Preparation of micromolecular phosphorus-magnesium flame retardant and application of micromolecular phosphorus-magnesium flame retardant in preparation of flame-retardant copolyester material

A technology of flame-retardant copolyester and flame retardant, which is applied in the direction of hypophosphorous acid, phosphorous acid, phosphorus oxyacid, etc., can solve the problems of affecting the mechanical properties of PET materials, poor dispersion of inorganic hydroxides, and easy agglomeration. Achieve excellent flame retardant and smoke suppression performance, good flame retardant and smoke suppression effect, and excellent flame retardant performance

Active Publication Date: 2021-05-28
NORTHWEST NORMAL UNIVERSITY +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Inorganic hydroxides (magnesium oxide, magnesium hydroxide, aluminum hydroxide) decompose when heated (340-490°C), absorb the surface heat of the combustibles, and play a role in flame retardancy; but due to the unmodified inorganic hydroxide Poor dispersibility, it is difficult to disperse uniformly in organic polymer materials, poor compatibility, easy to agglomerate, seriously affect the mechanical properties of PET materials, and to achieve a certain flame retardancy requires a large dose, therefore, the selection performance is excellent and the price is low. It is modified by cheap surface modifiers to improve its compatibility in PET polymer matrix materials, which can not only ensure the mechanical properties of PET materials, but also improve the flame retardancy

Method used

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  • Preparation of micromolecular phosphorus-magnesium flame retardant and application of micromolecular phosphorus-magnesium flame retardant in preparation of flame-retardant copolyester material
  • Preparation of micromolecular phosphorus-magnesium flame retardant and application of micromolecular phosphorus-magnesium flame retardant in preparation of flame-retardant copolyester material
  • Preparation of micromolecular phosphorus-magnesium flame retardant and application of micromolecular phosphorus-magnesium flame retardant in preparation of flame-retardant copolyester material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Add 300 mL of ethanol to a 500 mL round-bottomed flask, weigh 13.64 mL of phosphoric acid and add it to the round-bottomed flask. When the temperature rises to 60°C, the phosphoric acid is completely dissolved in ethanol, and then 5.83 g of magnesium hydroxide is weighed and added to the flask. Among them, the heating temperature was raised to 80°C, the reaction was carried out under stirring conditions for 5 hours, the product was filtered by hot filtration, the product was washed 3 times, and dried in a vacuum oven at 80°C for 6 hours to obtain a white solid powder, which was a phosphorus-magnesium flame retardant.

[0040] (2) 498g of terephthalic acid, 242g of ethylene glycol, 0.0498g of antimony trioxide and 4.98g of phosphorus-magnesium flame retardant were added to a 1.5L magnetic stirring reaction kettle, filled with nitrogen to make the pressure reach 0.05MPa, The temperature was raised to 235°C and the reaction was carried out for 4.5 hours. After the ester...

Embodiment 2

[0043] (1) Same as Example 1;

[0044] (2) Add 498g of terephthalic acid, 242g of ethylene glycol, 0.0498g of antimony trioxide and 14.9g of phosphorus-magnesium flame retardant to a magnetic stirring reaction kettle with a volume of 1.5L, and fill with nitrogen to make the pressure reach 0.05MPa , raise the temperature to 235°C and react for 4.5h. After the esterification reaction, remove the moisture produced by the reaction to keep the pressure in the kettle at normal pressure, close the esterification valve, and react at 100°C and normal pressure for 0.5h. After the normal pressure reaction is over, open the polycondensation valve and turn on the vacuum pump. In the semi-vacuum state, the semi-polycondensation reaction is carried out at 250 °C for 0.5 h. After the reaction is completed, the full polycondensation reaction is carried out at 275 °C for 6 h in a full vacuum state, and an appropriate amount of nitrogen is introduced to discharge the material. , dicing and dryin...

Embodiment 3

[0047] (1) Same as Example 1;

[0048] (2) Add 498g of terephthalic acid, 242g of ethylene glycol, 0.0498g of antimony trioxide and 24.9g of phosphorus-magnesium flame retardant into a 1.5L magnetic stirring reaction kettle, fill with nitrogen to make the pressure reach 0.05MPa, The temperature was raised to 235°C and the reaction was carried out for 4.5 hours. After the esterification reaction was completed, the moisture produced by the reaction was removed to keep the pressure in the kettle at normal pressure. After the normal pressure reaction is over, open the polycondensation valve and turn on the vacuum pump. In the semi-vacuum state, the semi-polycondensation reaction is carried out at 250 °C for 0.5 h. After the reaction is completed, the full polycondensation reaction is carried out at 275 °C for 6 h in a full vacuum state, and an appropriate amount of nitrogen is introduced to discharge the material. , dicing and drying to obtain a phosphorus-magnesium halogen-free a...

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Abstract

The invention discloses a preparation method of a micromolecular phosphorus-magnesium flame retardant. The method comprises the following steps: dissolving inorganic phosphoric acid in absolute ethyl alcohol, adding magnesium hydroxide, stirring and reacting at 60-80 DEG C for 5-6 hours, filtering, washing and drying to obtain white solid powder, namely the micromolecular phosphorus-magnesium flame retardant. The inorganic phosphoric acid is one of phosphoric acid, phosphorous acid and hypophosphorous acid. The small molecular phosphorus-magnesium flame retardant is used for preparing the phosphorus-magnesium type halogen-free low-smoke intrinsic flame-retardant copolyester material HAMH-PET. HAMH-PET has excellent flame retardance, smoke suppression, drip resistance and mechanical properties due to high compatibility of HAMH and a PET matrix and a compact spherical structure formed by a wrapping product generated by phosphorus and magnesium in a combustion process.

Description

technical field [0001] The invention relates to a preparation method of a small-molecule phosphorus-magnesium flame retardant, and also relates to the application of the small-molecule phosphorus-magnesium flame retardant in the preparation of flame-retardant copolyester materials, belonging to the technical field of flame-retardant materials and high Molecular materials technology field. Background technique [0002] Polyethylene terephthalate (PET) is a thermoplastic polymer material. Due to the special linear structure, it has the characteristics of high strength, chemical corrosion resistance, electrical insulation, friction resistance and excellent thermal stability. It can maintain excellent physical properties and dimensional stability in a wide temperature range, is easy to process and spin, and has low cost; therefore, it is widely used in the production of fibers, bottle flakes, films and engineering plastics. life has a very important impact. [0003] The oxyge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/34C01B25/163C01B25/165C08G63/692C08G63/78C09K21/04
CPCC01B25/34C01B25/163C01B25/165C08G63/6926C08G63/78C09K21/04
Inventor 雷自强李宏涛管洁陈登龙温娜李兴尧丁浩李晴刘金玲李菊赵璞芳
Owner NORTHWEST NORMAL UNIVERSITY
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