Method for preparing liquidized butyl diphenylamine/octyl diphenylamine

An octyldiphenylamine, liquefaction technology, used in the preparation of amino compounds from amines, organic chemistry, chemical recovery, etc., can solve the problems of unstable temperature, complicated recrystallization steps, etc.

Active Publication Date: 2015-05-20
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] CN1288000A discloses a method for preparing liquefied alkylated diphenylamine, which comprises contacting and reacting diisobutylene with diphenylamine at 170°C to 230°C and a pressure of 0.2 to 0.5Mpa in the presence of an activated clay catalyst. Stop the reaction when the content of bis-octyldiphenylamine in the product is less than 20%, which solves the disadvantage of unstable temperature in the reacti

Method used

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  • Method for preparing liquidized butyl diphenylamine/octyl diphenylamine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Add 128.8g of diphenylamine, 6.5g of catalyst and 75.0g of C8 olefins into a 500ml glass container equipped with a stirrer, thermometer, heating mantle, reflux condenser, water separator, and nitrogen pipeline, pass into nitrogen protection, and use a magnetic stirrer Stir, after melting at 80°C, gradually increase the temperature to 165°C, add 104g C8 olefin in 5-7 hours, control the reflux speed and heating temperature, so that the temperature of the reactant is not lower than 145°C, and the reaction time is 14 hours . According to the TLC tracking reaction until the DPA content does not change, it is properly cooled at 60 ° C and filtered, and the olefins are removed by vacuum distillation to obtain the final product. The olefins and catalyst are recovered. The product is a yellow clear liquid. The gas chromatography data shows that the content of diphenylamine is 5%, and the base number 122.

Embodiment 2

[0047] Add 128.8g of diphenylamine, 13g of catalyst and 75.0g of C8 olefin in a 500ml glass container equipped with stirrer, thermometer, heating mantle, reflux condenser, water separator, and nitrogen pipeline, pass into nitrogen protection, and add amount of polymerization inhibitor Stir with a magnetic stirrer, and after melting at 80°C, gradually increase the temperature to 155°C, add 104g of C8 olefin in 5 to 7 hours, control the reflux speed and heating temperature, so that the temperature of the reactant is not lower than 145 °C, and the reaction time was 14 hours. According to the TLC tracking reaction until the DPA content no longer changes, add 13g of polyisobutene, continue to react for 2 hours, after proper cooling, filter at 60°C, remove olefins by vacuum distillation to obtain the final product, recover olefins and catalyst, the product is yellow clear liquid, Gas chromatographic data showed a diphenylamine content of 1% and a base number of 166.

Embodiment 3

[0049] Add 128.8g of diphenylamine, 13g of catalyst and 179.0g of C8 olefin in a 500ml glass container equipped with stirrer, thermometer, heating mantle, reflux condenser, water separator, and nitrogen pipeline, pass into nitrogen protection, and add amount of polymerization inhibitor Stir with a magnetic stirrer. After melting at 80°C, gradually increase the temperature to 155°C. Control the reflux rate and heating temperature so that the temperature of the reactant is not lower than 145°C. The reaction time is 16 hours. According to the TLC tracking reaction until the DPA content does not change, add 25g of polyisobutene and continue the reaction for 2 hours. After proper cooling, filter at 60°C and remove the olefins by vacuum distillation to obtain the final product. Recover the olefins and catalyst. The product is an orange clear liquid. Gas chromatographic data showed a diphenylamine content of 2% and a base number of 162.

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Abstract

The invention relates to a method for preparing liquidized butyl diphenylamine/octyl diphenylamine. The method comprises the following steps: mixing diphenylamine with C8 alkene according to a mole ratio of 1:1.35-1:3.2, adding 5 to 25% of catalyst and polymerization inhibitor, carrying out alkylation reactions for 0.5 to 20 hours at a temperature of 80 to 165 DEG C under a reaction pressure of 0.25 to 0.5 MPa; wherein the addition amount of the polymerization inhibitor is 60 to 180 ppm; then adding ending alkene, wherein the adding amount of the ending alkene is 10 to 40% of the molar weight of the diphenylamine; heating the reaction product, filtering, then subjecting the filtrate to reduced pressure distillation, collecting the solid catalyst for cycle use, collecting and recovering the alkene, returning the collected alkene to the reaction system, and collecting the liquid namely the liquidized butyl diphenylamine/octyl diphenylamine. The color of obtained product is lightened, the product is clear and transparent, the base number reaches 140 to 180, the content of residual diphenylamine is less than 1%, the conversion of diphenylamine is increased, the performance of the product on controlling the viscosity increasing is excellent, the catalyst can be repeatedly used, and no wastewater is discharged.

Description

technical field [0001] The invention relates to a preparation method of butyl and octyl diphenylamine involving active olefins. Background technique [0002] Butyl and octylated diphenylamine antioxidants have excellent oxidation resistance, high thermal stability, good oil solubility, ash-free and phosphorus-free, etc., according to olefin isomerization, reaction conditions, and preparation processes. , There are two products of solidified and liquefied diphenylamine. The solidified product has stronger oxidation resistance, but the liquefied alkyl diphenylamine has better oil solubility and is easier to deploy, so it is more widely used in lubricating oil. [0003] The conventional preparation method of butyl and octylated diphenylamine is as follows: using diphenylamine as raw material, under the catalysis of Lewis acid or protonic acid catalyst, the initial product is obtained by alkylation reaction with C8 olefin, and then obtained through a series of post-reaction trea...

Claims

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Application Information

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IPC IPC(8): C07C211/55C07C209/68C10M133/12C10N30/10
CPCY02P20/584
Inventor 火鹏飞徐小红李涛蒋虎张丙伍周旭光薛卫国
Owner PETROCHINA CO LTD
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