Macromolecule triazine charring agent with main chain containing piperazidine structure, and preparation method thereof

A technology of triazine char-forming agent and macromolecule, which is applied in the field of char-forming agent, macromolecular triazine char-forming agent and its preparation, which can solve the problem of less side chains, achieve short reaction time, reduce production cost, and thermal stability good sex effect

Active Publication Date: 2014-04-09
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] As far as the current research reports are concerned, the focus of the research is on the composition and structure of the main chain, while there are relatively few studies on the side chains, especially the new macromolecular triazine char-forming agents with catalytic groups in the side chains have not yet been published. to report

Method used

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  • Macromolecule triazine charring agent with main chain containing piperazidine structure, and preparation method thereof
  • Macromolecule triazine charring agent with main chain containing piperazidine structure, and preparation method thereof
  • Macromolecule triazine charring agent with main chain containing piperazidine structure, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step (1). With 86 grams of anhydrous piperazine C 4 h 10 N 2 (1mol) mixed with 101 grams of triethylamine (1mol), in an argon atmosphere, stirred for 1 hour at 25°C;

[0029] Step (2). Add 1L of N-methylpyrrolidone solution of cyanuric chloride with a concentration of 1mol / L, and react for 8 hours at 25°C;

[0030] Step (3). Adding 1L concentration of HN(CH 3 )(CH 2 ) 10 SO 3 H in N-methylpyrrolidone solution, then add 101 grams of triethylamine (1mol), raise the temperature to 80°C, and react for 12 hours;

[0031] Step (4). After the reaction, suction filtration, water washing, and drying were performed to obtain a macromolecular triazine char-forming agent with the following structure. The average molecular weight of the macromolecular triazine char-forming agent was 29,400.

[0032]

Embodiment 2

[0034] Step (1). With 86 grams of anhydrous piperazine C4 h 10 N 2 (1mol) mixed with 112 grams of potassium hydroxide (2mol), in a nitrogen atmosphere, stirred at 30°C for 50 minutes;

[0035] Step (2). Add 1 L of N-N dimethylformamide solution of cyanuric chloride with a concentration of 0.5 mol / L, and react for 7 hours at 30° C.;

[0036] Step (3). Adding 1L concentration of HN(CH 3 )(CH 2 ) 5 SO 3 H N-N dimethylformamide solution, then add 28 grams of potassium hydroxide (0.5mol), raise the temperature to 90°C, and react for 12 hours;

[0037] Step (4). After the reaction, suction filtration, water washing, and drying were performed to obtain a macromolecular triazine char-forming agent with the following structure. The average molecular weight of the macromolecular triazine char-forming agent was 68,400.

[0038]

Embodiment 3

[0040] Step (1). With 86 grams of anhydrous piperazine C 4 h 10 N 2 (1mol) was mixed with 60 grams of sodium hydroxide (1.5mol), and stirred at 35° C. for 45 minutes in an argon atmosphere;

[0041] Step (2). Add 10L of N-N dimethylacetamide solution of cyanuric chloride with a concentration of 0.1mol / L, and react at 35°C for 6 hours;

[0042] Step (3). Adding 5L of concentration to the reaction solution is 0.1mol / L of HN(CH 3 )(CH 2 ) 8 SO 3 K's N-N dimethylacetamide solution, then add 32 grams of sodium hydroxide (0.8mol), raise the temperature to 100°C, and react for 11 hours;

[0043] Step (4). After the reaction, suction filtration, water washing, and drying, the macromolecular triazine char-forming agent with the following structure was obtained, and the average molecular weight of the macromolecular triazine char-forming agent was 126,600.

[0044]

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Abstract

The invention relates to a macromolecule triazine charring agent with main chains containing piperazidine structures and a preparation method thereof. According to the invention, a group with the catalytic action is introduced into a triazine macromolecule polymer with the main chains containing the piperazidine structures, and is integrated with a charring agent, so as to generate the catalytic action nearby; or, the group with the catalytic action can also be fixed on molecular chains of the polymer, so as to prevent migration and uneven dispersion and therefore greatly improve catalytic efficiency. The specific preparation method is as follows: firstly, a binary substance and an acid-binding agent are mixed, and then are stirred for 0.5 to 1 hour in inert gas atmosphere, so as to obtain a compound with bifunctional reactive hydrogen; the compound is added into a cyanuric chloride aprotic organic solvent to react for 4 to 8 hours, and then is added into an aprotic organic solvent containing sulfonic acid group activated monomers to react for 8 to 12 hours by adding the catalytic agent and the acid-binding agent; and finally, the product is obtained through filtering, washing and drying. The method provided by the invention has continuous reaction process, short reaction time and high reaction efficiency.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a char-forming agent, in particular to a macromolecular triazine char-forming agent whose main chain contains a piperazine structure and whose side chain has a catalytic effect and a preparation method thereof. Background technique [0002] Intumescent flame retardant is one of the types of flame retardants widely used in recent years. This flame retardant overcomes the fact that halogenated flame retardants are easy to emit irritating and corrosive gases and smoke when burning, pollute the environment, and endanger human health. , while corroding equipment and other shortcomings, it is a very promising green and environmentally friendly flame retardant. Intumescent flame retardants generally consist of three basic components: acid source, carbon source, and gas source. When burning, the "three sources" can be effectively matched to form a non-combustible carbon foam lay...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C08G73/06
Inventor李娟朱荧科陶慷石虎砚薛立新
OwnerNINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI