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Method for preparing pentaerythrite oleic ester used in cold-rolling oil

A technology of pentaerythritol oleate and pentaerythritol, which is applied in the field of preparation of pentaerythritol oleate, can solve the problems of slow reaction speed, low esterification rate, complicated process, etc., achieve fast reaction speed, improve overall performance, and good color Effect

Inactive Publication Date: 2011-05-11
LUOYANG XINZHONG PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the introduction of a basic catalyst, this method has complex processes, slow reaction speed and low esterification rate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 100 grams of pentaerythritol, 780 grams of oleic acid, and 176 grams of toluene solvent in the esterification reaction kettle, stir and heat up, and feed high-purity nitrogen, add 3.52 grams of p-toluenesulfonic acid at 60 ° C, continue to heat up, at 160 °C for 4.5 hours. After the reaction was completed, turn off the nitrogen gas, and vacuumize for 50 minutes under a vacuum condition of 50 Pa under heat preservation conditions. Cool to below 120°C and filter with a plate and frame filter to obtain pentaerythritol oleate with an acid value of 0.16 mgKOH / g and a yield of 94.3%.

Embodiment 2

[0021] Add 101 grams of pentaerythritol, 800 grams of oleic acid, and 270 grams of toluene solvent into the esterification reaction kettle, stir and heat up, and feed high-purity nitrogen, and add 2.25 grams of p-toluenesulfonic acid and 2.25 grams of tributyl phosphate at 60°C For ester, continue to heat up, and react at a temperature of 140° C. for 4 hours. After the completion of the reaction, turn off the nitrogen gas, and vacuumize for 60 minutes under a vacuum condition of 40 Pa under the condition of heat preservation. Cool to below 120°C and filter with a plate and frame filter to obtain pentaerythritol oleate with an acid value of 0.14 mgKOH / g and a yield of 94.2%.

Embodiment 3

[0023] Add 100 grams of pentaerythritol, 820 grams of oleic acid, and 350 grams of benzene solvent in the esterification reaction kettle, stir and heat up, and feed high-purity nitrogen, add 5.5 grams of tributyl phosphate at 60 ° C, continue to heat up, at 150 React for 6 hours under the temperature condition of -175°C. After completion of the reaction, turn off the nitrogen gas, and vacuumize for 40 minutes under a vacuum condition of 60 Pa under heat preservation conditions. Cool to below 120°C and filter with a plate and frame filter to obtain pentaerythritol oleate with an acid value of 0.18 mgKOH / g and a yield of 94.6%.

[0024] With embodiment 1, embodiment 2, embodiment 3 as composition of the present invention, as the purpose reference material of contrast is the pentaerythritol oleate sold on the market at present, and its acid value is greater than 3mgKOH / g, and appearance is brown. In the table is reference substance A.

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Abstract

A method for preparing pentaerythrite oleic ester used in cold-rolling oil belongs to the technical field of ester compound synthesis in organic chemistry. Pentaerythrite and oleinic acid are adopted as raw materials and p-toluenesulfonic acid or / and tributyl phosphate is / are adopted as catalyst; toluene or benzol is adopted as a water carrier, and esterification reaction lasting 4 to 6 hours is performed under the protection of high-purity nitrogen and under the temperature of 140 to 180 DEG C; after the reaction, continuous vacuumization lasting 40 to 60 mins is performed under the high-vacuum condition with a vacuity of 40 to 60Pa; and pentaerythrite oleic ester is obtained after the filtration of remains after vacuumizing. The pentaerythrite oleic ester prepared by adopting the method provided by the invention is specially used in cold-rolling oil, and has the advantages of excellent lubricity, temperature characteristics, annealing detergency and excellent mill housing cleanness.

Description

technical field [0001] The invention relates to a preparation method of pentaerythritol oleate used in cold-rolling rolling oil, and belongs to the technical field of synthesis of ester compounds in organic chemistry. Background technique [0002] In the cold rolling process of steel plates, the rolling oil is required to have a good anti-friction and anti-wear effect. The function of synthetic esters is to use their adsorption on the surface of the steel plate to prevent a large amount of wear between the steel plates in contact with each other. The oily agents used in cold rolling oil mainly include the following substances: [0003] Animal and vegetable oils: such as castor oil, palm oil, tallow, rapeseed oil, lard, whale oil, etc.; [0004] Polymerized fatty acids and their derivatives: such as dimer acid, trimer acid, etc.; fatty acids and their salts, fatty alcohols, fatty acid esters: such as oleic acid, stearic acid, octanol, lauryl alcohol, butyl oleate, hard Zinc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/58C07C67/08B01J31/02C10M129/74
Inventor 高建群
Owner LUOYANG XINZHONG PETROCHEM
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