CN106336935A - Titanium sol microemulsion cutting fluid and preparation method thereof - Google Patents

Titanium sol microemulsion cutting fluid and preparation method thereof Download PDF

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CN106336935A
CN106336935A CN201610761533.0A CN201610761533A CN106336935A CN 106336935 A CN106336935 A CN 106336935A CN 201610761533 A CN201610761533 A CN 201610761533A CN 106336935 A CN106336935 A CN 106336935A
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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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    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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    • C10M2227/06—Organic compounds derived from inorganic acids or metal salts
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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
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Abstract

The invention discloses a titanium sol microemulsion cutting fluid. The titanium sol microemulsion cutting fluid is prepared from, by weight, 0.3-1 part of polysorbate 80, 2-3 parts of casein, 1-2 parts of triethanolamine, 0.7-1 part of 8-hydroxyquinoline, 0.4-1 part of bromohexadecane, 0.3-1 part of tetrabutylammonium bromide, 6-7 parts of copper hydroxide, 20-30 parts of 10%-15% formic acid aqueous solution, 4-5 parts of carbon nanotubes, 50-60 parts of methyl silicone oil, 3-4 parts of sodium dodecyl sulfate, an appropriate amount of water, 5-7 parts of tetrabutyl titanate, 0.6-1 part of zinc sulfate, 2-3 parts of dithio-salicylic acid, 1-2 parts of fatty acid polyethylene glycol ester, 0.4-1 part of sodium pyrophosphate and 2-3 parts of polyethylene glycol adipate. According to the titanium sol microemulsion cutting fluid, esterified carbon noanotubes and copper formate are mixed to be subjected to ball milling, Cu<2+> can be adsorbed to the surfaces of the carbon nanotubes through pyrolysis, and copper nanoparticles are generated on the surfaces of the carbon nanotubes.

Description

A kind of titanium colloidal sol 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 titanium colloidal sol 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 titanium colloidal sol micro-emulsion cutting fluid and its system Preparation Method.
The present invention is achieved by the following technical solutions:
A kind of titanium colloidal sol micro-emulsion cutting fluid, it is made up of the raw material of following weight parts:
Polyoxyethylene sorbitan monoleate 0.3-1, casein 2-3, triethanolamine 1-2,8-hydroxyquinoline 0.7-1, bromohexadecane 0.4- 1st, tetrabutyl ammonium bromide 0.3-1, the aqueous formic acid 20-30 of Copper hydrate 6-7,10-15%, CNT 4-5, methyl-silicone oil 50-60, dodecyl sodium sulfate 3-4, appropriate amount of water, butyl titanate 5-7, zinc sulfate 0.6-1, dithio-salicylic acid 2-3, fat Acid polyethylene glycol ester 1-2, sodium pyrophosphate 0.4-1, polyadipate ethylene glycol 2-3.
A kind of preparation method of described titanium colloidal sol 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) by above-mentioned CNT be added to mass ratio be the sulphuric acid of 3-4:1, in 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 butyl titanate is added in the deionized water of its weight 24-30 times, stirs, rise high-temperature For 60-70 DEG C, sequentially add above-mentioned sodium pyrophosphate, purifying carbon nano-tube, insulated and stirred 20-30 minute, add above-mentioned poly- Pyrusussuriensiss Ester 80, stirs to room temperature, filters, be vacuum dried 1-2 hour, obtain modified purifying carbon nano-tube at being deposited in 50-60 DEG C；
(4) above-mentioned modification purifying carbon nano-tube is added to its weight 80-100 times, 0.2-1mol/l sodium hydroxide In solution, ultrasonic 20-30 minute, add above-mentioned bromohexadecane, tetrabutyl ammonium bromide, continue ultrasonic 17-20 minute, send into In 80-85 DEG C of water-bath, insulated and stirred 7-9 hour, discharging, Deca chloroform, no longer change to precipitation, stratification, take off layer Solution, adds the dehydrated alcohol of its weight 10-15%, sucking filtration after stirring, and precipitation is placed in 100-105 DEG C of vacuum drying It is dried completely in case, obtain esterification CNT；
(5) above-mentioned 8-hydroxyquinoline is added in the dehydrated alcohol of its weight 10-14 times, stirs, add fat Acid polyethylene glycol ester, rises high-temperature and is 70-76 DEG C, and insulated and stirred 6-10 minute adds above-mentioned esterification CNT, and stirring is all Even, filter, precipitation washing 3-4 time is vacuum dried 1-2 hour at 40-50 DEG C, obtains 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, sends in 190-200 DEG C of oil bath, insulated and stirred 27-30 minute, and discharging cools down, and obtains extreme-pressure anti-wear auxiliary agent；
(7) above-mentioned extreme-pressure anti-wear auxiliary agent, zinc sulfate are mixed, be added in the dehydrated alcohol of compound weight 4-6 times, rise High-temperature is 70-75 DEG C, adds above-mentioned triethanolamine, insulated and stirred 20-30 minute, filters, by precipitation washing 3-4 time, in 50- It is vacuum dried 1-2 hour at 60 DEG C, obtain modified extreme-pressure anti-wear auxiliary agent；
(8) above-mentioned modification extreme-pressure anti-wear auxiliary agent is mixed with dodecyl sodium sulfate, be added to compound weight 1.3-2 times Deionized water in, stir, add remaining each raw material, 700-800 rev/min stirring 20-30 minute, obtain final product.
The invention has the advantage that the present invention passes through first to Purification of Carbon Nanotubes, it is allowed to access carboxyl, then pass 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 with butyl titanate as presoma, the titanium colloidal sol of preparation, can effectively improve filler and cut Cut the dispersibility in liquid, improve the stability of finished product.
Specific embodiment
A kind of titanium colloidal sol micro-emulsion cutting fluid, it is made up of the raw material of following weight parts:
Polyoxyethylene sorbitan monoleate 0.3, casein 2, triethanolamine 1,8-hydroxyquinoline 0.7, bromohexadecane 0.4, the tetrabutyl Ammonium bromide 0.3, the aqueous formic acid 20 of Copper hydrate 6,10%, CNT 4, methyl-silicone oil 50, dodecyl sodium sulfate 3, Appropriate amount of water, butyl titanate 5, zinc sulfate 0.6, dithio-salicylic acid 2, fatty acid polyethylene glycol ester 1, sodium pyrophosphate 0.4, poly- oneself Diacid ethylene glycol 2.
A kind of preparation method of described titanium colloidal sol 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) by above-mentioned CNT be added to mass ratio be the sulphuric acid of 3:1, in 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 butyl titanate is added in the deionized water of 24 times of its weight, stirs, rising high-temperature is 60 DEG C, sequentially add above-mentioned sodium pyrophosphate, purifying carbon nano-tube, insulated and stirred 20 minutes, add above-mentioned polyoxyethylene sorbitan monoleate, stir to Room temperature, filters, and will be deposited in and be vacuum dried 1 hour at 50 DEG C, and obtain modified purifying carbon nano-tube；
(4) above-mentioned modification purifying carbon nano-tube is added in 80 times of its weight, 0.2mol/l sodium hydroxide solution, Ultrasonic 20 minutes, add above-mentioned bromohexadecane, tetrabutyl ammonium bromide, continue ultrasonic 17 minutes, send in 80 DEG C of water-bath, protect Temperature stirring 7 hours, discharging, Deca chloroform, no longer change to precipitation, stratification, take off a layer solution, add its weight 10% Dehydrated alcohol, sucking filtration after stirring, precipitation is placed in 100 DEG C of vacuum drying oven and is dried completely, obtain esterification CNT；
(5) above-mentioned 8 hydroxyquinoline are added in the dehydrated alcohol of 10 times of its weight, stir, add fatty acid polyglycol Glycol ester, rises high-temperature and is 70 DEG C, and insulated and stirred 6 minutes adds above-mentioned esterification CNT, stirs, filters, will sink Form sediment and wash 3 times, be vacuum dried 1 hour at 40 DEG C, 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, send in 190 DEG C of oil bath, insulated and stirred 27 minutes, discharging cools down, and obtains extreme-pressure anti-wear auxiliary agent；
(7) above-mentioned extreme-pressure anti-wear auxiliary agent, zinc sulfate are mixed, be added in the dehydrated alcohol of 4 times of compound weight, raise Temperature is 70 DEG C, adds above-mentioned triethanolamine, insulated and stirred 20 minutes, filters, and by precipitation washing 3 times, at 50 DEG C, vacuum is done Dry 1 hour, obtain modified extreme-pressure anti-wear auxiliary agent；
(8) above-mentioned modification extreme-pressure anti-wear auxiliary agent is mixed with dodecyl sodium sulfate, be added to 1.3 times of compound weight In deionized water, stir, add remaining each raw material, 700 revs/min are stirred 20 minutes, obtain final product.
Performance test:

Claims (2)

1. a kind of titanium colloidal sol micro-emulsion cutting fluid is it is characterised in that what it was made up of the raw material of following weight parts:
Polyoxyethylene sorbitan monoleate 0.3-1, casein 2-3, triethanolamine 1-2,8-hydroxyquinoline 0.7-1, bromohexadecane 0.4-1, four Butylammonium bromide 0.3-1, the aqueous formic acid 20-30 of Copper hydrate 6-7,10-15%, CNT 4-5, methyl-silicone oil 50- 60th, dodecyl sodium sulfate 3-4, appropriate amount of water, butyl titanate 5-7, zinc sulfate 0.6-1, dithio-salicylic acid 2-3, fatty acid Macrogol ester 1-2, sodium pyrophosphate 0.4-1, polyadipate ethylene glycol 2-3.
2. a kind of preparation method of titanium colloidal sol micro-emulsion cutting fluid as claimed in claim 1 is it is characterised in that include following walking Rapid:
(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) by above-mentioned CNT be added to mass ratio be the sulphuric acid of 3-4:1, in 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 butyl titanate is added in the deionized water of its weight 24-30 times, stirs, liter high-temperature is 60- 70 DEG C, sequentially add above-mentioned sodium pyrophosphate, purifying carbon nano-tube, insulated and stirred 20-30 minute, add above-mentioned polyoxyethylene sorbitan monoleate, Stir to room temperature, filter, be vacuum dried 1-2 hour at 50-60 DEG C will be deposited in, obtain modified purifying carbon nano-tube；
(4) above-mentioned modification 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 above-mentioned bromohexadecane, tetrabutyl ammonium bromide, continue ultrasonic 17-20 minute, send into 80-85 DEG C water-bath in, insulated and stirred 7-9 hour, discharging, Deca chloroform, to precipitation no longer change, stratification, take off a layer solution, Add the dehydrated alcohol of its weight 10-15%, sucking filtration after stirring, precipitation is placed in dry in 100-105 DEG C of vacuum drying oven Dry complete, obtain esterification CNT；
(5) above-mentioned 8-hydroxyquinoline is added in the dehydrated alcohol of its weight 10-14 times, stirs, add fatty acid polyglycol Glycol ester, rises high-temperature and is 70-76 DEG C, and insulated and stirred 6-10 minute adds above-mentioned esterification CNT, stirs, mistake Filter, precipitation washing 3-4 time is vacuum dried 1-2 hour at 40-50 DEG C, obtains 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, 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) above-mentioned extreme-pressure anti-wear auxiliary agent, zinc sulfate are mixed, be added in the dehydrated alcohol of compound weight 4-6 times, rise high temperature Spend for 70-75 DEG C, add above-mentioned triethanolamine, insulated and stirred 20-30 minute, filter, by precipitation washing 3-4 time, at 50-60 DEG C Lower vacuum drying 1-2 hour, obtains modified extreme-pressure anti-wear auxiliary agent；
(8) above-mentioned modification extreme-pressure anti-wear auxiliary agent is mixed with dodecyl sodium sulfate, be 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.
CN201610761533.0A 2016-08-30 2016-08-30 Titanium sol microemulsion cutting fluid and preparation method thereof Pending CN106336935A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104277900A (en) * 2014-09-25 2015-01-14 巢湖广丰金属制品有限公司 High-antiwear cutting fluid
CN104789311A (en) * 2015-04-22 2015-07-22 青岛承天伟业机械制造有限公司 Multifunctional cutting liquid

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104277900A (en) * 2014-09-25 2015-01-14 巢湖广丰金属制品有限公司 High-antiwear cutting fluid
CN104789311A (en) * 2015-04-22 2015-07-22 青岛承天伟业机械制造有限公司 Multifunctional cutting liquid

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* Cited by examiner, † Cited by third party
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