CN1362281A - Emulsifier for metal-machining emulsified oil and emulsified oil composition - Google Patents
Emulsifier for metal-machining emulsified oil and emulsified oil composition Download PDFInfo
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- CN1362281A CN1362281A CN01106029.8A CN01106029A CN1362281A CN 1362281 A CN1362281 A CN 1362281A CN 01106029 A CN01106029 A CN 01106029A CN 1362281 A CN1362281 A CN 1362281A
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Abstract
The emulsified oil composition for general machining metal comprises emulsifying agent, emulsification adjuvant, antirusting agent, extreme pressure compound, preservative, cosolvent, defoaming agent and basis oil, in which the emulsifying agent is obtained by the following steps: polymerizing mono-olefines in C4 and C5 to obtain low-molecular olefinic polymer (Mn=200-3000), then making it and carboxylic acid or carboxylic anhydride produce additive reaction to obtain polyolefine carboxylic acid or polyolefine carboxylic anhydride, then making them and polybasic alcohol, alcohol amine or alkali implement esterification or saponification react under the action of catalyst to obtain the invented emulsifying agent.
Description
The present invention relates to a kind of oil emulsion with emulsifying agent and emulsified oil composition thereof, especially for the oil emulsion emulsifying agent and the emulsified oil composition thereof of metal processing usefulness.
Metal-machining emulsified oil can be divided into 4 types by SY 1374-77 standard, 1,2,3, No. 4 oil emulsions, wherein No. 1 oil emulsion has excellent lubricity, rust-preventing characteristic, cleaning, cooling simultaneously, No. 2 oil emulsion rust-preventing characteristics, cooling property are better, No. 3 oil emulsion extreme pressure properties, cooling property are good, and No. 4 oil emulsion cooling property, cleaning are good.4 kinds of oil emulsions are according to different purposes, emulsifier type and addition difference separately.The lipophilic group of the used emulsifying agent of prior art generally is synthetic fatty acid, synthetic fatty alcohol, alkyl phenol, vegetable and animals oils.So emulsifying agent is C among the CN1031392A
8～C
30Fatty acid mixed, sulfonated castor oil, the emulsifying agent that relates among the CN1057478A is neopelex, dodecyl sodium sulfate, Nonyl pheno (10) ether, the lipophilic group reparation technology in the above-mentioned emulsifying agent is complicated, perhaps price is higher.
The object of the present invention is to provide a kind of emulsifying agent and preparation method thereof of metal-machining emulsified oil of abundant, cheap, the function admirable of originating, another object of the present invention is to provide the metal-machining emulsified oil composition.
Emulsifying agent of the present invention adopts following method preparation: polyolefin and carboxylic acid or acid anhydrides carry out addition reaction and generate polyolefin carboxylic acid or polyolefin acid anhydrides, and polyolefin carboxylic acid or polyolefin acid anhydrides and hydroxy compounds advance esterification and make emulsifying agent of the present invention; Or polyolefinic acid or polyolefin acid anhydrides and alkali carry out the emulsifying agent that saponification makes the another kind of type of the present invention.The viscosity of gained emulsifying agent is that viscosity is 3～1000, is preferably 5～200, is preferably 10～100, (100 ℃ of mm
2/ s).Polyolefin-based number-average molecular weight is 200～3000, better is preferably 300～2000, is preferably 400～1000.
Polyolefin carboxylic acid or polyolefin acid anhydrides and hydroxy compounds esterification condition are among the preparation method of emulsifying agent of the present invention: add polyolefin carboxylic acid or polyolefin acid anhydrides and hydroxy compounds (removing oxirane) in reaction vessel, its mol ratio is 1: 0.2～5, and adding concentration is NaOH, the KOH aqueous solution, the 98%H of 20w%-50w%
2SO
4Or a kind of in the p-methyl benzenesulfonic acid, its use amount is 0.05w%-1.5w%, be preferably the silicon oil foam killer (accounting for polyolefin carboxylic acid or acid anhydrides and hydroxy compounds mixture) of 0.5w%-1.0w% and 0.05w%-0.5w%, be preferably 0.05w%-0.1w%, reach-0.02MPa--0.10MPa at 100-250 ℃, be preferably-the 0.04MPa--0.08MPa condition under reaction 2-10 hour, preferably 3-8 hour, finally obtain emulsifying agent of the present invention.Above-mentioned reactant hydroxy compounds is one or more hydroxy compounds, and its hydroxyl value is at least 2.The reactant hydroxy compounds comprises poly-HO-(CH
2CH
2O)
n-H is n=1～50 wherein, preferably n=4～20, ethylene glycol 200, PEG400, polyethylene glycol 800, cetomacrogol 1000, Macrogol 2000, Macrogol 4000, cetomacrogol 1000 0, MEA, diethanol amine, triethanolamine, glycerine, sorbierite, pentaerythrite.
Above-mentioned reactant polyolefin carboxylic acid or polyolefin acid anhydrides are preferably selected the polyisobutenyl maleic anhydride for use, and its saponification number can be selected 30～350mgKOH/g for use, preferably select 100～250mgKOH/g for use.
The used defoamer of above-mentioned reaction can be selected polyethers or silicone oil defoamer for use, preferably selects the silicone oil defoamer for use.
If adopt saponification to prepare emulsifying agent of the present invention, then its reaction condition is: adding polyolefin-based carboxylic acid of reactant or acid anhydrides and alkali mol ratio in reaction vessel is 1: 1～5.Alkali is NaOH, potassium hydroxide, lithium hydroxide, calcium hydroxide, magnesium hydroxide, barium hydroxide.Preferably select NaOH, potassium hydroxide for use, polyolefin-based carboxylic acid or acid anhydrides and its mol ratio be preferably 1: 2.1～and 2.5.Reaction time is 5-60 minute, 50～100 ℃ of saponification temperatures.
Emulsifying agent of the present invention can be made and be easy to form oil-in-water emulsifiers, also can make and be easy to form water-in-oil emulsifier.The VB value of water-in-oil emulsifier should be 0.01～0.99; And the VB value of oil-in-water emulsifiers should be 1.01～6.The VB value that is used for the emulsifying agent of oil emulsion after the blending requires greater than 1." surfactant types decision method research---volumetric balance (VB) value method " paper in " the 9th the industrial surface activity agent Technological Economy in the whole nation with use open proceeding " that the VB value calculating method sees that " fine chemistry industry " editorial office 2000 publishes.
Emulsifying agent of the present invention can be used for various metal-machining emulsified oils, and its oil emulsion (except that emulsifying agent) is made up of assistant for emulsifying agent, antirust agent, extreme pressure agent, anticorrisive agent, cosolvent, defoamer, base oil.
Help emulsion to be selected from odium stearate, enuatrol, potassium stearate, potassium oleate, lecithin, phosphoric acid fat, AEO (10), aliphatic acid polyethenoxy ether (15), APES (7), aliphatic amine polyoxyethylene ether (15), polyethylene glycol (400), tall oil acid amides, dodecyl sodium sulfate, dodecyl alcohol acyl phosphate.
Antirust agent is divided into two kinds: oil-soluble antirust agent and water soluble anti-rust agent, oil-soluble antirust agent are selected from several mixtures in petroleum sodium sulfonate, calcium mahogany sulfonate, barium mahogany sulfonate, dinonyl naphthalene sulfonate barium, zinc naphthenate, aluminum stearate, oxidized petrolatum, oxidized petrolatum barium soap, dodecenylsuccinic acid, the BTA.Water soluble anti-rust agent is selected from one or more mixtures of natrium nitrosum, potassium chromate, sodium dichromate, sodium metasilicate, sodium pyrophosphate, sodium orthophosphate, Sodium Benzoate, triethanolamine.
Extreme pressure agent is selected from one or more mixtures of chlorinated paraffin wax, chlorination stearic acid, sulfuration oleic acid, sulfuration lard, sulfuration cotton seed oil, tributyl phosphate.
Anticorrisive agent is selected from pentachlorophenol, tetra-chloro-phenol, O-SyL, 2,4 dinitrophenol dinitrophenolates, 2-methylol-2 nitro-1, one or more mixtures of ammediol.
Cosolvent is selected from one or more mixtures of water, methyl alcohol, ethanol, diethanol amine, triethanolamine.
Defoamer is selected from one or more mixtures of polyethers, methyl-silicone oil, hydroxy silicon oil, amido silicon oil, silica.
Base oil be selected from subtract two cut dewaxed oils, subtract three cut dewaxed oils, a kind of or several mixtures of 150SN, 650SN, 120BS, 150BS.
The characteristics of No. 1 oil emulsion are antirust better, and the rust-preventing characteristic of its 2% emulsion is 48 hours to one-level cast iron monolithic, and lamination is 8 hours, compare all many one times of time requirement with other No. three oil emulsions.But cleaning is relatively poor, and cooling, lubricity is general.From composition, it has more base oil and less emulsifying agent, and the outward appearance of emulsion is creamy white for this reason.This class oil emulsion also is usually a large amount of employed a kind of, and its actual working concentration mostly is 2～5%.Sometimes in order to improve cleaning, can make concentration reduce to 1～2%, concentration can be brought up to 10～20% again in order to improve lubricity.
No. 1 oil emulsion by weight consists of:
One or more emulsifying agents of emulsifying agent of the present invention: 10～25%
Oil-soluble antirust agent: 5～15%
Water soluble anti-rust agent: 0.1～2.5%
Assistant for emulsifying agent: 1～5%
Cosolvent: 0.1～5%
Defoamer: 0.0001～0.2%
Anticorrisive agent: 0.01～1%
Base oil: surplus.
The characteristics ground of No. 2 oil emulsions cleans, cooling is better, antirust, lubricity is general, and it mainly is applicable to mill processing.Its good cleaning can prevent the sticking stifled emery wheel of abrasive dust thing, and good cooling can prevent that part from being burnt in mill processing.From composition, it contains the amount of base oil and lacks than No. 1 oil emulsion, and the amount of emulsifying agent than No. 1 oil emulsion for many, the outward appearance of the emulsion dispersed system that is translucent also promptly is bordering on the solubilising state more for this reason.Its working concentration in mill processing mostly is 2～3%.
No. 2 oil emulsions by weight consist of:
One or more emulsifying agents of emulsifying agent of the present invention: 15～30%, VB value＞1 of blending back emulsifying agent
Oil-soluble antirust agent: 3～5%
Water soluble anti-rust agent: 0.1～2.5%
Assistant for emulsifying agent: 1～5%
Cosolvent: 0.1～5%
Defoamer: 0.0001～0.2%
Anticorrisive agent: 0.01～1%
Base oil: surplus.
No. 3 oil emulsion can claim extreme emulsified oil again, and it is applicable to that mainly the higher machining of lubricating requirement makes lubricant usefulness, because this class process velocity is slower, cutting force is less, and heat radiation power is little, so less demanding to cooling property.This class oil emulsion has also added the extreme pressure oiliness additive except adding emulsifying agent, base oil, as chlorinated paraffin wax, chlorination stearic acid etc., to improve the boundary lubrication ability of aqueous emulsion, it is the P of aqueous emulsion really
kValue (being that oil film is destroyed from critical load) can be pressed the SY1374-77 standard, No. 3 P up to becoming more than 100 kilograms
kValue should be not less than kilogram.And the aqueous emulsion of general No. 1 oil emulsion is less than kilogram.The concentration that this class emulsion uses is higher, is generally 15～25%, and it is light brown to brown that the outward appearance of emulsion mostly is.In actual use, its aqueous emulsion can be made lubricant usefulness for edible oil and sulfurized oil, and the emulsion of 20% No. 1 extreme emulsified oil can be applicable to nut and reins in light according to reports.Service life of workpiece surface quality and cutter, mould is not had reach or be better than the level that edible oil and sulfurized oil are made lubricant.The aqueous emulsion of 24% No. 3 extreme emulsified oils can be applicable to tapping, operations such as gear shaping.
No. 3 oil emulsions by weight consist of:
One or more emulsifying agents of emulsifying agent of the present invention: 10～25%
Oil-soluble antirust agent: 5～15%
Water soluble anti-rust agent: 0.1～2.5%
Assistant for emulsifying agent: 2～5%
Extreme pressure agent: 10～25%
Cosolvent: 0.1～5%
Defoamer: 0.0001～0.2%
Anticorrisive agent: 0.01～1%
Base oil: surplus.
No. 4 oil emulsion is a transparent type, and it is applicable to the extraordinary metal processing cooling that requires, and also can make cooling liquid of IC engine.The NL oil emulsion promptly belongs to this class, and its aqueous emulsion is the semi-homogeneous dispersion, and this class oil emulsion is similar, but its emulsifier content is more than No. 2 missible oil, has been widely used as the train cooling liquid of IC engine at the NL oil emulsion.
No. 4 oil emulsions by weight consist of:
One or more emulsifying agents of emulsifying agent of the present invention: 20～40%
Oil-soluble antirust agent: 2～5%
Water soluble anti-rust agent: 0.1～2.5%
Assistant for emulsifying agent: 2～5%
Cosolvent: 0.1～5%
Defoamer: 0.0001～0.2%
Anticorrisive agent: 0.01～1%
Base oil: surplus.
The emulsifying agent of metal-machining emulsified oil provided by the invention has the following advantages:
1. the present invention is a primary raw material with the wide material sources that produced in oil refining, the chemical process, cheap carbon four, carbon pentaene hydrocarbon, and therefore the cost of the emulsifying agent of being produced is low.
2. carbon four, C 5 monoolefin are more unmanageable hydro carbons in addition, and other processing method such as hydration method etc. need the higher alkene of purity, and its purification and disposal cost are all very high.The purity requirement of emulsifying agent material carbon four, C 5 monoolefin that is used for oil emulsion of the present invention is not high, has saved the expense that a large amount of separation are purified.
3. the alkene of preparation emulsifying agent can be that mixture needn't separate, also needn't separate with the product behind binary acid or the anhydride reaction, directly also needn't separate and promptly can be used as emulsifying agent with the polyol reaction afterproduct, emulsifying agent has saved refining separation process in process of production like this, and producing cost reduces greatly.
4. emulsifying agent of the present invention not only has emulsifiability, also has rustless property, greasy property simultaneously, can prepare the oil emulsion of all kinds function admirable.
Below by instantiation the synthetic application that reaches in oil emulsion of emulsifying agent of the present invention is described.
Table 1 esterification prepares emulsifying agent of the present invention
| Embodiment | ????1 | ????2 | ????3 | ????4 | ????5 | ??6 | ??7 |
| Polyolefin acid anhydrides acid number (KOH/mg) | ????350 | ????30 | ????240 | ????75 | ????100 | ??160 | ??79 |
| The polyolefin number-average molecular weight | ????200 | ????3000 | ????350 | ????1200 | ????800 | ??500 | ??1100 |
| Hydroxy compounds | Triethanolamine | Polyoxyethylene mystery (40 | Diethanol amine | Triethanolamine | Glycerine | Polyoxyethylene mystery (10) | Pentaerythrite |
| Esterification temperature ℃ | ????100 | ????250 | ????120 | ????140 | ????160 | ??180 | ??200 |
| Esterification time (branch) | ????2 | ????10 | ????3 | ????4 | ????9 | ??6 | ??7 |
| Polyolefin acid anhydrides: hydroxy compounds | ????1∶3.5 | ????1∶0.5 | ????1∶2.2 | ????1∶2 | ????1∶2.5 | ??1∶4 | ??1∶4.5 |
| Esterification catalyst | ????NaOH | ????KOH | ????H 2SO 4 | ????NaOH | P-methyl benzenesulfonic acid | ??KOH | ??NaOH |
| Esterification catalyst consumption w% | ????0.05 | ????1.5 | ????0.07 | ????0.09 | ????0.1 | ??0.5 | ??0.8 |
| Esterification silicon oil foam killer w% | ????0.05 | ????0.5 | ????0.07 | ????0.09 | ????0.1 | ??0.2 | ??0.3 |
| Vacuum (MPa) | ????0.02 | ????0.10 | ????0.03 | ????0.04 | ????0.05 | ??0.06 | ??0.07 |
| Acid number (KOH/mg) | ????15 | ????20 | ????19 | ????28 | ????11.5 | ??17 | ??13 |
| The VB value | ????1.44 | ????1.01 | ????1.11 | ????0.24 | ????0.17 | ??1.51 | ??0.11 |
Table 2 saponification prepares emulsifying agent of the present invention
Embodiment 11:(1 oil emulsion)
| Embodiment | ????8 | ????9 | ????10 |
| The polyolefin number-average molecular weight | ????400 | ????450 | ????700 |
| Polyolefin acid anhydrides acid number (KOH/mg) | ????200 | ????150 | ????130 |
| Alkali | NaOH | Potassium hydroxide | Calcium hydroxide |
| Polyolefin acid anhydrides: alkali (mol ratio) | ????1∶2.5 | ????1∶3.5 | ????1∶1.5 |
| Saponification temperature ℃ | ????75 | ????85 | ????95 |
| Saponification time (branch) | ????35 | ????40 | ????45 |
| The VB value | ????2.01 | ????2.61 | ????0.38 |
Embodiment 1 emulsifying agent 12
Triethanolamine 3
Petroleum sodium sulfonate 3
Barium mahogany sulfonate 3
Sodium Benzoate 0.3
BTA 0.3
Water 0.4
150SN base oil surplus embodiment 12:(2 oil emulsion)
Embodiment 4 emulsifying agents 7
Embodiment 8 emulsifying agents 15
Triethanolamine 3
Tetra-chloro-phenol 0.2
Water 1
150SN base oil surplus embodiment 13:(3 oil emulsion)
Embodiment 6 emulsifying agents 20
Triethanolamine 3
No. 52 chlorinated paraffin waxs 6
Sodium Benzoate 0.5
BTA 1
Water 1.4
150SN base oil surplus embodiment 14:(4 oil emulsion)
Embodiment 2 emulsifying agents 22
Embodiment 9 emulsifying agents 12
Triethanolamine 3
No. 52 chlorinated paraffin waxs 3
Sodium Benzoate 0.3
BTA 0.3
Water 0.4
150SN base oil surplus
Comparative example 1: barium mahogany sulfonate 12
Dodecenylsuccinic acid 2
Oleic acid 11.5
Triethanolamine 3
No. 20 or No. 30 machine oil surpluses
Comparative example 2: higher fatty acids triethanolamine 6～9
OP-3??????????????????????9～6
Water 2～5
No. 5 or No. 7 high-speed engine oil surpluses
Comparative example 3: sulfonated castor oil 10
Chlorinated paraffin wax 40
No. 20 machine oil 40
40%NaOH transfers to alkalescent 10
Comparative example 4: petroleum sodium sulfonate 34.9
Triethanolamine 8.7
Oleic acid 16.6
Ethanol 4.9
No. 10 machine oil 34.9
Phenolethanolamine 0.2
Above-mentioned comparative example form come from " antirust technology " China rotten with the chief editor of protection association. the .1988 of Chemical Industry Press December.
The performance of table 3 oil emulsion of the present invention
| Embodiment | The mother liquor outward appearance | 5% dilution outward appearance | 5% dilution pH value | Extreme pressure property PB value, Kg | Rust-preventing characteristic (35 ℃, one-level cast iron sheet), h | |
| Monolithic | Lamination | |||||
| Embodiment 11 | Brown transparent | Milky | ??8.5 | ????/ | ??48 | ??8 |
| Embodiment 12 | Brown transparent | Microemulsion | ??8 | ????/ | ??24 | ??4 |
| Embodiment 13 | Brown transparent | Milky | ??8.5 | ????70 | ??24 | ??4 |
| Embodiment 14 | Brown transparent | Transparent | ??9 | ????/ | ??24 | ??4 |
| Comparative example 1 | Brown transparent | Milky | ??8.5 | ????/ | ??48 | ??8 |
| Comparative example 2 | Brown transparent | Microemulsion | ??8 | ????/ | ??24 | ??4 |
| Comparative example 3 | Brown transparent | Milky | ??8.5 | ????70 | ??24 | ??4 |
| Comparative example 4 | Brown transparent | Transparent | ??9 | ????/ | ??24 | ??4 |
As can be seen from the above table, oil emulsion of the present invention is suitable with classical oil emulsion performance, but owing to used cheap emulsified dose of the present invention, makes the cost of oil emulsion reduce greatly.
Claims (13)
1, a kind of machining oil emulsion emulsifying agent obtains by polyolefin-based carboxylic acid or acid anhydrides and hydroxy compounds esterification or with alkali soapization, and wherein polyolefin-based number-average molecular weight is 200～3000.
2, according to the described emulsifying agent of claim 1, it is characterized in that its VB value is 0.1～3, viscosity is 3～1000 (100 ℃ of mm
2/ s).
3,, it is characterized in that described polyolefin-based number-average molecular weight is 300～2000 according to claim 1 or 2 described emulsifying agents.
4,, it is characterized in that described acid or acid anhydrides substituting group are from maleic acid, maleic anhydride, fumaric acid, glutaric acid or adipic acid according to the described emulsifying agent of claim 1.
5,, it is characterized in that described acid or acid anhydrides substituting group are from maleic anhydride according to claim 1 or 4 described emulsifying agents.
6,, it is characterized in that described hydroxy compounds substituting group is from HO-(CH according to the described emulsifying agent of claim 1
2CH
2O)
n-H is one or more in n=1～50, Macrogol 200, PEG400, polyethylene glycol 800, cetomacrogol 1000, Macrogol 2000, Macrogol 4000, cetomacrogol 1000 0, MEA, diethanol amine, triethanolamine, glycerine, sorbierite, the pentaerythrite wherein.
7,, it is characterized in that described base substituting group is among Na, Ca, K, Mg, Ba, the Li one or more according to the described emulsifying agent of claim 1.
8, the preparation method of the described emulsifying agent of a kind of claim 1, its process comprises: polyolefin and carboxylic acid or acid anhydrides carry out addition reaction and generate polyolefin carboxylic acid or polyolefin acid anhydrides, and polyolefin carboxylic acid or polyolefin acid anhydrides and hydroxy compounds carry out esterification or carry out saponification with alkali making emulsifying agent of the present invention.
9, a kind of metal-machining emulsified oil,, assistant for emulsifying agent outer by the described emulsifying agent of claim 1, antirust agent, extreme pressure agent, anticorrisive agent, cosolvent, defoamer and base oil are formed.
10, according to the described oil emulsion of claim 9, it is characterized in that having following weight and form, constitute No. 1 oil emulsion:
One or more of claim 1 emulsifying agent: 10～25%
Oil-soluble antirust agent: 5～15%
Water soluble anti-rust agent: 0.1～2.5%
Assistant for emulsifying agent: 1～5%
Cosolvent: 0.1～5%
Defoamer: 0.0001～0.2%
Anticorrisive agent: 0.01～1%
Base oil: surplus.
11, according to the described oil emulsion of claim 9, it is characterized in that having following weight and form, constitute No. 2 oil emulsion:
One or more of claim 1 emulsifying agent: 15～30%
Oil-soluble antirust agent: 3～5%
Water soluble anti-rust agent: 0.1～2.5%
Assistant for emulsifying agent: 1～5%
Cosolvent: 0.1～5%
Defoamer: 0.0001～0.2%
Anticorrisive agent: 0.01～1%
Base oil: surplus.
12, according to the described oil emulsion of claim 9, it is characterized in that having following weight and form, constitute No. 3 oil emulsion:
One or more of claim 1 emulsifying agent: 10～25%
Oil-soluble antirust agent: 5～15%
Water soluble anti-rust agent: 0.1～2.5%
Assistant for emulsifying agent: 2～5%
Extreme pressure agent: 10～25%
Cosolvent: 0.1～5%
Defoamer: 0.0001～0.2%
Anticorrisive agent: 0.01～1%
Base oil: surplus.
13, according to the described oil emulsion of claim 9, it is characterized in that having following weight and form, constitute No. 4 oil emulsion:
One or more of claim 1 emulsifying agent: 20～40%
Oil-soluble antirust agent: 2～5%
Water soluble anti-rust agent: 0.1～2.5%
Assistant for emulsifying agent: 2～5%
Cosolvent: 0.1～5
Defoamer: 0.0001～0.2
Anticorrisive agent: 0.01～1%
Base oil: surplus.
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| CN1152737C CN1152737C (en) | 2004-06-09 |
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