阅读说明：本技术 一种三二甲苯基磷酸酯抗燃液压油及其制备方法 (Trixylyl phosphate fire-resistant hydraulic oil and preparation method thereof ) 是由 张继腾 吕冀川 于 2019-09-09 设计创作，主要内容包括：本发明公开了一种三二甲苯基磷酸酯抗燃液压油及其制备方法,属于液压油制备工艺技术领域,该液压油以磷酸三二甲苯酯为基础油,磷酸三二甲苯酯的原料为二甲酚和三氯氧磷,该液压油包括如下质量份数的原料：二甲酚1380～1450份；三氯氧磷625～635份；抗氧剂0.05～0.15份；抗泡剂0.02～0.04份；防锈剂0.030～0.035份；其制备方法为将二甲酚和三氯氧磷经上料、酯化反应、中和反应等步骤制得磷酸三二甲苯酯,再经蒸馏提纯后与抗氧剂、抗泡剂及防锈剂混合均匀,即得三二甲苯基磷酸酯抗燃液压油成品。本发明成分简单,原料易得,制得的产品具有较好的耐热抗燃、抗氧化性能和密封性,且产品质量稳定性高。(The invention discloses a tri-xylyl phosphate fire-resistant hydraulic oil and a preparation method thereof, belonging to the technical field of hydraulic oil preparation processes, wherein the hydraulic oil takes tri-xylyl phosphate as base oil, and the raw materials of tri-xylyl phosphate are xylenol and phosphorus oxychloride, and the hydraulic oil comprises the following raw materials in parts by weight: 1380-1450 parts of xylenol; 625-635 parts of phosphorus oxychloride; 0.05-0.15 part of antioxidant; 0.02-0.04 part of an antifoaming agent; 0.030-0.035 parts of antirust agent; the preparation method comprises the steps of carrying out feeding, esterification reaction, neutralization reaction and the like on the xylenol and the phosphorus oxychloride to prepare the trixylenyl phosphate, and then uniformly mixing the trixylenyl phosphate with the antioxidant, the antifoaming agent and the antirust agent after distillation and purification to obtain the finished product of the trinxylyl phosphate flame-retardant hydraulic oil. The invention has simple components and easily obtained raw materials, and the prepared product has better heat resistance, flame resistance, oxidation resistance and sealing property and high product quality stability.)

1. The trixylyl phosphate fire-resistant hydraulic oil is characterized by being prepared by taking trixylyl phosphate as base oil and adding an antioxidant, an antifoaming agent and an antirust agent, wherein the trixylyl phosphate is prepared from xylenol and phosphorus oxychloride, and the trixylyl phosphate fire-resistant hydraulic oil comprises the following raw materials in parts by weight:

1380-1450 parts of xylenol;

625-635 parts of phosphorus oxychloride;

0.05-0.15 part of antioxidant;

0.02-0.04 part of an antifoaming agent;

0.030-0.035 parts of antirust agent.

2. The trixylyl phosphate fire-resistant hydraulic oil of claim 1, wherein the trixylyl phosphate fire-resistant hydraulic oil comprises the following raw materials in parts by weight:

1393 parts of xylenol;

630 parts of phosphorus oxychloride;

0.1 part of antioxidant;

0.03 part of an antifoaming agent;

0.032 part of antirust agent.

3. The preparation method of the trixylyl phosphate fire-resistant hydraulic oil as claimed in claim 1 or 2, which is characterized by comprising the following steps:

s1, feeding: starting an injection pump, starting a negative pressure throttle, connecting a feeding pipeline communicated with an esterification kettle, and pumping xylenol into the esterification kettle when the vacuum degree in the esterification kettle is more than 300 mmHg; then adding the prepared catalyst; when the temperature in the esterification kettle is lower than 50 ℃, pumping phosphorus oxychloride into the esterification kettle, and opening a vent on the esterification kettle until no negative pressure exists in the esterification kettle;

s2, esterification:

s2-1: starting a normal pressure acid discharge system, filling cooling water into a condenser and a hydrochloric acid absorption tower, opening a normal pressure acid discharge throttle, starting a stirrer, and adjusting a negative pressure pipeline throttle on an acid circulating pump to maintain the pressure in the esterification kettle at 50mmHg in the step S1;

s2-2: feeding steam into an esterification kettle for heating treatment, rapidly heating to 75 ℃ within 1.5 hours, then heating at the speed of 4 ℃ per hour, and heating at the speed of 5-8 ℃ per hour after the temperature is raised to 95 ℃, wherein in the process, volatilized phosphorus oxychloride steam is condensed by a condenser and then reflows into the esterification kettle, and generated hydrogen chloride gas enters a falling film absorber through the condenser, is absorbed by water and then automatically flows into a strong acid circulation tank; when the reaction temperature rises to 135-140 ℃, closing the normal-pressure acid discharge system, starting the negative-pressure acid discharge system, allowing a small amount of residual hydrogen chloride gas in the esterification kettle to enter a jet pump through a vacuum-pumping pipeline and a buffer tank, absorbing the hydrogen chloride gas by water, and then entering a weak-acid circulation tank; unabsorbed hydrogen chloride gas is absorbed by tertiary water and then discharged by an exhaust funnel with the height of 15m, after acid discharge is finished, a negative pressure throttle is closed, a negative pressure pipeline is emptied, the interior of an esterification kettle is emptied to normal pressure, a sampling port is opened, sampling and testing are carried out, and the acid value is detected;

s3, neutralization reaction: according to the acid value detected in the step S2, adding soda ash for neutralization until the acid value is 2mgKOH/g, opening a rubber plug on a buffer tank, and closing a jet pump, a stirrer and a steam throttle valve to obtain a crude product of the tricresyl phosphate;

s4, distillation and purification: pumping the crude product of the tricresyl phosphate prepared in the step S3 into a distillation still, starting a Roots vacuum unit and a far infrared heating device, evaporating a superior product when the temperature reaches 280-310 ℃, condensing the superior product by a condenser, and then feeding the superior product into a superior product receiving tank to obtain a refined product of the tricresyl phosphate;

s5, final mixing: and (4) adding an antioxidant, an antifoaming agent and an antirust agent into the fine product of the trixylenyl phosphate obtained in the step S4 under the condition of stirring, and uniformly stirring to obtain a finished product of the flame-retardant hydraulic oil of the trixylyl phosphate.

4. The method for preparing the trixylyl phosphate fire-resistant hydraulic oil according to claim 3, wherein the catalyst in the step S1 is a calcium-magnesium composite catalyst.

5. The preparation method of the trixylyl phosphate fire-resistant hydraulic oil as claimed in claim 3, wherein in step S2-2, the reaction temperature is maintained at 135-150 ℃ and the pressure is 0.09KMPa during negative pressure acid discharge.

6. The preparation method of the trixylyl phosphate fire-resistant hydraulic oil according to claim 3, wherein the step S3 specifically comprises the following steps:

s3-1: adding soda ash for neutralization according to the acid value detected in the step S2, and starting a negative pressure acid discharge system;

s3-2: after acid is discharged by a negative pressure acid discharge system, sampling and testing, detecting the acid value, and if the detected acid value is more than 2mgKOH/g, continuously adding soda ash for neutralization until the acid value reaches the standard;

s3-3: and (3) after the acid value of the substances in the esterification kettle reaches the standard, closing the negative pressure acid discharge system, emptying the negative pressure pipeline, opening a rubber plug on the buffer tank, and closing the jet pump, the stirrer and the steam throttle valve to synthesize the crude product of the trixylenyl phosphate.

Technical Field

The invention relates to the technical field of hydraulic oil preparation processes, in particular to a tri-xylyl phosphate fire-resistant 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 trixylenyl phosphate product is colorless or light yellow viscous liquid, the color is less than or equal to 200, and the relative density is 1.130-1.160 g/cm³(20 ℃), acid value less than or equal to 0.1mgKOH/g, viscosity about 190 mPa.s (20 ℃), refractive index 1.551-1.555 (25 ℃), flash point (cup-opening method) more than or equal to 250 ℃, freezing point lower than-35 ℃, and boiling point temperature about 270 ℃ under 0.4 kPa. Is insoluble in water and is mutually soluble in dichloromethane, benzene, toluene, alcohol and methyl ethyl ketone. Is basically non-toxic. When the trixylenyl phosphate escapes due to fire in the environment where the trixylenyl phosphate is located, the liquid can be diluted into a non-combustible mixture after being sprayed by water, so that the flame retardant property can be exerted, and the liquid can be used for a flame retardant.

At present, the trixylenyl phosphate is not used for preparing the flame-retardant hydraulic oil in a precedent.

Disclosure of Invention

1. Technical problem to be solved

The invention aims to solve the technical problem of providing the tri-xylyl phosphate fire-resistant hydraulic oil and the preparation method thereof, wherein the tri-xylyl phosphate fire-resistant hydraulic oil takes the tri-xylyl phosphate as the base oil, the components are simple, the raw materials are easy to obtain, and the prepared product has better heat resistance, fire resistance, oxidation resistance and sealing property and high product quality stability.

2. Technical scheme

In order to solve the problems, the invention adopts the following technical scheme:

the trixylyl phosphate fire-resistant hydraulic oil is prepared by taking trixylyl phosphate (TXP) as base oil and adding an antioxidant, an antifoaming agent and an antirust agent, wherein the trixylyl phosphate is prepared from xylenol and phosphorus oxychloride, and the trixylyl phosphate fire-resistant hydraulic oil comprises the following raw materials in parts by weight:

1380-1450 parts of xylenol;

625-635 parts of phosphorus oxychloride;

0.05-0.15 part of antioxidant;

0.02-0.04 part of an antifoaming agent;

0.030-0.035 parts of antirust agent.

Further, the trixylyl phosphate fire-resistant hydraulic oil comprises the following raw materials in parts by weight:

1393 parts of xylenol;

630 parts of phosphorus oxychloride;

0.1 part of antioxidant;

0.03 part of an antifoaming agent;

0.032 part of antirust agent.

The invention also provides a preparation method of the tri-xylyl phosphate fire-resistant hydraulic oil, which comprises the following steps:

s1, feeding: starting an injection pump, starting a negative pressure throttle, connecting a feeding pipeline communicated with an esterification kettle, and pumping xylenol into the esterification kettle when the vacuum degree in the esterification kettle is more than 300 mmHg; then adding the prepared calcium-magnesium composite catalyst; when the temperature in the esterification kettle is lower than 50 ℃, pumping phosphorus oxychloride into the esterification kettle, and opening a vent on the esterification kettle until no negative pressure exists in the esterification kettle;

s2, esterification:

s2-1: starting a normal pressure acid discharge system, filling cooling water into a condenser and a hydrochloric acid absorption tower, opening a normal pressure acid discharge throttle, starting a stirrer, and adjusting a negative pressure pipeline throttle on an acid circulating pump to maintain the pressure in the esterification kettle at 50mmHg in the step S1;

s2-2: feeding steam into an esterification kettle for heating treatment, rapidly heating to 75 ℃ within 1.5 hours, then heating at the speed of 4 ℃ per hour, and heating at the speed of 5-8 ℃ per hour after the temperature is raised to 95 ℃, wherein in the process, volatilized phosphorus oxychloride steam is condensed by a condenser and then reflows into the esterification kettle, and generated hydrogen chloride gas enters a falling film absorber through the condenser, is absorbed by water and then automatically flows into a strong acid circulation tank; when the reaction temperature rises to 135-140 ℃, closing the normal-pressure acid discharge system, starting the negative-pressure acid discharge system, allowing a small amount of residual hydrogen chloride gas in the esterification kettle to enter a jet pump through a vacuum-pumping pipeline and a buffer tank, absorbing the hydrogen chloride gas by water, and then entering a weak-acid circulation tank; unabsorbed hydrogen chloride gas is absorbed by tertiary water and then discharged by an exhaust funnel with the height of 15m, when acid is discharged under negative pressure, the reaction temperature is kept at 135-150 ℃, the pressure is 0.09KMPa, after the acid is discharged, a negative pressure throttle is closed, a negative pressure pipeline is emptied, the interior of an esterification kettle is emptied to normal pressure, a sampling port is opened, sampling and testing are carried out, and the acid value is detected;

s3, neutralization reaction:

s3-1: adding soda ash for neutralization according to the acid value detected in the step S2, and starting a negative pressure acid discharge system;

s3-2: after acid is discharged by a negative pressure acid discharge system, sampling and testing, detecting the acid value, and if the detected acid value is more than 2mgKOH/g, continuously adding soda ash for neutralization until the acid value reaches the standard;

s3-3: after the acid value of the substances in the esterification kettle reaches the standard, closing the negative pressure acid discharge system, emptying a negative pressure pipeline, opening a rubber plug on a buffer tank, and closing a jet pump, a stirrer and a steam throttle valve to synthesize a crude product of the trixylenyl phosphate;

s4, distillation and purification: pumping the crude product of the tricresyl phosphate prepared in the step S3 into a distillation still, starting a Roots vacuum unit and a far infrared heating device, evaporating a superior product when the temperature reaches 280-310 ℃, condensing the superior product by a condenser, and then feeding the superior product into a superior product receiving tank to obtain a refined product of the tricresyl phosphate;

s5, final mixing: and (4) adding an antioxidant, an antifoaming agent and an antirust agent into the fine product of the trixylenyl phosphate obtained in the step S4 under the condition of stirring, and uniformly stirring to obtain a finished product of the flame-retardant hydraulic oil of the trixylyl phosphate.

3. Advantageous effects

The hydraulic oil is prepared by taking the phosphoric acid xylene ester as base oil and adding the antioxidant, the antifoaming agent and the antirust agent, so that the hydraulic oil has heat-resistant and flame-retardant properties, and the antioxidant can endow the hydraulic oil with antioxidant properties by adding the antioxidant, thereby prolonging the service life of the hydraulic oil; the addition of the anti-foaming agent can prevent the hydraulic oil from generating bubbles when in use, thereby avoiding the problem of poor sealing property caused by bubble rupture; the antirust agent and oil can be mutually dissolved together, so that molecules of the antirust agent are directionally arranged on the surface of the carrier to form an adsorptive protective film, and the sealing property can be further ensured. The raw materials of the trixylenyl phosphate are xylenol and phosphorus oxychloride. The invention has simple components and easily obtained raw materials, and the prepared product has better heat resistance, flame resistance, oxidation resistance and sealing property and high product quality stability.

Detailed Description