Full-bio-based polyamide and preparation method thereof

A bio-based polyamide and polyamide salt technology, which is applied in the field of chemical engineering, can solve the problems of increasing reaction steps and synthesis costs, the reaction rate and yield need to be improved, etc., and achieves abundant reserves, good reactivity and thermal stability, The effect of broadening the scope of application

Inactive Publication Date: 2020-11-13
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, on the one hand, the dimethyl furandicarboxylate monomer used in this patent needs further esterification of furandicarboxylic acid, which increases the reaction steps and synthesis costs. On the other hand, the patent uses enzyme-catalyzed polymerization, and the reaction rate and yield need to be improved.

Method used

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  • Full-bio-based polyamide and preparation method thereof
  • Full-bio-based polyamide and preparation method thereof
  • Full-bio-based polyamide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The air in the stainless steel salt-forming reactor was replaced three times by vacuuming and nitrogen gas. Under the protection of nitrogen, 1 mol of bio-based monomer 2,5-furandicarboxylic acid and 1.15 mol of bio-based monomer 1,4 -Butanediamine, 258mg of phosphorous acid catalyst and 400mL of deionized water were added to the salt-forming reactor to obtain a mixture; start stirring to mix the above mixture evenly, set the stirring speed to 300rpm, and heat the above mixture to 60 °C, reacted for 60 minutes, and the pH of the solution was 7.7 after the reaction, and a polyamide salt solution with a mass fraction of 36% was obtained.

[0054] Then check the air tightness of the stainless steel polymerization kettle. After the inspection is complete, replace the air in the stainless steel reaction kettle three times. Under the protection of nitrogen, transfer the polyamide salt solution obtained before to the polymerization kettle, and first heat it to 195°C. The react...

Embodiment 2

[0058] The air in the stainless steel salt-forming reactor was replaced three times by vacuuming and nitrogen gas. Under the protection of nitrogen, 1 mol of bio-based monomer 2,5-furandicarboxylic acid and 1.10 mol of bio-based monomer 1,5 - Add pentamethylenediamine, 536mg of phosphorous acid catalyst and 500mL of ethanol into the salt-forming reactor to obtain a mixture; start stirring to mix the above mixture evenly, set the stirring speed to 350rpm, and heat the above mixture to 72°C under normal pressure, After 75 minutes of reaction, the pH of the solution was 7.4 after the reaction, and a polyamide salt solution with a mass fraction of 38% was obtained.

[0059] Then check the air tightness of the stainless steel polymerization kettle. After the inspection is complete, replace the air in the stainless steel reaction kettle three times. Under the protection of nitrogen, transfer the polyamide salt solution obtained before to the polymerization kettle, and first heat it t...

Embodiment 3

[0063] The air in the stainless steel salt-forming reactor was replaced three times by vacuuming and nitrogen gas. Under the protection of nitrogen, 1 mol of bio-based monomer 2,5-furandicarboxylic acid and 1.08 mol of bio-based monomer 1,6 - Add hexamethylenediamine, 145mg of sodium phosphite catalyst and 350mL of deionized water into the salt-forming reactor to obtain a mixture; start stirring to mix the above mixture evenly, set the stirring speed to 200rpm, and heat the above mixture to 90° C., reacted for 120 minutes, and the pH of the solution was 7.2 after the reaction, thereby obtaining a polyamide salt solution with a mass fraction of 42%.

[0064] Then check the air tightness of the stainless steel polymerization kettle. After the inspection is complete, replace the air in the stainless steel reaction kettle three times. Under the protection of nitrogen, transfer the polyamide salt solution obtained before to the polymerization kettle, and first heat it to 225 ° C. T...

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Abstract

The invention discloses 2,5-furan dicarboxylic acid based polyamide with a full biomass source and a preparation method thereof, and belongs to the technical field of bio-based polyamide. The structural formula of the 2,5-furan dicarboxylic acid based polyamide is shown as (I), and in the formula, R is alkylene of C4, C5, C6 and C10. According to the method, 2,5-furan dicarboxylic acid and aliphatic diamine are used as raw materials, and 2,5-furan dicarboxylic acid based polyamide is prepared through a salt forming-pre-polycondensation-solid phase polycondensation process. 2,5-furan dicarboxylic acid and aliphatic diamine monomers are derived from biomass resources. The raw materials are wide in source, rich in reserves and renewable, and can be used as supplementation and partial substitution of non-renewable fossil raw material monomers, so that the high-performance environment-friendly polyamide is synthesized, is used in the fields of fibers, high-performance engineering plastics and the like, and has important scientific significance and application value.

Description

technical field [0001] The invention relates to a bio-based polyamide and a preparation method thereof, in particular to a method for synthesizing 2,5-furandicarboxylic acid-based polyamide with 2,5-furandicarboxylic acid and aliphatic diamine as raw materials, belonging to the field of chemical engineering . Background technique [0002] Polyamide (PA), also known as nylon, is a type of nitrogen-containing heterochain polymer containing amide groups (-NHCO-) ​​in the main chain of the polymer. Butylene glycol formate (PBT), polyoxymethylene (POM) and polyphenylene oxide (PPO) are known as the five general-purpose engineering plastics. According to the composition of the main chain, polyamides can be mainly divided into aliphatic polyamides, semi-aromatic polyamides and fully aromatic polyamides. The main chain of aliphatic polyamide is mainly composed of alkylene and amide groups, which is a typical linear structure. Although it has good comprehensive properties, the glas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/26C08G69/30
CPCC08G69/26C08G69/30
Inventor 马树刚周生远张雪芹郎笑梅胡泓梵李新乐孙鑫辛世煊
Owner PETROCHINA CO LTD
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