A polyester poly-alpha-olefin base oil, and a method for preparing and using the same

High-performance polyester polyalphaolefin base oil was prepared by addition polymerization of alpha-olefins and dibutyl itaconic acid. This solved the polarity and compatibility problems of existing lubricating oil base oils, achieving high viscosity index, low pour point and excellent oxidation stability, making it an ideal choice to replace traditional materials.

CN119192448BActive Publication Date: 2025-11-07OULUBO (TIANJIN) NEW MATERIAL TECH CO LTD
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Patent Information

Application Number
CN202411308963.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-19
Publication Date
2025-11-07
Estimated Expiration
2044-09-19

AI Technical Summary

Technical Problem

Existing synthetic esters and polyalphaolefin lubricating oil base oils each have problems such as high polarity, strong water absorption, poor compatibility with rubber materials, and incompatibility. Furthermore, the high reactivity of (meth)acrylates leads to self-polymerization, which increases the difficulty of reaction conditions and reduces product quality.

Method used

An addition polymerization reaction is carried out between α-olefins and dibutyl itaconic acid under the action of an initiator to form a polyester polyα-olefin base oil. By controlling the reaction conditions and the dropping method, the self-polymerization of dibutyl itaconic acid is avoided, thus ensuring the purity and performance stability of the product.

Benefits of technology

A polyester polyalphaolefin base oil with high viscosity index, low pour point, good compatibility with additives, and excellent oxidation stability was prepared, solving the quality degradation and compatibility problems existing in the prior art and improving lubrication performance and service life.

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Abstract

The present application relates to the technical field of chemical lubricating base oil, and particularly relates to a polyester poly-alpha-olefin base oil and a preparation method and application thereof. The preparation method of the polyester poly-alpha-olefin base oil comprises the following steps: firstly, mixing dibutyl itaconate and an initiator to obtain a mixed solution; then, adding the mixed solution into alpha-olefin dropwise, and under the action of the initiator, a free radical addition polymerization reaction occurs between the carbon-carbon double bond of the dibutyl itaconate and the carbon-carbon double bond of the alpha-olefin to obtain the polyester poly-alpha-olefin base oil. The preparation method has the characteristics of mild reaction conditions, easy control, easy-to-obtain raw materials and environmental protection and pollution-free, effectively solves the problem of quality decline of the existing polyester poly-alpha-olefin base oil caused by (methyl) acrylate self-polymerization, and can apply the polyester poly-alpha-olefin base oil as a lubricating oil base oil.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical lubricating base oil, and particularly relates to a polyester poly-alpha-olefin base oil and a preparation method and application thereof. BACKGROUND

[0002] In the field of lubricating oil, the selection of synthetic base oil is crucial for the performance of the product. Traditionally, synthetic esters and poly-alpha-olefins are widely used due to their unique physicochemical properties. However, each of these two base oils has significant limitations. Although synthetic esters have excellent lubricating properties and thermal stability, their problems of high polarity, strong water absorption, and poor compatibility with rubber materials limit the use of synthetic esters in certain high-end applications. On the other hand, poly-alpha-olefins are favored due to their good oxidation stability and low-temperature fluidity, but their incompatibility with ordinary sealing materials and poor compatibility with polar additives also pose challenges to their application range.

[0003] In order to overcome these defects, the prior art uses a copolymer of (meth)acrylate and alpha-olefin as an innovative attempt to significantly broaden the viscosity range of the product by combining the advantages of both. At 40℃, the kinematic viscosity of the product can rise from 100mm 2 / s to 90000mm 2 / s, bringing new possibilities to the field of lubricating oil additives. However, the high activity of (meth)acrylate leads to easy self-polymerization, which not only reduces the quality of the product, but also makes the copolymerization reaction conditions with alpha-olefin extremely harsh, requiring precise control to avoid the occurrence of side reactions. SUMMARY

[0004] In view of the deficiencies of the prior art, the present application provides a polyester poly-alpha-olefin base oil and a preparation method and application thereof. The present application uses alpha-olefin and dibutyl itaconate as raw materials, and under the action of an initiator, the alpha-olefin and the dibutyl itaconate undergo addition polymerization reaction to obtain a polyester poly-alpha-olefin base oil. The preparation method of the present application not only has the characteristics of mild reaction conditions, easy control, easy availability of raw materials, and environmental protection and no pollution, but also effectively solves the problem of quality decline of the existing polyester poly-alpha-olefin base oil due to self-polymerization of (meth)acrylate, and can apply the polyester poly-alpha-olefin base oil as a lubricating oil base oil.

[0005] In order to achieve the above-mentioned purposes, the technical scheme adopted by the present application is as follows:

[0006] The first object of the present application is to provide a preparation method of a polyester poly-alpha-olefin base oil, comprising the following steps:

[0007] S1, mixing dibutyl itaconate and an initiator to obtain a mixed solution;

[0008] S2, drop the mixed solution into the alpha-olefin, under the action of initiator, the carbon-carbon double bond of dibutyl itaconate and the carbon-carbon double bond of alpha-olefin occur free radical addition polymerization reaction, and polyester poly-alpha-olefin base oil is obtained.

[0009] Preferably, the molar ratio of alpha-olefin to dibutyl itaconate is 3-5:1, and the alpha-olefin is excessive, so as to ensure that there are enough reaction sites for addition polymerization with dibutyl itaconate during the reaction, and the excessive alpha-olefin acts as a diluent to reduce the concentration between the components in the reaction system, thereby reducing the probability of side reactions.

[0010] Preferably, the reaction conditions of the addition polymerization reaction are as follows: at 115℃-160℃, the reaction is carried out for 3h-10h, if the reaction temperature is lower than 115℃, the reaction rate is too slow, and the conversion rate is low; if the reaction temperature is higher than 160℃, the structure of the polyester poly-alpha-olefin base oil will be damaged, and the quality and performance of the product will be reduced.

[0011] Preferably, the initiator is selected from di-t-butyl peroxide or t-butyl peroxybenzoate.

[0012] Preferably, the mass of the initiator accounts for 1%-8% of the total mass of alpha-olefin and dibutyl itaconate.

[0013] Preferably, the dibutyl itaconate is selected from industrial-grade dibutyl itaconate, and the mass fraction of dibutyl itaconate in the industrial-grade dibutyl itaconate is ≥95%.

[0014] Preferably, the alpha-olefin is selected from one or two of alpha-octene, alpha-decene, alpha-dodecene or alpha-tetradecene, and the alpha-olefin is all industrial grade.

[0015] The second object of the present application is to provide a polyester poly-alpha-olefin base oil prepared by the above preparation method.

[0016] Preferably, the structural formula of the polyester poly-alpha-olefin base oil is as follows:

[0017] Wherein, m is 2-100; n is 2-100.

[0018] The third object of the present application is to provide an application of the above polyester poly-alpha-olefin base oil in preparing lubricating oil base oil, anti-emulsification additive or cutting fluid.

[0019] Compared with the prior art, the present application has the following beneficial effects:

[0020] 1. The application provides a preparation method of polyester poly-alpha-olefin base oil, which is prepared by using alpha-olefin and dibutyl itaconate as raw materials, and under the action of an initiator, the carbon-carbon double bond in the dibutyl itaconate molecule is activated to form an active free radical, which is added to the carbon-carbon double bond of the alpha-olefin to form a new active center and initiate chain growth. In this process, alpha-olefin and dibutyl itaconate molecules are alternately or randomly added to the polymer chain to form a polyester poly-alpha-olefin structure, and the polymerization is terminated when the active center encounters other active centers, thereby obtaining the polyester poly-alpha-olefin base oil.

[0021] In the application, the reaction activity of dibutyl itaconate is much lower than that of (meth)acrylate, the mixture of dibutyl itaconate and the initiator is added to the reaction system in a dropwise manner, the alpha-olefin is ensured to be in an excess state, the self-polymerization of dibutyl itaconate to form small molecule self-polymer is effectively prevented, and the unreacted dibutyl itaconate is also ensured to be not left after the reaction; after the reaction, the initiator and unreacted alpha-olefin are recovered by means of reduced pressure distillation, thereby the purity and quality of the polyester poly-alpha-olefin base oil are significantly improved; compared with (meth)acrylate, the application solves the problem of the quality decline of the polyester poly-alpha-olefin base oil caused by the self-polymerization of (meth)acrylate in the prior art, and makes the performance of the final product more stable and reliable.

[0022] 2. The application provides a polyester poly-alpha-olefin base oil, which has a high viscosity index and a low pour point characteristic compared with the copolymer of (meth)acrylate and alpha-olefin in the prior art, ensures the stable lubricating performance and good flowability of the polyester poly-alpha-olefin base oil in a wide temperature range, and has excellent oxidation stability, i.e., the oxidation induction time is more than 80 min, thereby significantly prolonging the service life of the oil product; in addition, the application also significantly improves the compatibility of the polyester poly-alpha-olefin base oil with various additives, and effectively inhibits the common emulsification tendency of ester base oil, and the polyester poly-alpha-olefin base oil can replace the copolymer of (meth)acrylate and alpha-olefin for use.

[0023] In the application, the polyester poly-alpha-olefin base oil is polymerized from alpha-olefin and dibutyl itaconate, and contains long-chain alkyl and ester groups in the molecular structure, which makes the base oil have good compatibility with various additives and lubricating components; the poly-alpha-olefin is a non-polar component, and the molecular structure thereof does not contain a strong polar functional group, which helps to reduce the interaction with other polar substances and avoid unnecessary phase separation or precipitation. Meanwhile, the poly-alpha-olefin is a non-polar component, and the molecular structure thereof does not contain any functional group that reacts with water, and with the increase of the content of alpha-olefin, the polarity of the copolymer is effectively reduced, and the hydrophobicity is significantly enhanced, which greatly reduces the interaction opportunity between the polyester and water molecules, thereby effectively inhibiting the common emulsification tendency of ester base oil.

[0024] 3. The application provides a preparation method of polyester poly-alpha-olefin base oil, which has simple process, high operability, mild reaction condition, high yield, easily obtained raw material, environmental protection and small environmental pollution. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 The technical route diagram for synthesizing the polyester poly-alpha-olefin base oil in the examples 1-9 of the application is shown.

[0026] Figure 2 The infrared spectrum of the polyester poly-alpha-olefin base oil synthesized in the example 1 of the application is shown.

[0027] Figure 3 The hydrogen nuclear magnetic resonance spectrum of the polyester poly-alpha-olefin base oil synthesized in the example 1 of the application is shown. DETAILED DESCRIPTION

[0028] The technical solutions of the application will be described clearly and completely in combination with the data in the examples of the application. Obviously, the described examples are only a part of the examples of the application, rather than all the examples. Based on the examples in the application, all the other examples obtained by those skilled in the art without creative labor fall within the protection scope of the application.

[0029] It should be noted that the professional terms used in the application are only for the purpose of describing the specific examples, and are not intended to limit the protection scope of the application. Unless otherwise specified, the various raw materials, reagents, instruments and equipment used in the following examples of the application can be purchased from the market or prepared by the existing method. The alpha-tetradecene, alpha-dodecene, alpha-octene and alpha-decene used in the application are all industrial grade and purchased from Aladdin Reagent Company; the dibutyl itaconate is industrial grade and purchased from Shenzhen Jintenglong Industry Co., Ltd.; the di-tert-butyl peroxide is industrial grade and purchased from Aladdin Reagent Company; and the tert-butyl peroxybenzoate is industrial grade and purchased from Aladdin Reagent Company.

[0030] The test method of the application is as follows:

[0031] Kinematic viscosity: tested according to GB / T 265-1988 Petroleum Products-Determination of Kinematic Viscosity and Calculation of Dynamic Viscosity.

[0032] Viscosity index: calculated according to GB / T 1995-1998 Petroleum Products-Determination of Viscosity Index.

[0033] Pour point: tested according to GB / T 3535-2006 Petroleum Products-Determination of Pour Point.

[0034] In the prior art, synthetic esters and poly-alpha-olefins have their respective advantages as lubricating oil base oils, but both have significant limitations: synthetic esters are limited in high-end applications due to their high polarity, strong water absorption and poor compatibility with rubber materials; and poly-alpha-olefins face the challenges of incompatibility with ordinary sealing materials and poor compatibility with polar additives. In addition, although copolymerization of (meth) acrylate and alpha-olefin can broaden the viscosity range, the high activity of (meth) acrylate can easily lead to self-polymerization, reducing the quality of polyester poly-alpha-olefin base oil and increasing the difficulty of controlling reaction conditions, which limits the further improvement of the performance of lubricating oil base oil.

[0035] To solve the problems in the prior art, the present application provides a preparation method of polyester poly-alpha-olefin base oil, comprising the following steps: mixing dibutyl itaconate and an initiator to obtain a mixed solution; and adding the mixed solution dropwise into alpha-olefin to carry out addition polymerization reaction to obtain polyester poly-alpha-olefin base oil.

[0036] In the present application, alpha-olefin and dibutyl itaconate are used as raw materials to carry out addition polymerization reaction under the action of an initiator, and polyester poly-alpha-olefin base oil is successfully prepared; wherein the reaction activity of dibutyl itaconate is relatively low, and when the alpha-olefin is ensured to be in an excess state, the mixed solution of dibutyl itaconate and the initiator is added into the reaction system in a dropwise manner, so that dibutyl itaconate will not self-polymerize to form small molecule self-polymer, and at the same time, it is also ensured that there is no unreacted dibutyl itaconate remaining after the reaction is completed, thereby significantly improving the purity and quality of the product; compared with (meth) acrylate, the preparation method of polyester poly-alpha-olefin base oil provided by the present application not only successfully avoids the common self-polymerization problem of (meth) acrylate, but also significantly improves the comprehensive performance and purity of polyester poly-alpha-olefin base oil; in addition, the polyester poly-alpha-olefin base oil prepared by the present application has a high viscosity index, a good pour point index and excellent product performance, which not only effectively makes up for the defects of traditional poly-alpha-olefin base oil and ester base oil, but also becomes an ideal choice for replacing or partially replacing these relatively expensive materials due to its cost-effectiveness advantage.

[0037] The reaction mechanism of the present application is as follows:

[0038]

[0039] wherein m is 2-100; and n is 2-100.

[0040] In order for those skilled in the art to more clearly understand the technical solutions of the present application, the technical solutions of the present application will be described in detail below in combination with specific examples, and the specific synthesis route is as shown in Figure 1

[0041] Example 1 ​

[0042] A method for preparing a polyester poly-alpha-olefin base oil, comprising the following steps:

[0043] S1, in a four-port reaction bottle with a temperature controller, a stirrer, a condenser, and a dropping funnel, 3 mol of alpha-tetradecene was added, and after being warmed to 145°C, 1 mol of dibutyl itaconate and 50 g of di-tert-butyl peroxide were mixed uniformly and then added to the four-port reaction bottle at a constant speed, with a dropping time of 2 h.

[0044] S2, after the dropping was completed, the reaction was continued at 145°C for 3 h, and then the temperature was increased to 210°C to distill the unreacted alpha-tetradecene under reduced pressure, to obtain the polyester poly-alpha-olefin base oil.

[0045] The physical and chemical indexes of the polyester poly-alpha-olefin base oil were as follows: a kinematic viscosity at 40°C of 175 mm 2 / s, a kinematic viscosity at 100°C of 21.99 mm 2 / s, a viscosity index of 150, and a pour point of -24°C.

[0046] Example 2

[0047] A method for preparing a polyester poly-alpha-olefin base oil, which was the same as the preparation method of Example 1, except that in S1, the alpha-tetradecene was replaced by alpha-dodecene, the amount of di-tert-butyl peroxide was replaced by 7.5 g, the dropping time was replaced by 1.5 h, and in S2, the reaction time was replaced by 1.5 h, comprising the following steps:

[0048] S1, in a four-port reaction bottle with a temperature controller, a stirrer, a condenser, and a dropping funnel, 3 mol of alpha-dodecene was added, and after being warmed to 145°C, 1 mol of dibutyl itaconate and 7.5 g of di-tert-butyl peroxide were mixed uniformly and then added to the four-port reaction bottle at a constant speed, with a dropping time of 1.5 h.

[0049] S2, after the dropping was completed, the reaction was continued at 145°C for 1.5 h, and then the temperature was increased to 210°C to distill the unreacted alpha-dodecene under reduced pressure, to obtain the polyester poly-alpha-olefin base oil.

[0050] The physical and chemical indexes of the polyester poly-alpha-olefin base oil were as follows: a kinematic viscosity at 40°C of 141.73 mm 2 / s, a kinematic viscosity at 100°C of 17.92 mm 2 / s, a viscosity index of 141, and a pour point of -35°C.

[0051] Example 3

[0052] A preparation method of a polyester poly-alpha-olefin base oil, which is the same as the preparation method of Example 1, except that in S1, the amount of alpha-tetradecene is replaced by 5 mol, the amount of di-tert-butyl peroxide is replaced by 24.44 g, and the dropping time is replaced by 3 h, and in S2, the continuous reaction time is replaced by 5 h, and the reaction temperature is replaced by 160°C, comprising the following steps:

[0053] S1, in a four-necked reaction bottle with a temperature controller, a stirrer, a condenser, and a dropping funnel, 5 mol of alpha-tetradecene is added, and after being heated to 160°C, 1 mol of itaconic acid dibutyl ester and 24.44 g of di-tert-butyl peroxide are uniformly mixed and then dropped into the four-necked reaction bottle at a constant speed, with a dropping time of 3 h.

[0054] S2, after the dropping is completed, the temperature is maintained at 160°C for 5 h of continuous reaction, and then the temperature is increased to 210°C to distill the unreacted alpha-tetradecene under reduced pressure, to obtain the polyester poly-alpha-olefin base oil.

[0055] The physical and chemical indicators of the polyester poly-alpha-olefin base oil are as follows: the 40°C kinematic viscosity is 195.3 mm 2 / s, the 100°C kinematic viscosity is 24.27 mm 2 / s, the viscosity index is 154, and the pour point is -24°C.

[0056] Example 4

[0057] A preparation method of a polyester poly-alpha-olefin base oil, which is the same as the preparation method of Example 2, except that in S1, the amount of alpha-dodecene is replaced by 4 mol, di-tert-butyl peroxide is replaced by peroxiobenzoic acid, the amount of peroxiobenzoic acid is replaced by 27.42 g, and the dropping time is replaced by 2 h, and in S2, the continuous reaction time is replaced by 5 h, and the reaction temperature is replaced by 115°C, comprising the following steps:

[0058] S1, in a four-necked reaction bottle with a temperature controller, a stirrer, a condenser, and a dropping funnel, 4 mol of alpha-dodecene is added, and after being heated to 115°C, 1 mol of itaconic acid dibutyl ester and 27.42 g of tert-butyl peroxiobenzoate are uniformly mixed and then dropped into the four-necked reaction bottle at a constant speed, with a dropping time of 2 h.

[0059] S2, after the dropping is completed, the temperature is maintained at 115°C for 5 h of continuous reaction, and then the temperature is increased to 210°C to distill the unreacted alpha-dodecene under reduced pressure, to obtain the polyester poly-alpha-olefin base oil.

[0060] The physical and chemical indicators of the polyester poly-alpha-olefin base oil are as follows: the 40°C kinematic viscosity is 142.31 mm 2 / s, 100℃ kinematic viscosity 18.36 mm 2 / s, viscosity index 145, pour point -36℃.

[0061] Example 5

[0062] A method for preparing a polyester poly-alpha-olefin base oil, which is the same as the preparation method of Example 1, except that in S1, alpha-tetradecene is replaced by alpha-decene, and di-tert-butyl peroxide is replaced by tert-butyl peroxybenzoate, the amount of which is replaced by 26.48g, the dropping time is replaced by 5h, and in S2, the continuous reaction time is replaced by 5h, and the reaction temperature is replaced by 125℃, comprising the following steps:

[0063] S1, in a four-necked reaction flask with a temperature controller, a stirrer, a condenser, and a dropping funnel, 3mol of alpha-decene is added, and after being heated to 125℃, 1mol of dibutyl itaconate and 26.48g of tert-butyl peroxybenzoate are mixed uniformly and then dropped into the four-necked reaction flask at a constant speed, with a dropping time of 5h.

[0064] S2, after the dropping is completed, the temperature is maintained at 125℃ for 5h of continuous reaction, and then the temperature is increased to 210℃ to distill the unreacted alpha-decene under reduced pressure, to obtain a polyester poly-alpha-olefin base oil.

[0065] The physical and chemical indicators of the polyester poly-alpha-olefin base oil are: 40℃ kinematic viscosity 129.41 mm 2 / s, 100℃ kinematic viscosity 15.73 mm 2 / s, viscosity index 128, pour point -46℃.

[0066] Example 6

[0067] A method for preparing a polyester poly-alpha-olefin base oil, which is the same as the preparation method of Example 5, except that in S1, the amount of alpha-decene is replaced by 4mol, the amount of di-tert-butyl peroxide is replaced by 64.16g, and the dropping time is replaced by 4h, and in S2, the continuous reaction time is replaced by 5h, and the reaction temperature is replaced by 160℃, comprising the following steps:

[0068] S1, in a four-necked reaction flask with a temperature controller, a stirrer, a condenser, and a dropping funnel, 4mol of alpha-decene is added, and after being heated to 160℃, 1mol of dibutyl itaconate and 64.16g of di-tert-butyl peroxide are mixed uniformly and then dropped into the four-necked reaction flask at a constant speed, with a dropping time of 4h.

[0069] S2, after the end of dropping, continue to react at 160℃ for 5h, then increase the temperature to 210℃ to distill the unreacted α-decene under reduced pressure, to obtain the polyester poly-α-olefin base oil.

[0070] The physical and chemical indexes of the polyester poly-α-olefin base oil are as follows: the kinematic viscosity at 40℃ is 115.34 mm 2 / s, the kinematic viscosity at 100℃ is 13.51 mm 2 / s, the viscosity index is 114, and the pour point is -50℃.

[0071] Example 7

[0072] A method for preparing a polyester poly-α-olefin base oil, which is the same as the preparation method of Example 1, except that in S1, α-tetradecene is replaced by α-octene, and di-tert-butyl peroxide is replaced by tert-butyl peroxybenzoate, the amount of which is replaced by 56.14g, and the dropping time is replaced by 4h, and in S2, the continuous reaction time is replaced by 4h, and the reaction temperature is replaced by 115℃, comprising the following steps:

[0073] S1, in a four-necked reaction bottle with a temperature controller, a stirrer, a condenser and a dropping funnel, 5mol of α-octene is added, and after being heated to 115℃, 1mol of itaconic acid dibutyl ester and 56.14g of di-tert-butyl peroxide are mixed uniformly and then dropped into the four-necked reaction bottle at a constant speed, and the dropping time is 4h.

[0074] S2, after the end of dropping, continue to react at 115℃ for 4h, then increase the temperature to 210℃ to distill the unreacted α-octene under reduced pressure, to obtain the polyester poly-α-olefin base oil.

[0075] The physical and chemical indexes of the polyester poly-α-olefin base oil are as follows: the kinematic viscosity at 40℃ is 115.34 mm 2 / s, the kinematic viscosity at 100℃ is 13.51 mm 2 / s, the viscosity index is 114, and the pour point is -50℃.

[0076] Example 8

[0077] A method for preparing a polyester poly-α-olefin base oil, which is the same as the preparation method of Example 1, except that in S1, α-tetradecene is replaced by a mixture of α-octene and α-decene, and di-tert-butyl peroxide is replaced by tert-butyl peroxybenzoate, the amount of which is replaced by 31g, and in S2, the continuous reaction time is replaced by 2h, and the reaction temperature is replaced by 125℃, comprising the following steps:

[0078] S1, in the four-port reaction bottle with temperature controller, stirrer, condenser, dropping funnel, add 3 mol of the mixture of a-octene and a-decene, after warming to 125℃, add 1 mol of dibutyl itaconate and 31 g of tert-butyl peroxybenzoate, mix uniformly, then drop into the four-port reaction product at a uniform speed, the dropping time is 2 h.

[0079] S2, after the dropping is completed, continue to react at 125℃ for 2 h, then increase the temperature to 180℃ to distill the mixture of a-octene and a-decene which does not participate in the reaction under reduced pressure, to obtain the polyester poly-a-olefin base oil.

[0080] The physical and chemical indexes of the polyester poly-a-olefin base oil are as follows: the kinematic viscosity at 40℃ is 115.34 mm 2 / s, the kinematic viscosity at 100℃ is 13.51 mm 2 / s, the viscosity index is 114, and the pour point is -45℃.

[0081] Example 9

[0082] A method for preparing a polyester poly-a-olefin base oil, which is the same as the preparation method of Example 1, except that in S1, the a-tetradecene is replaced by the mixture of a-octene and a-decene, the amount of di-tert-butyl peroxide is replaced by 52.22 g, the dropping time is replaced by 3 h, and the reaction temperature is replaced by 130℃, comprising the following steps:

[0083] S1, in the four-port reaction bottle with temperature controller, stirrer, condenser, dropping funnel, add 4 mol of the mixture of a-octene and a-decene, after warming to 130℃, add 1 mol of dibutyl itaconate and 52.22 g of di-tert-butyl peroxide, mix uniformly, then drop into the four-port reaction product at a uniform speed, the dropping time is 3 h.

[0084] S2, after the dropping is completed, continue to react at 130℃ for 3 h, then increase the temperature to 180℃ to distill the mixture of a-octene and a-decene which does not participate in the reaction under reduced pressure, to obtain the polyester poly-a-olefin base oil.

[0085] The physical and chemical indexes of the polyester poly-a-olefin base oil are as follows: the kinematic viscosity at 40℃ is 118.46 mm 2 / s, the kinematic viscosity at 100℃ is 13.97 mm 2 / s, the viscosity index is 116, and the pour point is -47℃.

[0086] Figure 2 The infrared spectrum of the polyester poly-a-olefin base oil synthesized in Example 1 in the application is observed Figure 2 It is known that, at 3000 cm -1 ~ 3100 cm -1The absence of obvious carbon-carbon double bond absorption peaks within the range indicates that the addition polymerization reaction between dibutyl itaconic acid and α-olefin proceeded very thoroughly during the synthesis process, with the carbon-carbon double bonds in the raw materials almost completely converted into saturated bonds in the polyester polyα-olefin polymer. Therefore, the infrared spectrum not only verifies the successful polymerization reaction.

[0087] Figure 3 The image shows the 1H NMR spectrum of the polyester polyα-olefin base oil synthesized in Example 1 of this invention. Figure 3 It was found that the range of 4.5 ppm to 6.0 ppm typically corresponds to the signal of hydrogen atoms near the carbon-carbon double bond in olefin compounds. However, in Figure 3 No obvious peaks were observed in the infrared spectrum, further confirming the results, indicating that the double bond between dibutyl itaconic acid and the α-olefin had been completely consumed through addition polymerization, resulting in a polyester polyα-olefin polymer without carbon-carbon double bonds. This characteristic of the 1H NMR spectrum not only proves the completeness of the polymerization reaction but also demonstrates the stability and consistency of the product structure. Combining the results of the infrared and 1H NMR spectra, it can be proven that this invention successfully synthesized a structurally stable polyester polyα-olefin base oil.

[0088] It should be noted that when numerical ranges are involved in this invention, it should be understood that both endpoints of each numerical range and any value between the two endpoints can be selected. Since the steps and methods used are the same as in the embodiments, preferred embodiments are described here to avoid redundancy. Although preferred embodiments of the invention have been described, those skilled in the art, once they understand the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments as well as all changes and modifications falling within the scope of this invention.

[0089] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.

Claims

1. A method for producing a polyester poly-α-olefin base oil, characterized by, The method comprises the following steps: mixing dibutyl itaconate and an initiator to obtain a mixed solution; dropping the mixed solution into the α-olefin, and under the action of the initiator, the carbon-carbon double bond of the dibutyl itaconate and the carbon-carbon double bond of the α-olefin undergo a free radical addition polymerization reaction to obtain a polyester poly-α-olefin base oil; the molar ratio of the α-olefin to the dibutyl itaconate is 3-5:1; the reaction conditions of the addition polymerization reaction are as follows: 115-160 ℃, and 3-10 h; the α-olefin is selected from one or two of α-octene, α-decene, α-dodecene or α-tetradecene.

2. The method for preparing a polyester polyα-olefin base oil according to claim 1, characterized in that, the initiator is selected from di-tert-butyl peroxide or tert-butyl peroxybenzoate.

3. The method for preparing a polyester polyα-olefin base oil according to claim 1, characterized in that, the mass of the initiator accounts for 1-8% of the total mass of the α-olefin and the dibutyl itaconate.

4. The method for preparing a polyester polyα-olefin base oil according to claim 1, characterized in that, the dibutyl itaconate is selected from industrial-grade dibutyl itaconate, and the mass fraction of the dibutyl itaconate in the industrial-grade dibutyl itaconate is ≥95%.

5. A polyester poly-α-olefin base oil prepared by the method of any one of claims 1-4.

6. The polyester polyalphaolefin base oil of claim 5, wherein, The structural formula of the polyester poly-alpha-olefin base oil is: ; wherein m is 2-100; and n is 2-100.

7. Use of the polyester poly-α-olefin base oil of claim 5 in the preparation of a lubricating oil base oil, an anti-emulsification additive or a cutting fluid.

Citation Information

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