Method for producing high-purity triazine-based charring agent

A production method and technology of triazines, which are applied in the field of production of high-purity triazines char-forming agents, can solve problems such as low yield, poor product stability, and poor polymer compatibility, so as to reduce loss rate and improve purity , the effect of easy temperature control

Inactive Publication Date: 2018-12-14
中山苏特宝新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] CN1709968A and document J.Journal of Applied Polymer Sci.94,1556~1561,2004 all disclose the structure and preparation method of triazine expansion flame retardant charring agent respectively; CN1715272A, CN101024632A and Li Bin etc. (J.Polymer Degration and Stability.91, 1380-1386, 2006) also reported linear polymeric triazine derivative char-forming agents and their synthesis methods, but because the polymeric triazine derivatives synthesized in the above literature are rich in hydroxyl groups, their water resistance It is still poor, and then has a greater impact on the flame retardant efficiency, and secondly, it has poor compatibility with polymers, and has a greater impact on the mechanical properties of materials;
Although the method disclosed in the above patent has achieved certain effects, the synthesis time of the triazine char-forming agent is long, the reaction process is discontinuous, the stability of the obtained product is poor, and the residual chlorine content is relatively high, and the yield is relatively low

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  • Method for producing high-purity triazine-based charring agent

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Experimental program
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Effect test

Embodiment 1

[0038] In a 500L reactor with a stirring and condensing device, when the temperature of the pure water in the reactor is lower than 10°C, suspend and disperse 25.00kg of cyanuric chloride in 250L of pure water, slowly add 184L of 25% ammonia solution, and control The reaction temperature is within 15°C, after the addition is completed, the temperature is kept at 58-60°C, and the reaction time is 2 hours; after the reaction is completed, the above solution is pressed into a filter press for press filtration to obtain a semi-finished product A with a solid content of 31.25%; at the same time The press filtrate can be recycled; then, add 62.41kg of the above-mentioned semi-finished product and 160L of pure water into a 500L reactor with a stirring and reflux device, after fully dispersing, control the temperature at 25-30°C, add 5.80kg of piperazine, After the addition is completed, the reaction temperature is controlled at 95-98°C, and then 18.83kg of 30% sodium hydroxide solutio...

Embodiment 2

[0040]In a 1000L reactor with a stirring and condensing device, when the temperature of the pure water in the reactor is lower than 10°C, suspend and disperse 50.00kg of cyanuric chloride in 450L of pure water, slowly add 430L of 25% ammonia solution, and control The reaction temperature is within 20°C. After the addition is complete, keep the temperature at 55°C and the reaction time is 3 hours; after the reaction, press the above solution into a filter press for press filtration to obtain a semi-finished product A with a solid content of 32.15%; It can be recycled; then, add 118.88kg of the above-mentioned semi-finished product and 350L of pure water into a 1000L reactor with a stirring and reflux device. After fully dispersing, control the temperature at 28-35°C, add 11.72kg of piperazine, and complete the addition , control the reaction temperature at 90-95°C, then add 37.66kg of 30% sodium hydroxide solution, the pH of the whole process is controlled at 8-9, after adding, ...

Embodiment 3

[0042] In a 3000L reactor with a stirring and condensing device, when the temperature of the pure water in the reactor is lower than 10°C, suspend and disperse 150.00kg of cyanuric chloride in 1500L of pure water, slowly add 1200L of 25% ammonia solution, and control The reaction temperature is within 14°C. After the addition is complete, the temperature is maintained at 57-60°C and the reaction time is 4 hours; after the reaction is completed, the above solution is pressed into a filter press for press filtration to obtain a semi-finished product A with a solid content of 31.75%; at the same time The press filtrate can be recycled; then, add 368.58kg of the above-mentioned semi-finished product and 1000L of pure water into a 3000L reactor with a stirring and reflux device, after fully dispersing, control the temperature at 28-35°C, add 34.71kg of piperazine, After adding, control the reaction temperature at 95-100°C, then add 112.98kg of 30% sodium hydroxide solution, control ...

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Abstract

The invention provides a method for producing a high-purity triazine-based charring agent. The method comprises the following steps: using cyanuric chloride, 25% aqueous ammonia solution and an aminesubstance as raw materials; using water as a solvent; and adding an alkali substance for production. The method provided by the invention uses the cyanuric chloride, the 25% aqueous ammonia solution and the amine substance as the raw materials, uses the water as the solvent, and adds the alkali substance to synthesize high-purity and high-yield triazine-based charring agent by controlling a reaction temperature and time in a reactor equipped with a stirring device, a condensing device and a refluxing device and in a vacuum drier.

Description

technical field [0001] The invention relates to heterocyclic triazine compounds, in particular to a production method of a high-purity triazine char-forming agent. Background technique [0002] The flame retardancy of polypropylene (PP) has been a research hotspot. But with people's requirements on the environment and the implementation of some environmental protection directives, a new type of halogen-free intumescent flame retardant (IFR) is considered to be a new generation of flame retardants for polyolefins. Halogen-free intumescent flame retardants have the characteristics of halogen-free and low toxicity, high flame retardant efficiency and good resin compatibility, and have attracted much attention in the flame retardant modification of polymers. Halogen-free intumescent flame retardants are generally composed of three components: char-forming agent, acid source (usually ammonium polyphosphate, APP) and gas source (such as nitrogen-containing compounds). Phosphoric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/40C08K5/3492C08L23/12
CPCC07D251/40C08K5/3492C08L2201/02C08L23/12
Inventor 不公告发明人
Owner 中山苏特宝新材料有限公司
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