阅读说明：本技术 控制聚α烯烃的运动粘度的方法 (Method for controlling kinematic viscosity of poly-alpha-olefins ) 是由 苏克迪普·考尔 乌沙拉尼·萨胡 古尔米特·辛格 纳雷什·帕普 贾伊·纳拉扬·潘迪 肖巴尚卡 于 2021-04-14 设计创作，主要内容包括：本发明涉及C6烯烃单体和更高级烯烃单体的低聚的方法,其中在固定的单体/卤化铝摩尔比下,通过控制低聚温度来制备具有期望的运动粘度的聚α烯烃。低聚在包含卤化铝的低聚催化剂和促进剂的存在下进行,以及低聚温度为约10℃至约120℃。(The present invention relates to a process for the oligomerization of C6 olefin monomers and higher olefin monomers, wherein polyalphaolefins having a desired kinematic viscosity are prepared by controlling the oligomerization temperature at a fixed monomer/aluminum halide molar ratio. The oligomerization is carried out in the presence of an oligomerization catalyst comprising an aluminum halide and a promoter, and the oligomerization temperature is from about 10 ℃ to about 120 ℃.)

1. A process for controlling the kinematic viscosity of a polyalphaolefin in the range of 1 centistokes to 70 centistokes, the process comprising the steps of:

oligomerizing a C6 olefin monomer and a higher olefin monomer in the presence of an aluminum halide, a promoter, and optionally a solvent to obtain a polyalphaolefin,

wherein the kinematic viscosity of the polyalphaolefin is controlled by adjusting the oligomerization temperature at a fixed molar ratio of olefin monomer to aluminum halide.

2. The process of claim 1, wherein the olefin monomer is selected from the group consisting of 1-decene, 1-dodecene, 1-octene, and any mixtures thereof.

3. The process of claim 1, wherein the molar ratio of the olefin monomer to the aluminum halide is from 10 to 500, more preferably from 10 to 350, most preferably from 40 to 300.

4. The process according to claim 1, wherein the molar ratio of the aluminum halide to the promoter is from 1 to 10, preferably from 1 to 5.

5. The method of claim 1, wherein the promoter is selected from the group consisting of a mixture of water, an alcohol, a carboxylic acid, an ester, a ketone, an ether, a halogenated hydrocarbon, or any combination thereof.

6. The method of claim 1, wherein the promoter is isobutanol.

7. The method of claim 1, wherein the moisture content of the monomer and the solvent is less than 20 ppm.

8. The method of claim 1, wherein the oligomerization temperature is in the range of 10 ℃ to 150 ℃.

9. The method of claim 1, wherein the oligomerization temperature is 25 ℃ and 90 ℃.

10. The process of claim 1, wherein the residence time during oligomerization is in the range of 0.5 hours to 8 hours.

11. The process of claim 1, wherein the solvent is selected from C5 to C19 alkanes.

12. The method of claim 1, wherein the conversion from the monomer to polyalphaolefin is greater than 95%.

13. The method of claim 1, wherein the oligomerizing comprises C20 to C24 dimers, C30 to C36 trimers, C40 to C48 tetramers, C50 to C60 pentamers, and C60+ heavies.

Technical Field

The invention relates to the use of aluminium halides as catalysts and promoters for the preparation of C₆A process for the oligomerization of olefin monomers and higher olefin monomers to Polyalphaolefin (PAO). More particularly, the present invention relates to a method for controlling the kinematic viscosity of polyalphaolefins by adjusting the oligomerization temperature at a fixed monomer/aluminum halide molar ratio.

Background

Oligomerization of higher olefins yields polyalphaolefins that are useful as synthetic base oils for lubricant applications. Polyalphaolefins are used in many synthetic products, such as lubricants, greases, and fluids, and have emerged as an essential component in many industries and applications. Polyalphaolefins are specifically designed chemicals that are uniquely made from alpha olefins. The increase in the use of polyalphaolefins is driven primarily by the stability of the polyalphaolefin molecule. This stability, along with many other unique performance characteristics, makes polyalphaolefins far superior to mineral oils in a variety of applications.

Efforts to improve the properties of polyalphaolefins have been the subject of significant research and development in the petroleum industry for decades. Industrial research efforts have been directed to synthetic processes for producing polyalphaolefins that exhibit useful viscosities over a wide temperature range, i.e., have improved Viscosity Indices (VI), while also exhibiting lubricity, thermal and oxidative stability, and pour point equal to or better than mineral oil lubricants.

Polyalphaolefins can be produced by using an olefin as a feed and using BF₃And AlCl₃And promoters are produced as catalysts. Evaluation of polyalphaolefins under various test conditions was performed only after hydrogenation of the polyalphaolefin after oligomerization. Usually by using BF₃The catalyst and alcohol promoter oligomerize 1-decene to typically produce polyalphaolefins in the range of 4cSt to 6 cSt.

Traditionally, the olefin feed for the oligomerization is 1-octene, 1-decene, 1-dodecene, 1-tetradecene, and possibly also mixtures, but the preferred olefin is 1-decene.

There are various known methods of forming polyalphaolefins in the prior art literature. Some of which are discussed herein below.

US 9708549 describes a process for oligomerizing olefins or producing polyalphaolefins using a catalyst mixture comprising an aluminum halide and an organic liquid carrier, wherein the organic liquid carrier comprises at least 75 mol% of a 1, 2-disubstituted olefin, a trisubstituted olefin, or any combination thereof. This patent teaches that a stable liquid solution can be formed between the aluminum halide and the organic liquid carrier, which can be prepared prior to its use and which can be stored for a long period of time.

US 5196635 describes the preparation of olefin oligomers by polymerizing an olefin or a mixture of olefins in the presence of a catalyst prepared by reacting an aluminum halide and a proton donor in an organic solvent. The resulting olefin oligomers have a kinematic viscosity at 100 ℃ of about 30cSt to 400 cSt.

US 5463158 describes a process for the catalytic oligomerization of light olefins such as ethylene or propylene using a liquid catalyst comprising a lewis acid and a lewis base component which forms a melt with the lewis acid which is liquid at room temperature. The Lewis acid being a metal halide, e.g. aluminium trichloride, and the Lewis base being an organic salt, e.g. an organic halide salt containing an N-heterocycle or containing a completely substituted Lewis acidA salt of an ion.

US 5451704 describes a process for producing a hydrocarbon lubricant base stock comprising contacting a C2 to C20 alpha-olefin feedstock or mixture under heterogeneous oligomerization conditions with AlCl anchored to an adsorptive inorganic oxide solid such as silica₃And (4) contacting.

US 4219691 describes a process for producing olefin oligomers from olefins having not less than 6 carbon atoms in the presence of an equal proportion of a reaction mixture of an aluminum halide and a secondary or tertiary alcohol. The olefin oligomers thus obtained have a high kinematic viscosity, a low pour point, a high viscosity index and good shear stability. It is also disclosed that the kinematic viscosity of the oligomer thus obtained does not change greatly even if the reaction ratio of the aluminum halide to the secondary or tertiary alcohol is changed within the above range.

US8865959B2 relates to a process for producing Polyalphaolefins (PAO), the process comprising: a) contacting one or more C4 to C24 alpha olefin monomers with a metallocene compound and optionally an activator to produce a low molecular weight PAO comprising a mixture of oligomers having a number average molecular weight in the range of 120 to 600 and a terminal olefin content of at least 25 wt% of total olefinic unsaturation; and b) subsequently contacting at least a portion of the low molecular weight PAO with a lewis acid catalyst and optionally one or more C4 to C24 alpha olefin monomers to produce a liquid PAO, wherein the liquid PAO has a mass average molecular weight of at least 988.

US10435491 relates to a method comprising: contacting in a reaction zone i) a monomer comprising a C6 to C20 olefin, ii) a haloaluminate ionic liquid, and iii) a halide component comprising a C1 to C12 organohalide; and oligomerizing the monomers in the reaction zone to form an oligomer product; wherein the oligomer product has an average molecular weight of 400 to 611 g/mol, wherein the oligomer product is formed in the presence of less than 8 mol% of an isoparaffin based on the moles of monomers in the reaction zone, wherein the molar ratio of halide in the halide component to aluminum in the haloaluminate ionic liquid is at least 0.14:1, and wherein the oligomer product is formed at a temperature of 15 to 125 ℃.

CN106957677 provides a process for the synthesis of low viscosity PAO4 from high purity linear alpha olefins by anhydrous AlCl 3. The method is characterized in that a catalyst selected from the group consisting of anhydrous aluminum chloride is added dropwise to a hot 1-decene monomer, and then a low viscosity PAO4 base oil is synthesized, wherein the hot 1-decene monomer is heated to 90 ℃ or higher. The invention provides a method for preparing a catalyst by anhydrous AlCl₃A process for synthesizing low viscosity PAO4 from high purity linear alpha olefins. The industrial catalyst adopted by the method is low in price; the catalyst is easy to obtain; in addition, the catalyst is easy to reactProcessing; the reaction condition is mild; the low viscosity PAO obtained by the preparation has good viscosity temperature characteristics.

US7550640 relates to the use of 1-decene/1-dodecene olefin mixtures to produce high viscosity Polyalphaolefins (PAOs) having a viscosity at 100 ℃ of from about 40cSt to about 100cSt (ASTM D-445) and a number average molecular weight of from about 1200 to about 4000, which are particularly useful as lubricant base stocks.

US7880047B2 relates to polyalphaolefins and processes and reaction systems for forming polyalphaolefins from alpha olefins, preferably C8 to C12 alpha olefins such as 1-decene, by co-feeding into a polymerization reaction mixture a C8 to C12 saturated hydrocarbon (preferably having the same number of carbon atoms) as the alpha olefin.

US8067652B2 relates to a process for forming a polyalphaolefin, the process comprising the steps of: polymerizing at least one C8 to C12 monomer, preferably decene such as 1-decene, in the presence of an alumoxane, an activator, and a metallocene to form a polyalphaolefin, wherein the molar ratio of alumoxane to metallocene is less than 250: 1.

US7259284B2 relates to a continuous process for making a high viscosity polyalphaolefin product from an alpha olefin feedstock using an ionic liquid catalyst, wherein the polyalphaolefin product has unique physical properties that make it useful as a lubricant or lubricant additive.

US8207390B2 relates to a process for producing Polyalphaolefins (PAO) in the presence of a metallocene catalyst with a non-coordinating anion activator and hydrogen.

There remains a need to provide a method for controlling the kinematic viscosity of polyalphaolefins at a fixed monomer/aluminum halide molar ratio.

The present invention provides a method for controlling the kinematic viscosity of polyalphaolefins by adjusting the oligomerization temperature at a fixed monomer/aluminum halide molar ratio. These newer methods of controlling the kinematic viscosity of polyalphaolefins provide polyalphaolefins with increased stability and mechanical efficiency over a wider range of operating conditions than mineral oil lubricants.

Object of the Invention

The main object of the present invention relates to C₆Process for the oligomerization of olefin monomers and higher olefin monomers in which the fixed monomer/aluminum halide mole isThe polyalphaolefin having a desired kinematic viscosity is prepared by controlling the oligomerization temperature at a molar ratio. The oligomerization is carried out in the presence of an oligomerization catalyst comprising an aluminum halide and a promoter, and the oligomerization temperature is from about 10 ℃ to about 120 ℃.

Furthermore, it is an object of the present invention that the oligomers obtained have a Br number > 0.2.

It is another object of the present invention to obtain oligomers with improved viscosity index.

It is another object of the present invention to use the oligomers as synthetic base oils after hydrogenation and distillation.

Disclosure of Invention

In one aspect of the invention, a process for controlling the kinematic viscosity of a polyalphaolefin to less than 70 centistokes is disclosed, the process comprising the steps of: oligomerizing a C6 olefin monomer and a higher olefin monomer in the presence of an aluminum halide, a promoter, and optionally a solvent to obtain a polyalphaolefin, wherein the kinematic viscosity of the polyalphaolefin is controlled by adjusting the oligomerization temperature at a fixed molar ratio of monomer to aluminum halide.

In one embodiment of the present invention, the olefin monomer or monomers are selected from the group consisting of 1-decene, 1-dodecene, 1-octene, and any mixtures thereof.

In one embodiment of the invention, the molar ratio of olefin monomer or monomers to aluminum halide is from 10 to 500, more preferably from 10 to 350, most preferably from 40 to 300.

In one embodiment of the invention, the molar ratio of aluminum halide to promoter is from 1 to 10, preferably from 1 to 5.

In one embodiment of the invention, the promoter is selected from the group/mixture consisting of water, alcohol, carboxylic acid, ester, ketone, ether, halogenated hydrocarbon, or any combination thereof.

In one embodiment of the invention, the promoter is isobutanol.

In one embodiment of the invention, the olefin monomer or monomers and solvent have a moisture content of less than 20 ppm.

In one embodiment of the invention, the oligomerization temperature is in the range of from 10 ℃ to 150 ℃.

In one embodiment of the invention, the oligomerization temperature is 25 ℃ and 90 ℃.

In one embodiment of the invention, the residence time during oligomerization is in the range of 0.5 hours to 8 hours.

In one embodiment of the invention, the solvent is selected from C5 to C19 alkanes.

In one embodiment of the invention, the conversion of olefin monomer or monomers to polyalphaolefin is greater than 95%.

In one embodiment of the invention, oligomerization comprises C20 to C24 dimers, C30 to C36 trimers, C40 to C48 tetramers, C50 to C60 pentamers, and C60+ heavies.

Detailed Description

The present invention relates to a process for the oligomerization of C6 olefin monomers and higher olefin monomers, wherein polyalphaolefins having a desired kinematic viscosity are prepared by controlling the oligomerization temperature at a fixed monomer/aluminum halide molar ratio. The oligomerization is carried out in the presence of an oligomerization catalyst comprising an aluminum halide and a promoter, and the oligomerization temperature is from about 10 ℃ to about 120 ℃.

Provide C to₆A process for the oligomerization of olefin monomers and higher olefin monomers to polyalphaolefins having a desired kinematic viscosity. In one embodiment, the process comprises the step of oligomerizing in the presence of an aluminum halide and a promoter, wherein the molar ratio of monomer to aluminum halide is from 10 to 500, preferably from 10 to 350.

In another embodiment, the invention relates to a process for oligomerizing C6 olefin monomers and higher olefin monomers to polyalphaolefins having a desired kinematic viscosity, the process comprising the step of oligomerizing in the presence of an aluminum halide and a promoter, wherein the aluminum halide is selected from those of formula R_3-nAlX_nWherein R is a hydrocarbyl group (i.e., alkyl group), X is a halide, and n ═ 0 to 3. In one embodiment, the halide may be chloride, bromide or iodide, preferably chloride or bromide. In one embodiment, the aluminum halide is aluminum chloride or aluminum bromide.

In one implementationIn scheme (B), C₆The olefin monomer and higher olefin monomer may be C₆To C₁₄Olefins in the range in which C can be used₆To C₁₄A mixture of olefin monomers. In another embodiment, recycled or re-distilled olefin monomers may be used.

In one embodiment, the invention relates to a method for reacting C₆A process for the oligomerization of olefin monomers and higher olefin monomers to polyalphaolefins having a desired kinematic viscosity, said process comprising the step of oligomerizing in the presence of an aluminum halide and a promoter, wherein the molar ratio of aluminum halide to promoter is from 1 to 10, preferably from 1 to 5.

In one embodiment, the promoter is selected from a mixture consisting of water, an alcohol, a carboxylic acid, an ester, a ketone, an ether, a halogenated hydrocarbon, or any combination thereof. In another embodiment, the accelerator is selected from a mixture consisting of water, an alcohol, an ester, a ketone, or any combination thereof. In one embodiment, the promoter is isobutanol.

The present inventors have unexpectedly discovered that by controlling the oligomerization temperature at a fixed monomer/Al weight ratio, polyalphaolefins having desirable kinematic viscosities are produced. In one embodiment, the oligomerization temperature is in the range of 10 ℃ to 150 ℃, although temperatures outside this range may be used. The preferred oligomerization temperature is 10 ℃ to 120 ℃. For non-adiabatic oligomerization, heat transfer capability may be required in order to maintain steady state conditions.

Furthermore, the present inventors have unexpectedly found that the addition of a promoter in addition to the olefin monomer not only improves the bromine number of the resulting polyalphaolefin, but also controls the exothermic nature of the oligomerization. Thus, the reaction proceeds in a controlled manner, so that the possibility of occurrence of hot spots or runaway is low.

Generally, the residence time to form the oligomer product is the time to achieve the desired conversion. In one embodiment, the residence time during oligomerization is from about 0.5 hours to 8 hours.

For any oligomerization carried out using an aluminum halide, the reactants and apparatus/equipment should be non-toxic, especially free of air and moisture. Thus, for this purpose all devices/equipment are heated and dried in vacuum or nitrogen while the monomer and solvent are distilled, passed through a desiccant column or stored on a desiccant. If necessary, operations before and during the oligomerization for maintaining inert conditions and atmosphere are performed.

In one embodiment, no solvent is used during oligomerization. In another embodiment, the choice of solvent may be related to the oligomerization temperature. In one embodiment, the solvent may be selected from C₅To C₁₉An alkane.

After oligomerization is complete, the conversion from monomer to oligomer is typically greater than 95%. The oligomerization is stopped by adding water or alcohol, followed by a catalyst removal step, such as water washing or filtration, adsorption or centrifugation. The next step is to remove the monomers, promoters and low boiling oligomers by distillation.

The oligomerization product is substantially hydrogenated and may optionally be hydrogenated before or after distillation. The hydrogenation is carried out using a metal catalyst and hydrogen. Generally, bromine numbers below 5, more preferably below 2, will yield oligomers with excellent oxidative stability. In one embodiment, the resulting product is typically hydrogenated to saturate the oligomers to provide a product having a desired viscosity, for example, 40cSt or 100cSt at 100 ℃.

Depending on the viscosity, the oligomeric product typically comprises C_20-24Dimer, C_30-36Trimer, C_40-48Tetramer, C_50-60Pentamer and C₆₀₊And (5) a heavy object.

One of the features of the present invention is that the oligomeric products can be used in a variety of applications, such as base oils in lubricants, additives for various compositions, viscosity index improvers, dispersants, and the like.

All monomers and solvents were used as obtained and contained less than 20ppm moisture. All chemicals based on aluminum halide were treated under nitrogen atmosphere and used as obtained.

Based on AlCl₃Is widely used for producing PAO. Variations in the molar ratio of reactants, the effect of changing substituents or solvents have been extensively studied. In the present invention, in the fixed monomerPAO with different viscosity is prepared by changing the temperature under the mol ratio of Al to the mixed solution. This is unique in itself, particularly for the preparation of low viscosity PAOs, as batches can be adjusted to produce, for example, high concentrations of PAO 4. Each batch will produce PAOs from dimer to pentamer, which can be separated by distillation.

Kinematic viscosity (sometimes also referred to as momentum diffusivity) is defined as the ratio of viscosity μ to fluid density ρ. Which is usually denoted by the Greek letter nu (nu) and dimensioned as (length)²Time/time.

A SVM 3000Stabinger viscometer was used to measure the dynamic viscosity and density of oils and fuels according to ASTM D7042-21. From the dynamic viscosity results/values, the SVM 3000 viscometer automatically calculates the kinematic viscosity and provides measurements equivalent to ISO 3104 or ASTM D445-19 a. The dynamic viscosity is a basic value for evaluating the lubrication behavior.

The viscosity index is a dimensionless number and is used to study the change in viscosity at different temperatures. The greater the Viscosity Index (VI), the less the change in fluid viscosity for a given change in temperature, and vice versa. The viscosity index is calculated from the kinematic viscosity at different temperature ranges.

In one aspect of the invention, a process for controlling the kinematic viscosity of a polyalphaolefin to less than 70 centistokes is disclosed, the process comprising the step of oligomerizing a C6 olefin monomer and a higher olefin monomer in the presence of an aluminum halide, a promoter, and optionally a solvent to obtain a polyalphaolefin; wherein the kinematic viscosity of the polyalphaolefin is controlled by adjusting the oligomerization temperature at a fixed monomer to aluminum halide molar ratio.

In one aspect of the invention, a process for controlling the kinematic viscosity of a polyalphaolefin in the range of 1 centistokes to 70 centistokes includes the step of oligomerizing a C6 olefin monomer and a higher olefin monomer in the presence of an aluminum halide, a promoter, and optionally a solvent to obtain a polyalphaolefin; wherein the kinematic viscosity of the polyalphaolefin is controlled by adjusting the oligomerization temperature at a fixed monomer to aluminum halide molar ratio.

According to a feature of the invention, the olefin monomer or monomers are selected from the group comprising 1-decene, 1-dodecene, 1-octene and any mixture thereof.

According to a feature of the invention, the molar ratio of olefin monomer or monomer to aluminum halide is from 10 to 500, more preferably from 10 to 350, and most preferably from 40 to 300.

According to one characteristic of the invention, the molar ratio of aluminium halide to promoter is between 1 and 10, preferably between 1 and 5.

According to a feature of the invention, the promoter is selected from the group/mixture consisting of water, alcohol, carboxylic acid, ester, ketone, ether, halogenated hydrocarbon, or any combination thereof.

According to one feature of the invention, the promoter is isobutanol.

According to one feature of the invention, the olefin monomer or monomers and solvent have a moisture content of less than 20 ppm.

According to a feature of the invention, the oligomerization temperature is in the range of 10 ℃ to 150 ℃.

According to a feature of the invention, the oligomerization temperature is 25 ℃ and 90 ℃.

According to a feature of the invention, the residence time during oligomerization is in the range of 0.5 hours to 8 hours.

According to a feature of the invention, the solvent is chosen from C5 to C19 alkanes.

According to a feature of the invention, the conversion of monomer to polyalphaolefin is greater than 95%.

According to one feature of the invention, the oligomerization comprises C20 to C24 dimers, C30 to C36 trimers, C40 to C48 tetramers, C50 to C60 pentamers, and C60+ heavies.

According to one characteristic of the invention, the kinematic viscosity decreases as the molar ratio of monomer to aluminium halide increases.

In another aspect of the invention, a process for preparing a polyalphaolefin is disclosed, the process comprising the steps of: a) oligomerizing one or more alpha olefin monomers having C6 to C14 carbon atoms in the presence of an aluminum halide, a promoter, and optionally a solvent under an inert atmosphere to obtain an oligomeric product in the reaction mass, wherein the aluminum halide is selected from the group consisting ofHas the formula R_3-nAlX_nWherein R is hydrocarbyl or alkyl, X is halide, and n ═ 0 to 3, wherein the halide is selected from chloride or bromide; b) stopping the oligomerization of the monomers in the reaction mass by adding water or alcohol; c) removing the aluminum halide from the reaction mass by water washing or filtration or adsorption or centrifugation or any combination thereof; d) separating unconverted monomers, promoters and oligomerization products from the reaction mass by distillation; e) hydrogenating the oligomerization product to saturate the oligomer to provide a polyalphaolefin, wherein the polyalphaolefin has a kinematic viscosity of less than 70 centistokes.

In another aspect of the invention, a process for preparing a polyalphaolefin is disclosed, the process comprising the steps of: a) oligomerizing a C6 olefin monomer and a higher olefin monomer under an inert atmosphere in the presence of an aluminum halide, a promoter, and optionally a solvent to obtain an oligomerization product in the reaction mass, wherein the aluminum halide is selected from those having the formula R_3-nAlX_nWherein R is hydrocarbyl or alkyl, X is halide, and n ═ 0 to 3, wherein the halide is selected from chloride or bromide; b) stopping the oligomerization of the monomers in the reaction mass by adding water or alcohol; c) removing the aluminum halide from the reaction mass by water washing or filtration or adsorption or centrifugation or any combination thereof; d) separating unconverted monomers, promoters and oligomerization products from the reaction mass by distillation; e) hydrogenating the oligomerization product to saturate the oligomer to provide a polyalphaolefin, wherein the polyalphaolefin has a kinematic viscosity of less than 70 centistokes.

In one feature of the invention, the hydrogenation is carried out using a metal catalyst and hydrogen.

In one feature of the invention, the conversion of monomer to oligomer is greater than 95%.

In another aspect of the invention, a process for preparing a polyalphaolefin is disclosed, the process comprising the steps of: a) oligomerizing C6 olefin monomers and higher olefin monomers under an inert atmosphere in the presence of an aluminum halide, a promoter, and optionally a solvent to obtain an oligomerization product, i.e., a polyalphaolefin, wherein the polyalphaolefin has a kinematic viscosity of less than 70 centistokes.

Table 1 shows the effect of temperature on the viscosity of PAO at a fixed monomer/Al ratio

Table 2 shows the effect of a fixed monomer/Al ratio during a runaway reaction

Example (b):

the invention is illustrated by the following non-limiting examples:

example 1:

in a 2L CSTR, 250ml of hexane, 13.6g of AlCl were added₃(0.10mol) and 4.0mL of isobutanol, and stirred for 15 minutes. The oligomerization temperature was set to 25 ℃. 1-decene (C10/AlCl) addition was started at a flow rate of 8.4 ml/min₃Molar ratio 83) for 3 hours. After the monomer addition was complete, the solution was stirred for an additional 1 hour. 100ml of deionized water was added to quench the reaction, followed by additional water washing. The subsequently obtained oil was kept over sodium sulfate overnight and filtered. After removal of the monomers, the oil was hydrogenated using nickel on a Kieselguhr catalyst. The hydrogenated oil had a KV of 45.6cSt @100 ℃ and a VI of 147.

Example 2:

the oligomerization procedure followed was the same as described in example 1, but instead the oligomerization temperature was set to 90 ℃. The hydrogenated oil had a KV of 23.5cSt @100 ℃ and a VI of 147.

Example 3:

the oligomerization procedure followed was the same as described in example 1, but alternatively, C10 was added/AlCl₃The molar ratio was maintained at 282. The hydrogenated oil had a KV of 12.1cSt @100 ℃, VI of 142.

Example 4:

the oligomerization procedure followed was the same as described in example 1, but alternatively C10/AlCl was used₃The molar ratio was maintained at 282 and the oligomerization temperature was set to 90 ℃. The hydrogenated oil had a KV of 4.5cSt @100 ℃, VI of 142.

Example 5:

the oligomerization procedure followed was the same as described in example 1, but alternatively C10/AlCl was used₃The molar ratio was maintained at 165. The hydrogenated oil had a KV of 23.4cSt @100 ℃, VI of 142.

Example 6:

the oligomerization procedure followed was the same as described in example 1, but alternatively C10/AlCl was used₃The molar ratio was maintained at 165 and the oligomerization temperature was set to 90 ℃. The hydrogenated oil had a KV of 5.8cSt @100 ℃, VI of 144.

Example 7:

the oligomerization procedure followed was the same as described in example 1, but alternatively C10/AlCl was used₃The molar ratio was kept at 100. The hydrogenated oil had a KV of 30.4cSt @100 ℃, VI of 142.

Example 8:

the oligomerization procedure followed was the same as described in example 1, but alternatively C10/AlCl was used₃The molar ratio was maintained at 100 and the oligomerization temperature was set to 90 ℃. The hydrogenated oil had a KV of 8.1cSt @100 ℃, VI of 141.

Example 9:

the oligomerization procedure followed was the same as described in example 1, but alternatively monomer/AlCl₃The molar ratio was kept at 48 and the monomer was 1-dodecene. The hydrogenated oil had a KV of 53.9cSt @100 ℃ and a VI of 147.

Example 10:

followingThe oligomerization step was the same as described in example 1, but alternatively the monomer/AlCl was used₃The molar ratio was maintained at 48 and the monomer was 1-dodecene, and the oligomerization temperature was set to 90 ℃. The hydrogenated oil had a KV of 25.4cSt @100 ℃, VI of 142.

The invention has the technical advantages that:

compared with the prior art, the invention has the following advantages:

using a fixed monomer/Al ratio, the viscosity of the resulting PAO can be controlled by varying the temperature.

In particular, useful advantages in the preparation of low viscosity PAOs, where any variation in the amount of catalyst does not lead to batch failures.

Addition of promoter to the feed controls the exotherm during oligomerization.