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Char-forming agent based on tripiperazine-triazine and preparation method thereof

A technology of char-forming agent and piperazine, which is applied in the field of macromolecular char-forming agent and its preparation, can solve problems such as difficult removal and uncontrollable product structure

Active Publication Date: 2020-10-23
JINHU JINLING NEW MATERIAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to: provide a kind of char-forming agent based on tripiperazine-triazine structure and its preparation method, pre-form tripiperazine-triazine, expand network structure, improve reaction probability, solve existing triazine char-forming agent There are problems that Cl is difficult to remove and the structure of the product is uncontrollable. Its raw materials come from a wide range of sources, and the preparation process is mild and controllable.

Method used

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  • Char-forming agent based on tripiperazine-triazine and preparation method thereof
  • Char-forming agent based on tripiperazine-triazine and preparation method thereof
  • Char-forming agent based on tripiperazine-triazine and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Example 1: Prepare a carbon-forming agent based on the tripiperazine-triazine structure according to the following steps

[0044] (1) Preparation of Boc-piperazine: Take 4.31g (0.05mol) of piperazine and add 100ml of CH at 25°C 2 Cl 2 In the solution, stir in a 250ml three-neck flask at a speed of 300r / min until uniform; 5.45g (0.025mol) of di-tert-butyl dicarbonate (Boc reagent), dissolved in 50ml of CH 2 Cl 2 The solution is placed in a constant pressure dropping funnel; after the piperazine dissolves, the Boc solution is added dropwise to the piperazine solution at a rate of 1-2 drops / s, and the temperature of the system is controlled at 25°C. React for 20h, TLC monitors the reaction end point; there will be a white precipitate during the dropwise addition, after the reaction is completed, the product is suction filtered to remove the white precipitate, and washed with water; the solution is transferred to a separatory funnel, and the 2 Cl 2 Extract three times,...

Embodiment 2

[0049] Example 2: Step (1)-step (3) is the same as Example 1; wherein, the preparation of step (4) prepolymer A2: take 2.40g (0.04mol) of ethylenediamine and add it to 60ml NMP solution at 20°C , while adding acid-binding agent pyridine 0.95g (0.012mol) and 5gCaCl 2 Stir in a three-necked flask at a speed of 300r / min until uniform, and the system passes through N 2 Protect and connect the tail gas absorption device; take phthaloyl chloride 9.34g (0.046mol) and dissolve it in 60ml NMP and place it in a constant pressure dropping funnel, drop the phthaloyl chloride solution at a rate of 1-2 drops / s Add it in the piperazine solution, control the system temperature at 25°C, continue to react for 0.5h after the dropwise addition, and obtain the solution of the prepolymer A2; step (5) preparation of the macromolecule char-forming agent: take 1.66g (0.005mol ) Tripiperazine-triazine is dissolved in 20ml NMP and placed in a constant pressure dropping funnel, after the prepolymer diss...

Embodiment 3

[0050] Example 3: Step (1)-step (3) is the same as Example 1; wherein, the preparation of step (4) prepolymer A2: take p-phenylenediamine 2.16g (0.02mol) and add 40ml NMP solution at 20°C , add 1.01g (0.01mol) of acid-binding agent triethylamine and 4g CaCl at the same time 2 Stir in a three-necked flask at a speed of 300r / min until uniform, and the system passes through N 2 Protect and connect the tail gas absorption device; take 5.07g (0.025mol) of isophthaloyl chloride and dissolve it in 40ml NMP and place it in a constant pressure dropping funnel, drop the isophthaloyl chloride solution at a rate of 1-2 drops / s Add it into the piperazine solution, control the system temperature at 40°C, continue to react for 1h after the dropwise addition, and obtain the solution of prepolymer A2; step (5) preparation of macromolecular char-forming agent: take 1.33g (0.004mol) Dissolve the tripiperazine-triazine in 20ml NMP and place it in a constant pressure dropping funnel; after the pr...

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Abstract

The invention relates to a tripiperazine-triazine based charcoal forming agent and a preparation method thereof. The general formula of the tripiperazine-triazine based charcoal forming agent is shown in picture 1, wherein B is tripiperazine-triazine, A is a prepolymer with a certain polymerization degree obtained from binary acyl chloride and diamine. The method includes substituting piperazine for three chlorines on cyanuric chloride to obtain tripiperazine-triazine (B3); preparing the prepolymer (A2) with a certain polymerization degree through reaction between the binary acyl chloride and the diamine; allowing polymerization reaction between the tripiperazine-triazine and the prepolymer to form the triazine-ring-containing macromolecular charcoal forming agent with a network structure. The tripiperazine-triazine based charcoal forming agent and the preparation method thereof have the advantages that the source of the raw materials is extensive, the raw materials are cheap and easy to get, the polymerization process is simple and easy to operate, and conditions are mild and controllable during forming of the network structure; the product has few chloride residues and high charcoal forming amount and can foam; the charcoal forming agent can be applied to intumescent flame retardants or non-charcoal-forming polymers.

Description

technical field [0001] The invention relates to a macromolecular char-forming agent and a preparation method thereof, in particular to a char-forming agent based on a tripiperazine-triazine structure and a preparation method thereof. Background technique [0002] Polymer materials are widely used in construction, transportation, automobiles, toys, electrical appliances, etc., but the flammability of these materials has brought huge losses to people's production and life. Therefore, people's requirements for the flame retardancy of polymer materials are also Higher and higher. Intumescent flame retardants are a kind of green and environmentally friendly flame retardants, which have played a good flame retardant effect in many polymers. However, the char-forming agent in the traditional intumescent flame retardant system is pentaerythritol, a small molecule, which is easy to absorb moisture and migrate, which affects its application in polymer materials. Therefore, many new ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06C07D251/54
CPCC07D251/54C08G73/06
Inventor 王文钦李娟凌坤华陈希磊孙立水
Owner JINHU JINLING NEW MATERIAL SCI & TECH
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