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Catalyst for synthesizing methylaniline from methylbenzene by one step and preparation method thereof

A technology of methylaniline and catalyst, applied in the field of aromatic hydrocarbon amination reaction synthesis, can solve the problems of large consumption, difficult product separation, unrecyclable homogeneous catalyst, etc., and achieves less usage, easily available raw materials, and a preparation process. simple effect

Inactive Publication Date: 2010-09-22
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst is a heterogeneous catalyst with high activity, which is used for the synthesis of methylaniline with toluene and hydroxylamine salt as raw materials. Disadvantages such as large consumption

Method used

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  • Catalyst for synthesizing methylaniline from methylbenzene by one step and preparation method thereof
  • Catalyst for synthesizing methylaniline from methylbenzene by one step and preparation method thereof
  • Catalyst for synthesizing methylaniline from methylbenzene by one step and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Select the active components CuO and V in the supported catalyst for the synthesis of methylaniline 2 O 5 The load capacity is 16.4%;

[0040] (2) Weigh 5g 20~40 mesh γ-Al 2 O 3 , Put it in a 100ml evaporating dish, use deionized water to measure the volume required for equal volume immersion to 5ml;

[0041] (3) CuO and V as the active components selected in step (1) 2 O 5 The loading amount is 16.4% to determine the required CuO and V 2 O 5 The total amount is 0.98g; according to CuO and V 2 O 5 The molar ratio of 0.25:1 to calculate the required precursor Cu(NO 3 ) 2 1.21mmol and NH 3 VO 3 9.70mmol;

[0042] (4) Weigh 5ml of deionized water determined in step (2), add 14.56mmol(COOH) 2 ·2H 2 O powder, mixed into a colorless and transparent oxalic acid solution;

[0043] (5) The NH determined in step (3) 3 VO 3 Add to the oxalic acid solution obtained in step (4) above to form a blue-green immersion solution;

[0044] (6) Weigh the catalyst carrier with the same mass as in...

Embodiment 2～4

[0056] The other steps are the same as in Example 1, except that the carrier used in the catalyst is silica, HZSM-5 molecular sieve (SiO 2 / Al 2 O 3 =135), titanium oxide, to prepare supported CuO-V for synthesis of methylaniline 2 O 5 Catalyst, in which active components CuO and V 2 O 5 The loading capacity is 16.4%.

[0057] Catalyst activity evaluation: Weigh 0.2 g of the supported catalysts prepared in Examples 2 to 4 into three three-necked flasks for performance evaluation. The reaction conditions are the same as the catalyst evaluation conditions in Example 1. The results of the reaction are shown in Table 2.

[0058] Table 2 The influence of carrier on catalyst performance

[0059] Example

Embodiment 5

[0061] (1) Select the active components CuO and V in the supported catalyst for the synthesis of methylaniline 2 O 5 The load capacity is 5.5%;

[0062] (2) Weigh 5g 20~40 mesh γ-Al 2 O 3 , Put it in a 100ml evaporating dish, use deionized water to measure the volume required for equal volume immersion to 5ml;

[0063] (3) CuO and V as the active components selected in step (1) 2 O 5 The loading amount is 5.5% to determine the required CuO and V 2 O 5 The total amount is 0.29g; according to CuO and V 2 O 5 The molar ratio of 0.25:1 to calculate the required precursor Cu(NO 3 ) 2 0.36mmol and NH 3 VO 3 2.90mmol;

[0064] (4) Weigh 5ml of deionized water determined in step (2), add 4.36mmol(COOH) 2 ·2H 2 O powder, mixed into a colorless and transparent oxalic acid solution;

[0065] Steps (5) to (10) are the same as in Example 1 to prepare supported CuO-V for the synthesis of methylaniline 2 O 5 Catalyst, in which active components CuO and V 2 O 5 The loading capacity is 5.5%.

[0066] C...

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Abstract

The invention belongs to the technical field of catalysis, in particular to a catalyst for synthesizing methylaniline from methylbenzene by one step. The catalyst consists of active ingredients and a carrier, wherein the active ingredients are CuO and V2O5; the molar ratio of the CuO to the V2O5 is 0.1-2:1; the carrier is silicon oxide, titanium oxide, alumina or a molecular sieve; and the load of the active ingredients CuO and V2O5 is 5 to 32 percent, wherein the load refers to the weight percentage of the active ingredients CuO and V2O5 in the integral supported catalyst. Compared with the conventional catalyst for amination of methylbenzene, the catalyst prepared by the method has low consumption; in the implementation, the weight ratio of the catalyst to a raw material hydroxylamine sulphate is reduced to be 1:8.2, the catalyst has good activity, and the conversion rate of the methylbenzene and the yield of the methylaniline are respectively 66.23 percent and 61.22 percent; and the preparation process for the catalyst is simple and the raw materials are readily available.

Description

Technical field [0001] The invention belongs to the synthesis of aromatic hydrocarbons by ammoniating reaction, and is specifically a catalyst for one-step synthesis of methylaniline from toluene, and a preparation method and application thereof. Background technique [0002] Methylaniline is an important organic chemical raw material, which has a wide range of applications in medicine, dyes, rubber and other industries. In recent years, its demand has continued to grow. Traditional methylaniline synthesis methods, such as nitrotoluene reduction method (Journal of Catalysis191(2000):467~473), methylphenol ammonification method (US Patent 3272865) and halogenated toluene ammonification method (CatalysisToday 37 (1997) ): 121 ~ 136), etc., these synthetic routes have complex processes, low atom utilization, and many by-products, which are prone to produce large amounts of toxic and harmful substances to the environment, which do not meet the needs of green synthetic chemistry idea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/847B01J29/48C07C211/47C07C209/02
Inventor 王延吉张东升高丽雅李佳李芳赵新强
Owner HEBEI UNIV OF TECH
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