CN116396795A - Water-based environment-friendly flame-retardant hydraulic fluid and preparation method thereof - Google Patents

Water-based environment-friendly flame-retardant hydraulic fluid and preparation method thereof Download PDF

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CN116396795A
CN116396795A CN202310358693.0A CN202310358693A CN116396795A CN 116396795 A CN116396795 A CN 116396795A CN 202310358693 A CN202310358693 A CN 202310358693A CN 116396795 A CN116396795 A CN 116396795A
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hydraulic fluid
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retardant hydraulic
sodium
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CN116396795B (en
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孙晓明
吴枫
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Tepulangke Chemical Yingkou Co ltd
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Abstract

The invention relates to the technical field of hydraulic fluid, and discloses an aqueous environment-friendly flame-retardant hydraulic fluid and a preparation method thereof. The main components of the water-based anti-flaming hydraulic fluid are triazine-based anti-rust agent, extreme pressure anti-wear agent, pour point depressant, thickener, water and the like, wherein sulfonate groups contained in the triazine-based anti-rust agent are not only anionic groups, but also very strong hydrophilic groups, so that the water solubility, thickening property, adsorptivity and rust resistance of the triazine-based anti-rust agent can be improved, and when open fire is encountered, moisture is evaporated to isolate air, thereby achieving the flame-retardant effect.

Description

Water-based environment-friendly flame-retardant hydraulic fluid and preparation method thereof
Technical Field
The invention relates to the technical field of hydraulic fluid, in particular to an aqueous environment-friendly flame-retardant hydraulic fluid and a preparation method thereof.
Background
The hydraulic fluid is a working medium for transmitting power and signals in the hydraulic system, different hydraulic fluids have different functions, and the flame-retardant hydraulic fluid is mainly water-based flame-retardant hydraulic fluid, fatty acid ester flame-retardant hydraulic fluid and phosphate ester flame-retardant hydraulic fluid, is widely applied to the fields of metallurgical industry, mechanical manufacturing, plastic processing, coal exploitation and the like in high-temperature open flame environments, and can effectively reduce the risk of ignition of the hydraulic system. The water-base fire-retarding hydraulic liquid has the advantages of no decomposition in water, safety and reliability, convenient waste liquid incineration treatment, low cost, etc., and is mainly composed of water, glycol or homolog and various functional additives. Because water is a polar compound, cations such as calcium ions and magnesium ions are contained in the water, calcium carbonate and magnesium carbonate precipitates are easy to generate, anions such as chloride ions and sulfate ions are also contained in the water, equipment is easy to corrode, and therefore, the selection of the additive is important for the water-based flame-retardant hydraulic fluid. For example, the document 'preparation and application of environment-friendly water-soluble antirust agent' discloses that several excellent compounds are screened from tens of compounds such as sodium salt, amine salt and amide salt synthesized by taking alkyl chain mono-and polycarboxylic acid as raw materials to serve as water-soluble antirust agents, and the excellent compounds are compounded with borate compounds to display excellent antirust performance and good microbial stability, and can be used as water-based antirust agents instead of sodium nitrite with carcinogenic action.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides the water-based environment-friendly flame-retardant hydraulic fluid and the preparation method thereof, and the prepared water-based hydraulic fluid has good performance in flame resistance effect.
(II) technical scheme
A preparation method of an aqueous environment-friendly flame-retardant hydraulic fluid comprises the following steps:
(1) Preparation of sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate
3-parahydroxybenzoyl propionic acid-2-alkene is placed in a flask filled with sodium sulfite for sulfonation reaction, and 2-parahydroxybenzoyl-1-carboxyl ethanesulfonic acid sodium salt is obtained.
(2) Preparation of triazinyl rust inhibitor
Dissolving 2-parahydroxybenzoyl-1-carboxyl sodium ethanesulfonate and sodium hydroxide in a flask filled with acetone and water, stirring and dissolving, adding cyanuric chloride into the flask under the protection of nitrogen at 0-10 ℃ for stirring and reacting for 1-2h, heating to 70-90 ℃ for reflux reaction for 6-12h, cooling, standing, suction filtering, washing with ice water, and vacuum drying to obtain the triazinyl antirust agent.
(3) Preparation of water-based flame-retardant hydraulic fluid
The formula of the water-based flame-retardant hydraulic fluid is as follows: 10-20% of defoamer, 2-3% of triazinyl antirust agent, 1-3% of extreme pressure antiwear agent, 30-35% of pour point depressant, 10-15% of thickener, 2-5% of triethanolamine PH regulator and the balance of deionized water.
Preferably, the sulfonation reaction time in the step (1) is 30-60min, and the temperature is 20-35 ℃.
Preferably, the molar ratio of the sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate to the sodium sulfite in the step (1) is 1:1-1.2.
Preferably, in the step (2), the molar ratio of the sodium 2-parahydroxybenzoyl-1-carboxyl ethanesulfonate, sodium hydroxide and cyanuric chloride is 1:0.8-1.2:0.3-0.5.
Preferably, in the step (2), the stirring and dissolving time is 5-10min, and the temperature is 20-35 ℃.
Preferably, the defoaming agent in the step (3) is one of tributyl phosphate and polyether modified organosilicon.
Preferably, the extreme pressure antiwear agent in the step (3) is one of potassium dimer, oleic acid soap and water-soluble molybdenum.
Preferably, the pour point depressant in the step (3) is one of diethylene glycol, ethanol and ethylene glycol.
Preferably, the thickener in the step (3) is one of polyether, polyethylene glycol and fatty alcohol acrylate copolymer.
(III) beneficial technical effects
According to the invention, 3-parahydroxybenzoyl propionic acid-2-alkene is subjected to sulfonation reaction under the condition of sodium sulfite to obtain 2-parahydroxybenzoyl-1-carboxyl sodium ethanesulfonate, and the obtained product reacts with cyanuric chloride to obtain the triazinyl antirust agent. The main components of the water-based anti-flaming hydraulic fluid are a triazine-based anti-rust agent, an extreme pressure anti-wear agent, a pour point depressant, a thickener, water and the like, wherein a sulfonate group contained in the triazine-based anti-rust agent is an anionic group and a very strong hydrophilic group, so that the water solubility, thickening property, adsorptivity and rust resistance of the triazine-based anti-rust agent can be improved, the triazine-based anti-rust agent can participate in tribochemical reaction in the rust prevention process, a complex and compact boundary film containing sulfur and nitrogen is formed on the surface of metal, and the contact of water, oxygen and metal is prevented from forming electrode potential and corroding equipment. When encountering open fire, the moisture evaporates to isolate the air, thereby achieving the flame-retardant effect.
Drawings
FIG. 1 is a route to a process for preparing a triazine-based rust inhibitor.
Detailed Description
Example 1
(1) Preparation of sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate
6mol of 3-parahydroxybenzoyl-propionic acid-2-alkene was placed in a flask containing 7.2mol of sodium sulfite at 20 ℃ for sulfonation for 40min to obtain sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate.
(2) Preparation of the triazinyl antirust agent 3mol of sodium 2-p-hydroxybenzoyl-1-carboxyethane sulfonate and 3mol of sodium hydroxide are dissolved in a flask filled with acetone and water at 30 ℃, stirred and dissolved for 8min, 1.2mol of cyanuric chloride is added into the flask under the protection of nitrogen at 5 ℃ for stirring reaction for 1.5h, the temperature is raised to 80 ℃ for reflux reaction for 9h, and then the triazinyl antirust agent is obtained through cooling, standing, suction filtration, ice water washing and vacuum drying.
(3) Preparation of water-based flame-retardant hydraulic fluid
The formula of the water-based flame-retardant hydraulic fluid is as follows: the anti-rust agent comprises, by mass, 15% of polyether modified organosilicon defoamer, 2.5% of triazine-based rust inhibitor, 4% of oleic acid soap extreme pressure anti-wear agent, 30% of ethanol pour point depressant, 12% of polyethylene glycol thickener, 4% of triethanolamine PH regulator and the balance of deionized water.
Example 2
(1) Preparation of sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate
6mol of 3-parahydroxybenzoyl-propionic acid-2-alkene was placed in a flask containing 6mol of sodium sulfite at 20 ℃ to carry out sulfonation reaction for 30min, and 2-parahydroxybenzoyl-1-carboxyethane sulfonic acid sodium salt was obtained.
(2) Preparation of triazinyl rust inhibitor
At 30 ℃, 3mol of 2-parahydroxybenzoyl-1-carboxyl sodium ethane sulfonate and 3mol of sodium hydroxide are dissolved in a flask filled with acetone and water, stirred and dissolved for 8min, 1.2mol of cyanuric chloride is added into the flask under the protection of nitrogen at 5 ℃ for stirring and reacting for 1.5h, the temperature is raised to 80 ℃ for reflux reaction for 9h, and then the triazinyl antirust agent is obtained through cooling, standing, suction filtration, ice water washing and vacuum drying.
(3) Preparation of water-based flame-retardant hydraulic fluid
The formula of the water-based flame-retardant hydraulic fluid is as follows: the anti-rust agent comprises, by mass, 15% of tributyl phosphate defoamer, 2-3% of triazinyl rust inhibitor, 2% of potassium dimer extreme pressure antiwear agent, 35% of ethanol pour point depressant, 12% of polyether thickener, 5% of triethanolamine PH regulator and the balance of deionized water.
Example 3
(1) Preparation of sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate
6mol of 3-parahydroxybenzoyl-propionic acid-2-alkene was placed in a flask containing 7mol of sodium sulfite at 30 ℃ to carry out sulfonation reaction for 40min, and 2-parahydroxybenzoyl-1-carboxyethane sulfonic acid sodium salt was obtained.
(2) Preparation of triazinyl rust inhibitor
3mol of 2-parahydroxybenzoyl-1-carboxyl sodium ethanesulfonate and 3.6mol of sodium hydroxide are dissolved in a flask filled with acetone and water at 35 ℃, stirred and dissolved for 10min, 1.5mol of cyanuric chloride is added into the flask under the protection of nitrogen at 10 ℃ for stirring and reacting for 2h, the temperature is raised to 90 ℃ for reflux reaction for 12h, and then the triazinyl antirust agent is obtained through cooling, standing, suction filtration, ice water washing and vacuum drying.
(3) Preparation of water-based flame-retardant hydraulic fluid
The formula of the water-based flame-retardant hydraulic fluid is as follows: tributyl phosphate defoamer, 2% triazinyl antirust agent, 1% potassium dimer extreme pressure antiwear agent, 30% diethylene glycol pour point depressant, 10% polyether thickener, 2% triethanolamine PH regulator and the balance deionized water.
Example 4
(1) Preparation of sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate
6mol of 3-parahydroxybenzoyl-propionic acid-2-alkene was placed in a flask containing 7.2mol of sodium sulfite at 35 ℃ for sulfonation for 60min to obtain sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate.
(2) Preparation of triazinyl rust inhibitor
3mol of 2-parahydroxybenzoyl-1-carboxyl sodium ethanesulfonate and 3mol of sodium hydroxide are dissolved in a flask filled with acetone and water at 30 ℃, stirred and dissolved for 8min, 1.5mol of cyanuric chloride is added into the flask under the protection of nitrogen at 0 ℃ for stirring and reacting for 1h, the temperature is increased to 80 ℃ for reflux reaction for 9h, and then the triazinyl antirust agent is obtained through cooling, standing, suction filtration, ice water washing and vacuum drying.
(3) Preparation of water-based flame-retardant hydraulic fluid
The formula of the water-based flame-retardant hydraulic fluid is as follows: the anti-rust agent comprises, by mass, 20% of polyether modified organosilicon defoamer, 2.5% of triazine-based rust inhibitor, 2% of potassium dimer extreme pressure antiwear agent, 32% of ethanol pour point depressant, 12% of poly fatty alcohol acrylate copolymer thickener, 4% of triethanolamine PH regulator and the balance of deionized water.
Example 5
(1) Preparation of sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate
6mol of 3-parahydroxybenzoyl-propionic acid-2-alkene was placed in a flask containing 6mol of sodium sulfite at 35 ℃ to carry out sulfonation reaction for 40min, and 2-parahydroxybenzoyl-1-carboxyethane sulfonic acid sodium salt was obtained.
(2) Preparation of triazinyl rust inhibitor
3mol of 2-parahydroxybenzoyl-1-carboxyl sodium ethanesulfonate and 2.4mol of sodium hydroxide are dissolved in a flask filled with acetone and water at 20 ℃, stirred and dissolved for 5min, 0.9mol of cyanuric chloride is added into the flask under the protection of nitrogen at 0 ℃ for stirring and reacting for 1h, the temperature is raised to 70 ℃ for reflux reaction for 6h, and then the triazinyl antirust agent is obtained through cooling, standing, suction filtration, ice water washing and vacuum drying.
(3) Preparation of water-based flame-retardant hydraulic fluid
The formula of the water-based flame-retardant hydraulic fluid is as follows: the anti-rust agent comprises, by mass, 20% of polyether modified organosilicon defoamer, 3% of triazinyl rust inhibitor, 3% of water-soluble molybdenum extreme pressure anti-wear agent, 35% of ethylene glycol pour point depressant, 15% of fatty alcohol acrylate copolymer thickener, 5% of triethanolamine PH regulator and the balance of deionized water.
Comparative example 1
(1) Preparation of water-based flame-retardant hydraulic fluid
The formula of the water-based flame-retardant hydraulic fluid is as follows: tributyl phosphate defoamer with the mass ratio of 15%, 1% of water-soluble molybdenum extreme pressure antiwear agent, 35% of diethylene glycol pour point depressant, 10% of fatty alcohol acrylate copolymer thickener, 4% of triethanolamine PH regulator and the balance of deionized water.
The hydraulic fluid was tested for flame retardancy using a manifold firing test according to the NB/SH/T10567 standard.
The hydraulic fluid was tested for flash point according to GB/T3536 standard.
The air release value was tested according to SH/T0308 standard.
Figure BDA0004164223800000061
According to GB/5096-2017 standard, a copper sheet corrosion tester is adopted to test the rust resistance. The test mode is as follows: selecting a test copper sheet with the length and width of 70mm,12mm and 2mm, the purity of not less than 99%, enabling the surface of the copper sheet to be smooth, cleaning the surface of the copper sheet by using normal hexane, then placing the copper sheet into a hydraulic liquid, heating the copper sheet at the constant temperature of 100 ℃ for 3 hours, washing the copper sheet by using normal hexane, and comparing the copper sheet with a standard colorimetric card to test the rust-proof effect.
Selecting cylindrical steel with a bright surface, a cross section of 1.0cm < 2 > and a length of 5.0cm, placing the cylindrical steel in hydraulic fluid, heating at a constant temperature of 35 ℃ for 24 hours, washing the cylindrical steel with ionized water and absolute ethyl alcohol, drying, and observing the appearance and liquid appearance of a test piece.
Figure BDA0004164223800000071
The water-based hydraulic fluids of examples 1, 3, 4, and 5 perform well in manifold firing experiments. The flash point of example 4 was high, reaching 290 ℃. The air release value of example 3 is preferably less than or equal to 7 minutes. And the corrosion resistance and rust resistance of each example were excellent.

Claims (9)

1. A preparation method of an aqueous environment-friendly flame-retardant hydraulic fluid is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) Preparation of sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate
3-parahydroxybenzoyl propionic acid-2-alkene is placed in a flask filled with sodium sulfite for sulfonation reaction, and 2-parahydroxybenzoyl-1-carboxyl sodium ethane sulfonate is obtained;
(2) Preparation of triazinyl rust inhibitor
Dissolving 2-parahydroxybenzoyl-1-carboxyl sodium ethanesulfonate and sodium hydroxide in a flask filled with acetone and water, stirring and dissolving, adding cyanuric chloride into the flask under the protection of nitrogen at 0-10 ℃ for stirring and reacting for 1-2h, heating to 70-90 ℃ for reflux reaction for 6-12h, cooling, standing, suction filtering, washing with ice water, and vacuum drying to obtain the triazinyl antirust agent;
(3) Preparation of water-based flame-retardant hydraulic fluid
The formula of the water-based flame-retardant hydraulic fluid is as follows: 10-20% of defoamer, 2-3% of triazinyl antirust agent, 1-3% of extreme pressure antiwear agent, 30-35% of pour point depressant, 10-15% of thickener, 2-5% of triethanolamine PH regulator and the balance of deionized water.
2. The method for preparing the aqueous environment-friendly flame-retardant hydraulic fluid according to claim 1, which is characterized in that: the sulfonation reaction time in the step (1) is 30-60min, and the temperature is 20-35 ℃.
3. The method for preparing the aqueous environment-friendly flame-retardant hydraulic fluid according to claim 1, which is characterized in that: the molar ratio of the sodium 2-parahydroxybenzoyl-1-carboxyethane sulfonate to the sodium sulfite in the step (1) is 1:1-1.2.
4. The method for preparing the aqueous environment-friendly flame-retardant hydraulic fluid according to claim 1, which is characterized in that: in the step (2), the molar ratio of the sodium 2-parahydroxybenzoyl-1-carboxyl ethanesulfonate, the sodium hydroxide and the cyanuric chloride is 1:0.8-1.2:0.3-0.5.
5. The method for preparing the aqueous environment-friendly flame-retardant hydraulic fluid according to claim 1, which is characterized in that: in the step (2), stirring and dissolving are carried out for 5-10min at 20-35 ℃.
6. The method for preparing the aqueous environment-friendly flame-retardant hydraulic fluid according to claim 1, which is characterized in that: and (3) the defoamer in the step (3) is one of tributyl phosphate and polyether modified organic silicon.
7. The method for preparing the aqueous environment-friendly flame-retardant hydraulic fluid according to claim 1, which is characterized in that: the extreme pressure antiwear agent in the step (3) is one of potassium dimer, oleic acid soap and water-soluble molybdenum.
8. The method for preparing the aqueous environment-friendly flame-retardant hydraulic fluid according to claim 1, which is characterized in that: and (3) the pour point depressant in the step (3) is one of diethylene glycol, ethanol and ethylene glycol.
9. The method for preparing the aqueous environment-friendly flame-retardant hydraulic fluid according to claim 1, which is characterized in that: the thickener in the step (3) is one of polyether, polyethylene glycol and fatty alcohol acrylate copolymer.
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