Halogen-free flame retardant melamine poly-phosphate borate as well as preparation method and application thereof

A technology of melamine polyphosphate borate and melamine polyphosphate, which is applied in the field of flame retardants, can solve the problems of low flame retardant efficiency, easy moisture absorption, and low carbon formation efficiency of melamine polyphosphate, and achieve high carbon formation efficiency and water absorption resistance Good performance, improved water absorption resistance and charcoal efficiency

Active Publication Date: 2019-04-26
JIANGSU LISIDE NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For red phosphorus, although its flame retardant effect is good, it faces two problems: one is the color of red phosphorus, which limits its application range, and is usually only used in black products; the other is that it is easy to generate phosphine during processing and other highly toxic substances, which bring environmental protection and safety problems, so red phosphorus is not the best choice for glass fiber reinforced engineering plastics
However, because melamine polyphosphate is easy to absorb moisture, it is inconvenient to use; at the same time, because melamine polyphosphate is low in charcoal efficiency and low in flame retardancy, the addition of melamine polyphosphate is relatively large, resulting in a decrease in the mechanical properties of the finished product. A series of problems, which limit the large-scale application of melamine polyphosphate in engineering plastics

Method used

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  • Halogen-free flame retardant melamine poly-phosphate borate as well as preparation method and application thereof
  • Halogen-free flame retardant melamine poly-phosphate borate as well as preparation method and application thereof
  • Halogen-free flame retardant melamine poly-phosphate borate as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] a. Add 500mL of deionized water and 186g of melamine to a 1000mL four-necked flask equipped with an electric stirrer, a thermometer and a reflux condenser, stir and heat to 80°C, slowly add 199g of 85wt% phosphoric acid dropwise, within about one hour After the dropwise addition, heat up and stir to 95°C, keep stirring for 2 hours, and increase the stirring speed when the viscosity becomes larger in the later stage. The suspension was filtered, washed several times with deionized water, and dried at 120° C. to obtain 323.7 g of an intermediate.

[0052] b. Add 1000mL of deionized water to a 2000mL four-necked flask equipped with an electric stirrer, a thermometer and a reflux condenser, add 27.2g of boric acid, heat up to 80°C to completely dissolve the boric acid, and add 323.7g of the intermediate obtained in step a , keep the temperature at 80°C, and stir the reaction for 3 hours. The suspension was cooled, filtered and washed several times with deionized water, the...

Embodiment 2

[0073] a. Add 500mL of deionized water and 186g of melamine to a 1000mL four-necked flask equipped with an electric stirrer, a thermometer and a reflux condenser, stir and heat to 60°C, then slowly add 154g of 85% phosphoric acid dropwise for about one hour After the internal dropwise addition, heat up and stir to 85° C., and stir for 1 hour. The viscosity increases later, and the stirring speed is increased. The suspension was filtered, washed several times with deionized water, and then dried at 120° C. to obtain 289.9 g of an intermediate.

[0074] b. Add 800mL of deionized water to a 2000mL four-necked flask equipped with an electric stirrer, a thermometer and a reflux condenser, add 31.6g of boric acid, heat up and stir to completely dissolve the boric acid, continue to heat up to 90°C, and add step a to obtain 289.9g of the intermediate was kept at 100°C, and the reaction was stirred for 3.5h. The suspension was cooled, filtered and washed several times with deionized w...

Embodiment 3

[0081] a. Add 500mL of deionized water and 186g of melamine to a 1000mL four-neck flask equipped with an electric stirrer, a thermometer and a reflux condenser, stir and heat to 100°C, then slowly add 199g of 85% phosphoric acid dropwise for about two hours After the internal dropwise addition, heat up and stir to 90°C for 2h, filter the obtained slurry, wash with deionized water several times, and then dry at 140°C to obtain 332.1g of an intermediate.

[0082] b. Add 1000mL of deionized water and 31.1g of boric acid to a 2000mL four-necked flask equipped with an electric stirrer, a thermometer and a reflux condenser, heat up and stir to completely dissolve the boric acid, continue to heat up to 100°C, and add the obtained in step a 332.1g of the intermediate was kept at a temperature of 92°C, and the reaction was stirred for 3h. The suspension was cooled, filtered, washed several times with deionized water, and dried at 140°C to yield 313.9 g of intermediate product.

[0083...

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Abstract

The invention discloses melamine poly-phosphate borate as well as a preparation method and an application thereof. The structural formula of melamine poly-phosphate borate is shown in the following formula (I) in the description, wherein m is the molar ratio of two structural units of melamine poly-phosphate borate and boric acid and is 3-6. The preparation process comprises the steps as follows:a. dispersing melamine in water, mixing the melamine solution with phosphoric acid, and performing thermal reaction at 70-100 DEG C to obtain an intermediate; b, mixing boric acid with water until boric acid is completely dissolved, then mixing the solution with the intermediate prepared in the step a, and continuously raising the temperature to 80-100 DEG C for thermal reaction to obtain an intermediate product; c, performing thermal treatment on the intermediate product prepared in step b at 300-360 DEG C. Melamine poly-phosphate borate prepared with the process has the advantages of good water absorption resistance and high carbonization efficiency, and can be compounded with organic hypophosphite for flame retardant treatment on engineering plastics such as glass fiber reinforced nylon, polyester and the like.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a halogen-free flame retardant polyphosphate borate melamine salt and its preparation method and application. Background technique [0002] Glass fiber reinforced engineering plastics, such as various nylons and polyesters (such as PBT, PET), etc., are favored due to their good rigidity and impact resistance, low warpage, high dimensional stability, and good surface appearance. Widely used in the field of electronic appliances. Applications in these fields require flame retardant materials, and most engineering plastics are flammable materials. After compounding with glass fibers, glass fiber reinforced engineering plastics are easier to burn due to the wick effect of glass fibers. Therefore, when glass fiber reinforced engineering plastics are applied in these fields, it is necessary to solve the problem of flame retardancy, and the existence of the wick effect makes i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/3492C07D251/56C08L77/06C08L67/00C08K5/5313C08K7/14
CPCC07D251/56C08K5/34928C08K5/5313C08K7/14C08K2201/003C08L2201/02C08L2201/22C08L77/06C08L67/02
Inventor 李金忠杨建伟
Owner JIANGSU LISIDE NEW MATERIAL
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