CN100448964C - A kind of continuously variable transmission transmission fluid composition - Google Patents
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Abstract
本发明提供一种无级变数器传动液组合物,以基础油的重量为100%计,包括:(1)双环己环类脂环烃基础油;(2)碱土金属盐清净剂,含量为0.05~3重%;(3)无灰分散剂,含量为1~15重%;(4)酚型或胺型抗氧剂,含量为0.01~1重%;(5)抗磨剂,含量为0.05~2重%;(6)摩擦改进剂,含量为0.05~3重%;(7)粘度指数改进剂,含量为0~20重%;(8)抗泡剂,含量为0~1000ppm。本发明提供的无级变速传动液组合物,具有优良的粘温性能和低温流动性,常温下具备较高的牵引系数,综合性能优良,完全能够满足CVT的使用要求。The invention provides a transmission fluid composition for a continuously variable variable speed changer, which comprises: (1) a dicyclohexyl cycloaliphatic base oil; (2) an alkaline earth metal salt detergent with a content of 0.05 to 3% by weight; (3) Ashless dispersant, the content is 1 to 15% by weight; (4) Phenolic or amine antioxidant, the content is 0.01 to 1% by weight; (5) Anti-wear agent, the content is 0.05-2% by weight; (6) Friction modifier, the content is 0.05-3% by weight; (7) Viscosity index improver, the content is 0-20% by weight; (8) Antifoaming agent, the content is 0-1000ppm. The continuously variable transmission fluid composition provided by the invention has excellent viscosity-temperature performance and low-temperature fluidity, high traction coefficient at normal temperature, excellent comprehensive performance, and can fully meet the requirements for use of CVT.
Description
技术领域 technical field
本发明涉及一种润滑油组合物,具体而言,本发明涉及的是一种高粘度指数、高牵引系数的性能优良的CVT专用传动液组合物。The invention relates to a lubricating oil composition, in particular to a CVT special-purpose transmission fluid composition with high viscosity index and high traction coefficient and excellent performance.
技术背景technical background
近年来,提高燃料经济性,减少排放,改进操纵灵活性成为汽车研制的发展趋势,而车用无级变速器(简称CVT)技术就是其中最有前景的一种。车用CVT常见类型有:带式CVT(Belt/Chain-CVT,B-CVT)和环型CVT(Torodial-CVT,T-CVT)。CVT技术在燃料经济性、超车加速性、乘坐舒适性、成本等方面优势显著。因此汽车自动变速器越来越多的采用CVT设计。In recent years, improving fuel economy, reducing emissions, and improving handling flexibility have become the development trend of automobile development, and the technology of continuously variable transmission (CVT for short) is one of the most promising. Common types of CVT for vehicles are: Belt CVT (Belt/Chain-CVT, B-CVT) and Ring CVT (Torodial-CVT, T-CVT). CVT technology has significant advantages in terms of fuel economy, overtaking acceleration, ride comfort, and cost. Therefore, more and more automatic transmissions of automobiles adopt CVT design.
CVT动力的传递实际上是依靠弹性流体动力润滑(EHL)接触区内油膜的剪切力完成的,因此,机械无级变速器性能的优劣在很大程度上取决于牵引液(CVTF)的牵引性能。CVTF是一种多功能的牵引传动液。在无级变速器传力元件接触区内,润滑油膜承受高压、高剪切应变率,同时还由于受到剪切而发热,因而对油品有许多特殊要求。CVTF除普通润滑油所具有的润滑高低温粘度要求、氧化稳定性能、分散性、抗泡性、材料相容性外,还对剪切稳定性能、抗磨损性能有严格的要求,特别是对牵引系数和抗粘滑性能很高的要求。而这些性能之间是相互矛盾,如牵引系数和低温粘度,高低温粘度和剪切稳定性,牵引系数和抗磨损性能等。The transmission of CVT power actually depends on the shearing force of the oil film in the contact area of elastohydrodynamic lubrication (EHL). Therefore, the performance of mechanical continuously variable transmission depends to a large extent on the traction of traction fluid (CVTF). performance. CVTF is a versatile traction transmission fluid. In the contact area of the force transmission element of the continuously variable transmission, the lubricating oil film bears high pressure, high shear strain rate, and heat due to shearing, so there are many special requirements for the oil. In addition to the lubricating high and low temperature viscosity requirements, oxidation stability, dispersibility, anti-foaming properties, and material compatibility of ordinary lubricating oils, CVTF also has strict requirements on shear stability and wear resistance, especially for traction coefficient and anti-stick-slip properties are very high requirements. These properties are contradictory, such as traction coefficient and low temperature viscosity, high and low temperature viscosity and shear stability, traction coefficient and wear resistance, etc.
合成型传动液就其分子结构而言可大致分为:(1)多环脂环族类型(多六元环);(2)合成聚烯烃型(高枝化度);(3)矿物油型;(4)酯类、醚类(分子结构中含多个六元环);(5)硅油型等。其中,多环己基脂环族类牵引液的牵引性能良好,特别是高温牵引系数较高,所以获得了广泛的使用。US 5043497公开了双(3,4,6-三甲基环己基)甲烷传动液的合成。US 3975278公开了2-甲基-2,4-二环己基戊烷传动液的合成。此外日本围绕此类分子结构也提出了大量的发明专利,如JP2001294880,JP11349968等,其中公开的传动液有共同的结构通式:不同处在环己环间的亚甲基个数的差异、以及亚甲基之间的联接方式的不同;此外,环己环上短链烷基R1、R2的类型、数量也各不相同。Synthetic transmission fluids can be roughly divided into the following molecular structures: (1) Polycyclic alicyclic type (multiple six-membered ring); (2) Synthetic polyolefin type (high degree of branching); (3) Mineral oil type ; (4) Esters, ethers (containing multiple six-membered rings in the molecular structure); (5) Silicone oil type, etc. Among them, polycyclohexyl cycloaliphatic traction fluid has good traction performance, especially high-temperature traction coefficient, so it has been widely used. US 5043497 discloses the synthesis of bis(3,4,6-trimethylcyclohexyl)methane transmission fluid. US 3975278 discloses the synthesis of 2-methyl-2,4-dicyclohexylpentane transmission fluid. In addition, Japan has also proposed a large number of invention patents around this type of molecular structure, such as JP2001294880, JP11349968, etc., wherein the disclosed transmission fluid has a common structural formula: The difference in the number of methylene groups between different cyclohexyl rings, and the difference in the connection mode between methylene groups; in addition, the types and quantities of short-chain alkyl groups R 1 and R 2 on the cyclohexyl rings are also different. same.
除了对基础油的研究及新型基础油的合成之外,人们对CVTF配方也进行了大量的研究。特许公开2000-63878,特许公开2000-1687,特许公开平11-293272,特许公开平11-181464,特许公开平9-263782,US 6809069,US 6746993,US6465399,US 6337309,US 6329327,US 6225266等专利给出了添加了粘度指数改进剂、清净剂、分散剂、摩擦改进剂等多种添加剂的以矿油为基础油的CVTF配方,这些CVTF具有较高的牵引系数,室温下的牵引系数最高达到0.07左右,可用于B-CVT,但是其牵引系数难于满足T-CVT的使用要求。JP2000239682,JP62001115178,JP2001019988,JP2000169866等专利给出了以1-环己基-1,3,3-三甲基二氢茚满、2,4-二环己基-2-甲基-戊烷等氢化二聚甲基苯乙烯合成油为基础油的CVTF配方,这些CVTF具有比矿油型CVTF更高的牵引系数,室温下的牵引系数最高达到0.12左右,能够满足T-CVT的使用要求。较为成功的商用传动液也多为多环己环类脂环烃,如Santotrac系列产品等。这些牵引液一般都具有较好的牵引系数,但它们的低温流动性能、及工作条件下的粘度各不相同,有的无法满足无级变数器的特殊要求。特别是在牵引系数与低温流动性之间存在着矛盾,高牵引系数往往伴随着高粘度、高倾点的同时出现。In addition to the research on base oils and the synthesis of new base oils, people have also done a lot of research on CVTF formulations. Patent Publication 2000-63878, Patent Publication 2000-1687, Patent Publication 11-293272, Patent Publication 11-181464, Patent Publication 9-263782, US 6809069, US 6746993, US6465399, US 6337309, US 6329327, US 6225266, etc. The patent provides CVTF formulations based on mineral oil with various additives such as viscosity index improvers, detergents, dispersants, and friction modifiers. These CVTFs have high traction coefficients, and the traction coefficients at room temperature are the highest Reaching about 0.07, it can be used in B-CVT, but its traction coefficient is difficult to meet the requirements of T-CVT. Patents such as JP2000239682, JP62001115178, JP2001019988, and JP2000169866 have provided hydrogenated dihydroindanes such as 1-cyclohexyl-1,3,3-trimethyldihydroindan, 2,4-dicyclohexyl-2-methyl-pentane, etc. CVTF formulations based on polymethylstyrene synthetic oil, these CVTFs have a higher traction coefficient than mineral oil-based CVTFs, and the maximum traction coefficient at room temperature can reach about 0.12, which can meet the requirements of T-CVT. More successful commercial transmission fluids are mostly polycyclohexyl cycloaliphatic hydrocarbons, such as Santotrac series products. These traction fluids generally have good traction coefficients, but their low-temperature flow properties and viscosities under working conditions vary, and some of them cannot meet the special requirements of continuously variable variables. In particular, there is a contradiction between traction coefficient and low-temperature fluidity, and high traction coefficient is often accompanied by high viscosity and high pour point.
发明内容 Contents of the invention
本发明提供了具备高的粘度指数、高的牵引系数、良好的低温流动性、正常的粘度特性的无级变数器传动液组合物。The invention provides a continuously variable variable transmission fluid composition with high viscosity index, high traction coefficient, good low-temperature fluidity and normal viscosity characteristics.
本发明提供的无级变数器传动液组合物,以基础油的重量为100%计,包括:The continuously variable variable transmission fluid composition provided by the present invention, based on the weight of the base oil as 100%, comprises:
(1)双环己环类脂环烃基础油;(1) Bicyclohexyl cycloaliphatic base oil;
(2)碱土金属盐清净剂,含量为0.05~3重%;(2) alkaline earth metal salt detergent, the content of which is 0.05 to 3% by weight;
(3)无灰分散剂,含量为1~15重%;(3) Ashless dispersant, the content is 1-15% by weight;
(4)酚型或胺型抗氧剂,含量为0.01~1重%;(4) phenolic or amine antioxidants, the content of which is 0.01 to 1% by weight;
(5)抗磨剂,含量为0.05~2重%;(5) anti-wear agent, the content is 0.05-2% by weight;
(6)摩擦改进剂,含量为0.05~3重%;(6) Friction modifier, the content of which is 0.05 to 3% by weight;
(7)粘度指数改进剂,含量为0~20重%;(7) Viscosity index improver, the content is 0~20% by weight;
(8)抗泡剂,含量为0~1000ppm。(8) Anti-foaming agent, the content is 0-1000ppm.
碱土金属盐清净剂为碱土金属的磺酸盐、硫化烷基酚盐和烷基水杨酸盐中的一种或几种。其中的碱土金属为钙、镁或钡。碱土金属盐的碱值可以是高碱值(>300TBN)、中碱值(100~300TBN)及低碱值(<100TBN)。优选的碱土金属盐清净剂是中碱值硫化烷基酚钙和高碱值硫化烷基酚钙。清净剂的含量为0.05~3重%,最好在0.5~2重%。The alkaline earth metal salt detergent is one or more of alkaline earth metal sulfonate, sulfurized alkylphenate and alkyl salicylate. The alkaline earth metals are calcium, magnesium or barium. The base number of the alkaline earth metal salt can be high base number (>300TBN), medium base number (100-300TBN) and low base number (<100TBN). Preferred alkaline earth metal salt detergents are medium base number sulfurized calcium alkylphenates and high base number sulfurized calcium alkylphenates. The content of the detergent is 0.05-3% by weight, preferably 0.5-2% by weight.
无灰分散剂为丁二酰亚胺分散剂、丁二酸酯分散剂、油溶性含磷或含硼的无灰分散剂中的一种或几种。优选的是硼化无灰分散剂及丁二酰亚胺分散剂。无灰分散剂的含量为1~15重%,最好在3~6重%。The ashless dispersant is one or more of succinimide dispersant, succinate dispersant, oil-soluble phosphorus-containing or boron-containing ashless dispersant. Preferred are boronated ashless dispersants and succinimide dispersants. The content of the ashless dispersant is 1-15% by weight, preferably 3-6% by weight.
抗氧剂为酚型或胺型抗氧剂中的一种或几种,优选的是胺型抗氧剂。抗氧剂的含量为0.01~1重%,最好在0.1~0.8重%。The antioxidant is one or more of phenolic or amine antioxidants, preferably amine antioxidants. The content of antioxidant is 0.01-1% by weight, preferably 0.1-0.8% by weight.
抗磨剂为烷基二硫代磷酸锌、二苄基二硫化物、硫化异丁烯、磷酸三甲酚酯、硼化油酰胺中的一种或几种。优选的是二苄基二硫化物及烷基二硫代磷酸锌。抗磨剂的含量为0.05~2重%,最好在0.1~1重%。The antiwear agent is one or more of zinc alkyl dithiophosphate, dibenzyl disulfide, isobutylene sulfide, tricresyl phosphate, and borated oleamide. Preferred are dibenzyl disulfide and zinc alkyl dithiophosphates. The content of the antiwear agent is 0.05-2% by weight, preferably 0.1-1% by weight.
摩擦改进剂为苯三唑脂肪酸铵盐(T406)、油酸乙二醇酯(T403)、硫化烯烃棉籽油(T405)、磷酸三辛酯、油酸、月桂酰胺二乙醇胺、羟乙基十七烷基咪唑啉、乙氧基化牛酯二胺中的一种或几种。优选的是苯三唑脂肪酸铵盐(T406),或羟乙基十七烷基咪唑啉与乙氧基化牛脂二胺的组合,组合中,两者的比例为1∶1~5∶1,优选1∶1~3∶1。摩擦改进剂的含量为0.05~3重%,最好在0.1~1重%。Friction modifiers are benzotriazole fatty acid ammonium salt (T406), ethylene glycol oleate (T403), sulfurized olefin cottonseed oil (T405), trioctyl phosphate, oleic acid, lauramide diethanolamine, hydroxyethyl seventeen One or more of alkyl imidazoline and ethoxylated tallow diamine. Preferred is benzotriazole fatty acid ammonium salt (T406), or the combination of hydroxyethyl heptadecyl imidazoline and ethoxylated tallow diamine, in the combination, the ratio of the two is 1:1~5:1, Preferably 1:1 to 3:1. The content of the friction modifier is 0.05-3% by weight, preferably 0.1-1% by weight.
粘度指数改进剂为聚甲基丙烯酸酯、乙丙共聚物、聚乙烯基正丁醚、聚异丁烯、苯乙烯马来酸酯中的一种或几种。最好使用分子量在10000~100000的范围内的聚甲基丙烯酸酯。粘度指数改进剂的含量可以为0~20重%,优选1~20重%,最好是1~10重%。The viscosity index improver is one or more of polymethacrylate, ethylene-propylene copolymer, polyvinyl n-butyl ether, polyisobutylene, and styrene maleate. It is preferable to use polymethacrylate having a molecular weight in the range of 10,000 to 100,000. The content of the viscosity index improver can be 0-20% by weight, preferably 1-20% by weight, most preferably 1-10% by weight.
抗泡剂为甲基硅油、乙基硅油、丙烯酸脂与醚共聚物(T911、T912)的一种或几种。优选的是T912,含量可以为0~1000ppm,优选50~1000ppm,最好是100~500ppm。The antifoaming agent is one or more of methyl silicone oil, ethyl silicone oil, acrylate and ether copolymer (T911, T912). T912 is preferred, the content can be 0-1000ppm, preferably 50-1000ppm, most preferably 100-500ppm.
所说的基础油为双环己环类脂环烃,优选的的是一种新型结构双环己环类脂环烃,它的2个环己基由1个亚甲基联接,且每个环己环上均有1~3个含有偕位二甲基结构的短链烷基取代基团,如异丙基、叔丁基、异戊基等。其结构式为:Said base oil is dicyclohexyl cycloaliphatic cyclohydrocarbon, preferably a novel structure bicyclohexyl cycloaliphatic cyclohydrocarbon, its 2 cyclohexyls are connected by 1 methylene, and each cyclohexyl cyclohexyl There are 1 to 3 short-chain alkyl substituent groups containing a geminal dimethyl structure, such as isopropyl, tert-butyl, isopentyl, etc. Its structural formula is:
其中R为含有偕位二甲基结构的C3~C5短链烷基,n为1~3的正整数。Wherein R is a C3-C5 short-chain alkyl group containing a geminal dimethyl structure, and n is a positive integer of 1-3.
所说的双环己环类脂环烃的制备可分为两步:即芳香中间体的合成和芳香中间体的氢化饱和。The preparation of said bicyclohexylcycloalicyclic hydrocarbon can be divided into two steps: the synthesis of the aromatic intermediate and the hydrogenation saturation of the aromatic intermediate.
(1)芳香中间体的合成(1) Synthesis of aromatic intermediates
以含有偕位二甲基结构的C1~C3烷基苯、甲醛为原料,在酸性催化剂的作用下,经缩合反应生成二芳基甲烷型芳香中间体。Using C1-C3 alkylbenzenes and formaldehyde containing geminal dimethyl structures as raw materials, under the action of acidic catalysts, diarylmethane-type aromatic intermediates are produced through condensation reactions.
催化剂可选用浓硫酸,磺酸或杂多酸,优选浓硫酸。甲醛原料可选用多聚甲醛或甲醛水溶液,优选37%的甲醛水溶液。反应温度可以是106~130℃。The catalyst can be selected concentrated sulfuric acid, sulfonic acid or heteropoly acid, preferably concentrated sulfuric acid. The formaldehyde raw material can be selected paraformaldehyde or formaldehyde aqueous solution, preferably 37% formaldehyde aqueous solution. The reaction temperature may be 106-130°C.
二芳基甲烷型芳香中间体通式如下: The general formula of diarylmethane-type aromatic intermediates is as follows:
由于烷基的不同取代位造成多个异构体同时存在,故芳香中间体实为混合物,但混合物对最终产品的性能无太大影响。Since multiple isomers exist at the same time due to the different substitution positions of the alkyl group, the aromatic intermediate is actually a mixture, but the mixture has little effect on the performance of the final product.
(2)芳香中间体的氢化饱和(2) Hydrogenation saturation of aromatic intermediates
将芳香中间体与加氢催化剂混合,置于高压釜内,于温度150~200℃,氢压5.0~10.0MPa的条件下,进行加氢饱和。产物经减压拔头后得最终产品。所说加氢催化剂可以是下列三大类:1)第VIII族金属(Fe、Co、Ni、Ru、Rh、Pd、Os、Ir、Pt)以及由合金制成的骨架催化剂或非晶合金催化剂;2)金属氧化物(MgO、ZnO、Cr2O3、Fe2O3等);3)复合氧化物或硫化物。上述物质,特别是金属本身,除骨架型催化剂外,最好分散在活性炭、分子筛等多孔性载体上,以增强活性。The aromatic intermediate is mixed with a hydrogenation catalyst, placed in an autoclave, and subjected to hydrogenation saturation at a temperature of 150-200° C. and a hydrogen pressure of 5.0-10.0 MPa. The final product is obtained after the product is decompressed and decapitated. Said hydrogenation catalyst can be the following three categories: 1) Group VIII metals (Fe, Co, Ni, Ru, Rh, Pd, Os, Ir, Pt) and skeleton catalysts or amorphous alloy catalysts made of alloys ; 2) metal oxides (MgO, ZnO, Cr 2 O 3 , Fe 2 O 3 , etc.); 3) composite oxides or sulfides. The above substances, especially the metal itself, except for the skeleton catalyst, are preferably dispersed on porous supports such as activated carbon and molecular sieves to enhance the activity.
以双(异丙苯基)甲烷为例说明芳香中间体经加氢后的产品构成。其最终产品的组成为双(异丙基环己基)甲烷。其中主要含有以下两种异构体:Taking bis(cumyl)methane as an example to illustrate the product composition of aromatic intermediates after hydrogenation. The composition of its final product is bis(isopropylcyclohexyl)methane. It mainly contains the following two isomers:
双(4-异丙基环己基)甲烷 Bis(4-isopropylcyclohexyl)methane
双(3-异丙基环己基)甲烷 Bis(3-isopropylcyclohexyl)methane
由于空间位阻的关系,前者的含量较高。分离上述混合物是困难的,同时对于本发明而言也是没有意义的。Due to the relationship of steric hindrance, the content of the former is higher. Separation of the above-mentioned mixture is difficult and at the same time meaningless for the present invention.
本发明提供的无级变速传动液组合物,具有优良的粘温性能和低温流动性,常温下具备较高的牵引系数,综合性能优良,完全能够满足CVT的使用要求。The continuously variable transmission fluid composition provided by the invention has excellent viscosity-temperature performance and low-temperature fluidity, high traction coefficient at normal temperature, excellent comprehensive performance, and can fully meet the requirements for use of CVT.
具体实施方式 Detailed ways
(1)牵引系数的测定(1) Determination of traction coefficient
牵引曲线的测定使用英国PCS Instruments公司生产的Mini Traction Machine(MTM)仪器,其几何接触型式为球-盘型。试验条件及试件参数见表1、表2。The measurement of the traction curve uses the Mini Traction Machine (MTM) instrument produced by British PCS Instruments, and its geometric contact type is ball-disk type. The test conditions and specimen parameters are shown in Table 1 and Table 2.
表1牵引性能试验条件Table 1 Traction performance test conditions
表2试件参数Table 2 Test piece parameters
(2)实施例(2) Example
在以下各表的实施例及比较例中列出了在实施本发明时适合使用的组合物,实施例及比较例采用了相同的添加剂组合,其中的百分数都以重量表示,以基础油的重量为100%。The compositions suitable for use when implementing the present invention are listed in the Examples and Comparative Examples of the following tables. The Examples and Comparative Examples have adopted the same combination of additives, and the percentages therein are expressed by weight, based on the weight of the base oil is 100%.
基础油I:双(4-异丙基环己基)甲烷,按照实施例1的方法制备。Base oil I: Bis(4-isopropylcyclohexyl)methane, prepared according to the method of Example 1.
基础油II:双(4-叔丁基环己基)甲烷,按照实施例2的方法制备。Base oil II: Bis(4-tert-butylcyclohexyl)methane, prepared according to the method in Example 2.
基础油III:双(3,4,6-三甲基环己基)甲烷,根据US 5043497合成。Base oil III: bis(3,4,6-trimethylcyclohexyl)methane, synthesized according to US 5043497.
基础油IV:2-甲基-2,4-二环己基戊烷,根据US 3975278合成。Base oil IV: 2-methyl-2,4-dicyclohexylpentane, synthesized according to US 3975278.
实施例1Example 1
取异丙苯(纯度99w%)240克,甲醛(37%水溶液)47.8克,硫酸(浓度98w%)58.2克为原料。其中异丙苯、硫酸混置于四颈瓶中搅拌,由室温升温至120℃。在达到设定温度后,将置于滴加漏斗中的甲醛水溶液,缓慢的滴加入四颈瓶。甲醛滴加完毕,保温反应约1小时后,出料入分液漏斗,用80℃左右的蒸馏水、正丁醇混合液(水∶醇体积比约为4∶1)萃取洗涤至PH=7,切出上层油相产品。油相产品汇集后,先在残压为24~40mmHg条件下蒸出未反应的原料异丙苯后,再在残压小于1mmHg的条件下,取176~186℃的减压馏份为目标中间体产物。Get cumene (purity 99w%) 240 grams, formaldehyde (37% aqueous solution) 47.8 grams, sulfuric acid (concentration 98w%) 58.2 grams are raw materials. Among them, cumene and sulfuric acid were mixed and stirred in a four-necked bottle, and the temperature was raised from room temperature to 120°C. After reaching the set temperature, the formaldehyde solution placed in the dropping funnel was slowly dropped into the four-necked bottle. After the dropwise addition of formaldehyde is completed, after the heat preservation reaction for about 1 hour, the material is discharged into a separatory funnel, extracted and washed with distilled water and n-butanol mixture (water:alcohol volume ratio is about 4:1) at about 80°C until pH = 7, Cut out the upper oil phase product. After the oil phase products are collected, the unreacted raw material cumene is first distilled under the condition of residual pressure of 24-40mmHg, and then under the condition of residual pressure of less than 1mmHg, the decompression distillate at 176-186°C is taken as the target intermediate body product.
将上述中间体——双(异丙苯基)甲烷139.6克,与10%Pd/C催化剂6.5克混合置于高压釜内。于温度190℃,氢压7.0MPa,搅拌速度250RPM的条件下,进行加氢饱和。产物经减压拔头后得最终产品126.2克,1H-NMR测定加氢饱和度为98.6%。13C-NMR分子结构鉴定表明,双(4-异丙基环己基)甲烷为其主要成份。Mix 139.6 grams of the above-mentioned intermediate, bis(isopropylphenyl)methane, with 6.5 grams of 10% Pd/C catalyst and place in an autoclave. Under the conditions of temperature 190° C., hydrogen pressure 7.0 MPa, and stirring speed 250 RPM, hydrogenation saturation was carried out. The product was decapitated under reduced pressure to obtain 126.2 g of the final product, and the degree of hydrogenation saturation was 98.6% as determined by 1 H-NMR. 13 C-NMR molecular structure identification shows that bis(4-isopropylcyclohexyl)methane is its main component.
实施例2Example 2
合成过程同实施例1,只是原料换为叔丁基苯268克,甲醛与浓硫酸的质量不变。120℃下进行缩合反应,并进行萃取分离及减压蒸馏,共得到中间体——双(叔丁苯基)甲烷产品125.5克。将它与10%Pd/C催化剂6.7克混合置于高压釜内。于温度190℃,氢压7.0MPa,搅拌速度250RPM的条件下,进行加氢饱和。产物经减压拔头后得最终产品115.3克,1H-NMR测定加氢饱和度为97.3%。13C-NMR分子结构鉴定表明,双(4-叔丁基环己基)甲烷为其主要成份。The synthesis process is the same as in Example 1, except that the raw material is changed to 268 grams of tert-butylbenzene, and the quality of formaldehyde and concentrated sulfuric acid remains unchanged. Condensation reaction was carried out at 120°C, followed by extraction, separation and vacuum distillation to obtain 125.5 grams of the intermediate bis(tert-butylphenyl)methane product. It was mixed with 6.7 g of 10% Pd/C catalyst and placed in an autoclave. Under the conditions of temperature 190° C., hydrogen pressure 7.0 MPa, and stirring speed 250 RPM, hydrogenation saturation was carried out. The product was decapitated under reduced pressure to obtain 115.3 g of the final product, and the degree of hydrogenation saturation was 97.3% as determined by 1 H-NMR. 13 C-NMR molecular structure identification shows that bis(4-tert-butylcyclohexyl)methane is its main component.
表3实施例及比较例的组合物The composition of table 3 embodiment and comparative example
表3实施例及比较例的组合物续The composition of table 3 embodiment and comparative example continues
表3实施例及比较例的组合物续The composition of table 3 embodiment and comparative example continues
表3实施例及比较例的组合物续The composition of table 3 embodiment and comparative example continues
表3实施例及比较例的组合物续The composition of table 3 embodiment and comparative example continues
对上述实施例及比较例的组合物进行性能测试,结果见表4The composition of above-mentioned embodiment and comparative example is carried out performance test, and the results are shown in Table 4
表4实施例及比较例数据对比表Table 4 embodiment and comparative example data comparison table
注:PHz为平均赫兹接触压力。Note: P Hz is the average hertz contact pressure.
通过表4可以看出,本发明提供的无级变速传动液组合物,具有比比较例高得多的粘度指数,更低的倾点,显示出优良的粘温性能及更好的低温流动性,常温下具备较高的牵引系数,虽然略低于比较例,但是完全能够满足CVT的使用要求。本发明提供的无级变速传动液组合物综合性能优于比较例。As can be seen from Table 4, the continuously variable transmission fluid composition provided by the present invention has a much higher viscosity index and lower pour point than the comparative examples, and shows excellent viscosity-temperature performance and better low-temperature fluidity , has a relatively high traction coefficient at room temperature, although it is slightly lower than that of the comparative example, it can fully meet the requirements of CVT use. The comprehensive performance of the continuously variable transmission fluid composition provided by the present invention is better than that of the comparative example.
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