Method for catalytically synthesizing diisooctyl dodecanedioate base oil by solid superacid

A technology of diisooctyl dodecanedioate and solid super acid, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc.

Inactive Publication Date: 2013-09-04
NANTONG ZHONGCHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Nowadays, the technical process and market strategy of ester synthetic oil are relatively mature, and the application fields have been expanded to precision instrument oil, synthetic compressor oil, automobile engine oil, marine engine oil, hydraulic oil, gear oil, metal processing oil and synthetic lubrication In addition, this type of synthetic ester can also be used as a stationary liquid for gas chromatography, an organic synthesis intermediate, and a plastic toughener and low-temperature plasticizer. Most of the ester synthetic base oils currently used in the market are composed of less than ten carbons Esters synthesized from dibasic acids, but ester base oils synthesized from dibasic acids with more than ten carbons are rare

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  • Method for catalytically synthesizing diisooctyl dodecanedioate base oil by solid superacid

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specific Embodiment approach

[0018] like figure 1 Show a kind of embodiment of the present invention with solid superacid catalyzed synthesis of di-isooctyl dodecanedioate base oil, comprising the following steps:

[0019] A. Preparation of solid superacid SO by precipitation and impregnation method 4 2- / ZrO 2 -TiO 2 Catalyst: Mix soluble titanium salt and soluble zirconium salt according to the molar ratio (1-10): 1, add the precipitant dropwise until the pH of the mixture reaches 5-14, wash the precipitate with water to neutral, dry and grind into powder, immersed in sulfuric acid or sulfate solution for 0.5-24 h, filtered and dried, and then calcined at 50-700 °C for 0.5-24 h, and finally the solid superacid SO 4 2- / ZrO 2 -TiO 2 catalyst;

[0020] B. Synthesis of base oil: using solid super acid SO 4 2- / ZrO 2 -TiO 2 As a catalyst, mix dodecanedioic acid and isooctyl alcohol in a molar ratio of 1: (1-10), catalyze the reaction at 50-200 °C for 0.5-16 h, vacuum filter out the catalyst, an...

Embodiment 1

[0022] Example 1: Add 4.7837g 99% zirconium oxychloride and 16.2353 g 98% titanium tetrachloride in a 500ml three-necked flask, shake until completely dissolved, add 25% ammonia water dropwise until the pH reaches 8-10, and obtain white Precipitate, wash the precipitate with water until neutral, dry and grind into powder, and then in 0.5 mol / L H 2 SO 4 The solid superacid SO 4 2- / ZrO 2 -TiO 2 Catalyst, seal the catalyst and place it in a desiccator for later use. Add 108.9753 g of 99% dodecanedioic acid, 199.3317 g of 98% isooctyl alcohol and 1.65 g of solid superacid catalyst to a 500 ml three-necked flask in turn, add 26.5 ml of distilled water to the water separator, and react the reaction solution at 140 °C After 7 hours, the catalyst was vacuum filtered after cooling, and the filtrate was the crude product; after the crude product was distilled under reduced pressure at 30-300 °C, a high-purity di-isooctyl dodecanedioate product was obtained. After testing, the puri...

Embodiment 2

[0023] Example 2: Add 4.8627g 99% zirconium oxychloride and 30.3318 g 98% butyl titanate to a 500ml three-neck flask, shake until completely dissolved, add 28% ammonia water dropwise until the pH reaches 8-10, and obtain white Precipitate, wash the precipitate with water to neutral, dry and grind into powder, and then in 0.4 mol / L H 2 SO 4 Immersed in the solution for 6 h, dried by suction filtration, and roasted in a muffle furnace at 550 °C for 4 h to obtain the solid superacid SO 4 2- / ZrO 2 -TiO 2 Catalyst, seal the catalyst and place it in a desiccator for later use. Add 116.3132 g of 99% dodecanedioic acid, 205.5325 g of 98% isooctyl alcohol and 2 g of solid superacid catalyst to a 500 ml three-neck flask in turn, add 26.5 ml of distilled water to the water separator, and react the reaction solution at 170 °C After 5 hours, the catalyst was vacuum filtered after cooling, and the filtrate was the crude product; after the crude product was distilled under reduced pres...

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Abstract

The invention discloses a method for obtaining high-purity diisooctyl dodecanedioate base oil by synthesizing solid superacid SO4<2-> / ZrO2-TiO2 catalyst with a precipitation-impregnation method, catalytically synthesizing diisooctyl dodecanedioate by dodecanedioic acid and isooctanol, and subjecting to separation and purification. The synthesized catalyst has the advantages of high activity, easiness in separation, capacity of recycling, good stability, high product yield and the like. The synthesized ester base oil has the advantages of high viscosity index and open cup flash point, low pour point and toxicity, good low temperature fluidity, wider operating temperature range, and excellent lubrication, environmental protection and biodegradation properties.

Description

technical field [0001] The invention relates to a method for synthesizing base oil in the field of organic chemical industry, in particular to a method for catalyzing and synthesizing diisooctyl dodecanedioate base oil with solid superacid. Background technique [0002] The technical requirements for lubricating base oils in the 21st century mainly include good thermal oxidation stability, low volatility, high viscosity index, low sulfur / sulfur-free, low viscosity and environmental friendliness. Synthetic base oils have significant advantages over mineral oils in terms of evaporation loss, pour point, viscosity index and stability to thermal oxidation, and their viscoelasticity under pressure is also superior to mineral oils. Due to the relatively expensive price of synthetic base oils, its use is limited to lubricating oils with demanding performance requirements. [0003] In the 1970s, various ester synthetic oils developed rapidly and were widely used in jet engine lubri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/34C07C67/08C10M105/36B01J27/053
Inventor 赵彦保徐吉上龚悦姚明忠
Owner NANTONG ZHONGCHENG BIOTECH
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