CN110724582A - Tert-butylated triphenyl phosphate flame-retardant hydraulic oil and preparation method thereof - Google Patents
Tert-butylated triphenyl phosphate flame-retardant hydraulic oil and preparation method thereof Download PDFInfo
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- CN110724582A CN110724582A CN201910970620.0A CN201910970620A CN110724582A CN 110724582 A CN110724582 A CN 110724582A CN 201910970620 A CN201910970620 A CN 201910970620A CN 110724582 A CN110724582 A CN 110724582A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/045—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution and non-macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/74—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing phosphorus
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/08—Inorganic acids or salts thereof
- C10M2201/081—Inorganic acids or salts thereof containing halogen
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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 tert-butyl triphenyl phosphate flame-retardant hydraulic oil and a preparation method thereof, wherein the tert-butyl triphenyl phosphate flame-retardant hydraulic oil comprises the following raw materials in mass; phosphorus oxychloride: 450 kg; phenol: 450 kg-650 kg; p-tert-butylphenol: 450 kg-600 kg; MgCL2：1.75kg；NH4CL: 0.75 kg; antioxidant: 1 kg; and (3) anti-foaming agent: 2.5 kg; antirust agent: 2kg, which is prepared by mixing p-tert-butylphenol, phenol and MgCL2、NH4CL and phosphorus oxychloride are sequentially fed and reacted, and then an antioxidant, an antifoaming agent and an antirust agent are added and uniformly mixed to obtain the finished product of the tert-butyl triphenyl phosphate flame-retardant hydraulic oil. The method is carried out under a closed condition when the tert-butyl triphenyl phosphate is prepared, the reaction is uniform and stable, the mass preparation can be carried out, the method has the characteristics of low labor intensity and good working environment, the mass preparation can be carried out, the labor intensity is low, the working environment is good, and meanwhile, the prepared product has good heat resistance, flame resistance, oxidation resistance and sealing property and high product quality stability.
Description
Technical Field
The invention relates to the technical field of hydraulic oil preparation, and particularly relates to tert-butylated triphenyl phosphate flame-retardant hydraulic oil and a preparation method thereof.
Background
The hydraulic oil is a hydraulic medium used by a hydraulic system utilizing hydraulic pressure energy, and plays roles of energy transfer, wear resistance, system lubrication, corrosion resistance, rust resistance, cooling and the like in the hydraulic system. For hydraulic oil, the requirements of a hydraulic device on the viscosity of liquid at working temperature and starting temperature are firstly met, and the viscosity change of lubricating oil is directly related to hydraulic action, transmission efficiency and transmission precision, so that the viscosity-temperature performance and the shear stability of the oil are also required to meet various requirements proposed by different purposes. Hydraulic oils are of various types and have been classified by their classification methods, which have been used for a long time to classify the oil according to its type, chemical composition or combustibility.
The tert-butyl triphenyl phosphate is colorless or light yellow viscous liquid, has the flash point of 224 ℃, the boiling point of 245-260 ℃, the viscosity of 65-75(38 ℃), and the acid value of 0.1mgKOH/g, and has excellent thermal stability and hydrolysis resistance. Its high thermal stability allows it to be used as a flame retardant for engineering plastics, and also to improve the melting properties of the plastics. The tert-butyl triphenyl phosphate is superior to TPP in performance, is liquid, has better durability and hydrolytic stability in resin, is not easy to generate surface stress cracking, and is widely applied to flame-retardant PVC, cellulose resin, synthetic rubber, phenolic resin, epoxy resin, polyester fiber and the like.
At present, tert-butyl triphenyl phosphate is not used for preparing the flame-retardant hydraulic oil in a precedent way.
Disclosure of Invention
1. Technical problem to be solved
The invention aims to provide tert-butyl triphenyl phosphate flame-retardant hydraulic oil and a preparation method thereof, so as to solve the problems in the background technology.
2. Technical scheme
In order to solve the problems, the invention adopts the following technical scheme:
the tert-butyl triphenyl phosphate fire-resistant hydraulic oil comprises the following raw materials in mass;
phosphorus oxychloride: 450 kg;
the phenol: 450 kg-650 kg;
p-tert-butylphenol: 450 kg-600 kg;
MgCL2：1.75kg；
NH4CL：0.75kg；
antioxidant: 1 kg;
and (3) anti-foaming agent: 2.5 kg;
antirust agent: 2 kg.
Preferably, the NH is4CL and MgCL2Drying for 4-5 hours.
5. The preparation method of the tert-butyl triphenyl phosphate fire-resistant hydraulic oil according to claim 1, comprising the following steps;
s1, feeding;
s1-1: putting p-tert-butylphenol into a manhole of a reaction kettle, closing the manhole of the reaction kettle, plugging the upper opening of a buffer tank by using a rubber plug, starting a jet pump, opening a negative pressure valve, and connecting a feeding pipeline;
s1-2: when the vacuum degree in the reaction kettle is more than 300mmHg, pumping phenol into the reaction kettle, introducing steam into the reaction kettle for heating, and controlling the temperature within 70 ℃;
s1-3: when the tert-butyl phenol is completely dissolved, starting stirring, introducing cooling water for cooling, and adding prepared NH into the reaction kettle in the process of cooling4CL and MgCL2；
S1-4: when the temperature in the reaction kettle is lower than 50 ℃, pumping phosphorus oxychloride into the reaction kettle;
s2, reacting;
s2-1: closing the negative pressure throttle, emptying the negative pressure pipeline, closing the jet pump, opening the rubber plug at the upper opening of the buffer tank and the emptying port on the reaction kettle until no negative pressure exists in the reaction kettle, starting the normal pressure acid discharging system, supplying cooling water to the hydrochloric acid absorption tower, opening the normal pressure acid discharging throttle, and starting stirring;
s2-2: heating steam in a jacket of the reaction kettle, raising the reaction temperature to 70-75 ℃, balancing for 1-1.5 hours, adjusting the temperature rise speed to 3-4 ℃ per hour after balancing, balancing for 1 hour when the reaction temperature is raised to 95 +/-2 ℃, adjusting the temperature rise speed to 5-6 ℃ per hour after balancing, and starting a negative pressure acid discharge system when the reaction temperature is raised to about 135-140 ℃;
s2-3: blocking the upper opening of the buffer tank by using a rubber plug, starting a jet pump, closing a normal-pressure acid discharge throttle, opening a negative-pressure throttle, closing a normal-pressure acid discharge system, after acid discharge is finished, closing the negative-pressure throttle, emptying a negative-pressure pipeline, closing the jet pump, emptying the reaction kettle to normal pressure, opening a sampling opening, sampling, testing and detecting the acid value;
s2-4: according to the acid value detected in the step S2-3, adding carbon and oxygen for neutralization until the acid value is less than or equal to 3mgKOH/g, namely, the synthesis is finished;
s3 final mixing: and (3) closing the negative pressure acid discharge system, emptying a negative pressure pipeline, opening a rubber plug on the buffer tank, closing the jet pump, closing stirring, closing a steam throttle, adding an antioxidant, an antifoaming agent and an antirust agent according to the proportion, stirring during adding, and uniformly stirring to obtain the finished tert-butyl triphenyl phosphate flame-retardant hydraulic oil.
Preferably, when acid is discharged under negative pressure in the step S2-3, the reaction temperature is kept at 135-150 ℃, the vacuum degree reaches 620-750 mmHg, and acid is discharged for 2 hours.
Preferably, in step S2-4, carbon and oxygen are added to neutralize according to the detected acid value, the negative pressure acid discharge system is started, acid discharge is continued for 2 hours, after acid discharge by the negative pressure acid discharge system, sampling and assay are performed, the acid value is detected, and if the detected acid value is greater than 3mgKOH/g, carbon and oxygen are continuously added to neutralize until the acid value is less than or equal to 3 mgKOH/g.
Preferably, the liquid stored in the waste acid absorption tank in the step S3 is not suitable for direct discharge, and needs to be recycled after centralized treatment in a sewage tank.
Preferably, when the alkali is added in the step S2-4, the solid can be added into the reaction kettle by a material circulation carrying method.
3. Advantageous effects
1. The invention takes tert-butyl triphenyl phosphate as base oil, and then antioxidant is added: the anti-foaming agent and the antirust agent are prepared, because tert-butylated triphenyl phosphate has excellent thermal stability and excellent hydrolysis resistance, and self can be used as a flame retardant, so that hydraulic oil has heat-resistant and flame-retardant properties, and the antioxidant resistance of the added antioxidant can improve the oxidation resistance of the hydraulic oil, thereby prolonging the service life of the hydraulic oil, the added anti-foaming agent can prevent the hydraulic oil from generating bubbles when in use, and further the problem of poor sealing property caused by bubble breakage can be avoided, and the added antirust agent: the antirust agent can be mutually dissolved with oil, so that antirust agent molecules are directionally arranged on the surface of a carrier to form an adsorptive protective film, and the sealing property can be further ensured, so that the product prepared by the invention has better heat resistance, flame resistance, oxidation resistance and sealing property, and the product quality stability is high.
2. The method is carried out under a closed condition when the tert-butyl triphenyl phosphate is prepared, the reaction is uniform and stable, in addition, hydrogen chloride generated in the reaction is discharged through an acid discharge system, the corrosion of acid to equipment can be avoided, the batch preparation can be carried out, and the method has the characteristics of low labor intensity and better working environment.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example one
The tert-butyl triphenyl phosphate fire-resistant hydraulic oil comprises the following raw materials in mass;
phosphorus oxychloride: 450 kg;
phenol: 450 kg;
p-tert-butylphenol: 600 kg;
MgCL2：1.75kg；
NH4CL：0.75kg；
antioxidant: 1 kg;
and (3) anti-foaming agent: 2.5 kg;
antirust agent: 2 kg.
NH4CL and MgCL2Drying treatment is carried out for 4 hours.
The preparation method of the tert-butyl triphenyl phosphate fire-resistant hydraulic oil according to claim 1, comprising the following steps;
s1, feeding;
s1-1: putting p-tert-butylphenol into a manhole of a reaction kettle, closing the manhole of the reaction kettle, plugging the upper opening of a buffer tank by using a rubber plug, starting a jet pump, opening a negative pressure throttle, connecting a feeding pipeline, canceling an original flexible connecting pipe, and metering by using an automatically controlled mass flow meter, so that the labor intensity is greatly reduced and the material preparation time is shortened;
s1-2: when the vacuum degree in the reaction kettle is more than 300mmHg, pumping phenol into the reaction kettle, introducing steam into the reaction kettle for heating, and controlling the temperature within 70 ℃;
s1-3: when the tert-butyl phenol is completely dissolved, starting stirring, introducing cooling water for cooling, and adding prepared NH into the reaction kettle in the process of cooling4CL and MgCL2；
S1-4: when the temperature in the reaction kettle is lower than 50 ℃, pumping phosphorus oxychloride into the reaction kettle;
s2, reacting;
s2-1: closing a negative pressure throttle, emptying a negative pressure pipeline, closing a jet pump, opening a rubber plug at the upper opening of a buffer tank and an emptying port on a reaction kettle until no negative pressure exists in the reaction kettle, starting a normal pressure acid discharging system, supplying cooling water to a hydrochloric acid absorption tower, connecting a hydrochloric acid tail gas absorption pipeline to the absorption tower in series or connecting the hydrochloric acid tail gas absorption pipeline to an independent absorption device, reducing the volatilization amount of hydrogen chloride gas, enhancing the airtightness, reducing the pollution to the environment, opening the normal pressure acid discharging throttle, and starting stirring;
s2-2: feeding steam into a jacket of a reaction kettle to heat, raising the reaction temperature to 70 ℃, balancing for 1 hour, adjusting the heating speed to 4 ℃ per hour after balancing, when the reaction temperature is raised to 94 ℃, balancing for 1 hour, adjusting the heating speed to 6 ℃ per hour after balancing, and when the reaction temperature is raised to about 136 ℃, starting a negative pressure acid discharge system;
s2-3: blocking the upper opening of a buffer tank by using a rubber plug, starting an injection pump, closing a normal-pressure acid discharge valve, opening a negative-pressure valve, keeping the reaction temperature at 150 ℃ when acid is discharged under negative pressure, keeping the vacuum degree at 620mmHg, discharging the acid for 2 hours, closing a normal-pressure acid discharge system, closing the negative-pressure valve after the acid is discharged, discharging a negative-pressure pipeline, closing the injection pump, discharging the reaction kettle to the normal pressure, opening a sampling opening, sampling, testing and detecting the acid value;
s2-4: adding carbon and oxygen for neutralization according to the acid value detected in the step S2-3, adding solid into a reaction kettle by adopting a material circulation carrying method during alkali addition to reduce alkali loss and effectively prevent the situation of long-term blockage of negative pressure, starting a negative pressure acid discharge system, continuing to discharge acid for 2 hours, after acid discharge through the negative pressure acid discharge system, sampling and testing, detecting the acid value, and if the detected acid value is more than 3mgKOH/g, continuing to add carbon and oxygen for neutralization until the acid value is less than or equal to 3 mgKOH/g;
s3 final mixing: and (3) closing the negative pressure acid discharge system, wherein the liquid stored in the waste acid absorption tank is not suitable for direct discharge, and is recycled after centralized treatment in a sewage tank, so that the production cost is reduced.
Example two
The tert-butyl triphenyl phosphate fire-resistant hydraulic oil comprises the following raw materials in mass;
phosphorus oxychloride: 450 kg;
phenol: 500 kg;
p-tert-butylphenol: 600 kg;
MgCL2：1.75kg；
NH4CL：0.75kg；
antioxidant: 1 kg;
and (3) anti-foaming agent: 2.5 kg;
antirust agent: 2 kg.
NH4CL and MgCL2Drying treatment is carried out for 4 hours.
The difference between the preparation method of the tert-butyl triphenyl phosphate fire-resistant hydraulic oil and the preparation method in the example 1 is that
Step S2-2, feeding steam into a jacket of a reaction kettle to heat, raising the reaction temperature to 75 ℃, balancing for 1.5 hours, adjusting the temperature rise speed to 3 ℃ per hour after balancing, balancing for 1 hour when the reaction temperature is raised to 95 ℃, adjusting the temperature rise speed to 5 ℃ per hour after balancing, and starting a negative pressure acid discharge system when the reaction temperature is raised to about 140 ℃;
in the step S2-3, the upper opening of the buffer tank is blocked by a rubber plug, the jet pump is started, the normal pressure acid discharge valve is closed, the negative pressure valve is opened, when acid is discharged under negative pressure, the reaction temperature is kept at 140 ℃, the vacuum degree reaches 650mmHg, the acid is discharged for 2 hours, the normal pressure acid discharge system is closed, after the acid discharge is finished, the negative pressure valve is closed, the negative pressure pipeline is emptied, the jet pump is closed, the reaction kettle is emptied to normal pressure, the sampling opening is opened, the sample is tested, and the acid value is detected.
Otherwise the same as example 1
EXAMPLE III
The tert-butyl triphenyl phosphate fire-resistant hydraulic oil comprises the following raw materials in mass;
phosphorus oxychloride: 450 kg;
phenol: 500 kg;
p-tert-butylphenol: 500 kg;
MgCL2：1.75kg；
NH4CL：0.75kg；
antioxidant: 1 kg;
and (3) anti-foaming agent: 2.5 kg;
antirust agent: 2 kg.
NH4CL and MgCL2Drying treatment is carried out for 4 hours.
The difference between the preparation method of the tert-butyl triphenyl phosphate fire-resistant hydraulic oil and the preparation method in the example 1 is that
Step S2-2, feeding steam into a jacket of a reaction kettle to heat, raising the reaction temperature to 75 ℃, balancing for 1.2 hours, adjusting the temperature rise speed to 4 ℃ per hour after balancing, balancing for 1 hour when the reaction temperature is raised to 95 ℃, adjusting the temperature rise speed to 6 ℃ per hour after balancing, and starting a negative pressure acid discharge system when the reaction temperature is raised to about 137 ℃;
in the step S2-3, the upper opening of the buffer tank is blocked by a rubber plug, the jet pump is started, the normal pressure acid discharge valve is closed, the negative pressure valve is opened, when acid is discharged under negative pressure, the reaction temperature is kept at 150 ℃, the vacuum degree reaches 700mmHg, acid is discharged for 2 hours, the normal pressure acid discharge system is closed, after the acid discharge is finished, the negative pressure valve is closed, the negative pressure pipeline is emptied, the jet pump is closed, the reaction kettle is emptied to normal pressure, the sampling opening is opened, sampling and testing are carried out, and the detected acid value is obtained.
Otherwise the same as example 1
It should be understood by those skilled in the art that the above embodiments are only for illustrating the present invention and are not to be used as a limitation of the present invention, and that changes and modifications to the above embodiments are within the scope of the claims of the present invention as long as they are within the spirit and scope of the present invention.
Claims (7)
1. The tert-butyl triphenyl phosphate flame-retardant hydraulic oil is characterized by comprising the following raw materials in mass;
phosphorus oxychloride: 450 kg;
phenol: 450 kg-650 kg;
p-tert-butylphenol: 450 kg-600 kg;
MgCL2：1.75kg；
NH4CL：0.75kg；
antioxidant: 1 kg;
and (3) anti-foaming agent: 2.5 kg;
antirust agent: 2 kg.
2. The tertiary butyl triphenyl phosphate fire-resistant hydraulic oil as claimed in claim 1, wherein the NH is4CL and MgCL2Drying for 4-5 hours.
3. The preparation method of the tert-butyl triphenyl phosphate fire-resistant hydraulic oil as claimed in claim 1, characterized by comprising the following steps;
s1, feeding;
s1-1: putting p-tert-butylphenol into a manhole of a reaction kettle, closing the manhole of the reaction kettle, plugging the upper opening of a buffer tank by using a rubber plug, starting a jet pump, opening a negative pressure valve, and connecting a feeding pipeline;
s1-2: when the vacuum degree in the reaction kettle is more than 300mmHg, pumping phenol into the reaction kettle, introducing steam into the reaction kettle for heating, and controlling the temperature within 70 ℃;
s1-3: when the tert-butyl phenol is completely dissolved, starting stirring, introducing cooling water for cooling, and adding prepared NH into the reaction kettle in the process of cooling4CL and MgCL2；
S1-4: when the temperature in the reaction kettle is lower than 50 ℃, pumping phosphorus oxychloride into the reaction kettle;
s2, reacting;
s2-1: closing the negative pressure throttle, emptying the negative pressure pipeline, closing the jet pump, opening the rubber plug at the upper opening of the buffer tank and the emptying port on the reaction kettle until no negative pressure exists in the reaction kettle, starting the normal pressure acid discharging system, supplying cooling water to the hydrochloric acid absorption tower, opening the normal pressure acid discharging throttle, and starting stirring;
s2-2: heating steam in a jacket of the reaction kettle, raising the reaction temperature to 70-75 ℃, balancing for 1-1.5 hours, adjusting the temperature rise speed to 3-4 ℃ per hour after balancing, balancing for 1 hour when the reaction temperature is raised to 95 +/-2 ℃, adjusting the temperature rise speed to 5-6 ℃ per hour after balancing, and starting a negative pressure acid discharge system when the reaction temperature is raised to about 135-140 ℃;
s2-3: blocking the upper opening of the buffer tank by using a rubber plug, starting a jet pump, closing a normal-pressure acid discharge throttle, opening a negative-pressure throttle, closing a normal-pressure acid discharge system, after acid discharge is finished, closing the negative-pressure throttle, emptying a negative-pressure pipeline, closing the jet pump, emptying the reaction kettle to normal pressure, opening a sampling opening, sampling, testing and detecting the acid value;
s2-4: according to the acid value detected in the step S2-3, adding carbon and oxygen for neutralization until the acid value is less than or equal to 3mgKOH/g, namely, the synthesis is finished;
s3 final mixing: and (3) closing the negative pressure acid discharge system, emptying a negative pressure pipeline, opening a rubber plug on the buffer tank, closing the jet pump, closing stirring, closing a steam throttle, adding an antioxidant, an antifoaming agent and an antirust agent according to the proportion, stirring during adding, and uniformly stirring to obtain the finished tert-butyl triphenyl phosphate flame-retardant hydraulic oil.
4. The preparation method of the tert-butylated triphenyl phosphate fire-resistant hydraulic oil as claimed in claim 2, wherein when acid is discharged under negative pressure in step S2-3, the reaction temperature is maintained at 135-150 ℃, the vacuum degree reaches 620-750 mmHg, and the acid is discharged for 2 hours.
5. The preparation method of tertiary butyl triphenyl phosphate fire-resistant hydraulic oil as claimed in claim 3, wherein in step S2-4, carbon and oxygen are added for neutralization according to the detected acid value, and the negative pressure acid discharge system is started, acid discharge is continued for 2 hours, after acid discharge by the negative pressure acid discharge system, sampling and testing are performed, the acid value is detected, and if the detected acid value is greater than 3mgKOH/g, carbon and oxygen are continuously added for neutralization until the acid value is less than or equal to 3 mgKOH/g.
6. The tertiary butyl triphenyl phosphate fire-resistant hydraulic oil and the preparation method thereof as claimed in claim 1, wherein the liquid stored in the waste acid absorption tank in the step S3 is not suitable for direct discharge, and needs to be recycled after centralized treatment in a sewage tank.
7. The flame-retardant hydraulic oil containing tert-butylated triphenyl phosphate and the preparation method of the flame-retardant hydraulic oil containing tert-butylated triphenyl phosphate according to claim 1, wherein solids can be added into a reaction kettle by a material circulation carrying method when alkali is added in the step S2-4.
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|---|---|---|---|---|
| CN114181757A (en) * | 2020-09-14 | 2022-03-15 | 安美科技股份有限公司 | Phosphate fire-resistant oil |
| CN114181757B (en) * | 2020-09-14 | 2022-06-28 | 安美科技股份有限公司 | Phosphate fire-resistant oil |
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Application publication date: 20200124 |