CN115433946A - Water-based metal cleaning agent and using method thereof - Google Patents
Water-based metal cleaning agent and using method thereof Download PDFInfo
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- CN115433946A CN115433946A CN202111261561.3A CN202111261561A CN115433946A CN 115433946 A CN115433946 A CN 115433946A CN 202111261561 A CN202111261561 A CN 202111261561A CN 115433946 A CN115433946 A CN 115433946A
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- Prior art keywords
- water
- acid
- based metal
- polyoxyethylene ether
- fatty alcohol
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 57
- 239000002184 metal Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000012459 cleaning agent Substances 0.000 title abstract description 35
- 238000004140 cleaning Methods 0.000 claims abstract description 31
- -1 nitrogen-containing heterocyclic compound Chemical class 0.000 claims abstract description 26
- 150000007524 organic acids Chemical class 0.000 claims abstract description 25
- 239000004094 surface-active agent Substances 0.000 claims abstract description 23
- 239000003381 stabilizer Substances 0.000 claims abstract description 15
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 86
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 86
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 57
- LVHBHZANLOWSRM-UHFFFAOYSA-N itaconic acid Chemical compound OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 57
- 239000002994 raw material Substances 0.000 claims description 29
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 24
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 23
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 22
- 235000002949 phytic acid Nutrition 0.000 claims description 22
- 239000000467 phytic acid Substances 0.000 claims description 22
- 229940068041 phytic acid Drugs 0.000 claims description 22
- 150000007942 carboxylates Chemical class 0.000 claims description 20
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 11
- 239000002736 nonionic surfactant Substances 0.000 claims description 11
- 239000000230 xanthan gum Substances 0.000 claims description 9
- 229920001285 xanthan gum Polymers 0.000 claims description 9
- 235000010493 xanthan gum Nutrition 0.000 claims description 9
- 229940082509 xanthan gum Drugs 0.000 claims description 9
- 150000002191 fatty alcohols Chemical class 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- QBYIENPQHBMVBV-HFEGYEGKSA-N (2R)-2-hydroxy-2-phenylacetic acid Chemical compound O[C@@H](C(O)=O)c1ccccc1.O[C@@H](C(O)=O)c1ccccc1 QBYIENPQHBMVBV-HFEGYEGKSA-N 0.000 claims description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- IWYDHOAUDWTVEP-UHFFFAOYSA-N R-2-phenyl-2-hydroxyacetic acid Natural products OC(=O)C(O)C1=CC=CC=C1 IWYDHOAUDWTVEP-UHFFFAOYSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 125000003438 dodecyl group Chemical group [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])* 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- 229960002510 mandelic acid Drugs 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- ONJQDTZCDSESIW-UHFFFAOYSA-N polidocanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO ONJQDTZCDSESIW-UHFFFAOYSA-N 0.000 claims description 2
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 2
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 2
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000013162 Cocos nucifera Nutrition 0.000 claims 1
- 244000060011 Cocos nucifera Species 0.000 claims 1
- 125000002252 acyl group Chemical group 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 12
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 3
- 238000005187 foaming Methods 0.000 abstract description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 23
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 19
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 19
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 19
- 239000005642 Oleic acid Substances 0.000 description 19
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 19
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 19
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 14
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 13
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000011734 sodium Substances 0.000 description 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 7
- 238000006116 polymerization reaction Methods 0.000 description 7
- 239000003112 inhibitor Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003599 detergent Substances 0.000 description 5
- 150000002391 heterocyclic compounds Chemical class 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- QJLCSFQWKBLNGJ-UHFFFAOYSA-N 3,4,5-trihydroxy-n-octylbenzamide Chemical group CCCCCCCCNC(=O)C1=CC(O)=C(O)C(O)=C1 QJLCSFQWKBLNGJ-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical compound NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 4
- 239000004519 grease Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910000737 Duralumin Inorganic materials 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001565 benzotriazoles Chemical class 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 150000005014 3-aminoquinolines Chemical class 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241001311547 Patina Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 150000001556 benzimidazoles Chemical class 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001012 protector Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
- C23G1/088—Iron or steel solutions containing organic acids
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/103—Other heavy metals copper or alloys of copper
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/12—Light metals
- C23G1/125—Light metals aluminium
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Detergent Compositions (AREA)
Abstract
The invention relates to the technical field of cleaning agents, belongs to the IPC class number of C23G1/08, and particularly relates to a water-based metal cleaning agent and a using method thereof. The water-based metal cleaner comprises, by mass, 5-20% of an organic acid, 10-30% of a surfactant, 0.5-5% of a stabilizer, 2-8% of a nitrogen-containing heterocyclic compound and water which is supplemented to 100%. The water-based metal cleaner can replace an acid-washing environment-friendly cleaner, has good cleaning effect and low foaming performance, can clean various different metal parts, and can increase the oxidation resistance of the cleaned parts.
Description
Technical Field
The invention relates to the technical field of cleaning agents, belongs to the IPC class number of C23G1/08, and particularly relates to a water-based metal cleaning agent and a using method thereof.
Background
The metal cleaning agent mainly comprises a solvent type cleaning agent and an aqueous cleaning agent, and is also used for cleaning metal by using strong acid, but the over-corrosion phenomenon is often caused, the solvent type cleaning mainly comprises organic solvent systems, the organic solvent has certain irritation to the skin protector of people after being used for a long time, and at present, the aqueous cleaning agent is concerned by people.
In order to find an aqueous cleaning agent capable of replacing an acid cleaning agent and a solvent cleaning agent, the inventor carries out a great deal of research, develops an environment-friendly cleaning agent which can replace the solvent cleaning agent and a strong acid cleaning agent, and applies for a related patent with the patent number of CN110684982A, but in use, the cleaned parts are easy to generate rust after being placed for a period of time, and the range of used metal parts is narrow.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the invention provides a water-based metal cleaner, which comprises, by mass, 5-20% of organic acid, 10-30% of surfactant, 0.5-5% of stabilizer, 2-8% of nitrogen-containing heterocyclic compound and water which are supplemented to 100%.
Preferably, the raw materials of the water-based metal cleaner comprise, by mass, 10-15% of organic acid, 12-18% of surfactant, 1-2% of stabilizer, 3-4% of nitrogen-containing heterocyclic compound and water to make up to 100%.
Further preferably, the raw materials of the water-based metal cleaner comprise, by mass, 12% of an organic acid, 15% of a surfactant, 1.5% of a stabilizer, 3.5% of a nitrogen-containing heterocyclic compound, 1% of an auxiliary agent and water to make up 100%.
The organic acid comprises at least one of acetic acid, glycolic acid, oxalic acid, phytic acid, tartaric acid, citric acid, succinic acid, mandelic acid, malic acid and azelaic acid.
The organic acid selected in the invention can dissociate out more protons, so that the cleaning performance is exerted, and the organic acid is low in toxicity or non-toxic and can be well biodegraded.
Preferably, the organic acid comprises a combination of phytic acid and citric acid.
The weight ratio of the phytic acid (CAS number is 83-86-3) to the citric acid (CAS number is 97-67-6) is 1: (0.5 to 1.5); preferably, the weight ratio of the phytic acid to the citric acid is 1: (0.6-1); further preferably, the weight ratio of the phytic acid to the citric acid is 1:0.8.
the phytic acid and citric acid can be obtained from the market.
The applicant found that when phytic acid is used in synergy with citric acid, the phytic acid can better react with metal oxides to produce complexes, and thus the rust removal effect is achieved.
The raw material of the water-based metal cleaner also comprises sulfamic acid (CAS No. 5329-14-6).
The weight ratio of the sulfamic acid to the phytic acid is (1-2.5): 1; preferably, the weight ratio of the sulfamic acid to the phytic acid is (1.5-2): 1; further preferably, the weight ratio of the sulfamic acid to the phytic acid is 1.8:1.
compared with the previous research, the inventor researches and discovers that the compatibility of the cleaning agent can be improved by using the synergistic effect of the sulfamic acid, the phytic acid and the citric acid in the system, and the stability of the cleaning agent can also be improved.
The surfactant comprises fatty alcohol polyoxyethylene ether carboxylate; the fatty alcohol polyoxyethylene ether carboxylate includes, but is not limited to, sodium fatty alcohol polyoxyethylene ether carboxylate.
Sodium fatty alcohol polyoxyethylene ether carboxylate is commercially available under the trade designation AEC-9Na.
The inventor finds that the fatty alcohol-polyoxyethylene ether carboxylate added into the system can better increase the removal of grease by the cleaning agent and further increase the removal of rust scale by the cleaning agent, probably because the fatty alcohol-polyoxyethylene ether carboxylate forms micelles in the system, and can better bring out metal ions chelated with organic acid out of the system.
The surfactant also includes a nonionic surfactant.
The nonionic surfactant comprises fatty alcohol polyoxyethylene ether itaconate.
The weight ratio of the fatty alcohol-polyoxyethylene ether itaconate to the fatty alcohol-polyoxyethylene ether carboxylate is (1.5-3): 1; preferably, the weight ratio of the fatty alcohol-polyoxyethylene ether itaconate to the fatty alcohol-polyoxyethylene ether carboxylate is (2-2.5): 1; further preferably, the weight ratio of the fatty alcohol-polyoxyethylene ether itaconate to the fatty alcohol-polyoxyethylene ether carboxylate is 2.3:1.
the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate comprise itaconic acid (CAS number 97-65-4), fatty alcohol-polyoxyethylene ether and p-toluenesulfonic acid.
The weight ratio of the itaconic acid to the fatty alcohol-polyoxyethylene ether is 1: (2.5-5); the weight ratio of the itaconic acid to the fatty alcohol-polyoxyethylene ether is 1: (3-4); the weight ratio of the itaconic acid to the fatty alcohol-polyoxyethylene ether is 1:3.5. ( The molar ratio is 1.05:1, if there is a data-based question, it can be answered from the molar ratio )
The weight of the p-toluenesulfonic acid is 2-3% (preferably 2.5%) of the total mass of the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate, and the p-toluenesulfonic acid mainly plays a role in catalyzing esterification, the using amount of the p-toluenesulfonic acid is not specifically limited, and the p-toluenesulfonic acid can play a role in catalyzing esterification.
In order to prevent self-polymerization, the raw material for preparing the fatty alcohol-polyoxyethylene ether itaconate also comprises a polymerization inhibitor; the polymerization inhibitor includes, but is not limited to, hydroquinone.
The weight of the polymerization inhibitor is 0.4-0.6% of the total mass of the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate.
The fatty alcohol-polyoxyethylene ether is selected from one of AEO-3, AEO-5, AEO-7 and AEO-9, preferably AEO-7.
The preparation method of the fatty alcohol-polyoxyethylene ether itaconate comprises the following steps: adding a raw material for preparing the fatty alcohol-polyoxyethylene ether itaconate into a device with a stirrer, a temperature agent and a condenser, heating to 125-135 ℃, reacting for 3.5-4.5 h, and continuously reducing pressure and removing water in the reaction process to obtain the fatty alcohol-polyoxyethylene ether itaconate.
The organic acid also includes oleic acid (CAS number 112-80-1).
Although the cleaning agent studied by the inventor before has a good cleaning effect on certain metals, the cleaning agent is cleaned by an ultrasonic instrument, more foams are generated under the vibration of ultrasonic, so the using effect of the cleaning agent is influenced. Oleic acid and fatty alcohol-polyoxyethylene ether itaconate can also better cleaning effect of the cleaning agent simultaneously, probably because fatty alcohol-polyoxyethylene ether itaconate and sodium fatty alcohol-polyoxyethylene ether carboxylate can further adsorb organic acid, make organic acid can be better with the dirt on metal surface, both synergism can be better not only can remove the grease better simultaneously, can also be better take away the rust scale that washs down.
The weight ratio of the oleic acid to the nitrogen-containing heterocyclic compound is 1: (2-8); preferably, the weight ratio of the oleic acid to the nitrogen-containing heterocyclic compound is 1: (3-4); further preferably, the weight ratio of the oleic acid to the nitrogen-containing heterocyclic compound is 1:3.5.
the nitrogen-containing heterocyclic compound refers to a compound having at least one nitrogen atom in addition to carbon atoms in the cyclic structure. For example, five-membered heterocyclic compounds, thiophene, pyrrole, thiazole and imidazole compounds, and the nitrogen-containing heterocyclic compound can also be a fused heterocyclic compound and the like.
As the nitrogen-containing heterocyclic compound, benzotriazoles, benzimidazoles, 3-aminoquinolines and the like can be mentioned, and benzotriazoles (CAS number 95-14-7) are preferred.
The inventor finds that the addition of a certain amount of oleic acid in the detergent is not only beneficial to the complexation of metal oxides, but also can better improve the corrosion resistance of the detergent under the action of citric acid, oleic acid and benzotriazol, so that the corrosion phenomenon of the detergent can not occur for a long time after the detergent is used, probably because a hydrophobic protective film is formed on the metal surface in a close arrangement manner on a non-polar group of a surfactant to prevent the corrosion reaction in the cleaning process, the benzotriazol has certain reducibility, nitrogen elements in the cleaned benzotriazol are adsorbed on the metal surface, the energy state of the metal surface tends to be stabilized, so that the corrosion speed of the metal surface is reduced, a smooth film can be formed under the interaction of the citric acid and the benzotriazol, the benzotriazol and the oleic acid can enable the corrosion potential to move positively, and simultaneously the benzotriazol and the oleic acid and the citric acid can enable the formed film to be more compact, so that the corrosion phenomenon cannot occur for a long time after the detergent is used.
The stabilizer is selected from one of polyvinyl pyrrolidone, carboxymethyl cellulose, xanthan gum, isomeric dodecyl polyoxyethylene ether, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600 and coconut oil diethanolyl; xanthan gum is preferred.
The xanthan gum is obtained by the market, and the market manufacturer comprises but is not limited to Anhui Zhonghong bioengineering Co., ltd.
Although fatty alcohol-polyoxyethylene ether itaconate can bring better effect, the inventor finds that the addition of fatty alcohol-polyoxyethylene ether itaconate can deteriorate the stability of the cleaning agent, and particularly, the cleaning agent is easy to generate turbidity at low temperature.
Although xanthan gum is not good for acid adhesion and has poor cleaning effect in the prior art, the applicant finds that the cleaning agent of the present invention has better cleaning effect, probably because two specific surfactants can better facilitate acid adhesion in the present invention.
The assistant is 3,4,5-trihydroxy-N-octyl benzamide.
The applicant found that the water-based metal cleaner LY12 of the present invention cleans duralumin.
The second aspect of the invention provides a preparation method of a water-based metal cleaner, which comprises the following steps:
(1) Evenly mixing sulfamic acid, a surfactant, a stabilizer and water to obtain a mixed material A;
(2) And adding the rest raw materials into the mixture A, and uniformly mixing and stirring to obtain the material.
The third aspect of the invention provides a use method of the water-based metal cleaner, which comprises the following steps:
s1: preparing a cleaning solution containing the water-based metal cleaner;
s2: filling the cleaning solution into an ultrasonic cleaning machine to perform ultrasonic cleaning on a workpiece to be cleaned;
s3: rinsing and drying the cleaned workpiece.
Wherein rinsing and drying are the means commonly used in the art.
The volume concentration of the water-based metal cleaning agent in the cleaning solution is 2-8%, and the balance is water.
The temperature for washing in step S2 is 40 to 60 ℃, preferably 50 ℃.
The inventors have found that the cleaning effect is better in the present application at a cleaning temperature of 40-60 c, probably because the dirt on the workpiece receives more ultrasonic energy at this temperature.
The number of the ultrasonic cleaning tanks in the step S2 is at least 3; ultrasonic wave selects a 25-80K vibration head; the stirring speed is 250-350 r/min, the ultrasonic frequency is 25-35 KHz, and the power is 300-350W.
The inventor finds that the period of mutual extrusion between cleaning liquid products is longer by selecting specific cleaning conditions, bubbles can be broken after reaching larger size, the cavitation effect is increased, and the cleaning is more beneficial.
Has the advantages that:
1. the water-based metal cleaning agent can replace an acid-washing environment-friendly cleaning agent, has a good cleaning effect, and can be used for promoting the dissolution of grease due to the mutual synergistic effect of the nonionic surfactant and simultaneously driving the diffusion of organic acid in the cleaning solution, so that the organic acid can well remove rust, patina, aluminum mildew and the like;
2. the water-based metal cleaner has better low-foaming performance probably due to the mutual synergistic action of oleic acid and a surfactant;
3. the water-based metal cleaner has better oxidation resistance and corrosion resistance, on one hand, the citric acid and the benzotriazol are possibly in mutual synergistic action, and on the other hand, the water-based metal cleaner is possibly adsorbed on the surface of metal by the physical adsorption or chemical adsorption of polar groups of elements such as nitrogen, sulfur, phosphorus and the like to form a layer of protective film;
4. the water-based metal cleaner disclosed by the invention can be used for cleaning various different metal parts and can be used for increasing the oxidation resistance of the cleaned parts.
Detailed Description
Specific examples of the present invention are given below, but the present invention is not limited by the examples; in addition, the starting materials in the present invention are all commercially available unless otherwise specified.
Example 1
A water-based metal cleaner comprises the following raw materials, by mass, 12% of organic acid, 15% of surfactant, 1.5% of stabilizer, 3.5% of nitrogen-containing heterocyclic compound, 1% of assistant and 100% of water;
the organic acid comprises a combination of phytic acid and citric acid; the weight ratio of the phytic acid to the citric acid is 1:0.8; the organic acid also includes oleic acid (CAS number 112-80-1); the weight ratio of the oleic acid to the nitrogen-containing heterocyclic compound is 1:3.5; the raw material of the water-based metal cleaner also comprises sulfamic acid (CAS No. 5329-14-6); the weight ratio of the sulfamic acid to the phytic acid is 1.8:1;
the surfactant comprises fatty alcohol polyoxyethylene ether carboxylate; the fatty alcohol-polyoxyethylene ether carboxylate comprises fatty alcohol-polyoxyethylene ether sodium carboxylate, and the sales grade of the fatty alcohol-polyoxyethylene ether sodium carboxylate is AEC-9Na;
the surfactant further comprises a nonionic surfactant; the nonionic surfactant comprises fatty alcohol-polyoxyethylene ether itaconate; the weight ratio of the fatty alcohol-polyoxyethylene ether itaconate to the fatty alcohol-polyoxyethylene ether carboxylate is 2.3:1;
the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate comprise itaconic acid (CAS number 97-65-4), fatty alcohol-polyoxyethylene ether, p-toluenesulfonic acid and hydroquinone; the weight ratio of the itaconic acid to the fatty alcohol-polyoxyethylene ether is 1:3.5; the weight of the p-toluenesulfonic acid is 2.5 percent of the total mass of the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate; the weight of the polymerization inhibitor is 0.5 percent of the total mass of the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate; the fatty alcohol-polyoxyethylene ether is AEO-7;
the preparation method of the fatty alcohol-polyoxyethylene ether itaconate comprises the following steps: adding a raw material for preparing the fatty alcohol-polyoxyethylene ether itaconate into a device with a stirrer, a temperature agent and a condenser, heating to 130 ℃, reacting for 4 hours, and continuously reducing pressure and removing water in the reaction process to obtain the fatty alcohol-polyoxyethylene ether itaconate;
the heterocyclic compound containing nitrogen is benzotriazol (CAS number is 95-14-7); the stabilizer is xanthan gum which is purchased from Anhui Zhonghong bioengineering limited company; the assistant is 3,4,5-trihydroxy-N-octyl benzamide.
The preparation method of the water-based metal cleaner comprises the following steps:
(1) Evenly mixing sulfamic acid, a surfactant, a stabilizer and water to obtain a mixed material A;
(2) And adding the rest raw materials into the mixture A, and uniformly mixing and stirring to obtain the material.
Example 2
A water-based metal cleaner comprises the following raw materials, by mass, 10% of organic acid, 12% of surfactant, 1% of stabilizer, 3% of nitrogen-containing heterocyclic compound and 100% of water;
the organic acid comprises a combination of phytic acid and citric acid; the weight ratio of the phytic acid to the citric acid is 1:0.6; the organic acid also includes oleic acid (CAS number 112-80-1); the weight ratio of the oleic acid to the nitrogen-containing heterocyclic compound is 1:3; the raw material of the water-based metal cleaner also comprises sulfamic acid (CAS No. 5329-14-6); the weight ratio of the sulfamic acid to the phytic acid is 1.5:1;
the surfactant comprises fatty alcohol polyoxyethylene ether carboxylate; the fatty alcohol-polyoxyethylene ether carboxylate comprises fatty alcohol-polyoxyethylene ether sodium carboxylate, and the sales grade of the fatty alcohol-polyoxyethylene ether sodium carboxylate is AEC-9Na;
the surfactant further comprises a nonionic surfactant; the nonionic surfactant comprises fatty alcohol-polyoxyethylene ether itaconate; the weight ratio of the fatty alcohol-polyoxyethylene ether itaconate to the fatty alcohol-polyoxyethylene ether carboxylate is 2:1;
the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate comprise itaconic acid (CAS number 97-65-4), fatty alcohol-polyoxyethylene ether, p-toluenesulfonic acid and hydroquinone; the weight ratio of the itaconic acid to the fatty alcohol-polyoxyethylene ether is 1:3.5; the weight of the p-toluenesulfonic acid is 2% of the total mass of the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate; the weight of the polymerization inhibitor is 0.4 percent of the total mass of the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate; the fatty alcohol-polyoxyethylene ether is AEO-7;
the preparation method of the fatty alcohol-polyoxyethylene ether itaconate comprises the following steps: adding a raw material for preparing the fatty alcohol-polyoxyethylene ether itaconate into a device with a stirrer, a temperature agent and a condenser, heating to 125 ℃, reacting for 4.5 hours, and continuously reducing pressure and removing water in the reaction process to obtain the fatty alcohol-polyoxyethylene ether itaconate;
the heterocyclic compound containing nitrogen is benzotriazol (CAS number is 95-14-7); the stabilizer is xanthan gum which is purchased from Anhui Zhonghong bioengineering limited company; the assistant is 3,4,5-trihydroxy-N-octyl benzamide.
The preparation method of the water-based metal cleaner is the same as that of example 1.
Example 3
A water-based metal cleaner is prepared from (by mass) organic acid 15%, surfactant 18%, stabilizer 2%, nitrogen-containing heterocyclic compound 4%, and water 100%;
the organic acid comprises a combination of phytic acid and citric acid; the weight ratio of the phytic acid to the citric acid is 1:1; the organic acid also includes oleic acid (CAS number 112-80-1); the weight ratio of the oleic acid to the nitrogen-containing heterocyclic compound is 1:4; the raw material of the water-based metal cleaner also comprises sulfamic acid (CAS No. 5329-14-6); the weight ratio of the sulfamic acid to the phytic acid is 2:1;
the surfactant comprises fatty alcohol polyoxyethylene ether carboxylate; the fatty alcohol-polyoxyethylene ether carboxylate comprises fatty alcohol-polyoxyethylene ether sodium carboxylate, and the sales grade of the fatty alcohol-polyoxyethylene ether sodium carboxylate is AEC-9Na;
the surfactant further comprises a nonionic surfactant; the nonionic surfactant comprises fatty alcohol-polyoxyethylene ether itaconate; the weight ratio of the fatty alcohol-polyoxyethylene ether itaconate to the fatty alcohol-polyoxyethylene ether carboxylate is 2.5:1;
the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate comprise itaconic acid (CAS number is 97-65-4), fatty alcohol-polyoxyethylene ether, p-toluenesulfonic acid and hydroquinone; the weight ratio of the itaconic acid to the fatty alcohol-polyoxyethylene ether is 1:4; the weight of the p-toluenesulfonic acid is 3% of the total mass of the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate; the weight of the polymerization inhibitor is 0.6 percent of the total mass of the raw materials for preparing the fatty alcohol-polyoxyethylene ether itaconate; the fatty alcohol-polyoxyethylene ether is AEO-7;
the preparation method of the fatty alcohol-polyoxyethylene ether itaconate comprises the following steps: adding a raw material for preparing fatty alcohol-polyoxyethylene ether itaconate into a device with a stirrer, a temperature agent and a condenser, heating to 135 ℃, reacting for 3.5h, and continuously reducing pressure and removing water in the reaction process to obtain the fatty alcohol-polyoxyethylene ether itaconate;
the heterocyclic compound containing nitrogen is benzotriazol (CAS number is 95-14-7); the stabilizer is xanthan gum which is purchased from Anhui Zhonghong bioengineering limited company; the assistant is 3,4,5-trihydroxy-N-octyl benzamide.
The preparation method of the water-based metal cleaner is the same as that of example 1.
Example 4
The specific implementation mode of the water-based metal cleaner is the same as that in example 1, except that no oleic acid is used, and the fatty alcohol-polyoxyethylene ether itaconate is replaced by oleic acid polyoxyethylene polyoxypropylene amine ether ester in patent CN 110684982A.
Example 5
A water-based metal cleaner was prepared in the same manner as in example 1, except that oleic acid was absent.
Example 6
The specific implementation mode of the water-based metal cleaner is the same as that of example 1, except that xanthan gum is not used.
Performance testing
1. The cleaning effect is as follows: cleaning rusty waste parts (the material is LY12 duralumin) by using the cleaning agent in the examples 1-6, wherein 30 parts are used in each group, the parts are heavy rust with oxide skin, the surfaces of the parts are matt, and the parts after rust removal are observed for evaluation, namely, the 0-grade parts have no rust and are glossy; grade 1, no rust and no luster on the surface; grade 2, light rust on the surface and uneven color; grade 3, large area of surface is rusted.
The cleaning method comprises the following steps:
s1: preparing a cleaning solution (with the volume concentration of 6 percent and the balance of water) containing the water-based metal cleaner;
s2: putting the cleaning solution into an ultrasonic cleaning machine to perform ultrasonic cleaning on a workpiece to be cleaned, wherein the temperature during cleaning is 50 ℃, the number of ultrasonic cleaning tanks is 3, 60K vibration heads are adopted as ultrasonic waves, and the stirring speed during cleaning is 300r/min, the ultrasonic frequency is 30KHz and the power is 320W;
s3: rinsing and drying the cleaned workpiece.
2. And (3) rust resistance detection: after the parts of each group of parts with the 0-1 level after being cleaned in the test 1 are placed for 30 days, the parts are evaluated according to the rating mode.
3. High-temperature stability: pouring the cleaning agent in the embodiment 1-6 into a measuring cylinder to 50mL of customers, plugging the measuring cylinder, putting the measuring cylinder into a constant-temperature water bath at 60 +/-2 ℃, taking out the measuring cylinder after the water surface is higher than the scale of 20mm and 6h, and observing the appearance after the room temperature is recovered, wherein the appearance is uniform, the cleaning agent is not layered to be qualified, and the cleaning agent is not layered to be qualified if the appearance is not the qualified.
4. Low-temperature stability: pouring the cleaning agent in the embodiment 1-6 into a measuring cylinder to 50mL of customers, plugging, putting into a refrigerator at minus 5 +/-2 ℃ for 24 hours, taking out, observing the appearance after the room temperature is recovered, and judging that the appearance is uniform, the delamination does not occur, no crystallization or precipitation is qualified, or else, the disqualification is determined.
The test results are shown in table 1.
5. The water-based metal cleaner of example 1 was tested according to QB-T2117-1995, and the results are shown in Table 2.
TABLE 1
TABLE 2
Claims (10)
1. The water-based metal cleaner is characterized in that the raw materials comprise, by mass, 5-20% of organic acid, 10-30% of surfactant, 0.5-5% of stabilizer, 2-8% of nitrogen-containing heterocyclic compound and 100% of water.
2. The water-based metal cleaner as defined in claim 1, wherein the organic acid comprises at least one of acetic acid, glycolic acid, oxalic acid, phytic acid, tartaric acid, citric acid, succinic acid, mandelic acid, malic acid, and azelaic acid.
3. The water-based metal cleaner according to claim 1 or 2, wherein the surfactant comprises a fatty alcohol polyoxyethylene ether carboxylate.
4. The water-based metal cleaner according to claim 3, wherein the surfactant further comprises a nonionic surfactant; the nonionic surfactant comprises fatty alcohol polyoxyethylene ether itaconate.
5. The water-based metal cleaner as claimed in claim 4, wherein the raw material for preparing the fatty alcohol-polyoxyethylene ether itaconate comprises itaconic acid, fatty alcohol-polyoxyethylene ether and p-toluenesulfonic acid.
6. The water-based metal cleaner as claimed in claim 5, wherein the fatty alcohol-polyoxyethylene ether is one selected from the group consisting of AEO-3, AEO-5, AEO-7 and AEO-9.
7. The water-based metal cleaner as claimed in claim 1, wherein the stabilizer is one selected from polyvinyl pyrrolidone, carboxymethyl cellulose, xanthan gum, isomeric dodecyl polyoxyethylene ether, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, and coconut diethanol acyl.
8. A method for using the water-based metal cleaner as claimed in any one of claims 1 to 7, which comprises the following steps:
s1: preparing a cleaning solution containing the water-based metal cleaner;
s2: filling the cleaning solution into an ultrasonic cleaning machine to perform ultrasonic cleaning on a workpiece to be cleaned;
s3: rinsing and drying the cleaned workpiece.
9. The use method of the water-based metal cleaner as claimed in claim 8, wherein the volume concentration of the water-based metal cleaner in the cleaning solution is 2-8%, and the balance is water.
10. The method as claimed in claim 8 or 9, wherein the temperature for cleaning in step S2 is 40-60 ℃.
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| CN110684982A (en) * | 2019-11-19 | 2020-01-14 | 上海赛敏环保科技有限公司 | Environment-friendly cleaning agent and preparation method thereof |
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| CN106283075A (en) * | 2016-08-03 | 2017-01-04 | 上海赛敏环保科技有限公司 | Water-solube and biodegradable abluent and Cleaning application method |
| CN110684982A (en) * | 2019-11-19 | 2020-01-14 | 上海赛敏环保科技有限公司 | Environment-friendly cleaning agent and preparation method thereof |
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