CN113073000A - Method for improving performance of phosphate flame-retardant hydraulic oil - Google Patents
Method for improving performance of phosphate flame-retardant hydraulic oil Download PDFInfo
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- C10M2207/10—Carboxylix acids; Neutral salts thereof
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- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
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- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
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- 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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- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/0405—Phosphate esters used as base material
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- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/041—Triaryl phosphates
- C10M2223/0415—Triaryl phosphates used as base material
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Abstract
The invention discloses a method for improving the performance of phosphate flame-retardant hydraulic oil, which comprises the following steps: adding the magnesium-aluminum hydrotalcite into the phosphate base oil, stirring and adsorbing for 0.5-10h at the temperature of 70-200 ℃, and then filtering and separating to obtain the magnesium-aluminum hydrotalcite and the improved phosphate base oil; controlling the mass ratio of the magnesium-aluminum hydrotalcite to the phosphate base oil to be 0.5-20: 100; sequentially adding a viscosity index improver, an antioxidant, an anticorrosive agent, an acid capture agent, an antifoaming agent and a dye into the improved phosphate base oil, and uniformly mixing to obtain phosphate flame-retardant hydraulic oil; the magnalium hydrotalcite can be recycled after being washed, filtered, dried, roasted and regenerated; according to the invention, the magnesium-aluminum hydrotalcite is used for treating the phosphate base oil, so that the volume resistivity and the spontaneous ignition point of the phosphate fire-resistant hydraulic oil can be obviously improved, and the operation method is simple and easy to implement. In addition, the hydrotalcite can be recycled after being filtered, roasted and regenerated, and has good economic benefit.
Description
Technical Field
The invention belongs to the technical field of synthetic lubricating oil, and particularly relates to a method for improving the performance of phosphate flame-retardant hydraulic oil.
Background
The phosphate flame-retardant hydraulic oil is artificially synthesized lubricating oil, and the base oil mainly comprises three types of trialkyl phosphate, triaryl phosphate and alkyl aryl phosphate. The triaryl phosphate ester has higher viscosity and viscosity-temperature performance compared with trialkyl phosphate ester with the same relative molecular mass, and is widely used as industrial flame-retardant hydraulic fluid. In addition, the phosphate fire-resistant hydraulic oil has good fire resistance and excellent abrasion resistance, and has irreplaceable positions in electric power, military, aircraft hydraulic systems and high-temperature and high-pressure hydraulic systems close to high-temperature heat sources and nearby open fires.
With the rapid development of the power industry, large-capacity and high-parameter steam turbine units are more and more put into operation, and the single-machine capacity of a thermal power plant reaches 300-800 MW. The unit with subcritical and supercritical parameters is widely applied, the steam temperature reaches about 550 ℃, the steam temperature can reach 565 ℃ higher, and the working pressure of a working medium, namely a regulating solution, of a speed regulating system is also increased to 3.0-14.0 Mpa[1,2]. The phosphate ester flame-retardant hydraulic oil is provided with various propertiesHigh requirements, in particular volume resistivity and self-ignition point. In general, the volume resistivity of the novel phosphate ester flame-retardant hydraulic oil is mainly related to the following factors, namely, the molecular structure of the phosphate ester base oil is higher, and the higher the proportion of alkane in the phosphate ester is, the higher the resistivity is; secondly, the content of polar substances, such as chloride ions, polar additives and the like, even though the addition amount is small, the resistivity is still adversely affected; and thirdly, the purity of the phosphate base oil is higher, and the higher the purity is, the higher the volume resistivity and the higher the self-ignition point are. In the current industrial production, the purity of the phosphate base oil is improved by means of water washing, alkali washing, distillation and the like, the self-ignition point and the volume resistivity of the phosphate base oil can be improved to a certain extent, but a large amount of electric energy is consumed in the process, and a large amount of waste water is generated at the same time.
[1] Application of Liu Yongluo phosphate fire-resistant oil in power plants in China [ J ] lubricating oil, 2006, 21 (5): 9-13.
[2] Zhengdongdong, Haoyudjie, Lichunchencheng, etc. State of the Art for the development of fire-resistant Hydraulic fluids [ J ] lubricating oils, 2012,27(2):5-9.
Disclosure of Invention
Aiming at the problems that the volume resistivity and the self-ignition point of the phosphate base oil sold in the market at present are low and can not meet the requirements of the power industry. The invention provides a method for adsorbing and treating phosphate base oil by using magnesium-aluminum hydrotalcite, and aims to reduce the energy consumption and cost for treating the phosphate base oil, remove impurities in the phosphate base oil in a simple and easy-to-operate mode, improve the purity and further improve the volume resistivity and the spontaneous combustion point of the phosphate base oil.
The invention can be realized by the following technical scheme:
a method for improving the performance of phosphate flame-retardant hydraulic oil comprises the following steps:
s1: adding the magnesium-aluminum hydrotalcite into the phosphate base oil, stirring and adsorbing for 0.5-10h at the temperature of 70-200 ℃, and then filtering and separating while hot to obtain the magnesium-aluminum hydrotalcite and the improved phosphate base oil; controlling the mass ratio of the magnesium-aluminum hydrotalcite to the phosphate base oil to be 0.5-20: 100;
s2: sequentially adding a viscosity index improver, an antioxidant, an anticorrosive agent, an acid capture agent, an antifoaming agent and a dye into the improved phosphate base oil, and uniformly mixing to obtain phosphate flame-retardant hydraulic oil;
s3: and the magnesium-aluminum hydrotalcite is recycled after being washed, filtered, dried and roasted.
Preferably, the magnesium-aluminum hydrotalcite is one or more of carbonate type, sulfate type, nitrate type or chloride type; the roasting regeneration temperature of the magnesium-aluminum hydrotalcite is 150-600 ℃.
Preferably, the viscosity index improver is a derivative of polyacrylate; such as: one or more of polyethylmethacrylate, polybutylmethacrylate, styrene-butadiene copolymer and polyisobutylene; wherein the addition amount of the viscosity index improver accounts for 0.5-10% of the mass fraction of the phosphate flame-retardant hydraulic oil.
Preferably, the antioxidant comprises a hindered phenolic antioxidant; the hindered phenol antioxidant is one or more of amine antioxidant and polyol ester antioxidant; such as: 2, 6-di-tert-butyl-p-cresol, N-phenyl-alpha-naphthylamine and the like, wherein the addition amount of the antioxidant accounts for 1-5% of the mass fraction of the phosphate flame-retardant hydraulic oil.
Preferably, the corrosion inhibitor is perfluorocycloalkyl sulfonate, such as one or more of perfluorooctyl sodium sulfonate and perfluorooctyl potassium sulfonate; wherein the addition amount of the anticorrosive agent accounts for 0.5-10% of the mass fraction of the phosphate flame-retardant hydraulic oil.
Preferably, the acid capturing agent is one or more of 7-oxabicyclo [4,1,0] heptane-3-carboxylic acid and 7-oxabicyclo [4,1,0] heptane-3, 4-dicarboxylic acid; wherein the addition amount of the acid catching agent accounts for 1-3% of the mass fraction of the phosphate flame-retardant hydraulic oil.
Preferably, the antifoaming agent is dimethicone; wherein the addition amount of the antifoaming agent accounts for 0.005-0.1% of the mass fraction of the phosphate flame-retardant hydraulic oil.
Preferably, the addition amount of the dye accounts for 0.001-0.005% of the mass fraction of the phosphate flame-retardant hydraulic oil.
Preferably, in S1, the specific process for preparing the improved phosphate base oil comprises the steps of:
s11: preparing magnesium-aluminum hydrotalcite: mixing Mg (NO)3)2··6H2O and Al (NO)3)39H2O is dissolved in deionized water and is marked as solution A; dissolving sodium hydroxide and sodium carbonate by using deionized water, and marking as a solution B; sequentially sucking the solution A and the solution B by using a dropper, dripping the solution A and the solution B into a beaker to obtain a suspension, uniformly stirring the suspension for 12 hours at 70 ℃, keeping the pH value of the suspension at 10, and finally placing the suspension into a centrifugal machine for centrifugal separation, drying and grinding to obtain carbonate magnesium-aluminum hydrotalcite;
s12: 500g of the carbonate magnesium-aluminum hydrotalcite obtained in S11 was placed in a reaction vessel containing 50Kg of a mixed solution of trixylyl phosphate, isopropylated triphenyl phosphate, tricresyl phosphate and tri (isobutyl) phosphate; carrying out adsorption reaction at 100 ℃ for 10h, and then filtering to obtain a clear mixed solution: namely the improved phosphate base oil; controlling the mass ratio of the tri (xylene) phosphate to the isopropylated triphenyl phosphate to the tricresyl phosphate to the tri (isobutyl) phosphate to be 7:2: 0.5: 0.5.
preferably, the magnesium-aluminum hydrotalcite in S3 is filtered and recovered, then washed with petroleum ether for 3 times, placed in a 100 ℃ oven for vacuum drying to constant weight, then placed in a muffle furnace for temperature programming to 300 ℃ for roasting for 5 hours, taken out and placed in a drying oven for cooling to room temperature to obtain regenerated magnesium-aluminum hydrotalcite for later use;
putting 40g of regenerated magnesium aluminum hydrotalcite in a three-necked bottle filled with 400g of mixed solution of tri (xylene) phosphate, isopropylated triphenyl phosphate, tricresyl phosphate and tri (isobutyl) phosphate; performing adsorption reaction for 2 hours at 100 ℃, and then filtering until clear mixed liquor is obtained; namely the phosphate base oil treated by the regenerated magnesium aluminum hydrotalcite
Compared with the prior art, the invention has the beneficial effects that: magnesium aluminum hydrotalcite (Mg-Al LDHs) is used as a layered double hydroxide, and has wide application in the fields of environment and adsorption materials due to simple preparation process, excellent ion exchange property, thermal stability and the like; considering the structure of the magnesium-aluminum hydrotalcite, the operation method for treating the phosphate base oil is simple and convenient, the volume resistivity and the self-ignition point of the treated phosphate base oil are obviously improved, the volume resistivity can reach 5.0 x 1011 omega cm, and the self-ignition point can reach 650 ℃. In addition, the used hydrotalcite can be reused for 5 times after being washed, filtered, dried, roasted and regenerated, the volume resistivity of the phosphate ester base oil treated for the fifth time is 8.0 x 1010 omega cm, the spontaneous combustion point can reach 580 ℃, and the temperature is higher than that of the phosphate ester flame-retardant hydraulic oil sold in the market;
various additives are required to be added in the preparation of lubricating oil, and the phosphate flame-retardant hydraulic oil mainly comprises the following additives: viscosity index improver is mainly used for improving the viscosity-temperature performance of phosphate ester fire-resistant oil; secondly, the working temperature of the antioxidant and the phosphate flame-retardant hydraulic oil is higher, and the antioxidant needs to be added, so that the high-temperature oxidation process of oil products is reduced; and thirdly, the acid value of the acid capturing agent exceeds the standard, so that the hydrolysis of the phosphate ester is accelerated, and a series of adverse effects are caused. Therefore, a small amount of an acid-replenishing agent is required to be added, the acid value is reduced, and hydrolysis is inhibited. Metal such as anticorrosive, steel, copper, etc. is a catalyst for oxidizing phosphate, and in order to slow down the oxidation process, anticorrosive is added to reduce the catalytic action of metal.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for improving the performance of phosphate flame-retardant hydraulic oil comprises the following steps:
s1: adding the magnesium-aluminum hydrotalcite into the phosphate base oil, stirring and adsorbing for 10 hours at the temperature of 200 ℃, and then filtering and separating to obtain the magnesium-aluminum hydrotalcite and the improved phosphate base oil; controlling the mass ratio of the magnesium-aluminum hydrotalcite to the phosphate base oil to be 20: 100;
s2: sequentially adding an antioxidant, an acid capture agent, an antifoaming agent and a dye into the improved phosphate base oil, and mixing to obtain phosphate flame-retardant hydraulic oil;
s3: and the magnesium-aluminum hydrotalcite is washed, filtered, dried, roasted and regenerated, and then recycled.
The magnesium-aluminum hydrotalcite is one or more of carbonate, sulfate, nitrate or chloride; the roasting regeneration temperature of the magnesium-aluminum hydrotalcite is 600 ℃.
The viscosity index improver is a derivative of polyacrylate; such as one or more of polyethyl methacrylate, polybutyl methacrylate, styrene-butadiene copolymers and polyisobutylene; wherein the addition amount of the viscosity index improver accounts for 0.5-10% of the mass fraction of the phosphate flame-retardant hydraulic oil.
Antioxidants include hindered phenolic antioxidants; the hindered phenol antioxidant is one or more of amine antioxidant and polyol ester antioxidant; wherein the addition amount of the antioxidant accounts for 5 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
The anticorrosive agent is perfluoronaphthenic sulfonate which is one or more of perfluorooctyl sodium sulfonate and perfluorooctyl potassium sulfonate; wherein the addition amount of the anticorrosive agent accounts for 10 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
The acid capturing agent is one or more of 7-oxabicyclo [4,1,0] heptane-3-carboxylic acid and 7-oxabicyclo [4,1,0] heptane-3, 4-dicarboxylic acid; wherein the addition amount of the acid catching agent accounts for 3 percent of the mass of the phosphate flame-retardant hydraulic oil.
The anti-foaming agent is dimethyl silicone oil; wherein the addition amount of the antifoaming agent accounts for 0.1 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
The addition amount of the dye accounts for 0.005 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
In S1, a specific process for preparing an improved phosphate base oil comprises the steps of:
s11: preparing magnesium-aluminum hydrotalcite: mixing Mg (NO)3)2··6H2O and Al (NO)3)39H2O is dissolved in deionized water and is marked as solution A; dissolving sodium hydroxide and sodium carbonate by using deionized water, and marking as a solution B; using a dropper to suck the solution A and the solution in sequenceB, dropwise adding the suspension into a beaker to obtain suspension, uniformly stirring the suspension for 12 hours at 70 ℃, keeping the pH value of the suspension at 10, and finally placing the suspension into a centrifuge for centrifugal separation, drying and grinding to obtain carbonate magnesium-aluminum hydrotalcite;
s12: 500g of the carbonate magnesium-aluminum hydrotalcite obtained in S11 was placed in a reaction vessel containing 50Kg of a mixed solution of trixylyl phosphate, isopropylated triphenyl phosphate, tricresyl phosphate and tri (isobutyl) phosphate; carrying out adsorption reaction at 100 ℃ for 10h, and then filtering to obtain a clear mixed solution: namely the improved phosphate ester base oil; controlling the mass ratio of the tri (xylene) phosphate to the isopropylated triphenyl phosphate to the tricresyl phosphate to the tri (isobutyl) phosphate to be 7:2: 0.5: 0.5.
in S1, the specific preparation process of the phosphate flame-retardant hydraulic oil includes the steps of:
and S13, adding a viscosity index improver, an antioxidant, an anticorrosive agent, an antifoaming agent and a dye into the improved phosphate base oil, and stirring and dissolving uniformly to obtain the phosphate flame-retardant hydraulic oil.
The recycling process of the magnesium-aluminum hydrotalcite comprises the following steps:
filtering and recovering the magnesium-aluminum hydrotalcite in the S3, washing for 3 times by using petroleum ether, putting the magnesium-aluminum hydrotalcite in an oven with the temperature of 100 ℃ for vacuum drying until the weight is constant, then putting the magnesium-aluminum hydrotalcite in a muffle furnace for temperature programming to 300 ℃ for roasting for 5 hours, taking out the magnesium-aluminum hydrotalcite and putting the magnesium-aluminum hydrotalcite in a drier for cooling to room temperature to obtain recovered magnesium-aluminum hydrotalcite for later use;
putting 40g of recovered magnesium aluminum hydrotalcite in a conical flask filled with 400g of mixed solution of tri (xylene) phosphate, isopropylated triphenyl phosphate, tricresyl phosphate and tri (isobutyl) phosphate; performing adsorption reaction for 2 hours at 100 ℃, and then filtering until clear mixed liquor is obtained; thus obtaining the recycled phosphate base oil treated by the magnalium hydrotalcite. And then adding a viscosity index improver, an antioxidant, an anticorrosive agent, an anti-foaming agent and a dye, and uniformly stirring and dissolving to obtain the phosphate flame-retardant hydraulic oil. Example 2
A method for improving the performance of phosphate flame-retardant hydraulic oil comprises the following steps:
s1: adding the magnesium-aluminum hydrotalcite into the phosphate base oil, stirring and adsorbing for 5 hours at the temperature of 150 ℃, and then filtering and separating to obtain the magnesium-aluminum hydrotalcite and the improved phosphate base oil; controlling the mass ratio of the magnesium-aluminum hydrotalcite to the phosphate base oil to be 10: 100;
s2: sequentially adding a viscosity index improver, an antioxidant, an acid capture agent, an antifoaming agent and a dye into the improved phosphate base oil, and mixing to obtain phosphate type anti-flaming hydraulic oil;
s3: and the magnesium-aluminum hydrotalcite is recycled after being washed, filtered, dried and roasted.
The magnesium-aluminum hydrotalcite is one or more of carbonate, sulfate, nitrate or chloride; the roasting regeneration temperature of the magnalium hydrotalcite is 400 ℃.
The viscosity index improver is a derivative of polyacrylate; the derivative of the polyacrylate is one or more of polyethylmethacrylate, polybutylmethacrylate, styrene-butadiene copolymer and polyisobutylene; wherein the addition amount of the viscosity index improver accounts for 0.5-10% of the mass fraction of the phosphate flame-retardant hydraulic oil.
Antioxidants include hindered phenolic antioxidants; the hindered phenol antioxidant is one or more of amine antioxidant and polyol ester antioxidant; wherein the addition amount of the antioxidant accounts for 3 percent of the mass of the phosphate flame-retardant hydraulic oil.
The anticorrosive agent is perfluoronaphthenic sulfonate which is one or more of perfluorooctyl sodium sulfonate and perfluorooctyl potassium sulfonate; wherein the addition amount of the anticorrosive agent accounts for 5 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
The acid capturing agent is one or more of 7-oxabicyclo [4,1,0] heptane-3-carboxylic acid and 7-oxabicyclo [4,1,0] heptane-3, 4-dicarboxylic acid; wherein the addition amount of the acid catching agent accounts for 2 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
The anti-foaming agent is dimethyl silicone oil; wherein the addition amount of the antifoaming agent accounts for 0.05 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
The addition amount of the dye accounts for 0.003 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
In S1, a specific process for preparing an improved phosphate base oil comprises the steps of:
s11: mixing Mg (NO)3)2·6H2O and Al (NO)3)39H2O is placed in deionized water and stirred uniformly to obtain a solution A; dissolving sodium hydroxide and sodium carbonate in deionized water, and stirring to obtain a solution B; sequentially sucking the solution A and the solution B by using a dropper, dripping the solution A and the solution B into a beaker to obtain a suspension, uniformly stirring the suspension for 12 hours at 70 ℃, keeping the pH value of the suspension at 10, and finally placing the suspension into a centrifuge for centrifugal treatment, drying and grinding to obtain carbonate magnesium-aluminum hydrotalcite;
s12: 500g of the carbonate magnesium-aluminum hydrotalcite obtained in S11 was placed in a reaction vessel containing 50Kg of a mixed solution of trixylyl phosphate, isopropylated triphenyl phosphate, tricresyl phosphate and tri (isobutyl) phosphate; carrying out adsorption reaction at 100 ℃ for 10h, and then filtering to obtain a clear mixed solution: namely the improved phosphate base oil; controlling the mass ratio of the tri (xylene) phosphate to the isopropylated triphenyl phosphate to the tricresyl phosphate to the tri (isobutyl) phosphate to be 7:2: 0.5: 0.5.
filtering and recovering the magnesium-aluminum hydrotalcite in the S3, washing for 3 times by using petroleum ether, putting the magnesium-aluminum hydrotalcite in an oven with the temperature of 100 ℃ for vacuum drying until the weight is constant, then putting the magnesium-aluminum hydrotalcite in a muffle furnace for temperature programming to 300 ℃ for roasting for 5 hours, taking out the magnesium-aluminum hydrotalcite and putting the magnesium-aluminum hydrotalcite in the oven for cooling to room temperature to obtain recovered magnesium-aluminum hydrotalcite for later use;
putting 40g of recovered magnesium aluminum hydrotalcite in a three-necked bottle filled with 400g of mixed solution of tri (xylene) phosphate, isopropylated triphenyl phosphate, tricresyl phosphate and tri (isobutyl) phosphate; performing adsorption reaction for 2 hours at 100 ℃, and then filtering until clear mixed liquor is obtained; thus obtaining the regenerated magnesium aluminum hydrotalcite treated phosphate ester base oil. And then adding a viscosity index improver, an antioxidant, an anticorrosive agent, an anti-foaming agent and a dye, and uniformly stirring and dissolving to obtain the phosphate flame-retardant hydraulic oil. Example 3
A method for improving the performance of a phosphate ester base oil, comprising the steps of:
s1: adding the magnesium-aluminum hydrotalcite into the phosphate base oil, stirring and adsorbing for 10 hours at the temperature of 200 ℃, and then filtering and separating to obtain the magnesium-aluminum hydrotalcite and the improved phosphate base oil; controlling the mass ratio of the magnesium-aluminum hydrotalcite to the phosphate base oil to be 20: 100;
s2: adding a viscosity index improver, an antioxidant, an acid capture agent, an antifoaming agent and a dye into the improved phosphate base oil in sequence, and mixing to obtain phosphate anti-flaming hydraulic oil;
s3: and the magnesium-aluminum hydrotalcite is recycled after being washed, filtered, dried and roasted.
The magnesium-aluminum hydrotalcite is one or more of carbonate, sulfate, nitrate or chloride; the roasting regeneration temperature of the magnesium-aluminum hydrotalcite is 600 ℃.
The viscosity index improver is a derivative of polyacrylate; the derivative of the polyacrylate is one or more of polyethylmethacrylate, polybutylmethacrylate, styrene-butadiene copolymer and polyisobutylene; wherein the addition amount of the viscosity index improver accounts for 10 percent of the mass of the phosphate flame-retardant hydraulic oil.
Antioxidants include hindered phenolic antioxidants; the hindered phenol antioxidant is one or more of amine antioxidant and polyol ester antioxidant; wherein the addition amount of the antioxidant accounts for 5 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
The anticorrosive agent is perfluoronaphthenic sulfonate which is one or more of perfluorooctyl sodium sulfonate and perfluorooctyl potassium sulfonate; wherein the addition amount of the anticorrosive agent accounts for 10 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
The acid capturing agent is one or more of 7-oxabicyclo [4,1,0] heptane-3-carboxylic acid and 7-oxabicyclo [4,1,0] heptane-3, 4-dicarboxylic acid; wherein the addition amount of the acid catching agent accounts for 3 percent of the mass of the phosphate flame-retardant hydraulic oil.
The anti-foaming agent is dimethyl silicone oil; wherein the addition amount of the antifoaming agent accounts for 0.1 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
The addition amount of the dye accounts for 0.005 percent of the mass fraction of the phosphate flame-retardant hydraulic oil.
In S1, a specific process for preparing an improved phosphate base oil comprises the steps of:
s11: mixing Mg (NO)3)2·6H2O and Al (NO)3)39H2O is placed in deionized water and stirred uniformly to obtain a solution A; dissolving sodium hydroxide and sodium carbonate in deionized water, and stirring to obtain a solution B; sequentially sucking the solution A and the solution B by using a dropper, dripping the solution A and the solution B into a beaker to obtain a suspension, uniformly stirring the suspension for 12 hours at 70 ℃, keeping the pH value of the suspension at 10, and finally placing the suspension into a centrifuge for centrifugal treatment, drying and grinding to obtain carbonate magnesium-aluminum hydrotalcite;
s12: 500g of the carbonate magnesium-aluminum hydrotalcite obtained in S11 was placed in a reaction vessel containing 50Kg of a mixed solution of trixylyl phosphate, isopropylated triphenyl phosphate, tricresyl phosphate and tri (isobutyl) phosphate; carrying out adsorption reaction at 100 ℃ for 10h, and then filtering to obtain a clear mixed solution: namely the improved phosphate base oil; controlling the mass ratio of the tri (xylene) phosphate to the isopropylated triphenyl phosphate to the tricresyl phosphate to the tri (isobutyl) phosphate to be 7:2: 0.5: 0.5.
filtering and recovering the magnesium-aluminum hydrotalcite in the S3, washing for 3 times by using petroleum ether, putting the magnesium-aluminum hydrotalcite in a drying oven at 100 ℃ for vacuum drying until the weight is constant, then putting the magnesium-aluminum hydrotalcite in a muffle furnace for temperature programming to 300 ℃ for roasting for 5 hours, taking out the magnesium-aluminum hydrotalcite and putting the magnesium-aluminum hydrotalcite in the drying oven for cooling to room temperature to obtain the recovered magnesium-aluminum hydrotalcite for later use;
putting 40g of recovered magnesium aluminum hydrotalcite in a conical flask filled with 400g of mixed solution of tri (xylene) phosphate, isopropylated triphenyl phosphate, tricresyl phosphate and tri (isobutyl) phosphate; performing adsorption reaction for 2 hours at 100 ℃, and filtering until clear mixed liquor is obtained; thus obtaining the recycled phosphate base oil treated by the magnalium hydrotalcite. And then adding a viscosity index improver, an antioxidant, an anticorrosive agent, an anti-foaming agent and a dye, and uniformly stirring and dissolving to obtain the phosphate flame-retardant hydraulic oil. Performance tests were performed on each set of examples:
the performance test is carried out by improving phosphate ester flame-retardant hydraulic oil prepared from phosphate ester base oil;
testing the performance of phosphate flame-retardant hydraulic oil prepared from the recovered magnalium hydrotalcite-treated phosphate base oil;
the preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. A method for improving the performance of phosphate flame-retardant hydraulic oil is characterized by comprising the following steps: the method comprises the following steps:
s1: adding the magnesium-aluminum hydrotalcite into the phosphate base oil, stirring and adsorbing for 0.5-10h at the temperature of 70-200 ℃, and then filtering and separating to obtain the magnesium-aluminum hydrotalcite and the improved phosphate base oil; controlling the mass ratio of the magnesium-aluminum hydrotalcite to the phosphate base oil to be 0.5-20: 100;
s2: sequentially adding a viscosity index improver, an antioxidant, an anticorrosive agent, an acid capture agent, an antifoaming agent and a dye into the improved phosphate base oil to obtain phosphate flame-retardant hydraulic oil;
s3: and the magnesium-aluminum hydrotalcite is washed, filtered, dried, roasted and regenerated, and then recycled.
2. The method of claim 1, wherein the magnesium aluminum hydrotalcite is one or more of carbonate, sulfate, nitrate, or chloride; the roasting regeneration temperature of the magnesium-aluminum hydrotalcite is 150-600 ℃.
3. The method for improving the performance of a phosphate ester fuel resistance hydraulic oil according to claim 1, wherein the viscosity index improver is a derivative of polyacrylate; comprises one or more of polyethyl methacrylate, polybutyl methacrylate, styrene-butadiene copolymer and polyisobutylene; wherein the addition amount of the viscosity index improver accounts for 0.5-10% of the mass fraction of the phosphate flame-retardant hydraulic oil.
4. The method of claim 1, wherein the antioxidant comprises a hindered phenolic antioxidant; the hindered phenol antioxidant is one or more of amine antioxidant and polyol ester antioxidant, such as 2, 6-di-tert-butyl-p-cresol, N-phenyl-alpha-naphthylamine, etc.; wherein the addition amount of the antioxidant accounts for 1-5% of the mass fraction of the phosphate flame-retardant hydraulic oil.
5. The method for improving the performance of the phosphate ester flame-retardant hydraulic oil, according to claim 1, wherein the corrosion inhibitor is perfluorocycloalkyl sulfonate, and the perfluorocycloalkyl sulfonate is one or more of perfluorooctyl sodium sulfonate and perfluorooctyl potassium sulfonate; wherein the addition amount of the anticorrosive agent accounts for 0.5-10% of the mass fraction of the phosphate flame-retardant hydraulic oil.
6. The method for improving the performance of the phosphate ester flame-retardant hydraulic oil, according to claim 1, wherein the acid capturing agent is one or more of 7-oxabicyclo [4,1,0] heptane-3-carboxylic acid and 7-oxabicyclo [4,1,0] heptane-3, 4-dicarboxylic acid; wherein the addition amount of the acid catching agent accounts for 1-3% of the mass fraction of the phosphate flame-retardant hydraulic oil.
7. The method for improving the performance of the phosphate ester flame-retardant hydraulic oil, as claimed in claim 1, wherein the antifoaming agent is dimethicone; wherein the addition amount of the antifoaming agent accounts for 0.005-0.1% of the mass fraction of the phosphate flame-retardant hydraulic oil.
8. The method for improving the performance of the phosphate flame-retardant hydraulic oil as claimed in claim 1, wherein the dye is added in an amount of 0.001-0.005% by mass of the phosphate flame-retardant hydraulic oil.
9. The method for improving the performance of the phosphate ester flame-retardant hydraulic oil as claimed in claim 1, wherein in S1, the specific preparation process of the improved phosphate ester base oil comprises the following steps:
s11: mixing Mg (NO)3)2·6H2O and Al (NO)3)3Dissolving 9H2O in deionized water, and uniformly stirring to obtain a solution A; dissolving sodium hydroxide and sodium carbonate in deionized water, and stirring to obtain a solution B; sequentially sucking the solution A and the solution B by using a dropper, dripping the solution A and the solution B into a beaker to obtain a suspension, uniformly stirring the suspension at 70 ℃ for 12 hours, keeping the pH value of the suspension at 10, and finally placing the suspension into a centrifuge for centrifugal treatment, drying and grinding to obtain carbonate magnesium-aluminum hydrotalcite;
s12: 500g of the carbonate magnesium-aluminum hydrotalcite obtained in S11 was placed in a reaction vessel containing 50Kg of a mixed solution of trixylyl phosphate, isopropylated triphenyl phosphate, tricresyl phosphate and tri (isobutyl) phosphate; carrying out adsorption reaction at 100 ℃ for 10h, and then filtering to obtain a clear mixed solution: namely the improved phosphate ester base oil; controlling the mass ratio of the tri (xylene) phosphate to the isopropylated triphenyl phosphate to the tricresyl phosphate to the tri (isobutyl) phosphate to be 7:2: 0.5: 0.5.
10. the method for improving the performance of the phosphate ester flame-retardant hydraulic oil is characterized in that the magnesium-aluminum hydrotalcite in S3 is filtered and recovered, then washed with petroleum ether for 3 times, placed in a 100 ℃ oven for vacuum drying to constant weight, then placed in a muffle furnace for roasting for 5 hours at the temperature of 300 ℃ by programming, taken out and placed in a drying oven for cooling to room temperature to obtain regenerated magnesium-aluminum hydrotalcite for later use;
placing 40g of regenerated magnesium aluminum hydrotalcite in a three-necked bottle containing 400g of mixed solution of tri (xylene) phosphate, isopropylated triphenyl phosphate, tricresyl phosphate and tri (isobutyl) phosphate; performing adsorption reaction for 2 hours at 100 ℃, and then filtering until clear mixed liquor is obtained; namely the phosphate base oil treated by the regenerated magnesium aluminum hydrotalcite.
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