパッキン、バブルキャップトレイ、又はデミスター等を設置してもよい。それらの理論段数は任意であり、必要に応じて増加させてもよい。また、共沸洗浄剤が共沸混合物以外の物質を含む場合には、蒸留により共沸混合物を得る工程の後に、得られた共沸混合物に上記共沸混合物以外の物質を加える工程を含み得る。 In one embodiment, the regeneration method comprises a step of vaporizing waste liquid, a step of concentrating, and a distillate obtained by a distiller equipped with a heat source such as a heater and a heat medium, and a condenser mechanism such as a condenser and a heat exchanger. Including a step of returning the liquid to the tank of the receiver or the washing machine, a step of removing contaminants concentrated as a kettle residue, and the like. In this distiller, a Raschig ring, a Dixon packing, a bubble cap tray, a demister, or the like may be installed as necessary for the purpose of increasing the purity of the distillate. The number of theoretical plates is arbitrary and may be increased as necessary. In addition, when the azeotropic cleaning agent contains a substance other than the azeotrope, it may include a step of adding a substance other than the azeotrope to the obtained azeotrope after the step of obtaining the azeotrope by distillation. .
上記再生方法の際に行われる蒸留の例は、単蒸留及び共沸蒸留等が挙げられるが、これに限定されるものではない。好ましくは常圧下、90〜110℃で共沸蒸留が行われる。 Examples of distillation performed during the regeneration method include simple distillation and azeotropic distillation, but are not limited thereto. Preferably, the azeotropic distillation is performed at 90 to 110 ° C. under normal pressure.
上記再生方法において、得られる共沸混合物の量の例は、再生前に共沸洗浄剤に含まれる共沸混合物の量の50質量%以上、60質量%以上、70質量%以上、80質量%以上、90質量%以上、95質量%以上、100質量%であり、好ましくは95質量%以上であり、最も好ましくは100質量%である。 In the above regeneration method, examples of the amount of the azeotrope obtained are 50% by mass, 60% by mass, 70% by mass, and 80% by mass of the amount of the azeotrope contained in the azeotropic detergent before regeneration. As mentioned above, it is 90 mass% or more, 95 mass% or more, and 100 mass%, Preferably it is 95 mass% or more, Most preferably, it is 100 mass%.
「共沸洗浄剤を含む液」の例は、共沸洗浄剤を用いて洗浄した後に生じる共沸洗浄剤を含む廃液(以下、共沸洗浄剤廃液ともいう)等が挙げられる。上記共沸洗浄剤廃液には、被洗浄物に付着していた汚染物質や本実施形態に係る共沸洗浄剤以外の洗浄液等を含み得る。 Examples of the “liquid containing an azeotropic cleaning agent” include a waste liquid containing an azeotropic cleaning agent (hereinafter, also referred to as an azeotropic cleaning agent waste liquid) generated after washing with an azeotropic cleaning agent. The azeotropic cleaning agent waste liquid may include a contaminant attached to the object to be cleaned, a cleaning liquid other than the azeotropic cleaning agent according to the present embodiment, and the like.
なお共沸洗浄剤を再生する際には、共沸洗浄剤廃液から本実施形態に係る共沸洗浄剤以外の剤(例えば汚染物質や本実施形態に係る共沸洗浄剤以外の洗浄剤等)が除去される。 When regenerating the azeotropic cleaning agent, an agent other than the azeotropic cleaning agent according to this embodiment (for example, a contaminant or a cleaning agent other than the azeotropic cleaning agent according to this embodiment) from the azeotropic cleaning agent waste liquid. Is removed.
上記再生方法において、除去される汚染物質の量の例は、共沸洗浄剤廃液に含まれる汚染物質の量の50質量%以上、60質量%以上、70質量%以上、80質量%以上、90質量%以上、95質量%以上、100質量%であり、好ましくは95質量%以上であり、最も好ましくは100質量%である。 In the above regeneration method, examples of the amount of contaminants to be removed include 50% by mass, 60% by mass, 70% by mass, 80% by mass, and 90% by mass of the amount of contaminants contained in the azeotropic detergent waste liquid. It is 95 mass% or more, 95 mass% or more, and 100 mass%, Preferably it is 95 mass% or more, Most preferably, it is 100 mass%.
上記再生方法において、除去される本実施形態に係る共沸洗浄剤以外の洗浄剤の量の例は、共沸洗浄剤廃液に含まれる本実施形態に係る共沸洗浄剤以外の洗浄液の量の50質量%以上、60質量%以上、70質量%以上、80質量%以上、90質量%以上、95質量%以上、100質量%であり、好ましくは95質量%以上であり、最も好ましくは100質量%である。 In the above regeneration method, an example of the amount of the cleaning agent other than the azeotropic cleaning agent according to this embodiment to be removed is the amount of the cleaning liquid other than the azeotropic cleaning agent according to this embodiment included in the azeotropic cleaning agent waste liquid. 50% by mass or more, 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, 95% by mass or more, 100% by mass, preferably 95% by mass or more, and most preferably 100% by mass. %.
(3.共沸洗浄剤を用いた洗浄(リンス)方法)
1つの局面において、本開示は、上記共沸洗浄剤を物品に付着している汚染物質又は洗浄剤と接触させる工程を含むが、物品に付着している洗浄剤は、上記共沸洗浄剤ではない、洗浄方法を提供する。本実施形態に係る共沸洗浄剤は容易に乾燥する。その結果、被洗浄物の表面に残らないことからリンス剤及びリンス剤使用後に生じるリンス剤廃液の量を低減させることが可能となる。さらに、本実施形態に係る共沸洗浄剤は、良好なリンス性及び良好な乾燥性を有することから、リンス剤としても用いることが可能である。
(3. Cleaning (rinsing) method using an azeotropic cleaning agent)
In one aspect, the present disclosure includes the step of contacting the azeotropic cleaning agent with a contaminant or cleaning agent attached to the article, wherein the cleaning agent attached to the article is not the azeotropic cleaning agent. Not provide a cleaning method. The azeotropic cleaning agent according to this embodiment is easily dried. As a result, since it does not remain on the surface of the object to be cleaned, it is possible to reduce the amount of the rinse agent and the rinse agent waste liquid generated after using the rinse agent. Furthermore, since the azeotropic cleaning agent according to this embodiment has good rinsing properties and good drying properties, it can also be used as a rinsing agent.
上記洗浄方法において、除去される汚染物質の量の例は、洗浄前に共沸洗浄剤に含まれる汚染物質の量の60質量%以上、70質量%以上、80質量%以上、90質量%以上、95質量%以上、100質量%である。上記除去される汚染物質の量は、好ましくは95質量%以上であり、最も好ましくは100質量%である。 In the above cleaning method, examples of the amount of contaminants to be removed are 60% by mass, 70% by mass, 80% by mass, 90% by mass or more of the amount of contaminants contained in the azeotropic cleaning agent before cleaning. 95 mass% or more and 100 mass%. The amount of contaminants removed is preferably 95% by weight or more, and most preferably 100% by weight.
上記洗浄方法において、除去される物品に付着している洗浄剤の量は、汚染物質の量の60質量%以上、70質量%以上、80質量%以上、90質量%以上、95質量%以上、100質量%であり、好ましくは100質量%である。上記除去される物品に付着している洗浄剤の量は、好ましくは95質量%以上であり、最も好ましくは100質量%である。 In the above cleaning method, the amount of the cleaning agent adhering to the article to be removed is 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, 95% by mass or more of the amount of contaminants, It is 100% by mass, preferably 100% by mass. The amount of the cleaning agent adhering to the article to be removed is preferably 95% by mass or more, and most preferably 100% by mass.
本実施形態に係る共沸洗浄剤を汚染物質等が付着した物品に接触させて物品を洗浄する手段は限定されず、洗浄手段の例は、浸漬洗浄、シャワー洗浄、スプレー洗浄、超音波洗浄、液中ジェット洗浄、直通式洗浄(ダイレクトパス(登録商標))等が挙げられる。また、公知の洗浄装置として、例えば、特開平7−328565号公報、特開2000−189912号公報、特開2001−932号公報、特開2005−144441号公報等が挙げられる。なお、本実施形態に係る共沸洗浄剤は、炭化水素溶剤系の洗浄剤とは異なり非危険物であるため燃焼しない。そのため防爆設備も不要となることから、シャワー洗浄やスプレー洗浄にも好適である。 Means for cleaning the article by bringing the azeotropic cleaning agent according to the present embodiment into contact with the article to which contaminants or the like are attached are not limited, and examples of the cleaning means include immersion cleaning, shower cleaning, spray cleaning, ultrasonic cleaning, Examples include submerged jet cleaning and direct-through cleaning (Direct Pass (registered trademark)). Moreover, as a well-known washing | cleaning apparatus, Unexamined-Japanese-Patent No. 7-328565, Unexamined-Japanese-Patent No. 2000-189912, Unexamined-Japanese-Patent No. 2001-932, Unexamined-Japanese-Patent No. 2005-144441 etc. are mentioned, for example. Note that the azeotropic cleaning agent according to the present embodiment does not burn because it is a non-hazardous material unlike the hydrocarbon solvent-based cleaning agent. Therefore, explosion-proof equipment is not necessary, and it is suitable for shower cleaning and spray cleaning.
(洗浄剤)
本開示において、「洗浄剤」とは洗って汚れを落とすために使う剤である。洗浄剤の例は、グリコールエーテル系洗浄剤、炭化水素系洗浄剤,アルコール系洗浄剤,塩素系洗浄剤,フッ素系洗浄剤,臭素系洗浄剤が挙げられる。
(Washing soap)
In the present disclosure, the “cleaning agent” is an agent used for washing and removing dirt. Examples of cleaning agents include glycol ether cleaning agents, hydrocarbon cleaning agents, alcohol cleaning agents, chlorine cleaning agents, fluorine cleaning agents, and bromine cleaning agents.
(汚染物質)
1つの実施形態において、上記汚染物質はハンダ付け用フラックス、ソルダペースト、及び工業油からなる群の少なくとも1つを含む。しかしこれらに限定されるものではない。
(Pollutant)
In one embodiment, the contaminant comprises at least one of the group consisting of soldering flux, solder paste, and industrial oil. However, it is not limited to these.
(ハンダ付け用フラックス)
本開示において、「ハンダ付け用フラックス」とは、ハンダ及び母材(金属電極等)表面の酸化皮膜を除去し、両者の接合を容易にするために用いられる組成物である。一般的には、ベース樹脂、活性剤及び有機溶剤を含み、必要に応じてチキソトロピック剤、酸化防止剤、その他の添加剤が含まれていてもよい。また、ハンダ付け用フラックスは、その組成により、ソルダペースト用フラックス、並びに糸はんだ用フラックス、ポストフラックス及びプレフラックス等の非ソルダペースト用フラックスに分類される。
(Soldering flux)
In the present disclosure, the “soldering flux” is a composition used to remove the oxide film on the surfaces of the solder and the base material (metal electrode or the like) and facilitate the joining of both. Generally, it contains a base resin, an activator and an organic solvent, and may contain a thixotropic agent, an antioxidant and other additives as necessary. The soldering flux is classified according to its composition into solder paste flux and non-solder paste flux such as yarn solder flux, post flux and preflux.
上記ベース樹脂の例は、ロジン系ベース樹脂及び非ロジン系ベース樹脂等が挙げられる。該ロジン系ベース樹脂の例は、天然ロジン、ロジン誘導体、及びこれらの精製物等が挙げられる。天然ロジンの例は、ガムロジン、トール油ロジン及びウッドロジン等が挙げられる。ロジン誘導体の例は、上記天然ロジンの水素化物及び不均化物;
重合ロジン、不飽和酸変性ロジン、ロジンエステル並びにそれらの水素化物及び不均化物等が挙げられる。上記重合ロジン、上記不飽和酸変性ロジン、及び上記ロジンエステルは、上記天然ロジン、又は上記天然ロジンの水素化物若しくは不均化物等を用いて製造され得る。上記ロジンエステルを構成する多価アルコールの例は、グリセリン、ペンタエリスリトール等が挙げられる。上記不飽和酸変性ロジンを構成する不飽和酸の例は、アクリル酸、フマル酸、マレイン酸等が挙げられる。非ロジン系ベース樹脂の例は、エポキシ樹脂、アクリル樹脂、ポリイミド樹脂、ナイロン樹脂、ポリアクリロニトリル樹脂、塩化ビニル樹脂、酢酸ビニル樹脂、ポリオレフイン樹脂、フッ素系樹脂、ABS樹脂、イソプレンゴム、スチレンブタジエンゴム(SBR)、ブタジエンゴム(BR)、クロロプレンゴム、ナイロンゴム、ナイロン系エラストマ、ポリエステル系エラストマ等が挙げられる。
Examples of the base resin include rosin base resins and non-rosin base resins. Examples of the rosin base resin include natural rosin, rosin derivatives, and purified products thereof. Examples of natural rosins include gum rosin, tall oil rosin and wood rosin. Examples of rosin derivatives are hydrides and disproportionates of the above natural rosins;
Examples thereof include polymerized rosin, unsaturated acid-modified rosin, rosin ester, hydrides and disproportionates thereof. The polymerized rosin, the unsaturated acid-modified rosin, and the rosin ester can be produced using the natural rosin or a hydride or disproportionate of the natural rosin. Examples of the polyhydric alcohol constituting the rosin ester include glycerin and pentaerythritol. Examples of the unsaturated acid constituting the unsaturated acid-modified rosin include acrylic acid, fumaric acid, maleic acid and the like. Examples of non-rosin base resins are epoxy resin, acrylic resin, polyimide resin, nylon resin, polyacrylonitrile resin, vinyl chloride resin, vinyl acetate resin, polyolefin resin, fluorine resin, ABS resin, isoprene rubber, styrene butadiene rubber ( SBR), butadiene rubber (BR), chloroprene rubber, nylon rubber, nylon elastomer, polyester elastomer and the like.
上記活性剤の例は、コハク酸、アジピン酸、アゼライン酸、グルタル酸、セバシン酸、ドデカン2酸、ダイマー酸、フマル酸、マレイン酸、イタコン酸、trans−2,3−ジブロモ−1,4−ブテンジオール、cis−2,3−ジブロモ−1,4−ブテンジオール、3−ブロモプロピオン酸、2−ブロモ吉草酸、5−ブロモ−n−吉草酸、2−ブロモイソ吉草酸、エチルアミン臭素酸塩、ジエチルアミン臭素酸塩、ジエチルアミン塩化水素酸塩、メチルアミン臭素酸等が挙げられる。 Examples of the activators are succinic acid, adipic acid, azelaic acid, glutaric acid, sebacic acid, dodecanedioic acid, dimer acid, fumaric acid, maleic acid, itaconic acid, trans-2,3-dibromo-1,4- Butenediol, cis-2,3-dibromo-1,4-butenediol, 3-bromopropionic acid, 2-bromovaleric acid, 5-bromo-n-valeric acid, 2-bromoisovaleric acid, ethylamine bromate, Examples include diethylamine bromate, diethylamine hydrochloride, methylamine bromate and the like.
上記有機溶剤の例は、エタノール、n−プロパノール、イソプロパノール、イソブタノール、ブチルカルビトール、ヘキシルジグリコール、ヘキシルカルビトール、酢酸イソプロピル、プロピオン酸エチル、安息香酸ブチル、アジピン酸ジエチル、n−ヘキサン、ドデカン、テトラデセン等が挙げられる。 Examples of the organic solvents are ethanol, n-propanol, isopropanol, isobutanol, butyl carbitol, hexyl diglycol, hexyl carbitol, isopropyl acetate, ethyl propionate, butyl benzoate, diethyl adipate, n-hexane, dodecane , Tetradecene and the like.
上記チキソトロピック剤の例は、ひまし油、硬化ひまし油、蜜ロウ、カルナバワックス、ステアリン酸アミド、12−ヒドロキシステアリン酸エチレンビスアミド等が挙げられる。 Examples of the thixotropic agent include castor oil, hydrogenated castor oil, beeswax, carnauba wax, stearamide, 12-hydroxystearic acid ethylenebisamide, and the like.
上記酸化防止剤の例は、ペンタエリスリチル−テトラキス〔3−(3,5−ジ−t−ブチル−4−ヒドロキシフェニル)プロピオネート〕、オクタデシル−3−(3,5−ジ−t−ブチル−4−ヒドロキシフェニル)プロピオネート、N,N’−ヘキサメチレンビス(3,5−ジ−t−ブチル−4−ヒドロキシ−ヒドロシンアミド)、1,3,5−トリメチル−2,4,6−トリス(3,5−ジ−t−ブチル−4−ヒドロキシベンジル)ベンゼン、2,6−ジ−t−ブチル−p−クレゾール、トリフェニルフォスファイト、トリエチルフォスファイト、トリラウリルトリチオフォスファイト、トリス(トリデシル)フォスファイト等が挙げられる。 Examples of the antioxidant are pentaerythrityl-tetrakis [3- (3,5-di-t-butyl-4-hydroxyphenyl) propionate], octadecyl-3- (3,5-di-t-butyl- 4-hydroxyphenyl) propionate, N, N′-hexamethylenebis (3,5-di-tert-butyl-4-hydroxy-hydrocinamide), 1,3,5-trimethyl-2,4,6-tris (3,5-di-t-butyl-4-hydroxybenzyl) benzene, 2,6-di-t-butyl-p-cresol, triphenyl phosphite, triethyl phosphite, trilauryl trithiophosphite, tris (tridecyl) ) Phosphite and the like.
上記その他の添加剤の例は、防黴剤、艶消し剤、増粘防止剤、界面活性剤等が挙げられる。 Examples of the other additives include an antifungal agent, a matting agent, an anti-thickening agent, and a surfactant.
(ソルダペースト)
本開示において「ソルダペースト」とはハンダ付け用フラックスとハンダ粉末とを混合してなる組成物である。ハンダ粉末としては、Sn−Ag系、Sn−Cu系、Sn−Sb系、Sn−Zn系の鉛フリーハンダ粉末、更に鉛を構成成分とする鉛含有ハンダ粉末が挙げられる。また、これらハンダ金属は、Ag、Al、Au、Bi、Co、Cu、Fe、Ga、Ge、In、Ni、P、Pt、Sb、Znの1種又は2種以上の元素がドープされたものであってよい。ソルダペーストは、スクリーン印刷によりメタルマスクを介して電極上に供給され、その上に電子部品が載置された後に、加熱下でハンダ付けが行われる。
(Solder paste)
In the present disclosure, “solder paste” is a composition formed by mixing a soldering flux and solder powder. Examples of the solder powder include Sn-Ag-based, Sn-Cu-based, Sn-Sb-based and Sn-Zn-based lead-free solder powders, and lead-containing solder powders containing lead as a constituent component. These solder metals are doped with one or more elements of Ag, Al, Au, Bi, Co, Cu, Fe, Ga, Ge, In, Ni, P, Pt, Sb, and Zn. It may be. The solder paste is supplied onto the electrode through a metal mask by screen printing, and after the electronic component is placed thereon, soldering is performed under heating.
上記ハンダ付け用フラックス又はソルダペーストが付着した物品の例は、スクリーン印刷用のメタルマスク、スキージ、ディスペンス方式用のノズル、シリンジ、及び基板固定用の治具等が挙げられる。 Examples of the article to which the soldering flux or solder paste is attached include a metal mask for screen printing, a squeegee, a nozzle for dispensing system, a syringe, a jig for fixing a substrate, and the like.
フラックス残渣は、ソルダペースト、糸ハンダ、プレフラックス、ポストフラックス等を用い、電子部品等を電極に接合した後に生ずる残渣である。フラックス残渣は、ハンダ金属及び母材を腐食したり、基板の絶縁抵抗を低下させたりするため、洗浄により除去する必要がある。 The flux residue is a residue that is generated after an electronic component or the like is bonded to an electrode using solder paste, yarn solder, preflux, postflux, or the like. The flux residue needs to be removed by cleaning in order to corrode the solder metal and the base material or to reduce the insulation resistance of the substrate.
上記フラックス残渣が付着した物品の例は、プリント回路基板、セラミック配線基板、半導体素子搭載基板、ウエハ、TABテープ、リードフレーム、パワーモジュール、及びカメラモジュール等が挙げられる。また、対応するものについては、IC、コンデンサ、抵抗器、ダイオード、トランジスタ、コイル、及びCSP等の電子部品がハンダ付けされていたり、BGA、PGA、及びLGA等が形成されていたり、ハンダレベリング等の前処理が施されていてもよい。 Examples of the article to which the flux residue is attached include a printed circuit board, a ceramic wiring board, a semiconductor element mounting board, a wafer, a TAB tape, a lead frame, a power module, and a camera module. In addition, as for the corresponding ones, electronic parts such as ICs, capacitors, resistors, diodes, transistors, coils, and CSPs are soldered, BGA, PGA, LGA, etc. are formed, solder leveling, etc. The pretreatment may be performed.
(工業油)
工業油の例は、加工油、切削油、鉱物油、機械油グリース、潤滑油、防錆油、ワックス、ピッチ、パラフィン、油脂、グリース等が挙げられる。これらは機械加工、金属加工等の分野において、材料と工具間の摩擦を低減して焼き付きを防止したり、加工に要する力を低減して形成し易くしたり、製品の錆や腐食を防止したりするために使用される。また、メッキ処理が予定されている部品に工業用油が残存しているとメッキ不良が生じ得るため、そうした部品の洗浄に本実施形態に係る洗浄剤は特に適している。
(Industrial oil)
Examples of industrial oils include processing oils, cutting oils, mineral oils, machine oil greases, lubricating oils, rust preventive oils, waxes, pitches, paraffins, oils and fats, greases and the like. These reduce the friction between materials and tools to prevent seizure in the fields of machining, metal processing, etc., reduce the force required for processing to make it easier to form, and prevent rust and corrosion of products. Used to In addition, if industrial oil remains in a part that is scheduled to be plated, defective plating may occur. Therefore, the cleaning agent according to this embodiment is particularly suitable for cleaning such parts.
工業油が付着した物品の例は、ボルト、ナット、フェルール、及びワッシャー等の成型部品をはじめ、エンジンピストン等の自動車部品、ギア、シャフト、スプロケット、及びチェーン等の産業機械部品、HDD用パーツ、及びリードフレーム等の電子部品等が挙げられる。 Examples of articles to which industrial oil adheres include molded parts such as bolts, nuts, ferrules and washers, automobile parts such as engine pistons, industrial machine parts such as gears, shafts, sprockets, and chains, HDD parts, And electronic components such as lead frames.
その他の汚染物質の例は、プリント回路基板、セラミック配線基板、半導体素子搭載基板、カバーガラス、及びウエハ等をダイシング加工した際に生じる切り粉等が挙げられる。 Examples of other contaminants include chips produced when dicing a printed circuit board, a ceramic wiring board, a semiconductor element mounting board, a cover glass, and a wafer.
(3.1.洗浄−リンス方法)
1つの実施形態において、上記洗浄方法は、
一般式(A):RA1−O−(CH2−CHRA2−O)a−RA3
(式中、RA1は炭素数1〜6のアルキル基又はベンジル基を表し、RA2はメチル基又は水素原子を表し、RA3は炭素数1〜5のアルキル基又は水素原子を表し、aは2〜4の整数を表す。)
で表される有機溶剤(A)、
一般式(B):
で表されるアミン(B)、
及びアミノ基非含有キレート剤(C)を含む非共沸洗浄剤を
物品に付着している汚染物質と接触させる工程、並びに
上記共沸洗浄剤を物品に付着している上記非共沸洗浄剤及び/又は汚染物質と接触させる工程を含む。
(3.1. Washing-rinsing method)
In one embodiment, the cleaning method comprises:
Formula (A): R A1 —O— (CH 2 —CHR A2 —O) a —R A3
(In the formula, R A1 represents an alkyl group having 1 to 6 carbon atoms or a benzyl group, R A2 represents a methyl group or a hydrogen atom, R A3 represents an alkyl group having 1 to 5 carbon atoms or a hydrogen atom, and a Represents an integer of 2 to 4.)
An organic solvent (A) represented by
Formula (B):
An amine (B) represented by
And a non-azeotropic cleaning agent containing an amino group-free chelating agent (C) and a contaminant attached to the article, and the non-azeotropic cleaning agent attached to the article. And / or contacting with contaminants.
炭素数5のアルキル基の例は、ペンチル基、1−メチルブチル基、2−メチルブチル基、3−メチルブチル基、1,1−ジメチルプロピル基、1,2−ジメチルプロピル基、1−エチルプロピル基、2,2−ジメチルプロピル基等が挙げられる。 Examples of the alkyl group having 5 carbon atoms are pentyl group, 1-methylbutyl group, 2-methylbutyl group, 3-methylbutyl group, 1,1-dimethylpropyl group, 1,2-dimethylpropyl group, 1-ethylpropyl group, Examples include 2,2-dimethylpropyl group.
炭素数6のアルキル基の例は、ヘキシル基、1−メチルペンチル基、2−メチルペンチル基、3−メチルペンチル基、4−メチルペンチル基、5−メチルペンチル基、1,1−ジメチルブチル基、2,2−ジメチルブチル基、3,3−ジメチルブチル基、1,2−ジメチルブチル基、1,3−ジメチルブチル基、2,3−ジメチルブチル基等が挙げられる。 Examples of the alkyl group having 6 carbon atoms are hexyl group, 1-methylpentyl group, 2-methylpentyl group, 3-methylpentyl group, 4-methylpentyl group, 5-methylpentyl group, 1,1-dimethylbutyl group. 2,2-dimethylbutyl group, 3,3-dimethylbutyl group, 1,2-dimethylbutyl group, 1,3-dimethylbutyl group, 2,3-dimethylbutyl group and the like.
炭素数7のアルキル基の例は、ヘプチル基、1−メチルヘキシル基、2−メチルヘキシル基、3−メチルヘキシル基、4−メチルヘキシル基、5−メチルヘキシル基等が挙げられる。 Examples of the alkyl group having 7 carbon atoms include heptyl group, 1-methylhexyl group, 2-methylhexyl group, 3-methylhexyl group, 4-methylhexyl group, 5-methylhexyl group and the like.
(有機溶剤(A)((A)成分ともいう))
有機溶剤(A)は2種以上を併用できる。(A)成分の例は、ジエチレングリコールエーテル、ポリエチレングリコールエーテル、プロピレングリコールエーテル(一般式(A)のRA2をメチル基としたグリコールエーテル)等が挙げられる。
ジエチレングリコールエーテルの例は、ジエチレングリコールモノアルキルエーテル、ジエチレングリコールジアルキルエーテル、ジエチレングリコールモノベンジルエーテル等が挙げられる。
ジエチレングリコールモノアルキルエーテルの例は、ジエチレングリコールモノメチルエーテル、ジエチレングリコールモノエチルエーテル、ジエチレングリコールモノプロピルエーテル、ジエチレングリコールモノブチルエーテル、ジエチレングリコールモノペンチルエーテル、ジエチレングリコールモノヘキシルエーテル等が挙げられる。
ジエチレングリコールジアルキルエーテルの例は、ジエチレングリコールジメチルエーテル、ジエチレングリコールジエチルエーテル、ジエチレングリコールメチルエチルエーテル、ジエチレングリコールジプロピルエーテル、ジエチレングリコールメチルプロピルエーテル、ジエチレングリコールエチルプロピルエーテル、ジエチレングリコールジブチルエーテル、ジエチレングリコールメチルブチルエーテル、ジエチレングリコールエチルブチルエーテル、ジエチレングリコールプロピルブチルエーテル、ジエチレングリコールジペンチルエーテル、ジエチレングリコールメチルペンチルエーテル、ジエチレングリコールエチルペンチルエーテル、ジエチレングリコールプロピルペンチルエーテル、ジエチレングリコールブチルペンチルエーテル等が挙げられる。
ポリエチレングリコールエーテルの例は、上記ジエチレングリコールエーテルに対応するトリエチレングリコールエーテル、テトラエチレングリコールエーテル等が挙げられる。
これらの中でも、共沸洗浄剤の共沸組成を崩さない観点より、トリエチレングリコールモノブチルエーテル、ジエチレングリコールモノベンジルエーテルが好ましい。
(Organic solvent (A) (also referred to as component (A)))
Two or more organic solvents (A) can be used in combination. Examples of the component (A) include diethylene glycol ether, polyethylene glycol ether, propylene glycol ether (glycol ether having R A2 in the general formula (A) as a methyl group) and the like.
Examples of diethylene glycol ether include diethylene glycol monoalkyl ether, diethylene glycol dialkyl ether, diethylene glycol monobenzyl ether and the like.
Examples of the diethylene glycol monoalkyl ether include diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, diethylene glycol monobutyl ether, diethylene glycol monopentyl ether, diethylene glycol monohexyl ether and the like.
Examples of diethylene glycol dialkyl ether are diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol methyl ethyl ether, diethylene glycol dipropyl ether, diethylene glycol methyl propyl ether, diethylene glycol ethyl propyl ether, diethylene glycol dibutyl ether, diethylene glycol methyl butyl ether, diethylene glycol ethyl butyl ether, diethylene glycol propyl butyl ether, Diethylene glycol dipentyl ether, diethylene glycol methyl pentyl ether, diethylene glycol ethyl pentyl ether, diethylene glycol propyl pentyl ether, diethylene glycol butyl pentyl ether Ether and the like.
Examples of the polyethylene glycol ether include triethylene glycol ether and tetraethylene glycol ether corresponding to the diethylene glycol ether.
Among these, triethylene glycol monobutyl ether and diethylene glycol monobenzyl ether are preferable from the viewpoint of not destroying the azeotropic composition of the azeotropic detergent.
また、上記非共沸洗浄剤には、必要に応じて上記(A)成分以外の非ハロゲン系有機溶剤が含まれる。非ハロゲン系有機溶剤の例は、エチレングリコールモノメチルエーテル、エチレングリコールモノエチルエーテル、エチレングリコールモノ−n−プロピルエーテル、エチレングリコールモノ−iso−プロピルエーテル、エチレングリコールモノ−n−ブチルエーテル、エチレングリコールモノ−iso−ブチルエーテル、エチレングリコールモノ−sec−ブチルエーテル、エチレングリコールモノ−tert−ブチルエーテル、プロピレングリコールモノメチルエーテル、プロピレングリコールモノエチルエーテル、プロピレングリコールモノ−n−プロピルエーテル、プロピレングリコールモノ−iso−プロピルエーテル、プロピレングリコールモノ−n−ブチルエーテル、プロピレングリコールモノ−iso−ブチルエーテル、プロピレングリコールモノ−sec−ブチルエーテル、プロピレングリコールモノ−tert−ブチルエーテル等のグリコールエーテル溶剤;1,3−ジメチル−2−イミダゾリジノン、1,3−ジエチル−2−イミダゾリジノン、1,3−ジプロピル−2−イミダゾリジノン、N−メチル−2−ピロリドン等の窒素含有化合物溶剤;ヘキサン、ヘプタン、オクタン等の炭化水素溶剤;メタノール、エタノール、ベンジルアルコール等のアルコール溶剤;アセトン、メチルエチルケトン等のケトン溶剤;ジエチルエーテル等のジアルキルエーテル溶剤;テトラヒドロフラン等の環状エーテル溶剤;酢酸エチル、酢酸メチル等のエステル溶剤等が挙げられる。これらは2種以上を併用できる。 The non-azeotropic cleaning agent contains a non-halogen organic solvent other than the component (A) as necessary. Examples of non-halogen organic solvents are ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol mono-n-propyl ether, ethylene glycol mono-iso-propyl ether, ethylene glycol mono-n-butyl ether, ethylene glycol mono- iso-butyl ether, ethylene glycol mono-sec-butyl ether, ethylene glycol mono-tert-butyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol mono-n-propyl ether, propylene glycol mono-iso-propyl ether, propylene Glycol mono-n-butyl ether, propylene glycol mono-iso-butyl ether, Glycol ether solvents such as propylene glycol mono-sec-butyl ether and propylene glycol mono-tert-butyl ether; 1,3-dimethyl-2-imidazolidinone, 1,3-diethyl-2-imidazolidinone, 1,3-dipropyl Nitrogen-containing compound solvents such as -2-imidazolidinone and N-methyl-2-pyrrolidone; hydrocarbon solvents such as hexane, heptane and octane; alcohol solvents such as methanol, ethanol and benzyl alcohol; ketone solvents such as acetone and methyl ethyl ketone A dialkyl ether solvent such as diethyl ether; a cyclic ether solvent such as tetrahydrofuran; and an ester solvent such as ethyl acetate and methyl acetate. Two or more of these can be used in combination.
(アミン(B)((B)成分ともいう))
アミン(B)は2種以上を併用できる。(B)成分の例は、N−メチルジエタノールアミン、N−エチルジエタノールアミン、N−ブチルジエタノールアミン、N−プロピルジエタノールアミン等のN−アルキルジアルカノールアミン;
一般式(B)中のRBをアルキル基とするオクチルアミン、デシルアミン、ドデシルアミン、テトラデシルアミン、ヘキサデシルアミン、2−エチルヘキシルアミン等の第1級脂肪族アミン等が挙げられる。これらの中でも、安全性等や、特に防汚染性及び低発泡性の観点より、前記N−アルキルジアルカノールアミンが好ましく、特にN−メチルジエタノールアミン、N−エチルジエタノールアミン、N−ブチルジエタノールアミン及びN−プロピルジエタノールアミンからなる群より選ばれる少なくとも1種がより好ましい。
(Amine (B) (also referred to as (B) component))
Two or more amines (B) can be used in combination. Examples of the component (B) include N-alkyl dialkanolamines such as N-methyldiethanolamine, N-ethyldiethanolamine, N-butyldiethanolamine, N-propyldiethanolamine;
Examples include primary aliphatic amines such as octylamine, decylamine, dodecylamine, tetradecylamine, hexadecylamine, 2-ethylhexylamine and the like, in which R B in general formula (B) is an alkyl group. Among these, the N-alkyl dialkanolamine is preferable from the viewpoints of safety and the like, in particular, antifouling property and low foaming property, and particularly N-methyldiethanolamine, N-ethyldiethanolamine, N-butyldiethanolamine and N-propyl. At least one selected from the group consisting of diethanolamine is more preferable.
(アミノ基非含有キレート剤(C)((C)成分ともいう))
アミノ基非含有キレート剤(C)は2種以上を併用できる。(C)成分は、分子内にアミノ基を有しないキレート剤であれば、各種公知のものを特に制限なく用いることができる。特に、隙間洗浄性や特に防汚染性の観点より、脂肪族ヒドロキシカルボン酸キレート剤及び/又は(ポリ)リン酸キレート剤が好ましい。
(Amino group-free chelating agent (C) (also referred to as component (C)))
Two or more amino group-free chelating agents (C) can be used in combination. As the component (C), various known compounds can be used without particular limitation as long as they are chelating agents having no amino group in the molecule. In particular, aliphatic hydroxycarboxylic acid chelating agents and / or (poly) phosphoric acid chelating agents are preferred from the viewpoints of gap cleaning properties and particularly antifouling properties.
脂肪族ヒドロキシカルボン酸キレート剤の例は、炭素数が2〜5程度の直鎖アルキル基を基本骨格として、これにカルボキシル基が2〜3個程度、及び水酸基が1〜3個程度結合したヒドロキシカルボン酸等が挙げられる。 Examples of the aliphatic hydroxycarboxylic acid chelating agent include hydroxy having about 2 to 3 carboxyl groups and about 1 to 3 hydroxyl groups bonded to a straight chain alkyl group having about 2 to 5 carbon atoms as a basic skeleton. A carboxylic acid etc. are mentioned.
上記ヒドロキシカルボン酸の例は、クエン酸、イソクエン酸、リンゴ酸、酒石酸や、これらの塩(ナトリウム塩、カリウム塩、アンモニウム塩、アルカノールアミン塩等が挙げられる。以下、同様。)等が挙げられる。これらの中でも、隙間洗浄性や特に防汚染性の観点より、クエン酸、イソクエン酸及びリンゴ酸からなる群より選ばれる少なくとも1種が好ましく、クエン酸がより好ましい。 Examples of the hydroxycarboxylic acid include citric acid, isocitric acid, malic acid, tartaric acid, and salts thereof (including sodium salt, potassium salt, ammonium salt, alkanolamine salt, etc. The same shall apply hereinafter). . Among these, at least one selected from the group consisting of citric acid, isocitric acid and malic acid is preferable, and citric acid is more preferable from the viewpoints of gap cleaning properties and particularly antifouling properties.
(ポリ)リン酸キレート剤の例は、隙間洗浄性や特に防汚染性の観点より、オルトリン酸、ピロリン酸及びトリリン酸からなる群より選ばれる少なくとも1種が好ましく、ピロリン酸がより好ましい。 The example of the (poly) phosphate chelating agent is preferably at least one selected from the group consisting of orthophosphoric acid, pyrophosphoric acid and triphosphoric acid, and more preferably pyrophosphoric acid, from the viewpoint of clearance cleaning properties and particularly antifouling properties.
(非共沸洗浄剤中の添加剤)
なお、非共沸洗浄剤には、各種公知の添加剤が含まれていてもよい。添加剤は2種以上を併用できる。添加剤の例は、ノニオン性界面活性剤(前記(A)成分及び(B)成分に相当するものを除く)、アニオン性界面活性剤、カチオン性界面活性剤等の各種界面活性剤や、消泡剤、防錆剤、酸化防止剤等が挙げられる。
(Additives in non-azeotropic detergents)
Note that various known additives may be included in the non-azeotropic cleaning agent. Two or more additives can be used in combination. Examples of the additive include various surfactants such as nonionic surfactants (excluding those corresponding to the components (A) and (B)), anionic surfactants, and cationic surfactants. Examples include foaming agents, rust inhibitors, and antioxidants.
ノニオン性界面活性剤の例は、一般式(D):Rd−O−(CH2−CH2−O)d−H(式中、Rdは炭素数8〜20のアルキル基を、dは0〜20の整数を表す。)で表される化合物や、脂肪酸アミドのエチレンオキサイド付加物、ソルビタン脂肪酸エステル、ショ糖脂肪酸エステル、脂肪酸アルカノールアミド、これらの対応するポリオキシプロピレン系界面活性剤等が挙げられる。 Examples of the nonionic surfactant are those represented by the general formula (D): R d —O— (CH 2 —CH 2 —O) d —H (wherein R d represents an alkyl group having 8 to 20 carbon atoms, d Represents an integer of 0 to 20)), ethylene oxide adducts of fatty acid amides, sorbitan fatty acid esters, sucrose fatty acid esters, fatty acid alkanolamides, their corresponding polyoxypropylene surfactants, etc. Is mentioned.
アニオン性界面活性剤の例は、硫酸エステル系アニオン性界面活性剤(高級アルコールの硫酸エステル塩、アルキル硫酸エステル塩、ポリオキシエチレンアルキル硫酸エステル塩等)、スルホン酸塩系アニオン性界面活性剤(アルキルスルホン酸塩、アルキルベンゼンスルホン酸塩等)等が挙げられる。 Examples of anionic surfactants include sulfate ester anionic surfactants (sulfate esters of higher alcohols, alkyl sulfate esters, polyoxyethylene alkyl sulfate salts, etc.), sulfonate anionic surfactants ( Alkyl sulfonates, alkyl benzene sulfonates, etc.).
カチオン性界面活性剤の例は、アルキル化アンモニウム塩、4級アンモニウム塩等が挙げられる。 Examples of the cationic surfactant include alkylated ammonium salts and quaternary ammonium salts.
両性界面活性剤の例は、アミノ酸型、ベタイン型両性界面活性剤等が挙げられる。 Examples of amphoteric surfactants include amino acid type, betaine type amphoteric surfactants and the like.
非共沸洗浄剤中、各成分の含有量は特に限定されない。(B)成分の含有量は、(A)成分100質量部に対して、(B)成分が0.01〜30質量部程度が好ましく、0.1〜5質量部がより好ましい。(C)成分の含有量は、(A)成分100質量部に対して、(C)成分が0.01〜10質量部程度が好ましく、0.02〜1質量部がより好ましい。水の含有量は、(A)成分100質量部に対して、0〜10質量部程度が好ましく、1〜8質量部がより好ましい。また、上記添加剤の含有量は、5質量部程度未満が好ましい。 In the non-azeotropic detergent, the content of each component is not particularly limited. The content of the component (B) is preferably about 0.01 to 30 parts by mass, more preferably 0.1 to 5 parts by mass with respect to 100 parts by mass of the component (A). As for content of (C) component, about 0.01-10 mass parts of (C) component is preferable with respect to 100 mass parts of (A) component, and 0.02-1 mass part is more preferable. About 0-10 mass parts is preferable with respect to 100 mass parts of (A) component, and, as for content of water, 1-8 mass parts is more preferable. Further, the content of the additive is preferably less than about 5 parts by mass.
(4.洗浄剤キット)
1つの局面において、本開示は、
一般式(A):RA1−O−(CH2−CHRA2−O)a−RA3
(式中、RA1は炭素数1〜6のアルキル基又はベンジル基を表し、RA2はメチル基又は水素原子を表し、RA3は炭素数1〜5のアルキル基又は水素原子を表し、aは2〜4の整数を表す。)
で表される有機溶剤(A)、
一般式(B):
で表されるアミン(B)、
及びアミノ基非含有キレート剤(C)を含む非共沸洗浄剤
並びに上記共沸洗浄剤を含む、洗浄剤キットを提供する。なお、有機溶剤(A)、アミン(B)及びアミノ基非含有キレート剤(C)の例は上述したものと同様である。
(4. Detergent kit)
In one aspect, the disclosure provides
Formula (A): R A1 —O— (CH 2 —CHR A2 —O) a —R A3
(In the formula, R A1 represents an alkyl group having 1 to 6 carbon atoms or a benzyl group, R A2 represents a methyl group or a hydrogen atom, R A3 represents an alkyl group having 1 to 5 carbon atoms or a hydrogen atom, and a Represents an integer of 2 to 4.)
An organic solvent (A) represented by
Formula (B):
An amine (B) represented by
And a non-azeotropic detergent containing the amino group-free chelating agent (C) and a detergent kit comprising the azeotropic detergent. Examples of the organic solvent (A), amine (B), and amino group-free chelating agent (C) are the same as those described above.
以下の製造例、作製例、調製例、実施例及び比較例に従って本発明をより具体的に説明するが、本発明はこれらに限定解釈されるものではなく、各実施例に開示された技術的手段を適宜組み合わせて得られる実施例も、本発明の範囲に含まれるものとする。 The present invention will be described more specifically according to the following production examples, preparation examples, preparation examples, examples and comparative examples, but the present invention is not construed as being limited thereto, and the technical disclosure disclosed in each example. Examples obtained by appropriately combining means are also included in the scope of the present invention.
製造例:共沸洗浄剤の調製
以下に示す手順により共沸洗浄剤を調製した。
Production Example: Preparation of Azeotropic Cleaning Agent An azeotropic cleaning agent was prepared by the following procedure.
製造例1:エチレングリコールモノメチルエーテルと水との共沸混合物を含む共沸洗浄剤の調製
200mlのナス型フラスコに、(1)成分:グリコールエーテルとしてエチレングリコールモノメチルエーテル(EM)を20g、及び水としてイオン交換水(以下、単に水という。)を80g入れ、よく混合することにより、溶液を調製した。
Production Example 1: Preparation of an azeotropic detergent containing an azeotropic mixture of ethylene glycol monomethyl ether and water In a 200 ml eggplant-shaped flask, (1) component: 20 g of ethylene glycol monomethyl ether (EM) as glycol ether and water As a solution, 80 g of ion exchange water (hereinafter simply referred to as water) was added and mixed well.
次いで、当該ナス型フラスコに、理論段数N=10に相当する蒸留カラム、ト字管、温度計及びリービッヒ冷却器を接続した。次いで、常圧下、当該ナス型フラスコをオイルバスで加熱し、当該共沸混合物を沸騰させることにより、沸点100℃以下の留分のみを採取することにより共沸洗浄剤を調製した。 Next, a distillation column, a T-tube, a thermometer, and a Liebig condenser corresponding to the theoretical plate number N = 10 were connected to the eggplant-shaped flask. Next, the eggplant-shaped flask was heated in an oil bath under normal pressure to boil the azeotropic mixture, whereby an azeotropic cleaning agent was prepared by collecting only a fraction having a boiling point of 100 ° C. or lower.
次いで、当該留分の組成比を、デジタル濃度計PR−201α(ATAGO社製)を用いて測定した。結果を表1に示す。 Subsequently, the composition ratio of the fraction was measured using a digital densitometer PR-201α (manufactured by ATAGO). The results are shown in Table 1.
製造例2〜11及び比較製造例1
製造例1において、(1)成分として表1で示されるものを使用した他は同様にして共沸洗浄剤を調製し、それぞれについて前記同様の方法での蒸留試験を行い、沸点100℃以下の留分の組成比を求めた。
In Production Example 1, azeotropic detergents were prepared in the same manner except that those shown in Table 1 were used as the component (1), and a distillation test was conducted in the same manner as described above. The composition ratio of the fraction was determined.
作製例:試験基材(被洗浄物品)の作製
以下に示す手順により基材A及び基材Bを試験基材(被洗浄物品)として作製した。
Production example: Production of test substrate (article to be cleaned) Substrate A and substrate B were produced as test substrates (articles to be cleaned) by the following procedure.
作製例1:基材Aの作製
市販の鉛フリーソルダーペースト(パインソルダーTAS LF−219−1、荒川化学工業(株)製)をSUS304テストピース(75×25×0.3mm)の上に1.0g均一に塗布する事で得られた試験片を基材Aとした。
Production Example 1: Production of Substrate A A commercially available lead-free solder paste (Pine Solder TAS LF-219-1, manufactured by Arakawa Chemical Industries, Ltd.) was placed on a SUS304 test piece (75 × 25 × 0.3 mm). A test piece obtained by uniformly coating 0.0 g was used as a base material A.
作製例2:基材Bの作製
市販の鉛フリーソルダーペースト(パインソルダーTAS LF−219−1、荒川化学工業(株)製)をリン脱酸銅板テストピース(40×40×0.3mm)の上に0.3g均一に塗布する事で得られた試験片を基材Bとした。
Production Example 2: Production of Substrate B A commercially available lead-free solder paste (Pine Solder TAS LF-219-1, manufactured by Arakawa Chemical Industry Co., Ltd.) was used for a phosphorus deoxidized copper plate test piece (40 × 40 × 0.3 mm). A test piece obtained by uniformly coating 0.3 g on top was used as a base material B.
調製例:リンス試験の際に用いる洗剤の調製
以下に示す手順により洗剤A及び洗剤Bをリンス試験の際に用いる洗剤として調製した。
Preparation Example: Preparation of detergent used in rinsing test Detergent A and detergent B were prepared as detergents used in the rinsing test by the following procedure.
調製例1:洗剤Aの調製
ベンジルアルコール(東京応化工業(株)製)と炭素数12〜14の第2級アルコール1モルに対して、9モル相当のエチレンオキシドを付加したもの(商品名ソフタノール90、日本触媒(株)製)とを99/1wt%で調合することにより、洗剤Aを調製した。
Preparation Example 1: Preparation of Detergent A A product obtained by adding 9 mol of ethylene oxide to benzyl alcohol (manufactured by Tokyo Ohka Kogyo Co., Ltd.) and 1 mol of a secondary alcohol having 12 to 14 carbon atoms (trade name Softanol 90 , Manufactured by Nippon Shokubai Co., Ltd.) was prepared at 99/1 wt% to prepare detergent A.
調製例2:洗剤Bの調製
ジプロピレングリコールモノ−n−ブチルエーテル(日本乳化剤(株)製)とソフタノール90(日本触媒(株)製)とを99/1wt%で調合することにより、洗剤Bを調製した。
Preparation Example 2: Preparation of Detergent B By preparing dipropylene glycol mono-n-butyl ether (manufactured by Nippon Emulsifier Co., Ltd.) and Softanol 90 (manufactured by Nippon Shokubai Co., Ltd.) at 99/1 wt%, detergent B was prepared. Prepared.
実施例1−1:洗浄試験
200mLビーカーに各製造例/比較製造例の共沸洗浄剤200gを入れ、70℃に加温した後、前記試験基材を浸漬し、28kHzの超音波を10分間照射させた後、該基材を取り出し、80℃の循風乾燥機の中で10分間乾燥させた。
Example 1-1: Cleaning test After 200 g of the azeotropic cleaning agent of each production example / comparative production example was placed in a 200 mL beaker and heated to 70 ° C, the test substrate was immersed, and 28 kHz ultrasonic waves were applied for 10 minutes. After irradiation, the substrate was taken out and dried for 10 minutes in an air circulation dryer at 80 ° C.
基材A及びBの評価方法及び評価基準
鉛フリーソルダーペーストの洗浄性は、洗浄前後の試験基材の質量差から除去率を求める事で判定した。尚、洗浄性の判定基準は下記の通りである。
除去率(%)={(洗浄前の試験基材質量−洗浄後の試験基材質量)/塗布量}×100
◎:除去率95%以上
○:除去率80%以上、かつ95%未満
△:除去率60%以上、かつ80%未満
×:除去率60%未満
Evaluation Method and Evaluation Criteria for Substrates A and B The detergency of the lead-free solder paste was determined by determining the removal rate from the difference in mass of the test substrate before and after cleaning. In addition, the criteria for determining the cleaning property are as follows.
Removal rate (%) = {(test substrate mass before cleaning−test substrate mass after cleaning) / coating amount} × 100
◎: Removal rate of 95% or more ○: Removal rate of 80% or more and less than 95% Δ: Removal rate of 60% or more and less than 80% ×: Removal rate of less than 60%
実施例1−1の結果を表2に示す。
実施例1−2:洗浄試験
基材A及びBの代わりに下記試験基材A及びBを用いる以外は、実施例1−1と同様にして、試験、評価を行った。その結果を表3に示す。
Example 1-2: Cleaning test A test and an evaluation were performed in the same manner as in Example 1-1 except that the following test substrates A and B were used instead of the substrates A and B. The results are shown in Table 3.
(試験基材A)
鉛フリーソルダペースト(商品名「パインソルダーTAS LF219−1」、荒川化学工業(株)製)を、ガラスエポキシ銅張積層板(30×30×T1.5mm)の銅パターン上にメタルマスクを介して印刷し、得られた積層板を、以下のプロファイルでリフローすることによって、フラックス残渣が付着した基板(試験基材A)を作製した。
(試験基板のリフロープロファイル)
雰囲気 : 大気
昇温速度 : 2℃/秒
プレヒート : 150℃、60秒間
ピーク温度 : 250℃、60秒間
(Test substrate A)
Lead-free solder paste (trade name “Pine Solder TAS LF219-1”, manufactured by Arakawa Chemical Industries, Ltd.) is placed on a copper pattern of a glass epoxy copper clad laminate (30 × 30 × T1.5 mm) through a metal mask. The substrate (test base material A) to which the flux residue was adhered was produced by reflowing the obtained laminated plate with the following profile.
(Test substrate reflow profile)
Atmosphere: Air heating rate: 2 ° C / second Preheating: 150 ° C, 60 seconds Peak temperature: 250 ° C, 60 seconds
(試験基材B)
ロジン系ポストフラックス(商品名「パインフラックスWHS−002」、荒川化学工業(株)製)50mgを、JIS2型の櫛形基板(50×50×T1.5mm)の銅パターン上に、軟毛ブラシを用いて均一に塗布し、100℃の乾燥機の中で5分間乾燥させた後、235±5℃の共晶ハンダ浴(錫−鉛合金)に5秒間浸すことによって、ポストフラックスの残渣が付着した基材(試験基材B)を作製した。
(Test substrate B)
Using a soft bristle brush with 50 mg of rosin-based postflux (trade name “Pineflux WHS-002”, manufactured by Arakawa Chemical Industries, Ltd.) on a copper pattern of a JIS2 type comb-shaped substrate (50 × 50 × T1.5 mm) And then uniformly applied, dried in a dryer at 100 ° C. for 5 minutes, and then immersed in a eutectic solder bath (tin-lead alloy) at 235 ± 5 ° C. for 5 seconds. A substrate (test substrate B) was prepared.
実施例2:リンス試験
リン脱酸銅板テストピース(40×40×0.3mm)を調製例において作成した洗浄剤A又はBに1分間浸漬した後、200mlビーカーに200g準備し、32℃に設定した各製造例/比較製造例の共沸洗浄剤に試験片を入れ、28kHzの超音波を3分間照射させた後、該試験片を取り出し、80℃の循風乾燥機の中で10分間乾燥させた。
Example 2: Rinse test Phosphorus deoxidized copper plate test piece (40 x 40 x 0.3 mm) was immersed in the cleaning agent A or B prepared in the preparation example for 1 minute, and then 200 g was prepared in a 200 ml beaker and set at 32 ° C. A test piece was placed in the azeotropic cleaning agent of each production example / comparative production example, irradiated with 28 kHz ultrasonic waves for 3 minutes, then taken out and dried for 10 minutes in an air circulation dryer at 80 ° C. I let you.
評価方法及び評価基準
前記洗剤A及びBのリンス性は、前記試験片に残留する油膜の有無を外観目視で判定した。尚、リンス性の判定基準は下記の通りである。
○:油膜無
×;油膜有
Evaluation Method and Evaluation Criteria The rinsing properties of the detergents A and B were determined by visual inspection of the presence or absence of an oil film remaining on the test piece. The criteria for rinsing properties are as follows.
○: No oil film ×: With oil film
実施例2の結果を表4に示す。
実施例3:乾燥試験
軟膏缶に各製造例/比較製造例の共沸洗浄剤1gを入れ、80℃に加温した循風乾燥機の中で乾燥するまでの時間を計測した。
Example 3: Drying test 1 g of the azeotropic cleaning agent of each production example / comparative production example was placed in an ointment can, and the time until drying was measured in an air circulation dryer heated to 80 ° C.
評価方法
試験前後の質量比較で乾燥性を評価した。具体的にはまず試験前の軟膏缶の質量及び軟膏缶に投入した各実施例の洗浄剤の質量を測定した。所定時間毎に乾燥機から各サンプルを取り出して計量し、乾燥したサンプルの質量が試験前の軟膏缶の質量と同じになるまでの所要時間で乾燥性を評価した。
Evaluation method Dryness was evaluated by mass comparison before and after the test. Specifically, first, the mass of the ointment can before the test and the mass of the cleaning agent of each example charged into the ointment can were measured. Each sample was taken out from the dryer every predetermined time and weighed, and the drying property was evaluated by the time required until the mass of the dried sample became the same as the mass of the ointment can before the test.
実施例3の結果を表5に示す。
実施例4−1:蒸留再生試験(洗浄剤入り廃液)
200mlのナス型フラスコに、製造例7の共沸洗浄剤を95g、及び市販の鉛フリー用洗浄剤(パインアルファST−180K、荒川化学工業(株)製)を5g入れ攪拌混合することにより廃液を調製した。
Example 4-1: Distillation regeneration test (waste liquid with detergent)
A 200 ml eggplant-shaped flask was charged with 95 g of the azeotropic cleaning agent of Production Example 7 and 5 g of a commercially available lead-free cleaning agent (Pine Alpha ST-180K, manufactured by Arakawa Chemical Co., Ltd.), and mixed by stirring. Was prepared.
次に、当該ナス型フラスコに、ト字管、温度計及びリービッヒ冷却器を取り付け、これをオイルバスに浸し、1気圧の下、該廃液を加熱して沸騰させた。そして初留区分を20g、中留区分を20gずつ3回、及び後留区分約20g未満をそれぞれ採取した。 Next, a toroid, a thermometer, and a Liebig condenser were attached to the eggplant-shaped flask, and this was immersed in an oil bath, and the waste liquid was heated to boiling under 1 atm. Then, 20 g of the first fraction, 3 times 20 g of the middle fraction, and less than about 20 g of the latter fraction were collected.
表6に、各蒸留区分におけるグリコールエーテルと水との比率(ガスクロマトグラフによる測定)を示す。表中に記載している通り、該廃液と留出液における組成比は、各蒸留区分において大きな変化がなく、蒸留前の洗浄液の組成比と大きく相違しないことがわかった。このことより、該廃液から共沸洗浄剤が再生されたことを確認した。
実施例4−2:蒸留再生試験(フラックス入り洗浄剤廃液)
200mlのナス型フラスコに、製造例7の共沸洗浄剤を99g、市販の鉛フリーソルダーペースト(パインソルダーTAS LF−219−1、荒川化学工業(株)製)のフラックス成分を1g入れ、攪拌混合することにより廃液を調製した。
Example 4-2: Distillation regeneration test (fluxed detergent waste liquid)
In a 200 ml eggplant-shaped flask, 99 g of the azeotropic cleaning agent of Production Example 7 and 1 g of a flux component of a commercially available lead-free solder paste (Pine Solder TAS LF-219-1, manufactured by Arakawa Chemical Industries, Ltd.) are stirred. A waste liquid was prepared by mixing.
次に、当該ナス型フラスコに、ト字管、温度計及びリービッヒ冷却器を取り付け、これをオイルバスに浸し、1気圧の下、該廃液を加熱して沸騰させた。そして初留区分を15g、中留区分を15gずつ3回、及び後留区分約15gをそれぞれ採取した。 Next, a toroid, a thermometer, and a Liebig condenser were attached to the eggplant-shaped flask, and this was immersed in an oil bath, and the waste liquid was heated to boiling under 1 atm. Then, 15 g of the first distillation section, 3 times of 15 g of the middle distillation section, and about 15 g of the rear distillation section were collected.
表7に、各蒸留区分におけるグリコールエーテルと水との比率(デジタル濃度計PR−201αによる測定)を示す。表中に記載している通り、該廃液と留出液における組成比は、各蒸留区分において大きな変化がなく、蒸留前の洗浄液の組成比と大きく相違しないことがわかった。このことより、該廃液から共沸洗浄剤が再生されたことを確認した。
実施例4−3:蒸留再生試験(各留分における各組成濃度の確認)
製造例7の共沸洗浄剤溶液を単蒸留にて蒸留再生し、液量が減った分、非共沸洗浄剤(トリエチレングリコールモノn−ブチルエーテル、N−n−ブチルジエタノールアミン及びクエン酸を含む非共沸洗浄剤)を濃度10%の割合で含む製造例7の共沸洗浄剤溶液を補充した。上記蒸留−補充の操作を繰返し、蒸留によって得られた各留分の組成を確認した。表8及び図1に、その結果(デジタル濃度計PR−201αによる測定)を示す。表8及び図1より、各留分の各組成の濃度が中央値から3%以内に収まっていることから、安定して共沸洗浄剤溶液が再生できていることを確認できた。
Example 4-3: Distillation regeneration test (confirmation of each composition concentration in each fraction)
The azeotropic detergent solution of Production Example 7 was distilled and regenerated by simple distillation, and the amount of liquid was reduced, so that a non-azeotropic detergent (containing triethylene glycol mono n-butyl ether, Nn-butyldiethanolamine and citric acid was included. The azeotropic detergent solution of Production Example 7 containing non-azeotropic detergent at a concentration of 10% was replenished. The above distillation-replenishment operation was repeated, and the composition of each fraction obtained by distillation was confirmed. The results (measurement with a digital densitometer PR-201α) are shown in Table 8 and FIG. From Table 8 and FIG. 1, since the density | concentration of each composition of each fraction was settled within 3% from the median, it has confirmed that the azeotropic cleaning agent solution was able to be reproduced | regenerated stably.
Claims (8)
(式中、Xが水素原子を表すとき、Rは、メチル基、エチル基、n−プロピル基、iso−プロピル基、及びtert−ブチル基からなる群から選択される基を表し、
Xがメチル基を表すとき、Rは、メチル基、及びエチル基からなる群から選択される基を表す。)
で表されるグリコールエーテル及び水、又は
前記グリコールエーテル、水、及びテトラメチルジアミノプロパン、若しくはテトラメチルジアミノブタンからなる
共沸混合物からなる共沸混合物からなる、曇点を有さない、共沸洗浄剤。 Formula (1): R—O—CH 2 —CHX—O—H
(Wherein, when X represents a hydrogen atom, R represents a radical selected from the group consisting of methyl group, ethyl group, n- propyl group, iso- propyl,及 Beauty tert- butyl group,
When X represents a methyl group, R represents a group selected from a methyl group, and ethyl group or Ranaru group. )
Glycol ether and water represented by
An azeotropic cleaning agent having no cloud point, comprising an azeotropic mixture comprising an azeotropic mixture comprising the glycol ether, water, and tetramethyldiaminopropane or tetramethyldiaminobutane .
(式中、RA1は炭素数1〜6のアルキル基又はベンジル基を表し、RA2はメチル基又は水素原子を表し、RA3は炭素数1〜5のアルキル基又は水素原子を表し、aは2〜4の整数を表す。)
で表される有機溶剤(A)、
一般式(B):
で表されるアミン(B)、
及びアミノ基非含有キレート剤(C)を含む非共沸洗浄剤を
物品に付着している汚染物質と接触させる工程、並びに
請求項1〜4のいずれか1項に記載の共沸洗浄剤を物品に付着している前記非共沸洗浄剤及び/又は汚染物質と接触させる工程を含む、請求項5に記載の洗浄方法。 Formula (A): R A1 —O— (CH 2 —CHR A2 —O) a —R A3
(In the formula, R A1 represents an alkyl group having 1 to 6 carbon atoms or a benzyl group, R A2 represents a methyl group or a hydrogen atom, R A3 represents an alkyl group having 1 to 5 carbon atoms or a hydrogen atom, and a Represents an integer of 2 to 4.)
An organic solvent (A) represented by
Formula (B):
An amine (B) represented by
And contacting the contaminants are amino group-free chelating agent a non-azeotropic cleaning agent containing (C) to adhere to the article, as well as the azeotropic cleaning agent according to any one of claims 1-4 The cleaning method according to claim 5 , comprising a step of contacting with the non-azeotropic cleaning agent and / or contaminant adhering to an article.
(式中、RA1は炭素数1〜6のアルキル基又はベンジル基を表し、RA2はメチル基又は水素原子を表し、RA3は炭素数1〜5のアルキル基又は水素原子を表し、aは2〜4の整数を表す。)
で表される有機溶剤(A)、
一般式(B):
で表されるアミン(B)、
及びアミノ基非含有キレート剤(C)を含む非共沸洗浄剤
並びに請求項1〜3のいずれか1項に記載の共沸洗浄剤を含む、洗浄剤キット。
Formula (A): R A1 —O— (CH 2 —CHR A2 —O) a —R A3
(In the formula, R A1 represents an alkyl group having 1 to 6 carbon atoms or a benzyl group, R A2 represents a methyl group or a hydrogen atom, R A3 represents an alkyl group having 1 to 5 carbon atoms or a hydrogen atom, and a Represents an integer of 2 to 4.)
An organic solvent (A) represented by
Formula (B):
An amine (B) represented by
And a non-azeotropic cleaning agent comprising an amino group-free chelating agent (C) and the azeotropic cleaning agent according to any one of claims 1 to 3 .
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