High-thermal stability macromolecular char-forming agent CPCA, preparation method, composition and application thereof

A technology with high thermal stability and macromolecules, which is applied in the field of flame retardant materials, can solve the problems affecting the mechanical properties of materials, large additions, large water solubility, etc., and achieve simple and efficient preparation methods, weakened combustion strength, and good thermal stability. Effect

Active Publication Date: 2019-10-15
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Abstract
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Problems solved by technology

[0002] With the development trend of various commodities towards lightweight in recent years, the amount of polymer materials is increasing day by day. Therefore, the requirements for the flame retardancy of polymer materials are becoming more and more stringent; intumescent flame retardants are a type of high-efficiency flame retardant developed in recent years. Flame retardants, which include acid sources, gas sources, and carbon sources, and the carbon source determines the shape of the charcoal layer generated when the flame-retardant material is burned and the quality of the barrier effect; although the traditional charcoal agent is low in cost and flame-retardant The effect is good, but it has a great impact on the physical and mechanical properties of flame-retardant products. For example, the typical pentaerythritol char-forming agent is often used in combination with ammonium polyphosphate, but its application is limited due to its large water solubility, while starch Although the price of sorbitol and sorbitol is low, it is added in a large amount when used, and it is easy to degrade and migrate, which affects the mechanical properties of the material, and its application is also limited; therefore, the development of new char-forming agents has attracted the attention of various research institutions.
[0003] Because triazine ring derivatives contain a tertiary nitrogen structure and have excellent char-forming effects, they can be used as carbon sources for intumescent flame retardants. In recent years, some patent applications for triazine derivative char-forming agents have been published, such as The Chinese patent No. CN103333336A "Preparation method of a hyperbranched triazine char-forming agent", the Chinese patent No. CN102702522A "A macromolecular triazine char-forming agent and its preparation method", the Chinese patent No. CN102702521A The patent "macromolecular triazine char-forming agent containing piperazine structure in the main chain and its preparation method" disclos

Method used

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  • High-thermal stability macromolecular char-forming agent CPCA, preparation method, composition and application thereof
  • High-thermal stability macromolecular char-forming agent CPCA, preparation method, composition and application thereof
  • High-thermal stability macromolecular char-forming agent CPCA, preparation method, composition and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 17.23g (0.20mol) of anhydrous piperazine and 330ml of chlorobenzene were added to the reaction vessel and stirred for dissolution, and 37.45g (0.35mol) of anhydrous sodium carbonate acid-binding agent was added to the reaction vessel; then 18.44g (0.10mol) of three Polycyanuric chloride is dissolved in 200ml of chlorobenzene solvent, 0.79g (0.01mol) pyridine is dissolved in 20ml of chlorobenzene solvent; At 25 ℃, the chlorobenzene solution containing cyanuric chloride is dripped into the reaction at a speed of 5ml / min. In the container, after the dropwise addition, the temperature of the reaction system was raised to 100°C for 1 hour, and then the pyridine solution was added to the system for 7 hours of reaction. After the reaction was completed, it was filtered and washed with water, each time for 25 minutes. After repeated washing for five times, it was dried to obtain high heat Stable macromolecular char-forming agent CPCA, the yield is 99.1%, and the temperature corr...

Embodiment 2

[0033] 25.84g (0.30mol) of anhydrous piperazine and 300ml of dioxane were added to the reaction vessel and stirred to dissolve, and 64.2g (0.6mol) of anhydrous sodium carbonate acid-binding agent was added to the reaction vessel; then 33.18g (0.18mol) ) cyanuric chloride is dissolved in 300ml dioxane solvent, 1.5g (0.025mol) urea is dissolved in 20ml dioxane solvent; Dioxane solution was dropped into the reaction container. After the dropwise addition, the reaction system was heated to 95°C for 4 hours, and then the urea solution was added to the system to react for 2 hours. After the reaction was completed, suction filtration and water washing were performed, and the washing was repeated for 20 minutes each time. After four times, the target product CPCA was obtained by drying, the yield was 98.1%, and the temperature corresponding to 5% of its decomposition was 424°C; the CPCA of 6wt.%, the ammonium polyphosphate of 25wt.% were uniformly mixed, and then mixed with 69wt.% The...

Embodiment 3

[0035] Add 25.84g (0.30mol) of anhydrous piperazine and 350ml of tetrahydrofuran into the reaction vessel and stir to dissolve, add 50.5g (0.5mol) of triethylamine acid-binding agent into the reaction vessel; Dissolve cyanogen in 300ml tetrahydrofuran solvent, dissolve 1.8g (0.03mol) ethylenediamine in 15ml tetrahydrofuran solvent; drop the dioxane solution containing cyanuric chloride into the reaction at a speed of 5ml / min at 30°C In the container, after the dropwise addition, the temperature of the reaction system was raised to 95°C for 7 hours, and then ethylenediamine solution was added to the system for 1 hour of reaction. After the reaction was completed, suction filtration and water washing were performed for 25 minutes each time. After repeated washing four times, it was dried Obtain the target product CPCA, the yield is 99.0%, and the temperature corresponding to its decomposition of 5% is 423°C; 3wt.% CPCA, 22wt.% ammonium polyphosphate are uniformly mixed, and then ...

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Abstract

The invention discloses a macromolecular char-forming agent (CPCA) with high thermal stability, a preparation method, a composition and application thereof. The macromolecular char-forming agent (CPCA) with high thermal stability is prepared mainly by dehydrochlorination of the C-Cl bond on cyanuric chloride and the N-H bond in anhydrous piperazine and introduction of a small amount of small molecular nitrogen-containing compounds which can react with the C-Cl bond on the cyanuric chloride. The invention also provides a composition containing the CPCA, the composition comprises the CPCA and ammonium polyphosphate. The composition containing the CPCA can be melted and blended with polyolefin resin to prepare halogen-free flame retardant polyolefin materials. The composition has excellent flame retardant efficiency under the condition of very low CPCA content, can obviously improve the limiting oxygen index (up to more than 40%) of polyolefin, has a vertical combustion (UL94) grade of V-0 grade, has a heat release rate peak value reduced by more than 80% when burning compared with a pure sample, and maintains a high carbon residue rate.

Description

technical field [0001] The invention belongs to the technical field of flame retardant materials, and in particular relates to a high thermal stability macromolecular char-forming agent CPCA, its preparation method and composition and its application. Background technique [0002] With the development trend of various commodities towards lightweight in recent years, the amount of polymer materials is increasing day by day. Therefore, the requirements for the flame retardancy of polymer materials are becoming more and more stringent; intumescent flame retardants are a type of high-efficiency flame retardant developed in recent years. Flame retardants, which include acid sources, gas sources, and carbon sources, and the carbon source determines the shape of the charcoal layer generated when the flame-retardant material is burned and the quality of the barrier effect; although the traditional charcoal agent is low in cost and flame-retardant The effect is good, but it has a gre...

Claims

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Application Information

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IPC IPC(8): C08G73/06C08L79/04C08L23/06C08L23/08C08L23/12
CPCC08G73/0633C08G73/0638C08G73/065C08L23/06C08L23/0853C08L23/12C08L79/04C08L2201/02C08L2201/08C08L2201/22
Inventor 钱立军汤维陈雅君许博
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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