CN100526444C - Preparing method of superfine borate grain as lubricant additive - Google Patents
Preparing method of superfine borate grain as lubricant additive Download PDFInfo
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- CN100526444C CN100526444C CNB200510133949XA CN200510133949A CN100526444C CN 100526444 C CN100526444 C CN 100526444C CN B200510133949X A CNB200510133949X A CN B200510133949XA CN 200510133949 A CN200510133949 A CN 200510133949A CN 100526444 C CN100526444 C CN 100526444C
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Abstract
The present invention discloses preparation process of superfine borate powder as lubricant additive. The process includes the following steps: dissolving boric acid in solvent to obtain precursor, spray drying in certain technological conditions to obtain spherical superfine borate powder of 0.1-3 micron size, capturing with the capturing liquid comprising dispersant and base oil, and heating to disperse and to obtain homogeneous transparent stably dispersed superfine borate powder as lubricant additive. The process has simple operation, short preparation period and high efficiency, and the prepared superfine borate powder is homogeneous in particle size and able to be dispersed stably in organic system without agglomeration.
Description
Technical field
The present invention relates to a kind of preparation method of superfine borate grain as lubricant oil additive.
Background technology
Lubricating oil additive is the marrow of various senior lubricants, can give base oil special performances (PeerSrudt. tribology collection of translations, 1992:1-6), be described as new and effective multi-functional inorganic borate lubricating oil additive, be always one of emphasis of each industrialized country's tribology scholar's research (west wind. the reasonable lubrication technical manual. Beijing: petroleum industry press, 1993:580-592).Borate additive for lubricating oil is a kind of lubricating oil additive with good anti-extreme pressure energy, high supporting capacity and outstanding abrasion resistance.Borate extreme pressure anti-wear additives extreme pressure property is good, and fabulous oil film strength is arranged, and agree trier at terraced nurse and can reach 45.4kg by load, and its contact pressure mean value is 2952.9kg/cm
2, almost be three times of lead-sulphur type gear oil, be two times of sulphur-phosphorus type gear oil (Adams J H.Borate-A New Generation EP GearLubricant..Lubr.Eng., Vol.33:241); The borate oil film thickness is 10～20 times of the extreme pressure film that forms of extreme pressure agent in the past, this film can bear contacting of metal and metal, can withstand shocks especially load (Huang Wenxuan. the eighties Saving Energy by Lubrication agent---borate. refining of petroleum, 1985,9:39-41); The borate lubricant also has outstanding characteristics, general extreme pressure anti-wear additives is diminishing along with lubricating oil viscosity, the withstand load degradation, and borate diminishing along with lubricating oil viscosity, the withstand load performance improved on the contrary (will is congratulated 3,000 men. ペ ト ロ テ Star Network, 1984,7 (8): 730-732); Thermal oxidation stability is good, under the high temperature copper there is not corrosion, iron and steel had good anti-rust properties, also has good seal compatibility, nonpoisonous and tasteless, compare sulphur, phosphorus is that performance is more superior, also obvious more (the JOST H P.Tribology:The first 25 years andbeyond-Achievements of environmental benefit, shortcomings and future tasks[C] .Industrial lubrication andtribiology.1992,44 (2): 22-27), (Liu Weimin, Xue Qunji, Huang Chunxiang. potassium borate is done the research [J] of the abrasion resistance of lubricating oil additive. tribology journal .1992,12 (2): 174-179), (Qiao Yulin. the tribological property [J] of surface modified boric acid salt lubricating oil additive. tribology journal .1998,18 (1): 25-31).
The preparation method that borate additive for lubricating oil is commonly used has polishing and double decomposition.Wherein, polishing is that a kind of preparation borate oil dispersion is the method that is relatively easy to, with borate in the presence of dispersion agent, make borate-oil dispersion with base oil grinding, barreling, vibration etc., the borate additive for lubricating oil particle of preparation is bigger, stability and water tolerance are all poor, are unfavorable for applying; Double decomposition is that boric acid and sodium hydroxide are dissolved in dispersion agent respectively, solubility promoter, make it reaction in the promotor, reaction product is through the dehydration that heats up, filter, make borate-oil dispersion, because of its complicated process of preparation, reaction and dehydration temperaturre all must strictly be controlled, be unfavorable for suitability for industrialized production (Adams J H, Calif S R.Lubricant containing potassium borateUSP 3997454.1976), (Inoue K, Nose Y.Method for producing an alkaline earthmetal borate dispersion.USP 4683126.1987).
Summary of the invention
The object of the present invention is to provide a kind of particle of superfine borate more simply and easily preparation process lubricant oil additive.
The principle of this method is borate solution to be atomized to become little drop earlier, and then the dry borate particulate that forms, after the liquid phase capture forms the slip additive product after disperseing.This method realizes the particle super-refinement by atomization technique, and the particulate fineness can be regulated and control easily by droplet size and strength of solution.
The present invention realizes by following measure:
A kind of preparation method of superfine borate grain as lubricant additive is characterized in that with concentration be the boratory aqueous solution of 0.5～1.5wt%, with 2～4kgf/cm
2The pressure of spraying, the sample introduction speed of 10～30ml/min sprays into drying chamber through nozzle and forms vaporific drop; With flow velocity is 4.5～5.5m
3/ min heated drying air is carried out drying to vaporific drop; Dried superfine powder fills base oil along with drying air stream feeds the liquid phase catch tank in the liquid phase catch tank, and the temperature of base oil continues to disperse in 90～150 ℃ of scopes, and obtaining grain diameter is 0.1～3um superfine borate slip additive.
Borate is selected from Sodium Tetraborate, potassium borate, sodium metaborate, potassium metaborate or sodium tetraborate.
The inlet temperature of heated drying air is 200～300 ℃, and temperature out is 70～90 ℃.
Base oil can be selected from whiteruss, Poly alpha Olefins (PAO), methyl phenyl silicone oil etc.
Method used in the present invention is expected product from former, and the preparation route is short, and simple to operate, cost is low, the assurance that also all is easy to get of the yield of product and quality.And the granularity of the borate ultra-fine grain product that makes with the inventive method is good, and grain diameter is between 0.1～3um.The single stage method that has realized high quality, superfine borate grain as lubricant additive that dispersion stabilization is good is synthetic.Particularly with after join to handle and combine with the superfine powder collection, join many steps of processing after both having saved, shorten preparation cycle greatly, can reach again and collect effect completely.
Description of drawings
For a better understanding of the present invention, be described further below by accompanying drawing:
Fig. 1 is the preparation process block diagram of superfine borate grain as lubricant additive.
A represents the feed liquid system, i.e. the boratory aqueous solution. The concentration of the used borate solution of the present invention 0.5～In the 1.5wt% scope, less than this concentration range, although the borate grain diameter that obtains is little, product yield Low, cause raw material and energy waste; Greater than this concentration range, because the droplet that high concentration liquid forms is bigger, Thereby the borate grain diameter that obtains is bigger, affects its dispersion stabilization in organic system.
The B representative is made A through process I the vaporific drop of borate.
The C representative obtains B through process II the superfine powder in dry gas stream. For guaranteeing with further Improve the quality of prepared superfine borate grain products, the employed hot-air of above-mentioned spray-drying is process Heated pure hot-air behind the filtering dust collecting.
The D representative is used for capturing the used liquid phase trapping system of borate superfine powder that obtains through process III, Liquid phase wherein is various base oils, and the kind of base oil is to not impact of preparation process.
The E representative is through the superfine borate grain as lubricant additive product of process IV gained. This product mesoboric acid The quality percentage composition of salt superfine powder is between 15～30%.
The I representative under certain experimental condition, is converted into the process of vaporific drop B with feed liquid system A. This mistake The related technological parameter of journey comprises atomisation pressure, sample introduction speed. Atomisation pressure is at 2～4kgf/cm2Scope In, atomizing pressure is the key parameter of spray drying technology, only reaches certain pressure and just can make borate molten Liquid forms vaporific drop. If atomisation pressure of the present invention just can't form vaporific drop B less than this pressure limit, Along with the increase of atomisation pressure, diameter of particle reduces, also can have a negative impact to particulate form but pressure is excessive, Such as phenomenons such as out-of-shape such as fragmentation, hole, depressions, affect properties of product. In addition, atomisation pressure is too big Also can cause heavy wear to nozzle. Sample introduction speed is in the scope of 10～30ml/min, if less than this speed Scope, the borate grain diameter that obtains is little, and drying effect is good, but product yield is low, causes energy waste, Increase cost; If greater than this velocity interval, undried drop number increases in the same time, phase between the drop Mutual collision and generation are poly-also, and product reunion situation increases the weight of. And sample introduction speed is unfavorable for feed liquid atomizing, shadow too soon Ring drying effect.
The II representative is carried out drying with vaporific drop B in thermal medium, obtain dry superfine borate powder C's Process. The related technological parameter of this process comprises that the inlet temperature of dry flow velocity with thermal current, thermal current reaches Outlet temperature. The flow velocity of the used thermal current of the present invention is 4.5～5.5m3/ min, less than this flow rates, ultra-fine Particle can not get abundant drying, and can affect ultra-fine grain and transport smoothly in spray drying system, greater than this Flow rates, air-flow at a high speed can make the liquid splash in the catch tank, cause danger, and also a large amount of borate is super Fine grained just has little time to be captured along with dry gas stream is discharged, and causes yield to reduce. Dry import with thermal current Temperature is 200～300 ℃, and outlet temperature is 70～90 ℃. Parameter inlet temperature outbalance is among the present invention If be lower than this inlet temperature scope, ultra-fine grain can not get abundant drying, affects its performance, if temperature is too high, Cause unnecessary energy waste.
The III representative is transported to dried superfine borate powder C the process of trapping solution D. This process is related The technological parameter that reaches is the drying medium flow velocity, i.e. aforesaid 4.5～5.5m3/ min, if flow velocity is too little, Then be not enough to ultra-fine grain is transported to trapping solution, but be gathered in the drying chamber, if flow velocity is too big, can lead Cause trapping solution and splash, a large amount of borate ultra-fine grains also can be along with drying medium be discharged, and the particle that traps is few, Can't guarantee the rate of recovery.
The IV representative fully is distributed to superfine borate particle C among the trapping solution D, finally obtains the mistake of product E Journey. The technological parameter that this process relates to comprises the temperature of trapping solution. The temperature range of trapping solution of the present invention is In 90 ℃～150 ℃ scopes, temperature is too low, and dispersant viscosity is too big, causes rate of dispersion extremely slow and inhomogeneous, Temperature is too high, can affect the performance of dispersant, causes C fully not disperse, affect product uniformity and Stability. After powder passes into the liquid phase catch tank, continue to disperse, can guarantee abundant dispersion, make ultra-fine boric acid Salt lubricating additive product.
Accompanying drawing 3 is the TEM photo of gained borate particle.
Embodiment
For a better understanding of the present invention, by concrete example foregoing of the present invention is described in further detail below.But above-mentioned subject area of the present invention not only is confined to following example.
Embodiment 1:
6.0g Sodium Tetraborate (it is heavy not contain crystal water) is dissolved in distilled water, is mixed with the solution that concentration is 0.5wt%, with 4kgf/cm
2Pressure, the sample introduction speed of 10ml/min is that the nozzle of 2.5mm sprays into drying chamber with dobell's solution through diameter, and forms vaporific drop in drying chamber, with desiccant warm air with 4.5m
3The flow velocity input drying tower of/min carries out drying to the dobell's solution droplet, and the inlet temperature of warm air is 200 ℃, and temperature out is 70 ℃.Dried powder is the Sodium Tetraborate ultrafine particle.Dried ultra-fine grain is along with drying air stream feeds the liquid phase catch tank, fill the whiteruss that quality is 14g in the liquid phase catch tank, the temperature of whiteruss is 150 ℃, after the Sodium Tetraborate ultrafine particle feeds the liquid phase catch tank, continue to add dissipation of heat 3 hours, and can obtain transparent ultra-fine Sodium Tetraborate slip additive product.The quality percentage composition of the ultra-fine Sodium Tetraborate slip additive mesoboric acid sodium that makes is 30%, keeps stable dispersion.Products obtained therefrom carries out the dynamic laser light scattering experimental sreen analysis, and shown in curve 1 in the accompanying drawing 2, its mean particle size is 134.9nm.
Embodiment 2:
6.0g sodium metaborate (it is heavy not contain crystal water) is dissolved in distilled water, is mixed with the solution that concentration is 0.7wt%, with 3.5kgf/cm
2Pressure, the sample introduction speed of 20ml/min is that the nozzle of 2.5mm sprays into drying chamber with sodium metaborate solution through diameter, and forms vaporific drop in drying chamber, with desiccant warm air with 5.0m
3The flow velocity input drying tower of/min carries out drying to the sodium metaborate solution droplet, and the inlet temperature of warm air is 200 ℃, and temperature out is 80 ℃.Dried powder is the sodium metaborate ultrafine particle.Dried ultra-fine grain is along with drying air stream feeds the liquid phase catch tank, fill the whiteruss that quality is 18g in the liquid phase catch tank, the temperature of whiteruss is 150 ℃, after the sodium metaborate ultrafine particle feeds the liquid phase catch tank, continue to add dissipation of heat 2 hours, and can obtain transparent ultra-fine sodium metaborate slip additive product.The quality percentage composition of sodium metaborate is 25% in the ultra-fine sodium metaborate slip additive that makes, and keeps stable dispersion.Products obtained therefrom carries out the dynamic laser light scattering experimental sreen analysis, and shown in curve 2 in the accompanying drawing 2, its mean particle size is about 195.9nm.
Embodiment 3:
6.0g potassium borate (it is heavy not contain crystal water) is dissolved in distilled water, is mixed with the solution that concentration is 1.0wt%, with 3.0kgf/cm
2Pressure, the sample introduction speed of 20ml/min is that the nozzle of 2.0mm sprays into drying chamber with potassium borate solution through diameter, and forms vaporific drop in drying chamber, with desiccant warm air with 5.0m
3The flow velocity input drying tower of/min carries out drying to potassium borate solution droplet, and the inlet temperature of warm air is 230 ℃, and temperature out is 70 ℃.Dried powder is the potassium borate ultrafine particle.Dried ultra-fine grain is along with drying air stream feeds the liquid phase catch tank, fill the Poly alpha Olefins (PAO) that quality is 24g in the liquid phase catch tank, the temperature of Poly alpha Olefins (PAO) is 90 ℃, after the potassium borate ultrafine particle feeds the liquid phase catch tank, continue to add dissipation of heat 2 hours, and can obtain transparent ultra-fine potassium borate slip additive product.The quality percentage composition of the ultra-fine potassium borate slip additive mesoboric acid potassium that makes is 20%, keeps stable dispersion.Products obtained therefrom carries out the dynamic laser light scattering experimental sreen analysis, and shown in curve 3 in the accompanying drawing 2, its mean particle size is about 512.5nm.
Embodiment 4:
6.0g potassium metaborate (it is heavy not contain crystal water) is dissolved in distilled water, is mixed with the solution that concentration is 1.2wt%, with 2.5kgf/cm
2Pressure, the sample introduction speed of 20ml/min is that the nozzle of 2.5mm sprays into drying chamber with potassium metaborate solution through diameter, and forms vaporific drop in drying chamber, with desiccant warm air with 4.5m
3The flow velocity input drying tower of/min carries out drying to potassium metaborate solution droplet, and the inlet temperature of warm air is 250 ℃, and temperature out is 80 ℃.Dried powder is the potassium metaborate ultrafine particle.Dried ultra-fine grain is along with drying air stream feeds the liquid phase catch tank, fill the methyl phenyl silicone oil that quality is 27g in the liquid phase catch tank, the temperature of methyl phenyl silicone oil is 150 ℃, after the potassium metaborate ultrafine particle feeds the liquid phase catch tank, continue to add dissipation of heat 2.5 hours, and can obtain transparent ultra-fine potassium metaborate slip additive product.The quality percentage composition of potassium metaborate is 18% in the ultra-fine potassium metaborate slip additive that makes, and keeps stable dispersion.Products obtained therefrom carries out the dynamic laser light scattering experimental sreen analysis, and shown in curve 4 in the accompanying drawing 2, its mean particle size is about 911nm.
Embodiment 5:
6.0g sodium tetraborate (it is heavy not contain crystal water) is dissolved in distilled water, is mixed with the solution that concentration is 1.5wt%, with 3kgf/cm
2Pressure, the sample introduction speed of 20ml/min is that the nozzle of 2.0mm sprays into drying chamber with sodium tetraborate solution through diameter, and forms vaporific drop in drying chamber, with desiccant warm air with 4.5m
3The flow velocity input drying tower of/min carries out drying to sodium tetraborate solution droplet, and the inlet temperature of warm air is 280 ℃, and temperature out is 75 ℃.Dried powder is the sodium tetraborate ultrafine particle.Dried ultra-fine grain is along with drying air stream feeds the liquid phase catch tank, fill the whiteruss that quality is 34g in the liquid phase catch tank, the temperature of whiteruss is 150 ℃, after the sodium tetraborate ultrafine particle feeds the liquid phase catch tank, continue to add dissipation of heat 3 hours, and can obtain transparent ultra-fine sodium tetraborate slip additive product.The quality percentage composition of sodium tetraborate is 15% in the ultra-fine sodium tetraborate slip additive that makes, and keeps stable dispersion.Products obtained therefrom carries out the dynamic laser light scattering experimental sreen analysis, and shown in curve 5 in the accompanying drawing 2, its mean particle size is about 1650nm.
Claims (2)
1, a kind of preparation method of superfine borate grain as lubricant additive is characterized in that with concentration be the boratory aqueous solution of 0.5～1.5wt%, with 2～4kgf/cm
2The pressure of spraying, the sample introduction speed of 10～30ml/min sprays into drying chamber through nozzle and forms vaporific drop; With flow velocity is 4.5～5.5m
3/ min heated drying air is carried out drying to vaporific drop; The inlet temperature of heated drying air is 200～300 ℃, and temperature out is 70～90 ℃; Dried superfine powder fills base oil along with drying air stream feeds the liquid phase catch tank in the liquid phase catch tank, and the temperature of base oil continues to disperse in 90～150 ℃ of scopes, and obtaining grain diameter is 0.1～3um superfine borate slip additive.
2, the method for claim 1 is characterized in that borate is selected from Sodium Tetraborate, potassium borate, sodium metaborate, potassium metaborate or sodium tetraborate.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1175621A (en) * | 1996-08-29 | 1998-03-11 | 中国人民解放军装甲兵工程学院 | Method for preparing superfine borate additive for lubricating oil |
| WO2004022676A1 (en) * | 2002-09-09 | 2004-03-18 | Ecurity Ab | A method for producing a solution having lubricating properties intended to be used as an additive to a liquid |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1175621A (en) * | 1996-08-29 | 1998-03-11 | 中国人民解放军装甲兵工程学院 | Method for preparing superfine borate additive for lubricating oil |
| WO2004022676A1 (en) * | 2002-09-09 | 2004-03-18 | Ecurity Ab | A method for producing a solution having lubricating properties intended to be used as an additive to a liquid |
Non-Patent Citations (1)
| Title |
|---|
| 我国喷雾干燥技术研究及进展. 黄立新，王宗濂，唐金鑫.化学工程，第VOL.29卷第NO.2期. 2001 * |
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