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Preparation method of iron-based catalyst for alkylation reaction

A technology of alkylation reaction and catalyst, which is applied in the field of preparation and synthesis of compounds, can solve the problems of decreased catalytic activity, low water tolerance, easy deactivation with water, etc., and achieves the effects of high activity, difficult hydrolysis, and wide application

Active Publication Date: 2015-04-29
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the catalytic systems described in the above disclosures have the characteristics of high activity, their catalytic activity decreases significantly after being recycled, and their tolerance to water is low, that is, they are easily deactivated by water.
[0005] Patent CN 1077808C and patent CN 1131107C etc. disclose the use of HY-type molecular sieve catalysts to catalyze the reaction of benzene and 1-dodecene to synthesize dodecylbenzene. Although it has the advantage of high selectivity, its reaction temperature is relatively high, and The reaction pressure is high, which limits the use of molecular sieves to a certain extent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-1

[0021] Take bisfluorosulfonimide HN(SO 2 F) 2 (3.1g, 18.8mmol) was dissolved in 10ml of distilled toluene. In a round bottom flask equipped with stirring and a gas vent, add ferric chloride FeCl 3 (1.02g, 6.3mmol). The bisfluorosulfonimide solution was slowly added dropwise into the round bottom flask. During the reaction process, the generated HCl needs to be continuously removed from the gas vent. The reaction was carried out in an ice-water bath. After reacting for about 30min, filter to obtain a solid, use 60ml of benzene to wash the solid three times, and then dry it in vacuum to obtain Fe(N(SO 2 F) 2 ) 3 . The yield is about 44%.

Embodiment 1-2

[0023] Take bisperfluorohexylsulfonimide HN(SO 2 C 6 f 13 ) 2 (4.65g, 6mmol) was dissolved in 10ml of distilled toluene. In a round bottom flask equipped with stirring and a gas vent, add ferric chloride FeCl 3 (0.19g, 1.2mmol). The bisfluorosulfonimide solution was slowly added dropwise into the round bottom flask. During the reaction process, the generated HCl needs to be continuously removed from the gas vent. The reaction was carried out in an ice-water bath. After reacting for about 30min, filter to obtain a solid, use 60ml of benzene to wash the solid three times, and then dry it in vacuum to obtain Fe(N(SO 2 C 6 f 13 ) 2 ) 3 . The yield is about 46%.

[0024] The embodiment that prepares catalyst and is used for synthetic Friedel-Crafts alkylation reaction is as follows:

[0025] The ionic liquid [1-butyl-3-methylimidazole] [bistrifluoromethylsulfonimide] used in the following examples needs to be vacuum-dried at 60-140° C. for 24 hours before use.

Embodiment 2-1

[0027] The ionic liquid [1-butyl-3-methylimidazole][bistrifluoromethylsulfonimide] (1.64g, 3.9mmol) was weighed and heated to 60°C under dry conditions. Weigh iron chloride FeCl 3 (0.49g, 3.0mmol), tris(difluorosulfonimide) iron Fe(N(SO 2 C 6 f 13 ) 2 ) 3 (2.40g, 1.0mmol), it was slowly added to the heated ionic liquid, stirred to fully dissolve, and the stirring time was 24h. Stirring was then stopped and allowed to slowly return to room temperature. That is, an ionic liquid catalyst with a perfluoroalkylsulfonimide structure is obtained.

[0028] Mix benzene (2.5g, 32.0mmol) with 1-dodecene (5.4g, 32.0mmol), preheat to a reaction temperature of 30°C, add 0.40g of the ionic liquid catalyst prepared by the present invention, start stirring, and react for 12 hours . Stand still, the system is layered, the lower layer is the catalyst, which can be recycled through separation; the upper layer is the product. The conversion of 1-dodecene was more than 90%, and the selecti...

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PUM

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Abstract

The invention discloses a preparation method of an iron-based catalyst for alkylation reaction. The preparation method comprises the following steps: firstly preheating ionic liquid with a perfluoroalkyl group sulfimide structure to 60-90 DEG C, then adding an iron-containing compound, stirring for uniform mixing, and then reducing temperature to normal temperature; reacting at normal temperature for 6-24 hours for interreaction to generate a coordination compound so as to obtain the catalyst used for catalyzing Friedel-Crafts alkylation reaction. The catalyst prepared through the method disclosed by the invention is used for synthesizing the Friedel-Crafts alkylation reaction, such as the reaction of synthesizing dodecylbenzene by using benzene and 1-laurylene; in addition, the catalyst has the characteristics of high activity, high 2-LAB (2-Linear Alkylbenzene) selectivity, moderation in use condition, good water resistance, low possibility in hydrolysis and good recycling property and can be recovered through a simple method.

Description

technical field [0001] The invention relates to the preparation and synthesis of compounds, and relates to a method for preparing an iron-based catalyst for alkylation reactions, specifically referring to a method for preparing an iron-containing catalyst system with a perfluoroalkylsulfonimide structure. Background technique [0002] Linear alkylbenzene (LAB), especially dodecylbenzene, is an important raw material for synthetic detergents. The annual demand for linear alkylbenzene in the world exceeds 3 million tons, and it is expected to grow at a rate of 4% per year. Since the first Pacol unit was used to produce linear alkylbenzenes in 1968, the HF / AlCl used in the Friedel-Crafts alkylation process 3 as a catalyst. Because HF is strongly corrosive and toxic, HF / AlCl 3 Technology has brought a series of problems to equipment maintenance and safe production. Use HF, AlCl 3 After the batch production is over, the catalytic components are difficult to separate and recy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C15/107C07C2/66
Inventor 詹晓力何逸波张庆华陈丰秋
Owner ZHEJIANG UNIV
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