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Catalyst of synthetic dodecylphenol and preparation method thereof

A dodecylphenol and catalyst technology, which is applied in the field of dodecylphenol synthesis from dodecylphenol and phenol, can solve the problems of less repetitions, more reaction by-products, poor product color, etc., to increase Si content, change The effect of catalytic performance

Active Publication Date: 2017-05-31
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Purpose of the present invention: the present invention aims at the shortcomings of existing catalysts such as complex preparation process, high cost, small application range, poor product color, low product yield, few repetitions, and many reaction by-products, and provides an acidified attapulgite As raw material, fluorinated with ammonium fluorosilicate solution, used to catalyze the synthesis of dodecylbenzene from dodecene and phenol

Method used

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  • Catalyst of synthetic dodecylphenol and preparation method thereof
  • Catalyst of synthetic dodecylphenol and preparation method thereof
  • Catalyst of synthetic dodecylphenol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 10 grams of purified attapulgite into a beaker filled with 40ml of dilute sulfuric acid solution with a concentration of 2mol / L, heat to 70°C, stir for 2 hours, cool, filter, wash until neutral, and dry at 110°C for 12 hours to obtain acidified unevenness Roast clay: Add 10g of acidified attapulgite into a beaker filled with 40ml of 1.5% ammonium fluorosilicate solution, heat to 70°C, stir for 2h, and dry by suction filtration; dry at 110°C for 12h, and roast at 550°C for 8h , to obtain a fluoridated acidified attapulgite catalyst (abbreviated as a fluorinated catalyst, the same below).

[0024] ① in N 2 Under the protection of 0.1 mol of dodecene and 0.2 mol of phenol and 0.49 g of the acidified attapulgite prepared in this example (the amount of acidified attapulgite is 5% of the mass of phenol) was added to the reactor, heated to 70 ° C, Stir for 4 hours. After the reaction, the product was filtered with suction and subjected to vacuum distillation to obtain ...

Embodiment 2

[0028] Weigh 10 grams of purified attapulgite into a beaker filled with 40ml of dilute sulfuric acid solution with a concentration of 2mol / L, heat to 90°C, stir for 2 hours, cool, filter, wash until neutral, and dry at 110°C for 12 hours to obtain acidified unevenness Roast clay: Add 10g of acidified attapulgite into a beaker filled with 40ml of 2% ammonium fluorosilicate solution, heat to 70°C, stir for 2h, filter and dry with suction; dry at 110°C for 12h, and roast at 550°C for 8h , to obtain a fluorination catalyst.

[0029] ① in N 2 Under the protection of 0.1mol dodecene, 0.2mol phenol and 0.25g acidified attapulgite prepared in this example (the amount of acidified attapulgite is 5% of the mass of phenol) was added to the reactor, heated to 50°C, Stir for 6 hours. After the reaction, the product was filtered with suction and subjected to vacuum distillation to obtain the distillate product at a vacuum degree of 1.3 mb and a temperature of 150° C., and finally stored u...

Embodiment 3

[0033] Weigh 10 grams of purified attapulgite into a beaker filled with 40ml of dilute hydrochloric acid solution with a concentration of 2mol / L, heat to 90°C, stir for 2h, cool, filter, wash until neutral, and dry at 110°C for 12h to obtain acidified attapulgite Roast clay: Add 10g of acidified attapulgite into a beaker filled with 40ml of 2.5% ammonium fluorosilicate solution, heat to 80°C, stir for 2h, filter and dry with suction; dry at 110°C for 12h, and roast at 550°C for 8h , to obtain a fluorination catalyst.

[0034] ① in N 2 Under the protection of 0.05 mol dodecene and 0.2 mol of phenol and 0.1 g of acidified attapulgite prepared in this example (the amount of acidified attapulgite is 1% of the mass of phenol) was added to the reactor, heated to 90 ° C, Stir for 8 hours. After the reaction, the product was filtered with suction and subjected to vacuum distillation to obtain the distillate product at a vacuum degree of 1.3 mb and a temperature of 150° C., and final...

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Abstract

The invention provides a catalyst of laurylene and phenol compounded dodecylphenol by taking acidified attapulgite as raw material and fluorating with ammonium fluosilicate. The reaction condition is: under the constant pressure, the reaction temperature is 50-90 DEG C, the reaction time is 4-8 h, the molar ratio of phenol and alkene is 2: 1-10: 1, the catalyst dosage is 0.5-5% (counted by laurylene mass). The catalyst has the advantages of long service life, low dosage, no frequent replacement and high product quality by comparing with the clay catalyst.

Description

technical field [0001] The invention relates to the field of petroleum product processing, in particular to a method for synthesizing dodecylphenol from dodecene and phenol. Background technique [0002] Alkylphenols are important fine chemical products, raw materials and intermediates. Alkylphenols are widely used in the synthesis of fine chemicals, such as non-ionic surfactants, phenolic resins, rubber antioxidants, antistatic agents, paints, coatings, etc. At present, dodecylphenol has been widely used in the research of surfactants due to its low cost, non-toxicity and easy degradation. Rigid aromatic rings and flexible carbon chains are the structural characteristics of this type of surfactants, and The surfactant has good temperature resistance. At present, the methods for synthesizing dodecylphenol mainly include n-dodecene, dodecane (halogenated hydrocarbon) and n-dodecyl alcohol as alkylation reagents, and the alkylation reaction catalyst mostly uses ionic liquid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/12B01J27/138C07C37/14C07C39/06
CPCY02P20/52B01J27/12B01J27/138C07C37/14C07C39/06
Inventor 李为民黄伟金天陈昶乐姚超
Owner CHANGZHOU UNIV
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