Polyamide-based intumescent flame retardant carbon-forming agent containing piperazine structure in main chain and preparation method and application thereof

A technology of intumescent flame retardant and polyamide, applied in the field of polyamide intumescent flame retardant charcoal agent and its preparation, which can solve the difficulty of deteriorating the mechanical properties, dielectric properties and processing properties of materials, and increasing the balance of various performance indicators , unsatisfactory charring effect, etc., to achieve the effect of simple and easy preparation process, improved vertical combustion level, and large molecules

Active Publication Date: 2018-11-02
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing studies have shown that small-molecule char-forming agents, such as pentaerythritol and its derivatives, not only have low char-forming efficiency, but also have disadvantages such as poor water resistance, easy moisture absorption, and easy migration, which are difficult to be widely used in practical applications (Polymer Degradation and Stability 97,1737-1744,2012 and Industrial&Engineering Chemistry Research,52,10905-10915,2013); while the traditional polyamide macromolecular charring agents represented by nylon 6, nylon 66 and nylon 1010 solve the problem of small Molecular char formers have disadvantages such as poor water resistance and easy migration, but due to the low nitrogen content in their structure, they do not contain heterocyclic or aromatized structures, and it is difficult to form a large number of stable carbon dioxide through rearrangement and cyclization during combustion. structure, so the charring effect is not ideal, and it is necessary to add a high content to make the flame-retardant polymer material reach the UL 94V-0 level, especially for polyethylene, polypropylene, ethylene-vinyl acetate copolymer, etc. For polyolefin materials that are difficult to flame-retardant, usually the total amount of flame retardant added needs to be more than 35wt%, so that in practical applications, the mechanical properties, dielectric properties, and processing properties of the material will be greatly deteriorated, which will not only increase the balance of various Difficulty of performance index, but also increase cost, such as patent CN104098836-A and literature ACS Applied Materials & Interfaces, 3,3754–3761,2011 and Polymer Engineering and Science, 55,6,1355-1360,2015, etc. Charcoal was reported

Method used

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  • Polyamide-based intumescent flame retardant carbon-forming agent containing piperazine structure in main chain and preparation method and application thereof
  • Polyamide-based intumescent flame retardant carbon-forming agent containing piperazine structure in main chain and preparation method and application thereof
  • Polyamide-based intumescent flame retardant carbon-forming agent containing piperazine structure in main chain and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 1 mol of oxalyl chloride into 1L of chloroform to make it evenly dispersed, and record it as liquid A; then add 1 mol of anhydrous piperazine and 2.0 mol of triethylamine acid-binding agent to 500 mL of chloroform to make it Disperse evenly, record it as liquid B, then add liquid B dropwise into liquid A while stirring at 0°C, raise the temperature to 60°C after the dropwise addition, and react for 12 hours. After the reaction is completed, remove the chloroform, add water to the remaining solid, stir and make a slurry, then suction filter, repeat this process at least 3 times, collect the solid, and dry it to obtain the charcoal agent CA-1.

Embodiment 2

[0038] Add 1 mol of malonyl chloride to 1L of 1,4-dioxane to disperse it evenly, and record it as liquid A; then add 0.95 mol of anhydrous piperazine and 2.1 mol of triethylamine acid-binding agent to Add it into 500mL of 1,4-dioxane to disperse it evenly, record it as liquid B, then drop liquid B into liquid A while stirring at 40°C, raise the temperature to 100°C after the dropwise addition, and react for 8 hours That's it. After the reaction is completed, remove 1,4-dioxane, add ethanol to the remaining solid, stir and beat, then suction filter, repeat this process at least 3 times, collect the solid, and dry it to obtain charcoal agent CA-2.

Embodiment 3

[0040] Add 1mol of succinyl chloride into 1L of chloroform to make it evenly dispersed, and record it as liquid A; then add 0.95mol of anhydrous piperazine and 2.1mol of triethylamine acid-binding agent to 500mL of chloroform to make If the dispersion is uniform, it is recorded as liquid B, and then liquid B is dripped into liquid A while stirring at 0°C. After the dropwise addition, the temperature is raised to 60°C, and the reaction is done for 12 hours. After the reaction is completed, remove the chloroform, add ethanol to the remaining solid, stir and make a slurry, then suction filter, repeat this process at least 3 times, collect the solid, and dry it to obtain the charcoal agent CA-3.

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Abstract

The invention discloses a polyamide intumescent flame-retardant char-forming agent having a main chain containing a piperazine structure; the char-forming agent has the structure general formula defined in the specification, wherein R1 is any one of H, straight-chain or branched-chain alkyl with the number of carbon atoms of 1-4, phenyl, benzyl or phenol, R2 represents straight-chain or branched-chain alkyl with the number of carbon atoms of 1-8, and n is more than or equal to 1. The invention also relates to a preparation method of the intumescent flame-retardant char-forming agent, an application of the intumescent flame-retardant char-forming agent as a carbon source of a novel intumescent flame-retardant system, and an application of the novel intumescent flame-retardant system in halogen-free flame retardancy of polyolefin, polyurethane, polylactic acid, polyamide, ethylene-propylene-diene monomer, silicone rubber and epoxy resin. The prepared intumescent flame-retardant char-forming agent has the advantages of no halogen, low smoke, low toxicity, good thermal stability, high char-forming efficiency, strong water resistance, relatively little influence on mechanical properties of flame-retardant polymers, and simple synthesis process, can be prepared by a one-step method, and is prone to industrialized production.

Description

technical field [0001] The invention belongs to the technical field of an intumescent flame-retardant char-forming agent and its preparation method and application, and in particular relates to a polyamide-based intumescent flame-retardant char-forming agent whose main chain contains a piperazine structure and a preparation method and application thereof. Background technique [0002] With the development of science and technology and the continuous improvement of people's living standards, polymer materials have been more and more widely used in aerospace, electronic appliances, automobiles, building materials, flame-retardant protective clothing and military uniforms, home decoration, packaging films and other fields. Its safety performance, especially its flame retardant performance, puts forward higher requirements. In order to solve the flammability problems of traditional polymer materials such as polyolefin, polyurethane, polyamide, polylactic acid, etc., the existing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/26C08G69/28C08L23/08C08L77/06C08K3/32C08L23/06C08L23/12C08L67/04C08L23/16C08L83/07C08L75/04C08L63/00C08K5/3492C08K9/04
CPCC08G69/26C08G69/28C08K2201/011C08L23/06C08L23/0815C08L23/0853C08L23/12C08L23/16C08L67/04C08L75/04C08L77/06C08L83/04C08L2201/02C08L2205/025C08L2207/066C08L77/02C08K2003/323C08K9/04C08K3/346C08K3/26C08L63/00C08K5/34928C08K3/32
Inventor 王玉忠董亮平邓聪陈宏黄胜超杨爱华李映明陈力
Owner SICHUAN UNIV
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