Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for recovering nylon 66 material by means of alcoholysis

A recovery method, nylon technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of amino compounds, etc., to achieve high purity, simple operation, easy control, and low cost

Active Publication Date: 2017-08-18
QINGDAO UNIV OF SCI & TECH
View PDF16 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are no literature or patent reports on the research on PA66 alcoholysis reaction. The present invention aims to provide a method for acid-catalyzed alcoholysis PA66 depolymerization to generate dialkyl adipate and hexamethylenediamine, and realize the separation of the two products. and refining, so as to achieve the purpose of efficient recycling of PA66, and provide a feasible route for industrialization

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
  • Method for recovering nylon 66 material by means of alcoholysis
  • Method for recovering nylon 66 material by means of alcoholysis
  • Method for recovering nylon 66 material by means of alcoholysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a high-pressure reaction kettle with a thermometer, add 1 mol of nylon 66 particles, 2 mol of sulfuric acid, and 20 mol of methanol in sequence, and stir the reaction at 160°C at a speed of 300r / min for 4 hours. Ethyl is extracted 5 times from the alcoholysis reaction mixture with ethyl ester at a volume ratio of 5:1, and the combined extracts are evaporated under reduced pressure to remove ethyl acetate, then distilled under reduced pressure by an oil pump, and collected at 109~110°C under a pressure of 12~14mmHg. Fraction dimethyl adipate, the yield is 86.85%; add 2mol calcium hydroxide to the raffinate phase hexamethylenediamine sulfate aqueous solution at room temperature, stir, react for a period of time and then heat to 50°C to make the reaction complete . Oil pump decompression distillation, under the pressure of 4-6mmHg, the fraction hexamethylenediamine at 90-110°C is collected, and the yield is 87.82%; the alcoholysis rate of nylon 66 is 100%.

[0023] Dep...

Embodiment 2

[0030]In a high-pressure reaction kettle with a thermometer, add 1 mol of nylon 66 particles, 3 mol of formic acid, and 25 mol of methanol in sequence, stir and react at 120°C at a speed of 400r / min for 6h, cool to room temperature naturally, open the kettle, and use the organic solvent tetrachloride Carbon dioxide extracts the mixed liquid after alcoholysis reaction for 4 times according to the volume ratio of 6:1, and the combined extraction phases are decompressed and rotary evaporated to remove carbon tetrachloride, and then the oil pump is distilled under reduced pressure. The fraction of dimethyl adipate has a yield of 80.85%; add 4.5 mol of sodium bicarbonate to the raffinate aqueous solution of hexamethylenediamine formate at room temperature, stir, and heat to 40°C after a period of reaction. to complete the reaction. Oil pump vacuum distillation, under the pressure of 4 ~ 6mmHg to collect the fraction of hexamethylenediamine at 90 ~ 110 ° C, the yield is 80.16%; the ...

Embodiment 3

[0032] In a high-pressure reaction kettle with a thermometer, add 1 mol of nylon 66 particles, 3.5 mol of phosphoric acid, and 15 mol of ethanol in sequence, and stir at 140°C for 8 hours at a speed of 350 r / min. The mixed solution of hexane and chloroform is extracted 7 times from the mixed solution after the alcoholysis reaction according to the volume ratio of 4:1, and the combined extraction phase is decompressed and rotary evaporated to remove the organic solvent, and the oil pump is distilled under reduced pressure. Collect diethyl adipate diethyl adipate at 110-120°C, and the yield is 82.85%; add 3 mol of sodium hydroxide to the raffinate phase hexamethylenediamine phosphate aqueous solution at room temperature, stir, react for a period of time and then heat to 55°C to complete the reaction. Oil pump decompression distillation, under the pressure of 4 ~ 6mmHg to collect the fraction of hexamethylenediamine at 90 ~ 110 ℃, the yield is 81.64%; the alcoholysis rate of nylo...

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 provides a method for recovering a nylon 66 material by means of alcoholysis. The method comprises the following steps: (1) putting nylon 66 particles, alcohol and a catalyst into a closed high-pressure reaction kettle according to a certain proportion, and carrying out an alcoholysis reaction under the conditions of stirring and heating; (2) after alcoholysis is finished, extracting for a plurality of times by using an organic solvent, merging extract phases, and carrying out reduced pressure rotary evaporation to obtain an extracting agent so as to obtain an dialkyl adipate crude product; then, carrying out reduced pressure distillation on the crude product, and collecting a corresponding fraction to obtain refined dialkyl adipate; (3) adding a certain amount of alkali into a raffinate phase obtained in the step (2) at the room temperature, and stirring; carrying out a reaction for a period of time, and then heating until the reaction is complete; after that, carrying out reduced pressure distillation, and collecting a corresponding fraction to obtain refined hexanediamine. Compared with the prior art, the method for recovering the nylon 66 material by means of alcoholysis is simple to operate and easy to control, mild in conditions, low in energy consumption, low in cost, stable in catalytic performance and easy to industrialize.

Description

technical field [0001] The invention relates to the field of high molecular polymer recovery, in particular to a method for recovering dialkyl adipate and hexamethylenediamine through alcoholysis of nylon 66 (PA66) material. Background technique [0002] Nylon 66 (PA66), also known as polyamide 66, is the first polyamide fiber variety successfully developed and industrialized by human beings. Due to its good wear resistance, solvent resistance and excellent mechanical properties, it is not only widely used in textile production, but also widely used in plastics industry, fishery and agriculture. Due to the increasing consumption demand for PA66, more and more wastes are generated. The landfill treatment method adopted in the early stage not only wastes renewable resources, but also occupies a large amount of land, and is easy to pollute groundwater resources. Mechanical recycling is to make new products through crushing, melting, extrusion, and injection molding, but the p...

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 Applications(China)
IPC IPC(8): C07C209/62C07C211/12C07C67/20C07C69/44
CPCC07C67/20C07C209/62C07C211/12C07C69/44
Inventor 宋修艳刘福胜赵瑞阳于世涛刘仕伟黄梅
Owner QINGDAO UNIV OF SCI & TECH