CN106467768A - A kind of antioxidation micro-emulsion cutting fluid and preparation method thereof - Google Patents

A kind of antioxidation micro-emulsion cutting fluid and preparation method thereof Download PDF

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CN106467768A
CN106467768A CN201610765001.4A CN201610765001A CN106467768A CN 106467768 A CN106467768 A CN 106467768A CN 201610765001 A CN201610765001 A CN 201610765001A CN 106467768 A CN106467768 A CN 106467768A
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江海涛
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Tianchang Runda Metal Antirust Auxiliary Co Ltd
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Tianchang Runda Metal Antirust Auxiliary Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00—Lubricating compositions containing more than 10% water
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/04—Metals; Alloys
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    • C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/285—Esters of aromatic polycarboxylic acids
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/287—Partial esters
    • C10M2207/289—Partial esters containing free hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/08—Amides
    • C10M2215/082—Amides containing hydroxyl groups; Alkoxylated derivatives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/221—Six-membered rings containing nitrogen and carbon only
    • C10M2215/222—Triazines
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/08—Thiols; Sulfides; Polysulfides; Mercaptals
    • C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/09—Heterocyclic compounds containing no sulfur, selenium or tellurium compounds in the ring
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    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
    • C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants

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  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses a kind of antioxidation micro-emulsion cutting fluid, it is made up of the raw material of following weight parts：Antioxidant 1010 12, isothiazolone 23,2 mercapto benzimidazoles 0.8 1, stearic acid monoglyceride 24, bromohexadecane 0.4 1, tetrabutyl ammonium bromide 0.3 1, the aqueous formic acid 20 30 of Copper hydrate 67,10 15%, CNT 45, methyl-silicone oil 50 60, dodecyl sodium sulfate 34, appropriate amount of water, phthalic acid ester 12, ammonium molybdate 23, aluminium stearate 0.6 1, N n-methylolacrylamide 12, sym-closene 0.8 1, lauryl mercaptan 24.By after the CNT after being esterified and Tubercuprose. mixing and ball milling, by pyrolysis, Cu2+ can be adsorbed in carbon nano tube surface to the present invention, generates nano copper particle in carbon nano tube surface.

Description

A kind of antioxidation micro-emulsion cutting fluid and preparation method thereof
Technical field
The present invention relates to cutting fluid technical field, more particularly, to a kind of antioxidation micro-emulsion cutting fluid and preparation method thereof.
Background technology
Because nanoparticle has the performance not available for a lot of Conventional solid, such as low melting point, high ductibility, easily diffusion Deng making its hardness, toughness！Anti-shearing degree etc. is it can also happen that change it means that cannot function as under normal circumstances lubricating material The solid particle of material, is possible to greasy property when being in Nano grade, and is likely to there is some different from tradition The boundary lubrication mechanism of additive；Secondly nano lubricating oil additive replaces the organic compound extreme-pressure anti-wears such as traditional S, P, Cl Additive is it is expected to solve S, P, Cl corrosion that parent metal is caused and the environmental problem brought；But nanoparticle is applied Friction-reducing and antiwear action in cutting fluid is it is also desirable to solve some difficult problems；
Because nanoparticle specific surface area is big！Surface energy is high, so in a solvent, especially in this non-aqueous Jie of lubricating oil In matter, easily reunite, if nanoparticle is agglomerated into big granule in lubricating oil, can drop on the contrary just as having impurity in oil Low lubricating oil performance " simultaneously, the dispersibility of nanoparticle and stability are two closely related and separate factors, Good dispersion, stability differs and reserves, in addition, cutting fluid be generally used for high temperature, under high pressure working environment, in cutting fluid itself The colloidal nanoparticles being in suspended state are highly vulnerable to breakage its stability under such working environment, thus occurring group poly and poly Heavy, finally make nanoparticle lose abrasion resistance；
Copper nanoparticle can effectively improve the frictional behaviour of cutting fluid as the additive of oiliness cutting fluid, but nanometer Stability in cutting fluid base oil for the copper powder needs to improve, so, this research and development bright by changing to the surface of CNT Property, prepares carbon nanotube/nano copper combined cut solution additive, to improve its in cutting fluid dispersion stabilization same When, reach the purpose improving cutting fluid frictional behaviour.
Content of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of antioxidation micro-emulsion cutting fluid and its system Preparation Method.
The present invention is achieved by the following technical solutions：
A kind of antioxidation micro-emulsion cutting fluid, it is made up of the raw material of following weight parts：
Antioxidant 1010 1-2, isothiazolone 2-3,2- mercapto benzimidazole 0.8-1, stearic acid monoglyceride 2-4, Bromohexadecane 0.4-1, tetrabutyl ammonium bromide 0.3-1, the aqueous formic acid 20-30 of Copper hydrate 6-7,10-15%, carbon nanometer Pipe 4-5, methyl-silicone oil 50-60, dodecyl sodium sulfate 3-4, appropriate amount of water, phthalic acid ester 1-2, ammonium molybdate 2-3, stearic acid Aluminum 0.6-1, N hydroxymethyl acrylamide 1-2, sym-closene 0.8-1, lauryl mercaptan 2-4.
A kind of preparation method of described antioxidation micro-emulsion cutting fluid, comprises the following steps：
(1) above-mentioned Copper hydrate is added in the deionized water of its weight 20-35 times, under stirring condition, Deca is above-mentioned The aqueous formic acid of 10-15%, rises high-temperature and is 80-85 DEG C, insulated and stirred to water is done, and obtains carboxylic acid nanometer after completion of dropping Copper；
(2) above-mentioned CNT being added to mass ratio is 3-4:In 1 sulphuric acid, the mixed solution of nitric acid, described sulfur The concentration of acid is 96-98%, the concentration of nitric acid is 65-70%, sends in 117-120 DEG C of constant temperature oil bath, insulated and stirred 100- 120 minutes, discharging cooled down, sucking filtration, and precipitation washing 4-5 time is vacuum dried 20-26 hour at 70-80 DEG C, obtains purified carbon and receive Mitron；
(3) above-mentioned 2- mercapto benzimidazole is added in the dehydrated alcohol of its weight 17-20 times, stirs, rise High-temperature is 65-70 DEG C, insulated and stirred 4-9 minute, adds above-mentioned aluminium stearate, stirs to room temperature, obtain alcohol dispersion liquid；
(4) above-mentioned purifying carbon nano-tube is added to its weight 80-100 times, 0.2-1mol/l sodium hydroxide solution In, ultrasonic 20-30 minute, add bromohexadecane, tetrabutyl ammonium bromide, continue ultrasonic 17-20 minute, send into 80-85 DEG C In water-bath, insulated and stirred 7-9 hour, discharging, Deca chloroform, no longer change to precipitation, stratification, take off a layer solution, add Above-mentioned alcohol dispersion liquid, sucking filtration after stirring, precipitation is placed in 100-105 DEG C of vacuum drying oven and is dried completely, obtain esterification CNT；
(5) above-mentioned isothiazolone is added in the dehydrated alcohol of its weight 10-13 times, stirs, add esterification CNT, rises high-temperature and is 60-67 DEG C, and insulated and stirred 4-10 minute adds above-mentioned N hydroxymethyl acrylamide, stirs to normal Temperature, filters, and precipitation washing 3-4 time, normal temperature drying obtain modified esterification CNT；
(6) by above-mentioned modified esterification CNT, the mixing of carboxylic acid Nanometer Copper, it is added in above-mentioned methyl-silicone oil, ball milling 10-13 hour, adds above-mentioned stearic acid monoglyceride, stirs, and sends in 190-200 DEG C of oil bath, insulated and stirred 27-30 Minute, discharging cools down, and obtains extreme-pressure anti-wear auxiliary agent；
(7) above-mentioned extreme-pressure anti-wear auxiliary agent, lauryl mercaptan are mixed, stir, add above-mentioned antioxidant 1010, Insulated and stirred 20-34 minute at 60-70 DEG C, is mixed with above-mentioned dodecyl sodium sulfate, is added to compound weight 1.3-2 times In deionized water, stir, add remaining each raw material, 700-800 rev/min of stirring 20-30 minute, obtain final product.
It is an advantage of the invention that：The present invention passes through first to Purification of Carbon Nanotubes, is allowed to access carboxyl, then passes through to replace instead Long chain alkane molecule should be accessed on ester group, the sterically hindered effect that exactly long chain alkane of carbon nano tube surface provides enhances Dispersion stabilization in methyl-silicone oil for the carbon nanotube/nano copper composite particles；Carbon nano tube surface through carboxylated resterification Containing a large amount of defects, free radical, oxygen-containing functional group etc., surface adsorption effect strengthens, by the CNT after esterification and Tubercuprose. After mixing and ball milling, by pyrolysis, Cu2+ can be adsorbed in carbon nano tube surface, generates nano copper particle in carbon nano tube surface, plus Esterification CNT long chain alkane sterically hindered effect, thus the carbon nanotube/nano copper-base pressure forming stably dispersing is anti- Milling aid；
Because copper nanoparticle has larger specific surface area, surface energy and activity, when highly active Nano-Cu Additive adds After being added to methyl-silicone oil, when nano copper particle is collided with wear surface in friction process, produced mechanical energy is most of Translate into heat energy, the groupuscule of very little can be agglomerated into after nano copper particle heat absorption, multiple groupuscules with certain energy are Certain thickness protecting film is formed at last on wear surface, reduces shear stress and the coefficient of friction of wear surface, additionally, Nano copper particle plays certain effect filled up and repair to the concavo-convex of wear surface, is equivalent to the work that traditional abrasive dust plays With, and nano copper particle is less, this action effect also becomes apparent from, so, the methyl-silicone oil sample containing proper amount of nano copper powder The extreme pressure property of product is remarkably improved；Further, since CNT has super-strong and super-toughened performance, and can pass through in stress , to discharging stress, so CNT rolls in lubricating fluid, CNT serves carrying for existing pentagon and heptagon Effect, reduce friction pair interface directly contact, improve cutting fluid greasy property；
Present invention adds antioxidant 1010,2- mercapto benzimidazole etc., can effectively improve finished product cutting fluid Antioxygenic property, improves the bin stability of finished product.
Specific embodiment
A kind of antioxidation micro-emulsion cutting fluid, it is made up of the raw material of following weight parts：
Antioxidant 1010 1, isothiazolone 2,2- mercapto benzimidazole 0.8, stearic acid monoglyceride 2, bromo 16 Alkane 0.4, tetrabutyl ammonium bromide 0.3, the aqueous formic acid 20 of Copper hydrate 6,10%, CNT 4, methyl-silicone oil 50,12 Sodium alkyl sulfonate 3, appropriate amount of water, phthalic acid ester 1, ammonium molybdate 2, aluminium stearate 0.6, N hydroxymethyl acrylamide 1, trichlorine are different Cyanuric acid 0.8, lauryl mercaptan 2.
A kind of preparation method of described antioxidation micro-emulsion cutting fluid, comprises the following steps：
(1) above-mentioned Copper hydrate is added in the deionized water of 20 times of its weight, Deca above-mentioned 10% under stirring condition Aqueous formic acid, after completion of dropping rise high-temperature be 80 DEG C, insulated and stirred to water do, obtain carboxylic acid Nanometer Copper；
(2) above-mentioned CNT being added to mass ratio is 3:In 1 sulphuric acid, the mixed solution of nitric acid, described sulphuric acid Concentration be 96%, the concentration of nitric acid be 65%, send in 117 DEG C of constant temperature oil bath, insulated and stirred 100 minutes, discharging cools down, Sucking filtration, precipitation washing 4 times is vacuum dried 20 hours at 70 DEG C, obtains purifying carbon nano-tube；
(3) above-mentioned 2 mercapto benzimidazoles are added in the dehydrated alcohol of 17 times of its weight, stir, rise high temperature Spend for 65 DEG C, insulated and stirred 4 minutes, add above-mentioned aluminium stearate, stir to room temperature, obtain alcohol dispersion liquid；
(4) above-mentioned purifying carbon nano-tube is added in 80 times of its weight, 0.2mol/l sodium hydroxide solution, ultrasonic 20 minutes, add bromohexadecane, tetrabutyl ammonium bromide, continue ultrasonic 17 minutes, send in 80 DEG C of water-bath, insulated and stirred 7 Hour, discharging, Deca chloroform, no longer change to precipitation, stratification, take off a layer solution, add above-mentioned alcohol dispersion liquid, stirring is all Even rear sucking filtration, precipitation is placed in 100 DEG C of vacuum drying oven and is dried completely, obtain esterification CNT；
(5) above-mentioned isothiazolone is added in the dehydrated alcohol of 10 times of its weight, stirs, add esterification carbon to receive Mitron, rises high-temperature and is 60 DEG C, and insulated and stirred 4 minutes adds above-mentioned N n-methylolacrylamide, stirs to room temperature, filters, will Precipitation washing 3 times, normal temperature drying, obtain modified esterification CNT；
(6) by above-mentioned modified esterification CNT, the mixing of carboxylic acid Nanometer Copper, it is added in above-mentioned methyl-silicone oil, ball milling 10 hours, add above-mentioned stearic acid monoglyceride, stir, send in 190 DEG C of oil bath, insulated and stirred 27 minutes, discharging Cooling, obtains extreme-pressure anti-wear auxiliary agent；
(7) above-mentioned extreme-pressure anti-wear auxiliary agent, lauryl mercaptan are mixed, stir, add above-mentioned antioxidant 1010, Insulated and stirred 20 minutes at 60 DEG C, are mixed with above-mentioned dodecyl sodium sulfate, are added to the deionized water of 1.3 times of compound weight In, stir, add remaining each raw material, 700 revs/min are stirred 20 minutes, obtain final product.
Performance test：

Claims (2)

1. a kind of antioxidation micro-emulsion cutting fluid is it is characterised in that what it was made up of the raw material of following weight parts：
Antioxidant 1010 1-2, isothiazolone 2-3,2- mercapto benzimidazole 0.8-1, stearic acid monoglyceride 2-4, bromo Hexadecane 0.4-1, tetrabutyl ammonium bromide 0.3-1, the aqueous formic acid 20-30 of Copper hydrate 6-7,10-15%, CNT 4- 5th, methyl-silicone oil 50-60, dodecyl sodium sulfate 3-4, appropriate amount of water, phthalic acid ester 1-2, ammonium molybdate 2-3, aluminium stearate 0.6-1, N hydroxymethyl acrylamide 1-2, sym-closene 0.8-1, lauryl mercaptan 2-4.
2. a kind of preparation method of antioxidation micro-emulsion cutting fluid as claimed in claim 1 is it is characterised in that include following walking Suddenly：
（1）Above-mentioned Copper hydrate is added in the deionized water of its weight 20-35 times, the above-mentioned 10-15% of Deca under stirring condition Aqueous formic acid, after completion of dropping rise high-temperature be 80-85 DEG C, insulated and stirred to water do, obtain carboxylic acid Nanometer Copper；
（2）It is 3-4 that above-mentioned CNT is added to mass ratio:In 1 sulphuric acid, the mixed solution of nitric acid, described sulphuric acid Concentration is 96-98%, the concentration of nitric acid is 65-70%, sends in 117-120 DEG C of constant temperature oil bath, insulated and stirred 100-120 is divided Clock, discharging cools down, sucking filtration, and precipitation washing 4-5 time is vacuum dried 20-26 hour at 70-80 DEG C, obtains purifying carbon nano-tube；
（3）Above-mentioned 2- mercapto benzimidazole is added in the dehydrated alcohol of its weight 17-20 times, stirs, rise high temperature Spend for 65-70 DEG C, insulated and stirred 4-9 minute, add above-mentioned aluminium stearate, stir to room temperature, obtain alcohol dispersion liquid；
（4）Above-mentioned purifying carbon nano-tube is added in its weight 80-100 times, 0.2-1mol/l sodium hydroxide solution, surpasses Sound 20-30 minute, adds bromohexadecane, tetrabutyl ammonium bromide, continues ultrasonic 17-20 minute, sends into 80-85 DEG C of water-bath In, insulated and stirred 7-9 hour, discharging, Deca chloroform, no longer change to precipitation, stratification, take off a layer solution, add above-mentioned Alcohol dispersion liquid, sucking filtration after stirring, precipitation is placed in 100-105 DEG C of vacuum drying oven and is dried completely, carbon must be esterified and receive Mitron；
（5）Above-mentioned isothiazolone is added in the dehydrated alcohol of its weight 10-13 times, stirs, add esterification carbon to receive Mitron, rises high-temperature and is 60-67 DEG C, and insulated and stirred 4-10 minute adds above-mentioned N hydroxymethyl acrylamide, stirs to room temperature, Filter, precipitation washing 3-4 time, normal temperature drying obtain modified esterification CNT；
（6）By above-mentioned modified esterification CNT, the mixing of carboxylic acid Nanometer Copper, it is added in above-mentioned methyl-silicone oil, ball milling 10-13 Hour, add above-mentioned stearic acid monoglyceride, stir, send in 190-200 DEG C of oil bath, insulated and stirred 27-30 minute, Discharging cools down, and obtains extreme-pressure anti-wear auxiliary agent；
（7）By above-mentioned extreme-pressure anti-wear auxiliary agent, lauryl mercaptan mixing, stir, add above-mentioned antioxidant 1010, in 60- Insulated and stirred 20-34 minute at 70 DEG C, is mixed with above-mentioned dodecyl sodium sulfate, is added to going of compound weight 1.3-2 times In ionized water, stir, add remaining each raw material, 700-800 rev/min of stirring 20-30 minute, obtain final product.
CN201610765001.4A 2016-08-30 2016-08-30 A kind of antioxidation micro-emulsion cutting fluid and preparation method thereof Pending CN106467768A (en)

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Application publication date: 20170301