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Catalyst for producing diethyltoluene diamine and preparation method and application of catalyst

A technology of diethyltoluenediamine and toluenediamine, which is applied in the field of supported catalysts and its preparation, can solve problems such as environmental pollution, cumbersome post-treatment process, high temperature and pressure, and solve the problems of three wastes and environmental pollution , reasonable acidity and acid distribution, high activity and selectivity

Active Publication Date: 2018-05-08
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] 1) complex reaction, many by-products, and poor product selectivity;
[0017] 2) Post-processing needs to go through steps such as alkali neutralization, filtration, extraction, rectification, etc., and there are problems such as cumbersome post-processing process, large amount of three wastes, difficult solid waste disposal, and environmental pollution;
[0018] 3) The product needs to pass rectification to be qualified, but because the boiling points of the by-product and the main product are very close, there are problems such as difficulty in product separation
The disadvantage of this invention is that the reaction conditions are harsh, especially for the alkylation reaction of ethylene needs higher temperature and pressure (temperature up to 375 ℃, pressure up to 3000psig)
At the same time, the conversion rate of raw materials is low, and the alkylation products are mainly monosubstituted ortho-cycloalkylation products, and a large amount of N-alkylated by-products are produced during the reaction.

Method used

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  • Catalyst for producing diethyltoluene diamine and preparation method and application of catalyst
  • Catalyst for producing diethyltoluene diamine and preparation method and application of catalyst
  • Catalyst for producing diethyltoluene diamine and preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-1

[0072] 2wt%Ru-4%Ni-6%Cu / Modified SiO 2 -Al 2 o 3 preparation of

[0073] At room temperature, 100g of SiO2 -Al 2 o 3 The carrier (Si:Al atomic ratio is 40) is completely immersed in 100ml of a mixed aqueous solution containing 26.0g of ammonium fluorosilicate and 1.4g of boric acid, soaked for 12h to allow for adsorption equilibrium, and then placed in an oven for 6h at 130°C, and finally transferred to Furnace, calcination at 500°C for 7h to obtain 8% SiO 2 and 0.7% B 2 o 3 Modified SiO 2 -Al 2 o 3 carrier.

[0074] Dissolve 6.9g of ruthenium nitrate, 21.7g of nickel nitrate hexahydrate and 24.8g of copper nitrate trihydrate in 100ml of deionized water, stir well, then add the above-mentioned modified SiO 2 -Al 2 o 3 The carrier was impregnated for 18 hours to allow for adsorption equilibrium, then baked in an oven at 120°C for 10 hours, and finally transferred to a muffle furnace and baked at 400°C for 6 hours. Get 2wt%Ru-4%Ni-6%Cu / Modified SiO 2 -Al 2 o 3 C...

Embodiment 1-2

[0076] 1wt%Pd-8%Ni-2%Fe / Modified SiO 2 -Al 2 o 3 preparation of

[0077] At room temperature, 100g of SiO 2 -Al 2 o 3 The carrier (Si:Al atomic ratio is 80) is completely immersed in 100ml of a mixed aqueous solution containing 19.0g of ammonium fluorosilicate and 0.9g of boric acid, soaked for 18h to allow for adsorption equilibrium, and then baked in an oven at 100°C for 9h, and finally transferred to Furnace, calcination at 450°C for 3h, to obtain 6% SiO 2 and 0.5% B 2 o 3 Modified SiO 2 -Al 2 o 3 carrier.

[0078] Dissolve 2.3g of palladium nitrate, 42.4g of nickel nitrate hexahydrate and 15.4g of ferric nitrate nonahydrate in 100ml of deionized water, stir well, then add the above-mentioned modified SiO 2 -Al 2 o 3 The carrier was impregnated for 14 hours to allow for adsorption equilibrium, then baked in an oven at 150°C for 4 hours, and finally transferred to a muffle furnace and baked at 350°C for 9 hours. Get 1wt%Pd-8%Ni-2%Fe / / Modified SiO 2 -Al 2 o ...

Embodiment 1-3

[0080] 2.5wt%Ru-10%Ni-4%Mo / Modified Al 2 o 3 preparation of

[0081] At room temperature, 100g of strip-shaped Al 2 o 3 The carrier is completely immersed in 100ml of a mixed aqueous solution containing 9.3g of ammonium fluorosilicate and 1.9g of boric acid, soaked for 14h to allow for adsorption equilibrium, then placed in an oven for 7h at 120°C, and finally transferred to a muffle furnace and roasted at 400°C for 8h to obtain Contains 3% SiO 2 and 1%B 2 o 3 Modified Al 2 o 3 carrier.

[0082] Dissolve 8.2g of ruthenium nitrate, 51.6g of nickel nitrate hexahydrate and 8.5g of ammonium molybdate in 100ml of deionized water, stir well, then add the above-mentioned modified Al 2 o 3 The carrier was impregnated for 16 hours to allow for adsorption equilibrium, then baked in an oven at 130°C for 6 hours, and finally transferred to a muffle furnace and baked at 450°C for 7 hours. Get 2.5wt%Ru-10%Ni-4%Mo / / Modified Al 2 o 3 Catalyst Precursor A-3.

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Abstract

The invention discloses a supported catalyst for producing diethyltoluene diamine. The supported catalyst for producing diethyltoluene diamine comprises a modified carrier and a supported active component, wherein the modified carrier contains SiO2 and B2O3 obtained by decomposing a soluble silicon-containing compound and a boron-containing compound through drying and roasting after introducing the soluble silicon-containing compound and the boron-containing compound into the carrier. The invention further discloses a preparation method and application of the catalyst. The catalyst disclosed by the invention is suitable for the alkylation of aromatic amines, especially has extremely high activity and selectivity for continuous production of diethyltoluene diamine with toluenediamine alkylation. The catalyst has a simple preparation process, high economy and better application prospects.

Description

technical field [0001] The invention relates to the field of preparation of diethyltoluenediamine, in particular to a supported catalyst for producing diethyltoluenediamine and its preparation method and application. Background technique [0002] Diethyltoluenediamine (abbreviated as DETDA) is a low-viscosity, non-toxic, odorless light yellow liquid, which is 3,5-diethyl-2,4-toluenediamine (about 80%) and 3, 5-diethyl-2,6-toluenediamine (about 20%) is a mixture of two isomers, the structural formula is as follows: [0003] [0004] DETDA is a sterically hindered aromatic diamine. The steric hindrance of ethyl and methyl groups makes its activity much lower than that of toluene diamine (TDA). It reacts with polyurethane prepolymers faster than DMTDA and twice as fast as MOCA is about 30 times faster. DETDA is a chain extender for polyurethane and polyurea elastomers. It can also be used as a curing agent for polyurethane and epoxy resins. It has the advantages of fast re...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J37/02C07C209/68C07C211/50
CPCB01J23/892B01J23/8926B01J23/8953B01J23/8993B01J37/0207C07C209/68C07C211/50
Inventor 任树杰张聪颖刘振国李鑫唐磊吴健姜庆梅黎源
Owner WANHUA CHEM GRP CO LTD
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