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Method for producing adipic acid, hexamethylenediamine hydrochloride and polyhexamethylene (di)guanidine chloride from nylon-66 through depolymerization

A technology of hexamethylene diamine hydrochloride and polyhexamethylene monoguanidine, which is applied in the field of industrial production of polyhexamethylene monoguanidine hydrochloride, can solve the problems of difficult separation, poor production efficiency, and art in other documents or patents None of the issues have been reported

Inactive Publication Date: 2013-04-17
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It not only overcomes the disadvantages of low yield and difficult separation in the production of monomer adipic acid and hexamethylenediamine from polynylon-66, but also solves the problems of poor production efficiency and high cost
The industrial production process of preparing polyhexamethylene mono(bi)guanidine hydrochloride with waste nylon-66 as raw material has not been reported in other documents or patents

Method used

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  • Method for producing adipic acid, hexamethylenediamine hydrochloride and polyhexamethylene (di)guanidine chloride from nylon-66 through depolymerization
  • Method for producing adipic acid, hexamethylenediamine hydrochloride and polyhexamethylene (di)guanidine chloride from nylon-66 through depolymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Depolymerization workshop section: add 30% industrial by-product hydrochloric acid of 1500Kg in the reaction kettle that reflux condenser and hydrochloric acid gas absorption device are housed on the top, add 500Kg water, heat, add waste nylon-66 fragment 1000Kg while stirring, Control the reaction temperature at 100-110° C., normal pressure, and time for 8 hours, and the reaction conversion rate reaches more than 90%, and the acid hydrolysis solution is obtained. The acid solution is filtered through a coarse filter and pressed into the crystallization tank, and the speed of cooling and crystallization is accelerated through top pumping and decompression. Circulating cooling water until the temperature of the crystallization tank drops to 30-40°C. After the crystallization is completed, a box-type filter press is used to separate the crude adipic acid crystals and the crude hexamethylenediamine hydrochloride solution.

[0028](2) Adipic acid refining section: heat...

Embodiment 2

[0032] The depolymerization section (1), adipic acid refining section (2) and hexamethylenediamine hydrochloride refining section (3) are the same as in Example 1.

[0033] (4) In the preparation section of polyhexamethylene mono(bi)guanidine hydrochloride, put dicyandiamide and ammonium chloride powder with a molar ratio of 1:2 into the reactor, under nitrogen protection, stir for 25min, and heat up to 180°C , stirred and reacted for 2h, slowly added the hexamethylenediamine hydrochloride powder obtained in the refining section (3) of hexamethylenediamine hydrochloride, and continued to react for 5h to obtain a mixture of polyhexamethylene monoguanidine hydrochloride and ammonium chloride, While hot, use nitrogen gas to slowly press the molten reaction liquid into a separation tank filled with industrial ethanol, stir well and then filter, and distill the polyhexamethylene monoguanidine hydrochloride ethanol filtrate to remove ethanol under reduced pressure to obtain light yel...

Embodiment 3

[0035] The depolymerization section (1), adipic acid refining section (2), hexamethylenediamine sulfate refining section (3) and polyhexamethylene mono(bi)guanidine sulfate preparation section (4) are the same as in Example 2.

[0036] Add 300Kg of hot water (80±5°C) to the crude ammonium chloride white powder obtained after the above filtration, stir, dissolve and filter, evaporate and concentrate under reduced pressure until crystals are precipitated, cool, filter, and vacuum dry to obtain 150Kg of refined sulfuric acid Ammonium solid, the yield is over 86%. According to the reaction equivalence ratio, fresh ammonium chloride is properly supplemented and recycled to the polyhexamethylene mono(bi)guanidine hydrochloride preparation section (4).

[0037] The general molar ratio herein refers to allowing the molar ratio to fluctuate by 10% on the basis of equivalent reaction.

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Abstract

The invention discloses a method for producing adipic acid, hexamethylenediamine hydrochloride and polyhexamethylene (di)guanidine chloride from waste nylon-66 serving as a raw amerial through depolymerization, which is characterized by comprising the following steps of: depolymerizing the waste nylon-66 by using hydrochloric acid to obtain refined adipic acid and hexamethylenediamine hydrochloride; polymerizing the hexamethylenediamine hydrochloride and dicyandiamide (in a molar ratio of 1:1) at the temperature of between 170 and 190DEG C for 1 to 3 hours to obtain a white or pale yellow solid polyhexamethylene diguanidine chloride; and adding dicyandiamide and ammonium chloride powder in a molar ratio of 1:2 into a reactor, performing reaction at high temperature for 1 to 3 hours, slowly adding hexamethylenediamine hydrochloride powder, continuously reacting for 3 to 7 hours to obtain a white or pale yellow solid polyhexamethylene guanidine chloride. The method improves production efficiency, reduces production cost, and solves the problems of difficult separation of the product hexamethylenediamine due to depolymerization, low yield and poor benefit; and the technological process is environment-friendly, simple and convenient, and is suitable for industrial production.

Description

technical field [0001] The present invention relates to the new method that utilizes nylon-66 waste depolymerization to produce adipic acid, hexamethylenediamine hydrochloride and polyhexamethylene mono(bi)guanidine hydrochloride disinfectant, especially introduces a kind of suitable for industrialized production New approach to polyhexamethylene mono(bi)guanidine hydrochloride. Background technique [0002] Nylon-66 is a polymer material formed by polycondensation of adipic acid and hexamethylenediamine. During its synthesis and processing, unqualified products and scraps will be produced. At the same time, various nylon 66 products are difficult to dispose of after being used, which not only causes waste, but also pollutes the environment. Therefore, the recycling of waste nylon-66 has attracted widespread attention from the society. How to turn waste into treasure and give full play to its economic and social benefits has become a research hotspot. At present, the main...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/14C07C51/06C07C211/12C07C209/50C08G73/00A01N47/44A61K31/785A01P1/00A61P31/00
Inventor 王邃李海龙张振民孙利民魏丹毅
Owner NINGBO UNIV
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