CN111303428A

CN111303428A - High-temperature stable silicon-based base oil and preparation method thereof

Info

Publication number: CN111303428A
Application number: CN202010111515.4A
Authority: CN
Inventors: 熊晶; 李博解; 杜志顺; 熊妮; 王辰; 熊萌
Original assignee: Wuhan Gaohuan New Material Technology Co Ltd
Current assignee: Wuhan Gaohuan New Material Technology Co Ltd
Priority date: 2020-02-24
Filing date: 2020-02-24
Publication date: 2020-06-19

Abstract

The invention discloses high-temperature stable silicon-based base oil and a preparation method thereof. The silicon-based base oil has high flash point, is acid and alkali resistant, has obviously improved high temperature resistance compared with common silicone oil, and is suitable for lubricating and using requirements of equipment under extremely severe conditions of high temperature, strong acid and strong alkali and the like.

Description

High-temperature stable silicon-based base oil and preparation method thereof

Technical Field

The invention relates to high-temperature stable silicon-based base oil which is mainly applied to the lubrication requirements of equipment in industries such as metallurgy, mining, power plants, machining and the like under high-temperature or strong acid and strong base conditions.

Background

The lubricating oil is commonly called industrial blood, is mainly used for lubrication, cleaning, rust prevention, heat dissipation and the like, and can be used for lubrication and protection of bearings, chains, sliding rails, gears and the like of various machines, such as automobile engine oil, turbine oil, hydraulic oil and the like. Lubricating oil is composed of base oil and additives, wherein the base oil accounts for about 90%, and the structure and performance of the lubricating oil have decisive influence on the lubricating oil. The base oil in the market is mainly mineral base oil. The mineral base oil mainly takes petroleum products as raw materials, and has the problems of poor lubricating property, high-temperature coking and equipment corrosion in the actual use process.

With the development of industries such as automobiles, machinery and the like, the relationship between lubricating oil and the general demand of the society is more and more compact, and the technical requirements on the lubricating oil are higher and higher. The traditional mineral base oil is far from meeting the actual use requirement. For this reason, the development of synthetic oils is receiving increasing attention.

Patent CN 105861040B and 103666552B disclose methods for preparing poly α olefin (PAO) based on the fourth base oil regulated by American Petroleum Institute (API), wherein PAO has excellent additive sensitivity but is easy to coke at high temperature to generate carbon deposition, patent CN105906795B discloses synthetic perfluoropolyether as lubricating oil which has excellent corrosion resistance and high performance, but the price of the perfluoropolyether lubricating oil is more than one hundred times of that of the traditional mineral oil product, which seriously limits the use of the perfluoropolyether, and patent CN105219480B discloses products based on fatty acid ester as a main component, which can be used for aeroengine oil.

The silicone oil represented by dimethyl silicone oil draws extensive attention because of the chemical inertness of the silicone oil, and phenyl hydroxyl silicone oil and branched chain silicone oil are respectively obtained by successfully designing and deriving the patents 104292464B and 105669981B, but the molecular weight of the product is smaller, the flash point is low, and the requirements of 200-260-DEG high-temperature use environment cannot be met.

Disclosure of Invention

The invention aims to solve the technical problem of providing the high-temperature stable silicon-based base oil and the preparation method thereof aiming at the defects in the prior art, the high-temperature stable silicon-based base oil has excellent stability and high-temperature performance, long service life and good corrosion resistance, can meet the requirements of 200-plus-260-DEG C high-temperature use environment, and is particularly suitable for the use requirements under the corrosion-prone conditions of easy contact of strong acid, strong alkali and the like.

The technical scheme adopted by the invention for solving the problems is as follows:

a preparation method of high-temperature stable silicon-based base oil mainly comprises the following steps:

(1) using methyl triallyl silane as monomer, adding platinum Catalyst (COD) PtCl₂The catalyst is used as a catalyst, is heated to 38-42 ℃ after being uniformly stirred and reacts for 95-100 hours, the complete reaction of the methyl triallyl silane monomer is confirmed through a TCL point plate, the polymethyl triallyl silane is obtained, the product is a semitransparent viscous oily substance, and the dosage of the catalyst is 0.02-0.05% of the mass of the methyl triallyl silane.

(2) And (2) taking 10 parts of the poly (methyl triallyl silane) obtained in the step (1), respectively adding 6-8 parts of dimethoxy dimethylsilane and 0.2-0.4 part of 37% concentrated hydrochloric acid, heating to 60 ℃ for reaction for 12-14 hours, then carrying out reduced pressure distillation, and removing unreacted small molecules to obtain colorless viscous liquid, namely the high-temperature stable silicon-based base oil.

In the preparation method, the reaction mechanism mainly involved is as follows:

(1) methyltriallylsilane in Catalyst (COD) PtCl₂The high-branched silicon-based polymer-poly (methyl triallyl silane) can be obtained by reacting for 95-100 hours at 38-42 ℃, the polymer forms a central core part, and the end group part of the polymer has C ═ C double bonds, so that the subsequent polymerization is facilitated, and the reaction formula is shown as formula 1.

(2) Dimethoxydimethylsilane and hydrochloric acid are added into the polymethyltriallyl silane according to the proportion, and the mixture is reacted for 12 hours at the temperature of 60 ℃, the polymerization degree n is controlled to be between 5 and 8, and the obtained product is shown in a formula 2.

The high-temperature stable silicon-based base oil designed by the invention is prepared by taking highly branched silicon-based macromolecules as the core and connecting long-chain silicon-based macromolecules to the edge of the core, so that the problem of high-temperature instability of carbon-based macromolecules is solved, and the problem of low flash point of low-polymer silicon-based macromolecules is solved. Moreover, the long chain is connected to the tail end of the high-branch-chain silicon-based polymer, so that the stability of the base oil can be improved, and the high-branch-chain silicon-based compound is prevented from undergoing chemical reaction at high temperature; the viscosity of the base oil can be increased, the thickness of an oil film in the using process can be increased, and the lubricating oil is more suitable for being used as lubricating oil; the cost of the lubricating oil can be reduced compared to polymerization with other silicon-based monomers. Compared with the prior art, the invention has the beneficial effects that:

1. the high-temperature stable silicon-based base oil is of a high-branched silicon-based polymer structure, has a high flash point, is not easy to decompose, has good high-temperature performance, and can be used for a long time in an environment of 200-260 ℃;

2. the silicon-based base oil stable at high temperature has low chemical activity and does not react with strong acid and strong base;

3. the preparation method of the high-temperature stable silicon-based base oil is simple, stable in quality and low in cost.

Detailed Description

In order to better understand the present invention, the following examples are further illustrative, but the present invention is not limited to the following examples.

Examples

A preparation method of high-temperature stable silicon-based base oil comprises the following preparation processes:

1) weighing 100 parts of methyl triallyl silane according to the parts by weight, adding the weighed materials into a flask, heating the flask to 40 ℃, and slowly adding 0.03 part of (COD) PtCl₂Keeping the temperature at 40 ℃ and mechanically stirring for 96 hours to finally obtain the polymethyl triallyl silane of the central core part;

2) weighing 68 parts of dimethoxydimethylsilane and 3 parts of 37% concentrated hydrochloric acid in parts by weight, adding the obtained product into the previous step, heating to 60 ℃, and continuously stirring for 12 hours to obtain a crude product;

3) standing the crude product for layering, and removing a lower water phase;

4) collecting the upper oil phase, distilling at 80 deg.C under reduced pressure to remove residual water, HCl molecules, unpolymerized monomers and oligomeric molecules to obtain colorless viscous liquid with flash point of about 360 deg.C. In addition, the high-temperature stable silicon-based base oil prepared by the method has stable chemical properties, is heated to 200 ℃ in the air and is kept for 72 hours, and the quality and the state are not obviously changed; is insoluble in water, and has no obvious change after being reacted for 24 hours at 100 ℃; dissolving in organic solvent such as diethyl ether and dichloromethane, and not dissolving in water; the acid and alkali resistance is excellent, and the reaction time with strong acid (1mol/L HCl) and strong base (1mol/L NaOH) at 80 ℃ is not obviously changed.

Comparative example 1: metallocene SpectraSyn Elite^TM300

Comparative example 2: ester oil composite ester 1851

Comparative example 3: dimethyl silicone oil

The results of comparing the parameters of the examples and the comparative examples are shown in Table 1.

TABLE 1

As can be seen from Table 1: the high-temperature stable silicon-based base oil obtained in the example has the best combination property. The embodiment improves the problem of poor high-temperature performance of the dimethyl silicone oil, improves the polymerization degree of the product by a catalytic grafting method, greatly improves the high-temperature resistance of the product, and can meet the requirement of long-time use at the temperature of 200-.

The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, which falls into the protection scope of the present invention.

Claims

1. A preparation method of high-temperature stable silicon-based base oil is characterized by mainly comprising the following steps:

(1) using methyl triallyl silane as monomer, platinum Catalyst (COD) PtCl₂As a catalyst, preparing poly (methyl triallyl silane);

(2) and (3) reacting the poly (methyl triallyl silane) with dimethoxy dimethylsilane and hydrochloric acid to obtain the high-temperature stable silicon-based base oil.

2. The method for preparing the silicon-based base oil with high temperature stability according to claim 1, wherein the amount of the catalyst is 0.02-0.05% of the mass of the methyl triallyl silane.

3. The method for preparing a high temperature stable silicon-based base oil according to claim 1, wherein the reaction temperature in the step (1) is 38-42 ℃ and the reaction time is 95-100 hours.

4. The method for preparing a high temperature stable silicon-based base oil according to claim 1, wherein in the step (2), the weight parts of the poly (methyl triallyl silane) are 10 parts, the weight parts of the dimethoxy dimethylsilane are 6 to 8 parts, and the weight parts of the concentrated hydrochloric acid are 0.2 to 0.4 part.

5. The method of claim 1, wherein the reaction temperature in step (2) is 55-65 ℃ and the reaction time is 12-14 hours.

6. A silicon-based base oil prepared by the process of claim 1.

7. The use of the silicon-based base oil of claim 6 as a lubricating oil in an environment of 200 ℃ and 260 ℃.

8. Use of the silicon-based base oil of claim 6 as a lubricating oil in a strong acid strong base environment.