阅读说明：本技术 桐油基水性极压润滑添加剂及其制备方法 (Tung oil-based water-based extreme pressure lubricating additive and preparation method thereof ) 是由 李梅 姚娜 丁海阳 李守海 张燕 许利娜 杨小华 于 2021-06-29 设计创作，主要内容包括：桐油基水性极压润滑添加剂及其制备方法,按比例,由以下步骤制得：将桐油与二乙醇胺在碱性催化剂作用下发生酰胺化反应,萃取提纯后制得桐油基脂肪酰胺；在酸性催化剂作用下,桐油基脂肪酰胺与硼酸在惰性有机溶剂中作用,发生酯化反应,制得桐油基硼酸酯；桐油基硼酸酯在酸性催化剂作用下,与聚乙二醇单甲醚在惰性有机溶剂中进行酯化反应,产物减压蒸出惰性有机溶剂,制得桐油基水性极压润滑添加剂。本发明的桐油基水性极压润滑添加剂兼有水解稳定性、润滑、环保和极压抗磨多重效果,具有反应条件温和、工艺简单的特点。(The tung oil-based water-based extreme pressure lubricating additive and the preparation method thereof are prepared by the following steps according to the proportion: carrying out amidation reaction on tung oil and diethanol amine under the action of an alkaline catalyst, and extracting and purifying to obtain tung oil-based fatty amide; under the action of an acid catalyst, tung oil-based fatty amide and boric acid act in an inert organic solvent to perform esterification reaction to prepare tung oil-based boric acid ester; tung oil-based boric acid ester and polyethylene glycol monomethyl ether are subjected to esterification reaction in an inert organic solvent under the action of an acid catalyst, and the inert organic solvent is evaporated out by the product under reduced pressure to prepare the tung oil-based aqueous extreme pressure lubricating additive. The tung oil-based aqueous extreme pressure lubricating additive has multiple effects of hydrolytic stability, lubrication, environmental protection and extreme pressure wear resistance, and has the characteristics of mild reaction conditions and simple process.)

1. A preparation method of a tung oil-based aqueous extreme pressure lubricating additive is characterized by comprising the following steps in proportion:

firstly, carrying out amidation reaction on 1mol of tung oil and 3mol of diethanolamine for 2-5 h at 90-120 ℃ under the action of an alkaline catalyst accounting for 0.05-1% of the total mass of the tung oil and the diethanolamine; adding the product into a saturated sodium chloride aqueous solution and carbon tetrachloride, standing for layering, removing the diethanolamine and the byproduct glycerol which are not completely reacted, and carrying out reduced pressure rotary evaporation to obtain tung oil-based fatty amide;

secondly, performing esterification reaction on 1mol of tung oil-based fatty amide and 1mol of boric acid in an inert organic solvent for 3-6 hours at 90-110 ℃ under the action of an acid catalyst accounting for 0.05-1% of the total mass of the tung oil-based fatty amide and the boric acid; decompressing, rotating and evaporating to obtain tung oil-based boric acid ester;

thirdly, performing esterification reaction on 1mol of tung oil-based borate and 1mol of polyethylene glycol monomethyl ether in an inert organic solvent for 3-6 hours at 90-110 ℃ under the action of an acid catalyst accounting for 0.05-1% of the total mass of the tung oil-based borate and the polyethylene glycol monomethyl ether; carrying out reduced pressure rotary evaporation to obtain the tung oil-based boron-nitrogen coordination annular structure lubricating additive;

and fourthly, dissolving the tung oil-based boron-nitrogen coordination ring-shaped structure lubricating additive obtained in the third step into water at room temperature to prepare the tung oil-based aqueous extreme pressure lubricating additive.

2. The method for preparing the tung oil-based aqueous extreme pressure lubricating additive of claim 1, characterized in that the basic catalyst used in the first step is sodium hydroxide, potassium hydroxide or sodium methoxide.

3. The method for preparing tung oil-based aqueous extreme pressure lubricating additive of claim 1 wherein the acidic catalyst used in the second step is concentrated sulfuric acid, benzenesulfonic acid or p-toluenesulfonic acid.

4. The method for preparing the tung oil-based aqueous extreme pressure lubricating additive of claim 1, wherein the molecular weight of the polyethylene glycol monomethyl ether used in the third step is 750, 1000 or 1200.

5. The method for preparing the tung oil-based aqueous extreme pressure lubricating additive of claim 1 wherein the inert organic solvent used in the second and third steps is toluene, xylene or cyclohexane.

6. The tung oil-based aqueous extreme pressure lubricant additive prepared by the preparation method of any one of claims 1 to 5.

Technical Field

The invention belongs to the technical field of lubricating additives, and particularly relates to a tung oil-based aqueous extreme pressure lubricating additive with stable hydrolysis and a preparation method thereof.

Background

Although the traditional petroleum-based lubricant can effectively control frictional wear to improve the mechanical operation efficiency and reduce the wear rate of a friction pair, the application of the traditional petroleum-based lubricant is limited by the defects of high cost, low heat conductivity coefficient, high flammability, low ignition point and the like, and serious ecological and environmental damage can be caused by direct discharge or leakage, which is contrary to the concept of sustainable development. With the development of industry, social progress and the improvement of environmental awareness, water-based lubricants are receiving more and more attention and tend to gradually replace petroleum-based lubricants due to their advantages of low cost, high cooling capacity, fire resistance, good thermal conductivity, environmental friendliness, etc., as compared to petroleum-based lubricants. Although the water-based lubricant meets the requirements of sustainable development, the water-based lubricant has the defects of low viscosity, high surface tension, low bearing capacity, easy corrosion and the like, so that the additive with excellent performance needs to be selected to meet the use requirements. The vegetable oil has biodegradability and lubrication effectiveness in nature, and the vegetable oil-based water-based extreme pressure lubricating additive prepared by using the vegetable oil as base oil and introducing hydrophilic groups, extreme pressure elements, boron and nitrogen into a molecular structure meets the current environmental protection and use requirements.

By utilizing the special structural characteristics of the tung oil which is rich in source and renewable, hydrophilic groups and extreme pressure elements such as boron, nitrogen and the like are introduced into a molecular structure, and the tung oil-based extreme pressure water-based lubricating additive is prepared and used for green lubricating oil. The boron and nitrogen elements are introduced into the molecular structure of the tung oil in a coordination ring structure mode to prepare the tung oil-based aqueous extreme pressure lubricating additive with stable hydrolysis.

Disclosure of Invention

The technical problem to be solved is as follows: in order to solve the problems of environmental pollution, poor wear resistance, poor hydrolysis stability and the like of the traditional lubricating additive raw materials, the invention provides the tung oil-based water-based extreme pressure lubricating additive with excellent hydrolysis stability and the preparation method thereof, and the tung oil-based water-based extreme pressure lubricating additive has multiple effects of environmental protection, wear resistance and hydrolysis stability.

The technical scheme is as follows: a preparation method of a tung oil-based aqueous extreme pressure lubricating additive comprises the following steps of performing amidation reaction on 1mol of tung oil and 3mol of diethanolamine for 2-5 hours at 90-120 ℃ under the action of an alkaline catalyst accounting for 0.05-1% of the total mass of the tung oil and the diethanolamine; adding the product into a saturated sodium chloride aqueous solution and carbon tetrachloride, standing for layering, removing the diethanolamine and the byproduct glycerol which are not completely reacted, and carrying out reduced pressure rotary evaporation to obtain tung oil-based fatty amide; secondly, performing esterification reaction on 1mol of tung oil-based fatty amide and 1mol of boric acid in an inert organic solvent for 3-6 hours at 90-110 ℃ under the action of an acid catalyst accounting for 0.05-1% of the total mass of the tung oil-based fatty amide and the boric acid; decompressing, rotating and evaporating to obtain tung oil-based boric acid ester; thirdly, performing esterification reaction on 1mol of tung oil-based borate and 1mol of polyethylene glycol monomethyl ether in an inert organic solvent for 3-6 hours at 90-110 ℃ under the action of an acid catalyst accounting for 0.05-1% of the total mass of the tung oil-based borate and the polyethylene glycol monomethyl ether; carrying out reduced pressure rotary evaporation to obtain the tung oil-based boron-nitrogen coordination annular structure lubricating additive; the ring structure increases the steric hindrance around the boron atom, thereby hindering the attack of water molecules, and the boron and the nitrogen generate coordination, so that the boron which is originally lack of electrons is not easy to be attacked and hydrolyzed by nucleophilic reagents (such as water molecules), and the hydrolysis stability of the borate is improved. The structural formula of the compound is compared with the conventional borate ester as follows:(conventional boronic esters of formula 1, wherein R is a hydrocarbyl or aliphatic chain),(formula 2 boron nitrogen coordination ring structure, wherein R₁,R₂Is a fatty chain); and fourthly, dissolving the tung oil-based boron-nitrogen coordination ring-shaped structure lubricating additive obtained in the third step into water at room temperature to prepare the tung oil-based aqueous extreme pressure lubricating additive.

Preferably, the basic catalyst used in the first step is sodium hydroxide, potassium hydroxide or sodium methoxide.

Preferably, the acidic catalyst used in the second step is concentrated sulfuric acid, benzenesulfonic acid or p-toluenesulfonic acid.

Preferably, the polyethylene glycol monomethyl ether used in the third step has a molecular weight of 750, 1000 or 1200.

Preferably, the inert organic solvent used in the second and third steps is toluene, xylene or cyclohexane.

The tung oil-based aqueous extreme pressure lubricating additive prepared by the preparation method.

Has the advantages that: 1. the tung oil-based aqueous extreme pressure lubricating additive prepared by the method has a hydrophilic group and boron-nitrogen extreme pressure elements in the molecular structure, and the boron and nitrogen elements are introduced into the tung oil molecular structure in a coordination ring structure mode, so that the problems of hydrolysis caused by the attack of electron-deficient boron by a nucleophilic reagent, further reduction of lubricating performance and metal corrosion can be solved. Therefore, the tung oil-based aqueous extreme pressure lubricating additive has multiple effects of environmental protection, lubricity, extreme pressure wear resistance and hydrolytic stability. 2. The tung oil-based aqueous extreme pressure lubricating additive has the characteristics of mild reaction conditions and simple process. 3. In the embodiment, the tung oil-based aqueous extreme pressure lubricating additive obviously improves the extreme pressure wear resistance of water and the hydrolytic stability.

Drawings

FIG. 1 is an infrared spectrogram of a preparation method of a tung oil-based aqueous extreme pressure lubricating additive.

Detailed Description

The invention adopts the following technical route to prepare the tung oil-based aqueous extreme pressure lubricating additive with hydrolytic stability.

(1) Synthesis of tung oil based fatty amides

Synthesis of tung oil-based borate

(3) Synthesis of tung oil base boron nitrogen coordination ring structure lubricating additive

(4) Synthesis of tung oil-based aqueous extreme pressure lubricating additive

Tung oil base boron nitrogen coordination ring structure lubricating additive + water → Tung oil base water-based extreme pressure lubricating additive

Firstly, carrying out amidation reaction on 1mol of tung oil and 3mol of diethanolamine for 2-5 h at 90-120 ℃ under the action of an alkaline catalyst accounting for 0.05-1% of the total mass of the tung oil and the diethanolamine; adding the product into a saturated sodium chloride aqueous solution and carbon tetrachloride, standing for layering, removing the diethanolamine and the byproduct glycerol which are not completely reacted, and carrying out reduced pressure rotary evaporation to obtain tung oil-based fatty amide;

(II) carrying out esterification reaction on 1mol of tung oil-based fatty amide and 1mol of boric acid in an inert organic solvent for 3-6 h at 90-110 ℃ under the action of an acid catalyst accounting for 0.05-1% of the total mass of the tung oil-based fatty amide and the boric acid; decompressing, rotating and evaporating to obtain tung oil-based boric acid ester;

(III) carrying out esterification reaction on 1mol of tung oil-based boric acid ester and 1mol of polyethylene glycol monomethyl ether in an inert organic solvent for 3-6 h at 90-110 ℃ under the action of an acid catalyst accounting for 0.05-1% of the total mass of the tung oil-based boric acid ester and the polyethylene glycol monomethyl ether; carrying out reduced pressure rotary evaporation to obtain the tung oil-based boron-nitrogen coordination annular structure lubricating additive;

and (IV) dissolving the tung oil-based boron-nitrogen coordination ring-shaped structure lubricating additive in water at 25 ℃ to prepare the tung oil-based water-based extreme pressure lubricating additive.

The alkaline catalyst used in the first step is one of sodium hydroxide, potassium hydroxide and sodium methoxide.

The acidic catalyst used in the second and third steps is one of concentrated sulfuric acid, benzenesulfonic acid and p-toluenesulfonic acid.

The molecular weight of the polyethylene glycol monomethyl ether used in the third step is one of 750, 1000 and 1200.

The inert organic solvent used in the second step and the third step is one of toluene, xylene and cyclohexane.

Example 1

Preparation of tung oil-based fatty amides

Adding 3mol of diethanolamine and sodium hydroxide which accounts for 0.05 percent of the total mass of the diethanolamine and the tung oil as catalysts into a 500mL three-neck flask provided with a heating jacket, a stirring device and a thermometer, heating to 90 ℃, dropwise adding 1mol of tung oil, continuously heating to 120 ℃, and reacting for 4 hours; and then adding the product into a saturated sodium chloride aqueous solution and carbon tetrachloride, standing for layering, removing the diethanolamine and the glycerol which are not completely reacted, reducing the pressure to-0.1 to-0.09 MPa, and evaporating the carbon tetrachloride which is a solvent to obtain the tung oil-based fatty amide.

Preparation of (di) tung oil-based boric acid ester

In a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator, adding 1mol of tung oil-based fatty amide obtained in the step (I) and 1mol of boric acid, and p-toluenesulfonic acid accounting for 0.1% of the total mass of the tung oil-based fatty amide and the boric acid as catalysts into toluene as a solvent, and reacting for 3h at 110 ℃; reducing the pressure to-0.1-0.09 MPa, and evaporating the solvent toluene to obtain the tung oil-based borate.

Preparation of tung oil-based boron-nitrogen coordination ring structure lubricating additive

In a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator, adding 1mol of tung oil-based borate and polyethylene glycol monomethyl ether with the molecular weight of 750 obtained in the step (II) and p-toluenesulfonic acid accounting for 0.1% of the total mass of the tung oil-based borate and the polyethylene glycol monomethyl ether as catalysts by taking toluene as a solvent, reacting for 6h, then reducing the pressure to-0.1 to-0.09 MPa, and evaporating the solvent toluene to obtain the tung oil-based boron-nitrogen coordination annular structure lubricating additive;

preparation of tung oil base hydraulic lubricating additive

And (3) dissolving 2% of the tung oil-based boron-nitrogen coordination ring-shaped structure lubricating additive obtained in the third step in water in a beaker to obtain the tung oil-based water-based extreme pressure lubricating additive.

The infrared spectrogram of the tung oil-based aqueous extreme pressure lubricating additive prepared in the embodiment is shown in figure 1: 1744cm in tung oil curve in spectrogram^-1The position is a stretching vibration characteristic peak of carbonyl; in the curves of the tung oil-based fatty amide, the tung oil-based boric acid ester and the tung oil-based boron-nitrogen coordination annular structure lubricating additive, characteristic peaks of carbonyl groups appear nearby. Tung oil based fatty amide is 3398cm^-1﹑1622cm^-1N-H bond stretching vibration and bending vibration absorption peaks respectively appear, which shows that tung oil and diethanol amine have amidation reaction; in the tung oil based borate curve, a new symmetric stretching vibration with a peak of B-O bond appears at 1363, and the formation of B-O bond in the borate indicates that the alcohol is connected to the boron atom to generate the borate. The characteristic peak also appears at 1348 of the tung oil based boron nitrogen coordination annular structure lubricating additive, and the characteristic peak is further enhanced, which shows that-OH on polyethylene glycol monomethyl ether and boric acid are subjected to esterification reaction, and a strong absorption peak at 1093 corresponds to a characteristic peak of an ether bond, and further shows that the polyethylene glycol monomethyl ether and tung oil based borate are subjected to esterification reaction. The products prepared in the following examples have IR spectra similar to that of example 1 and will not be described in detail.

Example 2

Preparation of tung oil-based fatty amides

Adding 3mol of diethanolamine and potassium hydroxide accounting for 0.1 percent of the total mass of the diethanolamine and the tung oil as catalysts into a 500mL three-neck flask provided with a heating jacket, a stirring device and a thermometer, heating to 90 ℃, dropwise adding 1mol of tung oil, continuously heating to 120 ℃, and reacting for 4 hours; and then adding the product into a saturated sodium chloride aqueous solution and carbon tetrachloride, standing for layering, removing the diethanolamine and the glycerol which are not completely reacted, reducing the pressure to-0.1 to-0.09 MPa, and evaporating the carbon tetrachloride which is a solvent to obtain the tung oil-based fatty amide.

Preparation of (di) tung oil-based boric acid ester

Adding 1mol of tung oil-based fatty amide obtained in the step (I) and 1mol of boric acid into a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator by taking dimethylbenzene as a solvent, and adding concentrated sulfuric acid which accounts for 0.05 percent of the total mass of the tung oil-based fatty amide and the boric acid as a catalyst to react for 3 hours at 100 ℃; reducing the pressure to-0.1 to-0.09 MPa, and evaporating the xylene solvent to obtain the tung oil-based borate.

Preparation of tung oil-based boron-nitrogen coordination ring structure lubricating additive

Adding 1mol of tung oil-based borate and polyethylene glycol monomethyl ether with the molecular weight of 1000 obtained in the step (II) and concentrated sulfuric acid accounting for 0.05 percent of the total mass of the tung oil-based borate and the polyethylene glycol monomethyl ether into a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator by taking dimethylbenzene as a solvent, reacting for 6 hours at 100 ℃, then reducing the pressure to-0.1 to-0.09 MPa, and evaporating the solvent dimethylbenzene to obtain the tung oil-based boron-nitrogen coordination annular structure lubricating additive;

preparation of tung oil base hydraulic lubricating additive

And (3) dissolving 2% of the tung oil-based boron-nitrogen coordination ring-shaped structure lubricating additive obtained in the third step in water in a beaker to obtain the tung oil-based water-based extreme pressure lubricating additive.

Example 3

Preparation of tung oil-based fatty amides

Adding 3mol of diethanolamine and sodium methoxide accounting for 0.2 percent of the total mass of the diethanolamine and the tung oil as catalysts into a 500mL three-neck flask provided with a heating jacket, a stirring device and a thermometer, heating to 90 ℃, dropwise adding 1mol of tung oil, continuously heating to 120 ℃, and reacting for 4 hours; and then adding the product into a saturated sodium chloride aqueous solution and carbon tetrachloride, standing for layering, removing the diethanolamine and the glycerol which are not completely reacted, reducing the pressure to-0.1 to-0.09 MPa, and evaporating the carbon tetrachloride which is a solvent to obtain the tung oil-based fatty amide.

Preparation of (di) tung oil-based boric acid ester

Adding 1mol of tung oil-based fatty amide obtained in the step (I) and 1mol of boric acid into a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator by taking cyclohexane as a solvent, and adding benzenesulfonic acid accounting for 0.1 percent of the total mass of the tung oil-based fatty amide and the boric acid as a catalyst to react for 3 hours at 100 ℃; reducing the pressure to-0.1 to-0.09 MPa, and evaporating the solvent cyclohexane to obtain the tung oil-based borate.

Preparation of tung oil-based boron-nitrogen coordination ring structure lubricating additive

Adding 1mol of tung oil-based borate and polyethylene glycol monomethyl ether with the molecular weight of 1200 obtained in the step (II) and benzenesulfonic acid accounting for 0.1 percent of the total mass of the tung oil-based borate and the polyethylene glycol monomethyl ether as catalysts into a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator, reacting for 6 hours at 100 ℃, then reducing the pressure to-0.1 to-0.09 MPa, and evaporating the solvent cyclohexane to obtain the tung oil-based boron-nitrogen coordination annular structure lubricating additive;

preparation of tung oil base hydraulic lubricating additive

And (3) dissolving 2% of the tung oil-based boron-nitrogen coordination ring-shaped structure lubricating additive obtained in the third step in water in a beaker to obtain the tung oil-based water-based extreme pressure lubricating additive.

Example 4

Preparation of tung oil-based fatty amides

Adding 3mol of diethanolamine and potassium hydroxide accounting for 0.1 percent of the total mass of the diethanolamine and the tung oil as catalysts into a 500mL three-neck flask provided with a heating jacket, a stirring device and a thermometer, heating to 90 ℃, dropwise adding 1mol of tung oil, continuously heating to 120 ℃, and reacting for 4 hours; and then adding the product into a saturated sodium chloride aqueous solution and carbon tetrachloride, standing for layering, removing the diethanolamine and the glycerol which are not completely reacted, reducing the pressure to-0.1 to-0.09 MPa, and evaporating the carbon tetrachloride which is a solvent to obtain the tung oil-based fatty amide.

Preparation of (di) tung oil-based boric acid ester

Adding 1mol of tung oil-based fatty amide obtained in the step (I) and 1mol of boric acid into a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator by taking toluene as a solvent, and adding benzene sulfonic acid accounting for 0.05 percent of the total mass of the tung oil-based fatty amide and the boric acid as a catalyst to react for 3 hours at 100 ℃; reducing the pressure to-0.1-0.09 MPa, and evaporating the solvent toluene to obtain the tung oil-based borate.

Preparation of tung oil-based boron-nitrogen coordination ring structure lubricating additive

Adding 1mol of tung oil-based borate and polyethylene glycol monomethyl ether with the molecular weight of 750 obtained in the step (II) and benzenesulfonic acid accounting for 0.1 percent of the total mass of the tung oil-based borate and the polyethylene glycol monomethyl ether into a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator by taking dimethylbenzene as a solvent, reacting for 6 hours at 100 ℃, then reducing the pressure to-0.1 to-0.09 MPa, and evaporating the solvent dimethylbenzene to obtain the tung oil-based boron-nitrogen coordination annular structure lubricating additive;

preparation of tung oil base hydraulic lubricating additive

And (3) dissolving 5 percent of the tung oil-based boron-nitrogen coordination ring-shaped structure lubricating additive obtained in the third step in water in a beaker to obtain the tung oil-based water-based extreme pressure lubricating additive.

Example 5

Preparation of tung oil-based fatty amides

Adding 3mol of diethanolamine and sodium methoxide accounting for 0.05 percent of the total mass of the diethanolamine and the tung oil as catalysts into a 500mL three-neck flask provided with a heating jacket, a stirring device and a thermometer, heating to 90 ℃, dropwise adding 1mol of tung oil, continuously heating to 120 ℃, and reacting for 4 hours; and then adding the product into a saturated sodium chloride aqueous solution and carbon tetrachloride, standing for layering, removing the diethanolamine and the glycerol which are not completely reacted, reducing the pressure to-0.1 to-0.09 MPa, and evaporating the carbon tetrachloride which is a solvent to obtain the tung oil-based fatty amide.

Preparation of (di) tung oil-based boric acid ester

Adding 1mol of tung oil-based fatty amide obtained in the step (I) and 1mol of boric acid into a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator by taking dimethylbenzene as a solvent, and adding concentrated sulfuric acid which accounts for 0.1% of the total mass of the tung oil-based fatty amide and the boric acid as a catalyst to react for 3h at 100 ℃; reducing the pressure to-0.1 to-0.09 MPa, and evaporating the xylene solvent to obtain the tung oil-based borate.

Preparation of tung oil-based boron-nitrogen coordination ring structure lubricating additive

Adding 1mol of tung oil-based borate and polyethylene glycol monomethyl ether with the molecular weight of 1000 obtained in the step (II) and concentrated sulfuric acid accounting for 0.2 percent of the total mass of the tung oil-based borate and the polyethylene glycol monomethyl ether into a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator by taking cyclohexane as a solvent, reacting for 6 hours at 100 ℃, then reducing the pressure to-0.1 to-0.09 MPa, and evaporating the solvent cyclohexane to obtain the tung oil-based boron-nitrogen coordination annular structure lubricating additive;

preparation of tung oil base hydraulic lubricating additive

And (3) dissolving 5 percent of the tung oil-based boron-nitrogen coordination ring-shaped structure lubricating additive obtained in the third step in water in a beaker to obtain the tung oil-based water-based extreme pressure lubricating additive.

Example 6

Preparation of tung oil-based fatty amides

Adding 3mol of diethanolamine and sodium hydroxide which accounts for 0.2 percent of the total mass of the diethanolamine and the tung oil as catalysts into a 500mL three-neck flask provided with a heating jacket, a stirring device and a thermometer, heating to 90 ℃, dropwise adding 1mol of tung oil, continuously heating to 120 ℃, and reacting for 4 hours; and then adding the product into a saturated sodium chloride aqueous solution and carbon tetrachloride, standing for layering, removing the diethanolamine and the glycerol which are not completely reacted, reducing the pressure to-0.1 to-0.09 MPa, and evaporating the carbon tetrachloride which is a solvent to obtain the tung oil-based fatty amide.

Preparation of (di) tung oil-based boric acid ester

Adding 1mol of tung oil-based fatty amide obtained in the step (I) and 1mol of boric acid and p-toluenesulfonic acid accounting for 0.1 percent of the total mass of the tung oil-based fatty amide and the boric acid as catalysts into a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator by taking cyclohexane as a solvent, and reacting for 3 hours at 100 ℃; reducing the pressure to-0.1 to-0.09 MPa, and evaporating the solvent cyclohexane to obtain the tung oil-based borate.

Preparation of tung oil-based boron-nitrogen coordination ring structure lubricating additive

Adding 1mol of tung oil-based borate and polyethylene glycol monomethyl ether with the molecular weight of 1200 obtained in the step (II) and p-toluenesulfonic acid accounting for 0.2 percent of the total mass of the tung oil-based borate and the polyethylene glycol monomethyl ether as catalysts into a 500mL four-neck flask provided with a heating jacket, a stirring device, a thermometer and a water separator, reacting at 100 ℃ for 6 hours, then reducing the pressure to-0.1 to-0.09 MPa, and evaporating the solvent toluene to obtain the tung oil-based boron-nitrogen coordination annular structure lubricating additive;

preparation of tung oil base hydraulic lubricating additive

And (3) dissolving 5 percent of the tung oil-based boron-nitrogen coordination ring-shaped structure lubricating additive obtained in the third step in water in a beaker to obtain the tung oil-based water-based extreme pressure lubricating additive.

Experiment of hydrolytic stability

Good water solubility and hydrolytic stability of aqueous lubricant additives is a prerequisite as a lubricant additive. In the present invention, the above examples were added to water (0.1%), dissolved by stirring at the same room temperature, and the state of the additive was observed at the same humidity and temperature, and the experimental results are shown in table 1:

item	Half a month	1 month	2 months old
				Example 1	-	-	-
Example 2	-	-	-
				Example 3	-	-	#
Example 4	-	-	-
				Example 5	-	-	-
Example 6	-	-	#

In the figure, "-" indicates clear and transparent; "#" indicates the occurrence of stratification or precipitation

As can be seen from the experimental results in Table 1, the products of examples 1, 2, 4 and 5 have good water solubility, and after being placed at room temperature for 2 months, the products can be kept clear and transparent at the addition concentrations of 2% and 5%, have no precipitation and delamination phenomena, and meet the basic conditions of being used as water-based lubricating additives. Examples 3 and 6 started to develop turbidity and demixing when left at room temperature for 2 months, with 5% added concentration indicating that the greater concentration of 3 and 6 products, which were stable at room temperature for 1 month.

Extreme pressure antiwear property

The 6 examples were tested using a four-ball tester (Dalian Intelligent Instrument and meters Co., Ltd., DZY-S10A)

Item	Extreme pressure (P)B/N)	Coefficient of friction	Motorcycle spot diameter (mm)
				Water (W)	<88	0.247	0.88
Example 1	596	0.153	0.66
				Example 2	667	0.123	0.34
Example 3	631	0.150	0.47
				Example 4	674	0.148	0.36
Example 5	726	0.107	0.18
				Example 6	685	0.135	0.26