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Preparation method of methylcyclohexanediamine

A technology of methylcyclohexanediamine and methylphenylenediamine, applied in the field of preparation of methylcyclohexanediamine, can solve the problems of harsh process, many by-products, low production capacity, etc. Hydrogen pressure, effect of elevated temperature

Inactive Publication Date: 2016-09-07
本源精化环保科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the above-mentioned deficiencies in the prior art, the object of the present invention is to provide a method for preparing methylcyclohexanediamine, which aims to solve the problem of many by-products, low production capacity, and harsh processes in the existing production process of methylcyclohexanediamine. question

Method used

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  • Preparation method of methylcyclohexanediamine

Examples

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Comparison scheme
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Embodiment 1

[0030] Example 1: Preparation of catalyst

[0031] Alumina supported catalyst: 0.26g RuCl 3 ·3H 2 O, 0.06g RhCl 3 Dissolve together in 200 mL of an aqueous solution containing 0.5 g of polyethylene glycol, stir at 1000 rpm, add 100 mL of hydrazine hydrate solution (mass concentration of 10%), add 2 g of alumina to the mixed system after reduction, stir for 1.5 h, filter, THF (tetrahydrofuran) was rinsed 5 times to obtain a ruthenium-rhodium-alumina catalyst (ruthenium-rhodium mass ratio of about 4:1) with a loading rate of 99.5%.

Embodiment 2

[0032] Example 2: Preparation of 2-methyl-1,3-cyclohexanediamine

[0033] In a 1L autoclave, add 150g of 2-methyl-1,3-phenylenediamine, add 300g of isopropanol, stir to dissolve (slightly hot), quickly add 6g of fresh (that is, freshly prepared) palladium-carbon catalyst, turn off the high pressure The kettle is replaced by hydrogen for 3-5 times (such as 4 times), and the temperature is raised to 140 ° C. The pressure of the reaction system is controlled to about 6-8 MPa (such as 7 MPa), and the reaction is stirred for 8 hours. The product 2-methyl-1,3 - The yield of cyclohexanediamine was 59%, and the by-products in the reaction system were mainly 1-amino-2-methylcyclohexane (18%), isopropylated 1-amino-2-methylcyclohexane and Isopropylated 2-methyl-1,3-cyclohexanediamine (13%) and some other impurities. The catalyst in this example was reused for the second time, and the reaction basically did not proceed.

Embodiment 3

[0034] Example 3: Preparation of 2-methyl-1,3-cyclohexanediamine

[0035] In a 1L autoclave, add 150g of 2-methyl-1,3-phenylenediamine, add 250g of dioxane, stir to dissolve (slightly hot), add 8g of anhydrous sodium sulfate, and quickly add 6g of fresh palladium-carbon catalyst, Close the autoclave, replace it with hydrogen for 3-5 times (such as 4 times), start to heat up to 180 ° C, control the pressure of the reaction system to about 10 MPa, stir and react for 6 hours, and the product 2-methyl-1,3-cyclohexanediamine is recovered. The ratio was 91%, the content of the by-product 1-amino-2-methylcyclohexane in the reaction system was 1.7%, and no isobutylated by-product was found. When the catalyst in this example was reused for the third time, the activity remained at 60%.

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Abstract

The invention discloses a preparation method of methylcyclohexanediamine, wherein the preparation method comprises: dissolving methylphenylenediamine as a material in an organic solvent, and stirring and reacting at 150-200 DEG C under hydrogen pressure of 8-12 Mpa in the presence of a supporting metal catalyst and an inorganic salt aid for 5-10 hours to obtain the methylphenylenediamine. The preparation method provided herein solves the problems that existing preparation process of methylcyclohexanediamine is low in capacity and brings mass byproducts, and popularization of this product in more fields is reliably guaranteed.

Description

technical field [0001] The invention relates to the technical field of preparation of alicyclic amine curing agents, in particular to a preparation method of methylcyclohexanediamine. Background technique [0002] Epoxy resin is a thermosetting plastic with excellent comprehensive properties, which is widely used in coatings, civil engineering, automobiles, factory equipment, ships, containers and many other fields. The curing agent is one of the important components of the epoxy resin composition, and the quality of the curing agent directly determines the performance of the resin. Curing agents can be divided into several types according to chemical composition, application, etc., including aliphatic amines, aromatic amines, amidoamines, latent curing amines, urea substitutes, etc. Among them, aliphatic amine curing agents have many advantages, such as high reactivity, fast curing at low temperature, insensitivity to humidity, stable color, good chemical corrosion resista...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/36C07C209/72
CPCC07C209/72C07C211/36
Inventor 赵智全范丽芬
Owner 本源精化环保科技有限公司
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