Supercharge Your Innovation With Domain-Expert AI Agents!

A kind of preparation method of cycloaliphatic amine curing agent

A technology of alicyclic amine curing agent and metal catalyst, which is applied in a new preparation field, can solve the problems of high proportion of by-products, affecting the production capacity of alicyclic amine, and large amount of catalyst usage, so as to save production time and increase hydrogen pressure , the effect of improving the total yield

Active Publication Date: 2017-02-08
本源精化环保科技有限公司
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing synthesis methods have problems such as harsh processes, many by-products, large amount of catalyst used, and few times of use, especially the high proportion of by-products, which seriously affects the production capacity of alicyclic amines.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of cycloaliphatic amine curing agent
  • A kind of preparation method of cycloaliphatic amine curing agent
  • A kind of preparation method of cycloaliphatic amine curing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1: Preparation of 2-methyl-1,3-cyclohexanediamine (general method)

[0024] In a 1L autoclave, add 150g of 2-methyl-1,3-phenylenediamine, add 300g of isopropanol, stir to dissolve with slight heat, quickly add 6g of fresh palladium-carbon catalyst, close the autoclave, and replace with hydrogen for 3-5 The second time, start to heat up to 140°C, control the pressure of the reaction system to about 6-8MPa, and stir the reaction for 8 hours. The yield of the product 2-methyl-1,3-cyclohexanediamine is 59%, and the by-products in the reaction system mainly include 1 -amino-2-methylcyclohexane (18%), isopropylated 1-amino-2-methylcyclohexane and isopropylated 2-methyl-1,3-cyclohexanediamine (13 %) and some other impurities. The catalyst is reused for the second time, and the reaction does not proceed substantially.

Embodiment 2

[0025] Embodiment 2: the preparation of catalyst

[0026] (1) Activated carbon carrier catalyst: 0.26g RuCl 3 ·3H 2 O, 0.27g Span20 (sorbitan laurate), 0.19g Brij35 (polyethylene glycol ether) were dissolved in 500mL water, stirred at 1000rpm, and 200mL containing 0.14g NaBH was added dropwise 4 After the reduction, add 2g of activated carbon into the mixed system, continue to stir for 1.5h, filter, and rinse with THF (tetrahydrofuran) 5 times to obtain a ruthenium activated carbon catalyst with a loading capacity of 5%, and a loading rate of 99.8%.

[0027] (2) Alumina carrier catalyst: 0.26g RuCl 3 ·3H 2 O, 0.06g RhCl 3 Dissolve together in 200mL aqueous solution containing 0.5g polyethylene glycol, stir at 1000rpm, add 100mL hydrazine hydrate solution (mass concentration: 10%), add 2g alumina to the mixed system after reduction, stir for 1.5h, filter, THF Rinse 5 times to obtain about 5% ruthenium rhodium alumina catalyst (mass ratio is 4:1), and the loading rate is 99...

Embodiment 3

[0028] Embodiment 3: Preparation of 2-methyl-1,3-cyclohexanediamine

[0029] In a 1L autoclave, add 150g of 2-methyl-1,3-phenylenediamine, add 250g of dioxane, stir to dissolve with slight heat, add 10g of anhydrous sodium sulfate, quickly add 6g of fresh palladium carbon catalyst, turn off the high pressure The kettle was replaced by hydrogen for 3-5 times, the temperature was raised to 220°C, the pressure of the reaction system was controlled at about 14MPa, and the reaction was stirred for 6 hours. The yield of the product 2-methyl-1,3-cyclohexanediamine was 91%, and the reaction system The content of by-product 1-amino-2-methylcyclohexane is 1.7%, and no isobutylated by-product is seen. When the catalyst was reused for the third time, the activity remained 60%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of alicyclic amine curing agent. The method includes steps of dissolving methylphenylenediamine, as a raw material, in an organic solvent and performing a reaction with stirring for 5-12 hours in the presence of a supported metal catalyst and an inorganic salt promoter under a hydrogen pressure of 6-15 MPa at 150-240 DEG C for obtaining the alicyclic amine curing agent. A reaction yield can reach 90-97%. By means of the method in the invention, the alicyclic amine curing agent is high in amine value, is high in curing speed, is excellent in curing performance and is good in compounding property. Based on the method, alicyclic amine curing agents such as various alicyclic isocyanate and alicyclic derivatives with N-alkyl substituted alicyclic amine and the like can be prepared. The curing agent is widely applied in industries including blades of wind turbines, floors, extra-heavy corrosion-proof paints, exercisers, vehicles and the like.

Description

technical field [0001] The invention belongs to the technical field of curing agents, and in particular relates to a new preparation method of an alicyclic amine curing agent. Background technique [0002] Epoxy resin is a kind of thermosetting plastic with excellent comprehensive properties. It is widely used in many fields such as coatings, civil engineering, automobiles, factory equipment, ships, and containers. 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 and usage, including aliphatic amines, aromatic amines, amidoamines, latent curing amines, urea substitutes, etc. Among them, the aliphatic amine curing agent has many advantages such as high reactivity, rapid curing at low temperature, insensitivity to humidity, stable color, good chemical corrosion resistance, and...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/72C07C211/36C08G59/50
Inventor 赵智全
Owner 本源精化环保科技有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com