Method for synthesizing polyamide through olefin hydroamine carbonylation
An alkene hydrogen amine carbonyl and hydrogen amine carbonyl technology, applied in the field of polyamides, can solve the problems of oxygen sensitivity and harsh reaction conditions, and achieve the effects of simple raw materials, strong practicability and high step economy.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0047] Example 1: Without adding alkali as additive
[0048]
[0049] Aryldiene (213.1 mg), hydroxylamine hydrochloride (55.6 mg), bisacetonitrile palladium(II) chloride (10.4 mg), 2-dicyclohexylphosphorus-2',6' were added to a strictly dry ampoule in this order. - Diisopropoxy-1,1'-biphenyl (41.1 mg) and anisole (2.0 mL). The ampoule bottle was put into the autoclave, carbon monoxide replaced the air in the autoclave three times and filled with 20 atm carbon monoxide, heated to 120° C. for reaction for 24 hours. After the autoclave was cooled, the carbon monoxide in the autoclave was slowly released. The reaction solution was poured into methanol, and the mixture was centrifuged to obtain a crude product, which was subsequently washed with methanol and water in turn, and vacuum-dried to obtain a polyamide product with a yield of 11%.
Embodiment 2
[0050] Example 2: 2-cyano-6-methylpyridine as base
[0051]
[0052] Aryldiene (213.1 mg), hydroxylamine hydrochloride (55.6 mg), bisacetonitrile palladium(II) chloride (10.4 mg), 2-dicyclohexylphosphorus-2',6' were added to a strictly dry ampoule in this order. -Diisopropoxy-1,1'-biphenyl (41.1 mg), 6-methyl-2-pyridinecarbonitrile (18.9 mg) and anisole (2.0 mL). The ampoule bottle was put into the autoclave, carbon monoxide replaced the air in the autoclave three times and filled with 20 atm carbon monoxide, heated to 120° C. for reaction for 24 hours. After the autoclave was cooled, the carbon monoxide in the autoclave was slowly released. The reaction solution was poured into methanol, and the mixture was centrifuged to obtain a crude product, which was then washed with methanol and water in turn, and vacuum-dried to obtain a polyamide product with a yield of 62% and a number-average molecular weight of 3.1×10 4 , the polymer dispersibility index is 1.84.
Embodiment 3
[0053] Example 3: Preparation of polyamide from aryl dienes
[0054]
[0055] Aryldiene (240.1 mg), hydroxylamine hydrochloride (34.7 mg), bisacetonitrile palladium(II) chloride (6.5 mg), 2-dicyclohexylphosphorus-2',6' were added to a strictly dry ampoule in this order. - Diisopropoxy-1,1'-biphenyl (25.7 mg) and N-methylpyrrolidone (4.0 mL). The ampoule bottle was put into the autoclave, carbon monoxide replaced the air in the autoclave three times and filled with 20atm carbon monoxide, heated to 120°C and reacted for 12 hours. After the autoclave was cooled, the carbon monoxide in the autoclave was slowly released. The reaction solution was poured into methanol, and the mixture was centrifuged to obtain a crude product, which was then washed with methanol and water in turn, and vacuum-dried to obtain a polyamide product with a yield of 73% and a number-average molecular weight of 9×10 3 , the polymer dispersibility index is 3.79.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More