CN108107142B - Analysis method of surfactant in wax removal water - Google Patents
Analysis method of surfactant in wax removal water Download PDFInfo
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- CN108107142B CN108107142B CN201711390727.5A CN201711390727A CN108107142B CN 108107142 B CN108107142 B CN 108107142B CN 201711390727 A CN201711390727 A CN 201711390727A CN 108107142 B CN108107142 B CN 108107142B
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- fluoroquinoline
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000004094 surface-active agent Substances 0.000 title claims abstract description 45
- 238000004458 analytical method Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 36
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000527 sonication Methods 0.000 claims abstract description 19
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 19
- NLEPLDKPYLYCSY-UHFFFAOYSA-N 2-fluoroquinoline Chemical compound C1=CC=CC2=NC(F)=CC=C21 NLEPLDKPYLYCSY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 15
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 claims abstract description 15
- RMDCSDVIVXJELQ-UHFFFAOYSA-N 6-fluoroquinoline Chemical compound N1=CC=CC2=CC(F)=CC=C21 RMDCSDVIVXJELQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- XUIRHRWOJCYEDJ-UHFFFAOYSA-N 7-fluoroquinoline Chemical compound C1=CC=NC2=CC(F)=CC=C21 XUIRHRWOJCYEDJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- WMFXCDGQRHJFKL-UHFFFAOYSA-N 5-fluoroquinoline Chemical compound C1=CC=C2C(F)=CC=CC2=N1 WMFXCDGQRHJFKL-UHFFFAOYSA-N 0.000 claims abstract description 7
- RNAAXKYOTPSFGV-UHFFFAOYSA-N 8-fluoroquinoline Chemical compound C1=CN=C2C(F)=CC=CC2=C1 RNAAXKYOTPSFGV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001819 mass spectrum Methods 0.000 claims abstract description 7
- UFIGOYSEDNHKGT-UHFFFAOYSA-N 3-fluoroquinoline Chemical compound C1=CC=CC2=CC(F)=CN=C21 UFIGOYSEDNHKGT-UHFFFAOYSA-N 0.000 claims abstract description 5
- IZCUJTLKJPQFSY-UHFFFAOYSA-N 4-fluoroquinoline Chemical compound C1=CC=C2C(F)=CC=NC2=C1 IZCUJTLKJPQFSY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001993 wax Substances 0.000 claims description 80
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 7
- 239000010962 carbon steel Substances 0.000 claims description 7
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
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- 239000002184 metal Substances 0.000 description 18
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- 239000002563 ionic surfactant Substances 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
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- 239000002244 precipitate Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
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- 238000001179 sorption measurement Methods 0.000 description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 2
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- 238000005202 decontamination Methods 0.000 description 2
- 230000003588 decontaminative effect Effects 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
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- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- ONJQDTZCDSESIW-UHFFFAOYSA-N polidocanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO ONJQDTZCDSESIW-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000003381 solubilizing effect Effects 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 244000236521 Bupleurum rotundifolium Species 0.000 description 1
- 235000015221 Bupleurum rotundifolium Nutrition 0.000 description 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N CHCl3 Substances ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
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- 125000002091 cationic group Chemical group 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
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- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
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- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 229910003480 inorganic solid Inorganic materials 0.000 description 1
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- 238000004811 liquid chromatography Methods 0.000 description 1
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- 238000004949 mass spectrometry Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002381 microspectrum Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 235000011008 sodium phosphates Nutrition 0.000 description 1
- 235000019351 sodium silicates Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical class [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000002888 zwitterionic surfactant Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
A method for analyzing a surfactant in wax removal water comprises the following steps: filtering the wax removing water, adding fluoroquinoline in 0.5-1.5 wt% of the wax removing water, and ultrasonic treating. After sonication, analysis was performed by HPLC or LC-MS. The filtration was first through a buchner funnel and then through a 0.45 μm filter. The temperature of the ultrasonic treatment is 55-65 ℃. The ultrasonic treatment time is 10-30 min. The fluoroquinoline is selected from one of 3-fluoroquinoline, 4-fluoroquinoline, 5-fluoroquinoline, 6-fluoroquinoline, 7-fluoroquinoline and 8-fluoroquinoline. The mobile phase of the HPLC is methanol and water, and the chromatographic column is a C18 column. The mass spectrum in the LC-MS is a triple quadrupole.
Description
Technical Field
The invention relates to the field of micro-spectrum analysis, in particular to an analysis method of a surfactant in wax removal water.
Background
After the metal workpiece is treated by a mechanical procedure through polishing wax, wax scales are adhered to the metal workpiece, and the wax scales are mainly remained on the workpiece in the forms of molecule-to-molecule adsorption, mechanical adsorption, electrostatic adsorption and the like. The main components of the wax scale include animal and vegetable oil, rosin soap, powder and oxide which are ground into a metal matrix, metal oxide, paraffin, organic acid and the like.
The method for removing wax stain from metal includes chemical method, water-based cleaning agent method, organic solvent method and electrochemical method. The common organic solvent method can not completely remove wax scale, especially can not effectively clean polishing materials such as metal oxides, carbides and the like on the surface of a metal workpiece, and the contained organic solvent has high toxicity and is likely to be hydrolyzed, and the metal workpiece can be corroded in a humid environment. The chemical and electrochemical methods for removing wax need strong acid or strong alkali, so that the method is not suitable for cleaning steel parts.
The wax removing water is a water-based multifunctional cleaning agent which mainly comprises a surfactant and is supplemented with components with a corrosion inhibition effect on metals, a solvent and the like, and has emulsifying capacity on waxy dirt and cleaning capacity on oil dirt. The multifunctional wax remover has the functions of thorough wax removal, clean oil removal, no corrosion to workpieces, no color change after cleaning, no oxidation and no rust. The research of the wax removing water mainly comprises the compounding and the preparation of some surfactants, auxiliary agents, corrosion inhibitors, latent solvents and the like.
The wax scale of polishing waxes is mainly composed of paraffin wax, fatty acids, rosin soaps, metal oxides and certain inorganic solids milled small particles such as: corundum, silicon carbide, high-alumina porcelain and the like. The solid particles are uniformly distributed in the polishing wax system mainly in a powdery state, and some polishing cloth rumble residual pieces, powder materials of a polished metal matrix and oxides thereof are also provided. The wax scale is mainly adhered to the workpiece in a mechanical adhesion mode, an intermolecular force adhesion mode, an electrostatic force adhesion mode and the like, and is difficult to remove when the mechanically adhered wax scale particles are less than 011 mu m, which is a conclusion obtained by observing various wax scales for a long time. The key of the preparation of the wax removing water is the reasonable compounding of various surfactants, assistants, corrosion inhibitors and the like, and the wetting and penetrating performance and the emulsifying, dissolving, solubilizing and other performances are improved by reducing the surface tension, so that the penetrating capacity and the dissolving capacity are enhanced. The compounding of the nonionic surfactant and the anionic surfactant is widely applied for a long time, and the addition of the ionic surfactant can ensure that the cloud point of the nonionic surfactant has a wider range and can form mixed micelles; the nonionic surfactant molecules are inserted into the micelles, so that the repulsion between ion heads of the subsequent ionic surfactants is weakened, and the interaction between hydrophobic chains of the two surfactants is added, so that the micelles are more easily generated, the CMC of the mixed liquid is reduced, the surface tension is also reduced, and the surface activity is increased.
The wax removing water is widely applied to the wax removing process after polishing of hardware industrial workpieces such as electroplating, clocks, artware, ornaments and the like. The wax removing water is compounded with surfactant, assistant, corrosion inhibitor, cosolvent, etc. and thus the product may be used in normal temperature, heating, ultrasonic treatment, soaking and other technological process to eliminate wax scale fast and completely without producing corrosion, oxidation and other negative effect on stainless steel, carbon steel, zinc alloy, aluminum alloy, magnesium alloy, copper alloy and other base material and has long service life and environment friendship.
Because the wax removing water contains more surfactants, when the composition analysis is carried out, the sample is easily foamed after being treated, flocculent precipitates with fine particles are formed, the subsequent operation steps such as centrifugation are interfered, and the analysis difficulty is higher.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides an analysis method of a surfactant in wax removing water, which comprises the following steps: filtering the wax removing water, adding fluoroquinoline in 0.5-1.5 wt% of the wax removing water, and ultrasonic treating.
In some embodiments, the filtration is first through a buchner funnel and then through a 0.45 μm filter.
In some embodiments, the temperature of the sonication is between 55 and 65 ℃.
In some embodiments, the sonication time is 10-30 min.
In some embodiments, the fluoroquinoline is selected from one of 3-fluoroquinoline, 4-fluoroquinoline, 5-fluoroquinoline, 6-fluoroquinoline, 7-fluoroquinoline, 8-fluoroquinoline.
In some embodiments, the fluoroquinoline is selected from one of 5-fluoroquinoline, 6-fluoroquinoline, 7-fluoroquinoline, 8-fluoroquinoline.
In some embodiments, the dewaxed water is used for stainless steel and/or carbon steel.
In some embodiments, the method further comprises the step of performing the analysis by HPLC or LC-MS after the ultrasonic treatment.
In some embodiments, the mobile phase of the HPLC is methanol and water and the chromatography column is a C18 column.
In some embodiments, the mass spectrum in the LC-MS is a triple quadrupole.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
Water-based wax removers, emulsion-based wax removers, and oil-based wax removers. The oil-based wax remover is a solvent with large wax dissolving amount, can effectively dissolve wax stains formed, and is mainly used in oil fields. The solvents of this type, which have been widely used at home and abroad up to now, are mainly the following: CS2、CCl4、CHCl3Aromatic hydrocarbon solvent, condensate oil, diesel oil, gasoline, naphtha and byproducts in chemical synthesis processes. The mechanism of action is to inject the solvent which is easy to dissolve and carry away the deposited wax into the oil well in batches or repeatedly after dissolving, and dissolve and carry away the deposited wax. When the amount of wax precipitation is very serious, a large amount of wax remover can be added into the pipeline for removing wax by the repeated action of circulation. In the oil-based wax remover, a surfactant is usually added to the oil-based wax remover to further improve the wax removing effect of the organic solvent by utilizing the wetting, penetrating, emulsifying and cleaning capabilities of the surfactant.
The wax removing water belongs to an important branch product in industrial cleaning agents. Cleaning processes are required in various fields of production and industrial processing, and the surfaces of workpieces such as metal, glass, plastic, spray coating, etc. are cleaned. The surface properties of various cleaned workpieces are different, but the cleaning purpose is consistent, the cleaning aims are to remove grease, wax dirt, organic residues, inorganic coating, metal oxide layers and other substances, and the cleaning effect also comprises a sterilization effect in the food industry and factory sanitation.
The wax removing water is one kind of industrial detergent, which is compounded with water as solvent and surfactant as active matter and has certain functions as assistant, and is used as chemical agent for polishing and cleaning hardware, and may be used widely in electroplating, clock, tableware, handicraft, etc. The wax removing water is mainly used for removing and cleaning wax stains by reducing the interfacial tension of the wax stains and workpieces through comprehensive processes of wetting, permeating, stripping, compatibilization and the like.
The water-based wax remover takes water as a dispersion medium, a surfactant as a main agent and a solvent as an auxiliary agent, and simultaneously, some inorganic salts and corrosion inhibitors are added. The surfactant is prepared by a wetting inversion method, so that the wax deposition surface is inverted from the original oleophilic surface to the hydrophilic surface, and the wax removal is facilitated. And the penetration of the surfactant can weaken the force between the wax molecules and the metal workpiece and thus can be removed from the surface of the metal workpiece. Commonly used surfactants are water soluble 6501, AEO-9, peregal type, etc. Inorganic salt assistants include phosphates, pyrophosphates, sodium silicates, sodium phosphates, and the like, and therefore they have a synergistic effect on surfactants. Commonly used metal corrosion inhibitor inhibitors include triethanolamine, potassium pyrophosphate, oleic soap, and the like. The water-based wax remover mainly removes wax attached to the surface of a metal workpiece through the reverse action, wetting action, penetrating action and cleaning action of a surfactant. Therefore, its use effect is temperature controlled.
A method for analyzing a surfactant in wax removal water comprises the following steps: filtering the wax removing water, adding fluoroquinoline in 0.5-1.5 wt% of the wax removing water, and ultrasonic treating.
In some embodiments, the filtration is first through a buchner funnel and then through a 0.45 μm filter.
In some embodiments, the temperature of the sonication is between 55 and 65 ℃.
In some embodiments, the sonication time is 10-30 min.
In some embodiments, the fluoroquinoline is selected from one of 3-fluoroquinoline, 4-fluoroquinoline, 5-fluoroquinoline, 6-fluoroquinoline, 7-fluoroquinoline, 8-fluoroquinoline.
In some embodiments, the fluoroquinoline is selected from one of 5-fluoroquinoline, 6-fluoroquinoline, 7-fluoroquinoline, 8-fluoroquinoline.
In some embodiments, the dewaxed water is used for stainless steel and/or carbon steel.
The wax removing water for stainless steel or carbon steel has high requirements, and has high requirements on rust resistance, low foaming property, stability and wax removing capability. Antirust property: the metal sample is required to have the functions of rust prevention and corrosion inhibition after being washed by the wax removing agent. Low foaming property: at present, common cleaning is completed by the action of an ultrasonic instrument, but under the vibration of ultrasonic waves, the wax remover generates more foams, and in order to avoid using effects, the product is required to have low-foam performance. Stability: it must be ensured that the wax remover should not precipitate, delaminate and suspend during use, which requires a good compatibility of the wax remover. No corrosion: in order not to corrode the metal parts and not to damage the appearance of the finished parts, the wax remover must have the ability not to corrode the metal specimen. After the antirust property, the low foaming property and the stability meet the requirements, the wax removing capability of the wax remover becomes the only factor for the good and bad water performance of the wax. The type and formulation of the selected surfactant in the wax removing water formula determine the wax removing rate. The cleaning agent prepared by only using one surfactant has unsatisfactory wax removing effect and low foaming property, but the cleaning agent prepared by compounding two or more surfactants has excellent wax removing effect and foaming resistance and can be used for rinsing. But also remarkably increases the rust resistance and the corrosiveness. At present, the wax removing water on the market in China basically contains 6 to 8 or more surfactants. The main purpose is to improve the wax removal efficiency. In fact, people already compound the nonionic surfactant and the anionic surfactant, and the cloud point range of the nonionic surfactant is expanded by adding the ionic surfactant, so that mixed micelles can be formed. Due to the insertion of the molecules of the nonionic surfactant, the repulsion of the ion parts between the ionic surfactants is reduced, and then through the interaction between the hydrophobic chain micelles of the two surfactants, the generation of micelles is easier, so that the critical micelle value of the solution is reduced, the surface tension is also reduced, and the surface activity is increased.
Because of the large number of surfactants, it is a very important question of how well the surfactants are qualitatively and quantitatively accurate when performing the analysis.
There are many types of surfactants, if classified according to their uses, but the classification is rather vague, and the chemical structure of the surfactant is not clearly indicated, but only one use is emphasized. The surfactants are classified herein into four broad categories, primarily based on their ionization characteristics in aqueous solutions: anionic, cationic, amphoteric and nonionic surfactants.
The anionic surfactant has the characteristics of good penetration, wetting, dispersion, neutrality and the like, and except the sulfonate, other varieties are not acid-resistant. The cationic surfactant has good penetration and decontamination capability, high foam, bactericidal effect and corrosion inhibition effect on metals, but has higher price. The zwitterionic surfactant has good decontamination, bubble and emulsification capabilities, good hard water resistance, corrosion inhibition and small irritation to skin. The nonionic surfactant has high surface activity, acid and alkali resistance and cloud point.
In the dewaxing water for stainless steel or carbon steel, many surfactants with better emulsifying, penetrating and solubilizing abilities are adopted, and the considered components include but are not limited to: coconut oil diethanolamide (6501), coconut oil diethanolamide phosphate (6503), fatty alcohol polyoxyethylene ether (AEO-9), nonylphenol polyoxyethylene ether phosphate (TX-10), fatty alcohol polyoxyethylene ether sodium sulfate (AES), sodium dodecyl benzene sulfonate (LAS), and the like.
Due to the wide variety of surfactants, the polarity and boiling point are very close. The prior art has technical resistance when analyzing wax removing water, particularly when analyzing by adopting liquid chromatography. In the invention, the inventor finds that the fluoroquinoline is added in the analysis process of the wax removing water, so that a good bubble inhibiting effect can be achieved on the wax removing water, the subsequent operations of centrifugation, filtration and the like are facilitated, and after the fluoroquinoline is added, the inaccurate qualitative and quantitative result caused by flocculent precipitates can not be generated. However, the fluoroquinoline is filtered before being added, and metal-containing components in the wax removing water are removed, so that the accuracy of the analysis result is influenced. The inventors speculate that fluoroquinoline may be easily coordinated with metal ions.
In some embodiments, the method further comprises the step of performing the analysis by HPLC or LC-MS after the ultrasonic treatment.
In some embodiments, the mobile phase of the HPLC is methanol and water and the chromatography column is a C18 column.
In some embodiments, the mass spectrum in the LC-MS is a triple quadrupole.
The operation of the analysis by HPLC or LC-MS and the resolution of the spectra are well known to the person skilled in the art. The qualitative determination can be carried out by mass spectrometry, and can also be carried out by an internal standard method or an external standard method. Quantification can be analyzed in terms of peak area.
The invention is further illustrated by the following specific examples.
The paraffin removal water sample is the paraffin removal water for carbon steel directly purchased from the market, and comprises AEO-74 wt%, AEO-94 wt%, AEO-106 wt%, 65012 wt% and 65038 wt%.
Example 1
A method for analyzing a surfactant in wax removal water comprises the following steps: the dewaxing water was filtered, and then 1 wt% of 6-fluoroquinoline to the dewaxing water was added and subjected to ultrasonic treatment. After sonication, analysis was performed by HPLC.
The filtration was first through a buchner funnel and then through a 0.45 μm filter. The temperature of the sonication was 60 ℃. The time of the ultrasonic treatment is 20 min. The mobile phase of the HPLC is methanol and water, and the chromatographic column is a C18 column.
And (3) testing results: contains AEO-74 wt%, AEO-94 wt%, AEO-106 wt%, 65012 wt% and 65038 wt%.
Example 2
A method for analyzing a surfactant in wax removal water comprises the following steps: the dewaxing water was filtered, and then 1 wt% of 6-fluoroquinoline to the dewaxing water was added and subjected to ultrasonic treatment. After sonication, analysis was performed by LC-MS.
The filtration was first through a buchner funnel and then through a 0.45 μm filter. The temperature of the sonication was 60 ℃. The time of the ultrasonic treatment is 20 min. The mass spectrum in the LC-MS is a triple quadrupole.
And (3) testing results: contains AEO-74 wt%, AEO-94 wt%, AEO-106 wt%, 65012 wt% and 65038 wt%.
Example 3
A method for analyzing a surfactant in wax removal water comprises the following steps: the dewaxing water was filtered, and then 0.5 wt% of 3-fluoroquinoline with respect to the dewaxing water was added and subjected to ultrasonic treatment. After sonication, analysis was performed by HPLC.
The filtration was first through a buchner funnel and then through a 0.45 μm filter. The temperature of the sonication was 60 ℃. The time of the ultrasonic treatment is 20 min. The mobile phase of the HPLC is methanol and water, and the chromatographic column is a C18 column.
And (3) testing results: contains AEO-73.8 wt%, AEO-94.1 wt%, AEO-106.2 wt%, 65012.2 wt% and 65038.1 wt%.
Example 4
A method for analyzing a surfactant in wax removal water comprises the following steps: the dewaxing water was filtered, and then 1.5 wt% of 7-fluoroquinoline with respect to the dewaxing water was added and subjected to ultrasonic treatment. After sonication, analysis was performed by LC-MS.
The filtration was first through a buchner funnel and then through a 0.45 μm filter. The temperature of the sonication was 60 ℃. The time of the ultrasonic treatment is 20 min. The mass spectrum in the LC-MS is a triple quadrupole.
And (3) testing results: contains AEO-74.1 wt%, AEO-94.2 wt%, AEO-105.8 wt%, 65012 wt% and 65037.8 wt%.
Comparative example 1
A method for analyzing a surfactant in wax removal water comprises the following steps: 6-fluoroquinoline was added to the wax removing water in an amount of 1 wt% relative to the wax removing water, and the mixture was subjected to ultrasonic treatment. After sonication, analysis was performed by HPLC.
The filtration was first through a buchner funnel and then through a 0.45 μm filter. The temperature of the sonication was 60 ℃. The time of the ultrasonic treatment is 20 min. The mobile phase of the HPLC is methanol and water, and the chromatographic column is a C18 column.
And (3) testing results: comprises AEO-71 wt%, AEO-92 wt%, AEO-103 wt%, 65010 wt% and 65034 wt%.
Comparative example 2
A method for analyzing a surfactant in wax removal water comprises the following steps: 7-fluoroquinoline was added to the wax removing water in an amount of 1.5% by weight relative to the wax removing water, and the mixture was subjected to ultrasonic treatment. After sonication, analysis was performed by LC-MS.
The filtration was first through a buchner funnel and then through a 0.45 μm filter. The temperature of the sonication was 60 ℃. The time of the ultrasonic treatment is 20 min. The mass spectrum in the LC-MS is a triple quadrupole.
And (3) testing results: contains AEO-71 wt%, AEO-93 wt%, AEO-104 wt%, 65010.5 wt% and 65036 wt%.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (9)
1. An analytical method of a surfactant in wax removal water is characterized by comprising the following steps: filtering the wax removing water, adding fluoroquinoline in 0.5-1.5 wt% of the wax removing water, and performing ultrasonic treatment; after sonication, analysis was performed by HPLC or LC-MS.
2. The method of claim 1, wherein the filtration is performed by a Buchner funnel followed by a 0.45 μm filter.
3. The method of claim 1, wherein the temperature of the sonication is between 55 ℃ and 65 ℃.
4. The method for analyzing surfactant in wax-removed water according to claim 1, wherein the time of the ultrasonic treatment is 10-30 min.
5. The method for analyzing surfactant in wax-removing water according to claim 1, wherein the fluoroquinoline is one selected from the group consisting of 3-fluoroquinoline, 4-fluoroquinoline, 5-fluoroquinoline, 6-fluoroquinoline, 7-fluoroquinoline and 8-fluoroquinoline.
6. The method for analyzing surfactant in wax-removing water according to claim 1, wherein the fluoroquinoline is one selected from the group consisting of 5-fluoroquinoline, 6-fluoroquinoline, 7-fluoroquinoline and 8-fluoroquinoline.
7. The method for analyzing surfactant in paraffin removal water according to claim 1, wherein the paraffin removal water is used for stainless steel and/or carbon steel.
8. The method for analyzing surfactant in wax-removed water according to claim 1, wherein the mobile phase of HPLC is methanol and water, and the chromatographic column is C18 column.
9. The method of claim 1, wherein the mass spectrum in LC-MS is a triple quadrupole.
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