CN101812349B - Lubricating oil and grease base oil, and preparation method and applications thereof - Google Patents
Lubricating oil and grease base oil, and preparation method and applications thereof Download PDFInfo
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Abstract
The invention provides base oil, in particular to a neopentyl polyalcohol dibasic acid complex ester. The neopentyl polyalcohol dibasic acid complex ester is prepared in a way that: completely esterifying C5-12 binary fatty acid carboxyl with the mixture of neopentyl glycol, trimethylolpropane and pentaerythritol, and blocking with C14-20 unsaturated monobasic fatty acid. The base oil provided by the invention has the characteristics of high flash point, high flammability point, low pour point, high viscosity index, low evaporation loss, high thermal oxidation stability and high biodegradation rate. The invention can be used as syntholube and grease base oil, especially syntholube base oil used under the conditions of high temperature and high pressure. The invention is especially suitable to be used in fire resistant hydraulic fluid, high-temperature chain oil, high-temperature grease and the like in severe working spaces at which naked flame can is accessible under the conditions of high temperature and high pressure.
Description
Technical field
The present invention relates to a kind of lubricating oil and grease base oil and preparation method thereof and application, especially relate to a kind of preparation and application of hydraulic efficiency oil base oil, belong to the industrial lubricant technical field.
Background technology
Hydraulic machinery has been widely used in the industries such as iron and steel, electric power, coal and machinery.Hydraulic efficiency oil as dynamic medium is the critical material of hydraulic transmission technology, also is one of three kinds of important oil products of industrial lubrication oil consumption maximum.Along with the development of modern hydraulic technology, the hydraulic efficiency system that has usually is under high pressure, the hot conditions works.Employed hydraulic efficiency oil has been proposed the more harsh requirement of non-flame properties.Before 20 century 70s, various countries are devoted to develop water type emulsion (W/O and O/W type), water-ethylene glycol type and water-free phosphate type, hydrochloric ether type fire resistant hydraulic oil.But the working pressure of water type anti-flame hydraulic fluid generally is lower than 10Mpa, and poor lubricity, can not satisfy the long lifetime service requirements of hydraulic efficiency system under high temperature, the condition of high voltage.Water-free phosphoric acid ester and hydrochloric ether fire resistant hydraulic oil are owing to be subject to the restriction of the factors such as environmental requirement of adaptability for materials, toxicity, price and increasingly stringent, and use range will more and more be subject to stricter restriction.Along with the progress of society and the development of science and technology, economizing on resources has become the two large problems that Faced In Sustainable Development is realized in countries in the world with environment protection.Energy-conservation, reduction of discharging, environmental contamination reduction are direction and the power of industrial sustainable development.A new generation's ester type fire resistant hydraulic oil adopts ester compound to make base oil, have high flash point, high burning-point, low vaporization losses, high viscosity index (HVI), excellent lubricity, nontoxic, biodegradable and good adaptability for materials and main raw material from reproducible animal-plant oil through advantages such as chemical process form, be a kind of " green science and technology product " that meets environmental requirement.
Because the Working environment of fire resistant hydraulic fluid is extremely harsh, be quite comprehensively with strict to the performance requriements of lubricating oil therefore.Main manifestations is:
(1) sticking warm nature: the working point of hydraulic efficiency system is under the high-temperature and high-pressure conditions for a long time, and this just requires fire resistant hydraulic fluid to have good viscosity temperature characteristic, high viscosity index (HVI), can use in wide temperature range;
(2) non-flame properties: the working point of hydraulic efficiency system is under the high-temperature and high-pressure conditions for a long time, and contact with naked light easily, this safe handling to oil product is a greatly test, this just requires the non-flame properties of fire resistant hydraulic fluid to get well, it is high that the flash-point burning-point of oil product is wanted, and volatility is low; Mineral hydraulic efficiency oil and general synthetic hydraulic fluid are very inaccessible;
(3) High Temperature High Pressure oxidation-resistance: hydraulic efficiency system is worked under high-temperature and high-pressure conditions for a long time, and temperature is that oil product causes the principal element that oxidizing reaction is accelerated, and measures to show 10 ℃ of the every risings of temperature, and oxidation rate increases by 2～4 times.Equally, oxygen partial pressure increases with compressed-air actuated pressure and improves, the oxygenizement of hydraulic efficiency oil and the increase of oxygen partial pressure and accelerate, and this just requires hydraulic efficiency oil to have good antioxidant property;
(4) environmental protection: along with the progress of the development of society and science and technology, more and more stricter to the requirement of environmental protection, energy-conservation, reduction of discharging, environmental contamination reduction are direction and the power of industrial sustainable development; For the hydraulic efficiency oil that accounts for very large composition in the lubricating oil, biological degradation, nontoxicity, free from environmental pollution, meeting environmental requirement also is the trend that develops in the future;
(5) long lifetime work: synthetic main advantage of fire resistant hydraulic fluid is to adopt novel synthesizing ester oil as base oil, has realized long lifetime work; Generally can reach 3 years at present, and safe and reliable, so work long hours, hydraulic efficiency oil stands the severe condition such as heating, cooling repeatedly, plays the effects such as lubricated, cooling, antirust and sealing, and general hydraulic efficiency oil is very inaccessible.
For synthetic fire resistant hydraulic fluid, the ratio of base oil is up to more than 95%, and the performance of base oil has just determined the salient features of product.Although present synthetic fire resistant hydraulic fluid has adopted synthesizing ester oil as base oil, can satisfy the requirement of the aspects such as environmental protection, work-ing life, but because its synthetic ester that adopts is single ester, also be difficult to satisfy the harsh requirement of fire resistant hydraulic fluid at aspects such as viscosity, pour point, flash-points.
Summary of the invention
The object of the invention is to overcome above the deficiencies in the prior art, a kind of lubricating oil and grease base oil are provided, on viscosity, pour point, flash-point, can't meet the requirements of technical problem to solve existing base oil.
It is lower and be easy to realize the preparation method of industrialized above-mentioned lubricating oil and grease base oil to the present invention also aims to disclose a kind of preparation cost, and above-mentioned lubricating oil and grease base oil particularly easily contact application in the hydraulic efficiency installation under the naked light condition in High Temperature High Pressure in the lubricating oil field.
The present invention solves above technical problem by the following technical solutions:
A kind of base oil is the multiple ester of amyl-based polyol diprotic acid, and the multiple ester of described amyl-based polyol diprotic acid is by first with C
5～12The complete esterification of alcohol mixture that forms with neopentyl glycol, TriMethylolPropane(TMP) and new penta tetrol of the carboxyl of binary of fatty acids after, use again C
14～20Unsaturated unary fatty acid end-blocking and make.
In the above-mentioned base oil, in the described alcohol mixture, the molar percentage of described neopentyl glycol, TriMethylolPropane(TMP), new penta tetrol is as follows:
Neopentyl glycol: 20～30%;
TriMethylolPropane(TMP): 50～60%;
New penta tetrol: 10～30%.
Preferably, in the described alcohol mixture, the molar percentage of described neopentyl glycol, TriMethylolPropane(TMP), new penta tetrol is as follows:
Neopentyl glycol: 20～25%
TriMethylolPropane(TMP): 50～60%
New penta tetrol: 20～25%
Better, described C
5～12Binary of fatty acids be two kinds of C
5～12The mixing of straight chain binary of fatty acids, described two kinds of C
5～ 12The mol ratio 1: 1～1: 4 of straight chain binary of fatty acids.Preferably, described C
5～12Binary of fatty acids be two kinds of C
6～10The mixing of straight chain binary of fatty acids, described two kinds of C
6～10The mol ratio of straight chain binary of fatty acids be 1: 1～1: 2
Described straight chain binary of fatty acids can be selected from pentanedioic acid, hexanodioic acid, pimelic acid, suberic acid, nonane diacid, sebacic acid, undecane diacid or dodecanedioic acid.
Better, described C
14～20Unsaturated unary fatty acid be selected from vegetable oil acid or hexadecylenic acid.
In the above-mentioned base oil, described with C
5～12The carboxyl of binary of fatty acids with the complete esterification of alcohol mixture that neopentyl glycol, TriMethylolPropane(TMP) and new penta tetrol form, referring to needs to guarantee that the carboxyl of described binary of fatty acids is by fully esterification.Can pass through integral molar quantity and the described C of the alcohol mixture of the described neopentyl glycol of control, TriMethylolPropane(TMP) and new penta tetrol composition
5～12The ratio of molar weight of binary of fatty acids esterification be to realize that the error about 1% can be arranged between the two in about 2: 1.
The described C that uses
14～20Unsaturated unary fatty acid end-blocking refer to, after described neopentyl glycol, TriMethylolPropane(TMP) and new penta tetrol and the described binary of fatty acids generation esterification polyreaction, the whole hydroxyls that have more again with C
14～20Unary fatty acid carry out the esterification end-blocking.The final multiple ester of the amyl-based polyol diprotic acid that comprises DOPCP, TriMethylolPropane(TMP) alcohol ester and new Doutrate that forms, the structural formula that comprises is as follows:
[C
nH
2n+1COOC
5H
10COO]
2C
mH
2m n＝13～19，m＝3～10；
{[C
nH
2n+1COO]
2C
6H
11COO}
2C
mH
2m n＝13～19，m＝3～10；
{[C
nH
2n+1COO]
3C
5H
8COO}
2C
mH
2m n＝13～19，m＝3～10。
The present invention also provides the preparation method of a kind of above-mentioned lubricating oil and grease base oil, may further comprise the steps:
1) makes C
5～12Binary of fatty acids and the alcohol mixture that neopentyl glycol, TriMethylolPropane(TMP) and new penta tetrol form, esterification occurs under the katalysis of catalyzer;
2) after reaction was finished described in the step 1, adding molar weight was described C
5～12At least 4 times C of binary of fatty acids integral molar quantity
14～20Unary fatty acid mixing esterification, obtain reaction product;
3) remove unreacted excess fatty acids and the described catalyzer of step 1 in the products therefrom in the step 2, obtain the multiple ester of described amyl-based polyol diprotic acid.
Step 1) in, described catalyzer is zirconic acid four monooctyl esters and tosic acid, and wherein, the molar weight of described zirconic acid four monooctyl esters is described C
5～12The binary of fatty acids integral molar quantity 0.95～1.05%, the molar weight of described tosic acid is described C
5～12The binary of fatty acids integral molar quantity 1.9～2.1%; The temperature of described esterification is 160～180 ℃, and the reaction times is 140～180 minutes.
Step 2) in, the temperature of reaction is 200～220 ℃, and the reaction times is 100～120 minutes; Described C
14～20The integral molar quantity of unary fatty acid need in the more described alcohol mixture not with the integral molar quantity of the hydroxyl of described binary of fatty acids reaction more excessive so that the second step esterification is complete.
Step 3) in, removes described unreacted excess fatty acids by the mode of underpressure distillation.According to the character of selected lipid acid, those skilled in the art can determine the condition of described underpressure distillation, distills under in 200 ℃, the vacuum condition of 3.2Kpa.
Step 3) in, removes described catalyzer by the mode of alkali cleaning and washing.The method of this alkali cleaning and washing is known by those skilled in the art, as: reaction product can be added first 3～5% water-soluble neutralization of yellow soda ash, then wash.After catalyzer is removed, after dehydration, filtration treatment, can obtain again the multiple ester of the amyl-based polyol diprotic acid described in the present invention.
The preparation method of above-mentioned base oil provided by the present invention has the advantage that processing condition are simple, preparation cost is lower and be easy to realize the aspects such as industrialization.
The base oil (the multiple ester of amyl-based polyol diprotic acid) that adopts aforesaid method to obtain has high flash point burning-point, low pour point, high viscosity index (HVI), low vaporization losses, thermal oxidation stability, the characteristics that biological degradation rate is high.Its flash-point can reach more than 295 ℃, and burning-point can reach more than 330 ℃, and pour point is below-28 ℃, and biological degradation rate is greater than 95%, and is safe and reliable.Can be used as synthetic lubricant base oil and grease base oil, particularly as the synthetic lubricant base oil that uses under the high-temperature and high-pressure conditions, be particularly useful in High Temperature High Pressure and be easy to contact in the hydraulic efficiency installation of naked light using, such as the base oil of the fire resistant hydraulic fluid that uses in the hydraulic efficiency system as Steel Plant or power station etc., high-temperature chain oil, high temperature grease etc.
Described high-temperature and high-pressure conditions typically refers to temperature and is higher than 80 ℃, and pressure is higher than the occasion of 20MPa.
Base oil described in the present invention (the multiple ester of amyl-based polyol diprotic acid), when using as the base oil of fire resistant hydraulic fluid, high-temperature chain oil, high temperature grease etc., only need according to different needs, add other corresponding functional additive, stir with the physical method intensification, dissolving evenly gets final product.
The present invention also provides a kind of fire resistant hydraulic fluid, comprises the component of following weight percent:
Oxidation inhibitor 1.9～4.5%;
Extreme pressure anti-wear additives 1.5～3.5%;
Defoamer 5～50ppm;
Rust-preventive agent 0.1～0.4%;
Base oil 92～97%;
Wherein, the multiple ester of the above-mentioned amyl-based polyol diprotic acid that provides among the present invention is provided described base oil.
In the above-mentioned fire resistant hydraulic fluid provided by the present invention, the adding of described oxidation inhibitor, extreme pressure anti-wear additives, defoamer and rust-preventive agent is in order to satisfy all round properties requirement of hydraulic efficiency installation under the high temperature and high pressure environment, as satisfies the lubricity, high-temperature thermal oxidation stability, anti-foaming properties, corrosion resistance of oil product under the long term operation etc.
Preferably, described fire resistant hydraulic fluid comprises the component of following weight percent:
Oxidation inhibitor 2.4～3.9%;
Extreme pressure anti-wear additives 2.3～2.6%;
Defoamer 10～30ppm;
Rust-preventive agent 0.1～0.2%;
Base oil 93.9～94.5%.
Fire resistant hydraulic fluid is in work, and the temperature of working point is generally 80～90 ℃, and local temperature may be higher.The easier deterioration by oxidation of oil product under hot conditions generates acidic substance, and the parts generation corrosion to hydraulic efficiency installation affects the normal operation of hydraulic efficiency installation; Viscosity can increase after the simultaneous oxidation, and this also can affect the operating accuracy of hydraulic efficiency installation and increase energy consumption.In order to prolong the work-ing life of hydraulic efficiency installation, slow down the deterioration by oxidation of oil product, need to add various oxidation inhibitor.In addition, also must pay attention to Research on synergistic effect between oxidation inhibitor, primary antioxidant and the antioxygen auxiliary agent.Through lot of experiments, the present invention selects by di-iso-octyldiphenylamine, phenyl-a-naphthylamine, 2, the composite oxidation inhibitor that forms of 6 DI-tert-butylphenol compounds and thiocarbamate, the performance advantage that has reached various antioxidants is complementary, has improved greatly the long term high temperature anti-oxidative stability of fire resistant hydraulic fluid.
Better, described oxidation inhibitor comprises di-iso-octyldiphenylamine, phenyl-a-naphthylamine, 2,6 DI-tert-butylphenol compounds and thiocarbamate, the proportioning of each component is as follows:
Di-iso-octyldiphenylamine 4～10 weight parts;
Phenyl-a-naphthylamine 4～10 weight parts;
2,6 DI-tert-butylphenol compounds, 5～10 weight parts;
Thiocarbamate 6～15 weight parts.
Preferably, the proportioning of each component is as follows in the described oxidation inhibitor:
Di-iso-octyldiphenylamine 5～8 weight parts;
Phenyl-a-naphthylamine 5～8 weight parts;
2,6 DI-tert-butylphenol compounds, 6～9 weight parts;
Thiocarbamate 8～14 weight parts.
Above-mentioned oxidation inhibitor provided by the present invention can be about to each raw material and mix by conventional physical mixed method preparation, and stirring gets final product.
Above-mentioned oxidation inhibitor provided by the present invention, also can be used with lubricating oil or the grease base plinth oil phase of routine, the base oil of described routine as, mineral oil, high-precision (refining) mineral oil, alkylation mineral oil, poly-alpha olefins, polyethers synthetic oil, alkylbenzene oil, biodegradable ester class wet goods.Among the present invention, preferably with the present invention in above-mentioned base oil (the amyl-based polyol diprotic acid multiple ester) use that matches that provides, be higher than 80 ℃ fire resistant hydraulic fluid as working point temperature in the hydraulic efficiency system.
Better, described extreme pressure anti-wear additives is tritolyl phosphate and thiophosphatephosphorothioate.Better, described tritolyl phosphate accounts for 2～4 weight parts, and described thiophosphatephosphorothioate accounts for 1～3 weight part.
Described defoamer is methyl-silicone oil.
Described rust-preventive agent is benzotriazole and Benzotriazole Derivative.Better, described benzotriazole accounts for 1～4 weight part, and described Benzotriazole Derivative accounts for 1～4 weight part.
Described Benzotriazole Derivative is domestic additive T551.
Above-mentioned fire resistant hydraulic fluid provided by the present invention can be about to each raw material and mix by conventional physical mixed method preparation, and stirring gets final product.
Above-mentioned fire resistant hydraulic fluid provided by the present invention, at first by adopting base oil of the present invention (the multiple ester of amyl-based polyol diprotic acid) as the base oil of environmentally friendly synthetic fire resistant hydraulic fluid, satisfied the non-flame properties of hydraulic efficiency system under the High Temperature High Pressure, the job requirement of sticking warm nature, can reach biodegradable environmental requirement, biological degradation rate＞80%; Secondly, by selecting the composite collaborative of several oxidation inhibitor, reach various antioxidant properties and have complementary advantages, improved greatly the long term high temperature anti-oxidative stability of fire resistant hydraulic fluid; At last, by selecting the optimum combination of extreme pressure anti-wear additives, rust-preventive agent, kilfoam, so that environmentally friendly synthetic fire resistant hydraulic fluid of the present invention has excellent over-all properties.
Evidence, environmentally friendly synthetic fire resistant hydraulic fluid of the present invention can further improve the high temperature antioxygen that improves oil product, improve the lubricated abrasion resistance of oil product and increase the service life; Have high flash point, high burning-point, low vaporization losses, high viscosity index (HVI), excellent lubricity, nontoxic, biodegradable and good adaptability for materials and main raw material from reproducible animal-plant oil through performances such as chemical process form.
Above-mentioned fire resistant hydraulic fluid provided by the present invention has excellent viscosity temperature characteristic, high-temperature oxidation resistant stability, non-flame properties, lubricity, rust-preventing characteristic, anti-bubble, easily contact applicable to various High Temperature High Pressure in the hydraulic efficiency system of naked light, such as continuous casting and rolling hydraulic efficiency system, desulfurizing iron system and the RH vacuum oven equipment of Steel Plant.Described high-temperature and high-pressure conditions typically refers to temperature and is higher than 80 ℃, and pressure is higher than the occasion of 20MPa.Compare with mineral base (compressor) hydraulic efficiency oil: have energy-conservation, as to reduce oil consumption, minimizing environmental pollution and increase the service life (more than 3 times) advantage, can satisfy the job requirement that High Temperature High Pressure easily contacts the hydraulic efficiency system of naked light fully.
Embodiment
Further set forth the present invention below in conjunction with embodiment.Should be understood that these embodiment only are used for explanation the present invention, but not limit the scope of the invention.The reagent of the experimental technique of unreceipted actual conditions and undeclared prescription is according to the condition of normal condition or manufacturers suggestion and carries out or dispose in the following example.
The preparation of embodiment 1 base oil
Preparation process is as follows:
1, selecting carbon number is two kinds of diprotic acid of 5～12, add amount of substance and be the alcohol mixture that is formed by neopentyl glycol, TriMethylolPropane(TMP) and new penta tetrol of 2 times of this diprotic acid, add again amount of substance for the tosic acid of zirconic acid four monooctyl esters of this mixed dibasic acid 0.95～1.05% and 1.9～2.1% as catalyzer, stirring reaction is 140～180 minutes under 160～180 ℃ temperature, finishes the first step esterification.
2, adding amount of substance is that the carbon number of mixed dibasic acid more than 4 times is 14 to 20 unary fatty acid, (it is more excessive that unary fatty acid is wanted, so that the second step esterification is complete), stirring reaction is 100～120 minutes under 200～220 ℃ temperature, finishes the second step esterification.
3, with reaction product at 200 ℃, carry out underpressure distillation under the condition of 3.2Kpa, can remove unreacted excess fatty acids.
4, reaction product is cooled to 60 ℃ and puts into the alkali cleaning still, add first 3～5% water-soluble neutralization of yellow soda ash, can remove catalyzer and part unreacted reactant; Then washing, also is in order to remove the residual and catalyzer after the alkali cleaning.
5, under vacuum condition, dehydrate, filter and namely get the multiple ester of desired amyl-based polyol diprotic acid.
Each raw material and consumption are as shown in table 1:
Table 1
Annotate: the data in the table 1 all represent the mole proportion relation of each stock yard.
The properties of the multiple ester of the amyl-based polyol diprotic acid that employing above-mentioned raw materials proportioning and preparation method obtain is as shown in table 2:
Table 2
* Comparative Examples is Uniflex 212 base oils of Arizona chemical company.
The preparation of embodiment 2 oxidation inhibitor
Press the weight part formulated oxidation inhibitor in the table 3.
Compound method: raw material mixed by proportioning get final product.
Table 3
| 1# | 2# | 3# | 4# | |
| Di-iso-octyldiphenylamine (weight part) | 5 | 8 | 4 | 10 |
| Phenyl-a-naphthylamine (weight part) | 5 | 8 | 4 | 10 |
| 2,6 DI-tert-butylphenol compounds (weight part) | 9 | 6 | 10 | 5 |
| Thiocarbamate (weight part) | 14 | 8 | 15 | 6 |
The structural formula of thiocarbamate is (C in the table 3
4H
9)
2NCS
2CS
2CN (C
4H
9)
2
The performance of embodiment 3 oxidation inhibitor
4# prescription base oil among the employing embodiment 1 and the various oxidation inhibitor in the following table mix, and wherein said base oil accounts for 98wt%, and the total amount of oxidation inhibitor accounts for 2wt%.Each raw material is mixed by proportioning, stir.
Table 4
Annotate: the total amount of oxidation inhibitor is 2.0%, and wherein, the structural formula of thiocarbamate is (C
4H
9)
2NCS
2CS
2CN (C
4H
9)
2
Data can be found out from table 4, the present invention selects by di-iso-octyldiphenylamine, phenyl-a-naphthylamine, 2, the composite oxidation inhibitor that forms of 6 DI-tert-butylphenol compounds and thiocarbamate, the performance advantage that has reached various antioxidants is complementary, has improved greatly the long term high temperature anti-oxidative stability of oil product.
The preparation of embodiment 4 environmentally friendly synthetic fire resistant hydraulic fluids
By following weight percent preparation raw material, mix, can obtain environmentally friendly synthetic fire resistant hydraulic fluid.
Di-iso-octyldiphenylamine 0.5%
Phenyl-a-naphthylamine 0.5%
2,6 DI-tert-butylphenol compounds 0.9%
Thiocarbamate 1.4%
Tritolyl phosphate 1.8%
Thiophosphatephosphorothioate 0.8%
Methyl-silicone oil 10ppm
Benzotriazole 0.14%
Benzotriazole Derivative (T551) 0.06%
1# prescription base oil 93.9% among the embodiment 1
The structural formula of described thiocarbamate is (C
4H
9)
2NCS
2CS
2CN (C
4H
9)
2
Environmentally friendly synthetic fire resistant hydraulic fluid to present embodiment detects, and the result is as follows:
Table 5
| Project | Technical indicator | Measured data | Test method |
| 40 ℃ of mm of kinematic viscosity 2/s 100℃ mm 2/s | 68 # 68±6.8 | 62.16 11.86 | GB/T265 |
| Viscosity index | ≥180 | 191 | GB/T2541 |
| Flash-point (opening) ℃ | ≥260 | 296 | GB/T3536 |
| Burning-point ℃ | ≥310 | 334 | GB/T3536 |
| Pour point ℃ | ≤-20 | -30 | GB/T3535 |
| Moisture % | ≤ vestige | Nothing | GB/T 260 |
| Acid number mgKOH/g | ≤2.6 | 0.22 | GB/T 264 |
| Copper corrosion (100 ℃ * 3h) level | ≤1 | 1a | GB/T5096 |
| 24 ℃, 93 ℃, rear 24 ℃ of foaming properties ml/ml | ≤ 100/0 100/0 100/0 | 5/0 15/0 5/0 | GB/T12579 |
| 54 ℃ of min of demulsification performance (40-37-3) | ≤30 | 13 | GB/T 7305 |
| Mechanical impurity % | Nothing | Nothing | GB/T 511 |
| Oxidation stability min | Actual measurement | 936 | SH/T 0193 |
The performance of the fire resistant hydraulic fluid that present embodiment obtains and the like product of import (Quintolubric 888) compares: pour point is low, and the flash-point burning-point is high, excellent demulsification performance, and anti-foaming properties is excellent, and extreme pressure anti-wear is excellent, the results are shown in Table 6.
Table 6
The fire resistant hydraulic fluid that present embodiment obtains is on probation at the RH of steelworks vacuum oven, through nearly 5 years use, should synthesize the normal working performance requirement that (ester type) fire resistant hydraulic fluid can satisfy equipment, indices is all normal, has substituted original import fire resistant hydraulic oil (table 7 is the analytical results of uninterrupted sampling over 5 years) fully.
The practical application of table 7 fire resistant hydraulic fluid (I)
The preparation of embodiment 5 environmentally friendly synthetic fire resistant hydraulic fluids
By following weight percent preparation raw material, mix, can obtain environmentally friendly synthetic fire resistant hydraulic fluid.
Di-iso-octyldiphenylamine 0.8%
Phenyl-a-naphthylamine 0.8%
2,6 DI-tert-butylphenol compounds 0.6%
Thiocarbamate 0.8%
Tritolyl phosphate 1.1%
Thiophosphatephosphorothioate 1.2%
Methyl-silicone oil 30ppm
Benzotriazole 0.08%
Benzotriazole Derivative (T551) 0.12%
2# prescription base oil 94.5% among the embodiment 1
The structural formula of described thiocarbamate is (C
4H
9)
2NCS
2CS
2CN (C
4H
9)
2
Above-mentioned environmentally friendly synthetic fire resistant hydraulic fluid is detected result such as table 8.
Table 8
| Project | Technical indicator | Measured data | Test method |
| 40 ℃ of mm of kinematic viscosity 2/s 100℃ mm 2/s | 68# 68±6.8 | 62.64 12.08 | GB/T265 |
| Viscosity index | ≥180 | 194 | GB/T2541 |
| Flash-point (opening) ℃ | ≥260 | 300 | GB/T3536 |
| Burning-point ℃ | ≥310 | 332 | GB/T3536 |
| Pour point ℃ | ≤-20 | -30 | GB/T3535 |
| Moisture % | ≤ vestige | Nothing | GB/T 260 |
| Acid number mgKOH/g | ≤2.6 | 0.30 | GB/T 264 |
| Copper corrosion (100 ℃ * 3h) level | ≤1 | 1a | GB/T5096 |
| 24 ℃, 93.5 ℃, rear 24 ℃ of foaming properties ml/ml | ≤ 100/0 100/0 100/0 | 10/0 20/0 10/0 | GB/T12579 |
| 54 ℃ of min of demulsification performance (40-37-3) | ≤30 | 8 | GB/T 7305 |
| Mechanical impurity % | Nothing | Nothing | GB/T 511 |
| Oxidation stability min | Actual measurement | 984 | SH/T 0193 |
The performance of the fire resistant hydraulic fluid that present embodiment obtains and the like product of import (Quintolubric 888) compares: pour point is low, and the flash-point burning-point is high, excellent demulsification performance, and anti-foaming properties is excellent, and extreme pressure anti-wear is excellent, the results are shown in Table 9.
Table 9
The fire resistant hydraulic fluid replace imported oil product of the same type that present embodiment obtains is brought into use in import equipment continuous casting and rolling hydraulic efficiency system, through many uses half a year, satisfied equally the normal working performance requirement of equipment, obtained satisfied effect.Afterwards, in the enterprising enforcement usefulness of the desulfurizing iron system of steelworks, through the use in 1 year, the normal working performance that satisfies equipment fully required (table 10 is for using year afterwards analytical results of sampling of half a year/one) with this fire resistant hydraulic fluid
The practical application of table 10 fire resistant hydraulic fluid (II)
Use by three systems each 5 years, a year and half a year, to seeing carrying out conventional physics and chemistry detected result with oil sample, all test items change little, namely still meet the standard-required that dispatches from the factory through the oil sample that works long hours, show synthetic (ester type) fire resistant hydraulic fluid steady quality of the present invention, dependable performance, and continue in addition the potentiality that increase the service life.
The preparation of embodiment 6 environmentally friendly synthetic fire resistant hydraulic fluids
By following weight percent preparation raw material, mix, can obtain environmentally friendly synthetic fire resistant hydraulic fluid.
Di-iso-octyldiphenylamine 0.7%
Phenyl-a-naphthylamine 0.7%
2,6 DI-tert-butylphenol compounds 1.3%
Thiocarbamate 1.8%
Tritolyl phosphate 2.3%
Thiophosphatephosphorothioate 1.1%
Methyl-silicone oil 50ppm
Benzotriazole 0.02%
Benzotriazole Derivative (T551) 0.08%
2# prescription base oil 92% among the embodiment 1
The structural formula of described thiocarbamate is (C
4H
9)
2NCS
2CS
2CN (C
4H
9)
2
Above-mentioned environmentally friendly synthetic fire resistant hydraulic fluid is detected result such as table 11.
Table 11
| Project | Technical indicator | Measured data | Test method |
| 40 ℃ of mm of kinematic viscosity 2/s 100℃mm 2/s | 68# 68±6.8 | 64.45 12.74 | GB/T265 |
| Viscosity index | ≥180 | 202 | GB/T2541 |
| Flash-point (opening) ℃ | ≥260 | 310 | GB/T3536 |
| Burning-point ℃ | ≥310 | 338 | GB/T3536 |
| Pour point ℃ | ≤-20 | -36 | GB/T3535 |
| Moisture % | ≤ vestige | Nothing | GB/T 260 |
| Acid number mgKOH/g | ≤2.6 | 0.16 | GB/T 264 |
| Copper corrosion (100 ℃ * 3h) level | ≤1 | 1a | GB/T5096 |
| 24 ℃, 93 ℃, rear 24 ℃ of foaming properties ml/ml | ≤ 100/0 100/0 100/0 | 5/0 10/0 10/0 | GB/T12579 |
| 54 ℃ of min of demulsification performance (40-37-3) | ≤30 | 8 | GB/T 7305 |
| Mechanical impurity % | Nothing | Nothing | GB/T 511 |
The preparation of embodiment 7 environmentally friendly synthetic fire resistant hydraulic fluids
By following weight percent preparation raw material, mix, can obtain environmentally friendly synthetic fire resistant hydraulic fluid.
Di-iso-octyldiphenylamine 0.7%
Phenyl-a-naphthylamine 0.7%
2,6 DI-tert-butylphenol compounds 0.2%
Thiocarbamate 0.3%
Tritolyl phosphate 0.5%
Thiophosphatephosphorothioate 1.0%
Methyl-silicone oil 5ppm
Benzotriazole 0.32%
Benzotriazole Derivative (T551) 0.08%
2# prescription base oil 96.2% among the embodiment 1
The structural formula of described thiocarbamate is (C
4H
9)
2NCS
2CS
2CN (C
4H
9)
2
Above-mentioned environmentally friendly synthetic fire resistant hydraulic fluid is detected result such as table 12.
Table 12
| Project | Technical indicator | Measured data | Test method |
| 40 ℃ of mm of kinematic viscosity 2/s 100℃ mm 2/s | 68# 68±6.8 | 63.74 12.48 | GB/T265 |
| Viscosity index | ≥180 | 199 | GB/T2541 |
| Flash-point (opening) ℃ | ≥260 | 310 | GB/T3536 |
| Burning-point ℃ | ≥310 | 338 | GB/T3536 |
| Pour point ℃ | ≤-20 | -33 | GB/T3535 |
| Moisture % | ≤ vestige | Nothing | GB/T 260 |
| Acid number mgKOH/g | ≤2.6 | 0.15 | GB/T 264 |
| Copper corrosion (100 ℃ * 3h) level | ≤1 | 1a | GB/T5096 |
| 24 ℃, 93 ℃, rear 24 ℃ of foaming properties ml/ml | ≤ 100/0 100/0 100/0 | 0/0 10/0 5/0 | GB/T12579 |
| 54 ℃ of min of demulsification performance (40-37-3) | ≤30 | 9 | GB/T 7305 |
| Mechanical impurity % | Nothing | Nothing | GB/T 511 |
The preparation of embodiment 8 high-temperature chain oils
By following weight percent preparation raw material, mix, can obtain high-temperature chain oil.
2# prescription base oil 65% among the embodiment 1
PRIOLUBE 1929 16％
Polyisobutene 15%
Di-iso-octyldiphenylamine 1.5%
Thiocarbamate 1.0%
Phosphoric acid ester 1.5%
Described PRIOLUBE 1929 is the product of CRODA company,
The molecular weight of described polyisobutene is 2400;
Described phosphoric acid ester is the product hostaphat 1322 of Clariant company;
The structural formula of described thiocarbamate is (C
4H
9)
2NCS
2CS
2CN (C
4H
9)
2
Above-mentioned synthesizing high temperature chain oils is detected result such as following table:
Table 13
Claims (6)
1. base oil is the multiple ester of amyl-based polyol diprotic acid, and the multiple ester of described amyl-based polyol diprotic acid is by first with C
5～12The complete esterification of alcohol mixture that forms with neopentyl glycol, TriMethylolPropane(TMP) and new penta tetrol of the carboxyl of binary of fatty acids after, use again C
14～20Unsaturated unary fatty acid end-blocking and make; Described C
14～20Unsaturated unary fatty acid be selected from vegetable oil acid, hexadecylenic acid; In the described alcohol mixture, the molar percentage of neopentyl glycol, TriMethylolPropane(TMP), new penta tetrol is as follows:
Neopentyl glycol: 20～30%;
TriMethylolPropane(TMP): 50～60%;
New penta tetrol: 10～30%;
Described C
5～12Binary of fatty acids be two kinds of C
5～12The mixing of straight chain binary of fatty acids, described two kinds of C
5～12The mol ratio of straight chain binary of fatty acids be 1:1～1:4;
Described straight chain binary of fatty acids is selected from pentanedioic acid, hexanodioic acid, pimelic acid, suberic acid, nonane diacid, sebacic acid, undecane diacid and dodecanedioic acid.
2. the preparation method of a base oil as claimed in claim 1 may further comprise the steps:
1) makes C
5～12Binary of fatty acids and the alcohol mixture that neopentyl glycol, TriMethylolPropane(TMP) and new penta tetrol form, esterification occurs under the katalysis of catalyzer;
2) after reaction was finished described in the step 1), adding molar weight was described C
5～12At least 4 times C of binary of fatty acids integral molar quantity
14～20Unsaturated unary fatty acid mixing esterification, obtain reaction product;
3) removal step 2) unreacted excess fatty acids and the described catalyzer of step 1) in the products therefrom obtain the multiple ester of amyl-based polyol diprotic acid.
3. preparation method as claimed in claim 2 is characterized in that, in the step 1), described catalyzer is zirconic acid four monooctyl esters and tosic acid.
4. preparation method as claimed in claim 3 is characterized in that, in the step 1), the molar weight of described zirconic acid four monooctyl esters is described C
5～12The binary of fatty acids integral molar quantity 0.95～1.05%, the molar weight of described tosic acid is described C
5～12The binary of fatty acids integral molar quantity 1.9～2.1%.
5. the application of base oil as claimed in claim 1 in lubricating oil or lubricating grease.
6. application as claimed in claim 5 is characterized in that, described lubricating oil or lubricating grease are fire resistant hydraulic fluid, high-temperature chain oil or high temperature grease.
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| CN102010772A (en) * | 2010-12-01 | 2011-04-13 | 中国科学院新疆理化技术研究所 | Ester lubricating base oil with dumbbell-type structure and preparation method thereof |
| WO2013129910A1 (en) | 2012-02-28 | 2013-09-06 | Petroliam Nasional Berhard | Composition of matter polyols for polyurethane applications |
| CN104302612B (en) * | 2012-02-28 | 2017-07-18 | 马来西亚国家石油公司 | Lubricant compositions of material and preparation method thereof |
| CN104271546B (en) | 2012-02-28 | 2017-06-09 | 马来西亚国家石油公司 | Production method of ester and application thereof |
| CN103013635B (en) * | 2012-12-27 | 2014-01-15 | 安陆市奥森石油化学有限责任公司 | Ester type fire-resistant hydraulic fluid and preparation method thereof |
| MY169226A (en) | 2013-02-28 | 2019-03-19 | Petroliam Nasional Berhad | Preparation of biopolyol esters for lubricant application |
| CN104845700B (en) * | 2013-06-05 | 2021-06-01 | 中国科学院微生物研究所 | Lubricating oil base oil with long carbon chain dibasic acid complex ester structure and preparation method and application thereof |
| CN105331427B (en) * | 2014-08-11 | 2018-10-12 | 中国石油化工股份有限公司 | A kind of biodegradable plant oil-base fluid pressure oil composition |
| EP3305878A4 (en) * | 2015-06-08 | 2018-12-05 | NOF Corporation | Ester for refrigeration oil and working fluid composition for refrigeration oil |
| CN107586398A (en) * | 2017-09-27 | 2018-01-16 | 浙江锦润生物科技有限公司 | A kind of colorless and odorless liquid plasticses lubricant and synthetic method |
| CN109294705A (en) * | 2018-10-18 | 2019-02-01 | 广州领扬科技有限公司 | Compressor lubricant oil |
| CN111100750A (en) * | 2018-10-29 | 2020-05-05 | 台境企业股份有限公司 | Waste fluoride oil treatment method and system |
| CN113088363B (en) * | 2021-04-14 | 2022-10-21 | 海南热带海洋学院 | Preparation method of coconut oil fatty acid composite ester |
| CN114621804A (en) * | 2021-12-25 | 2022-06-14 | 科特龙流体科技（扬州）有限公司 | Composite extreme pressure additive and preparation method thereof |
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