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Synergistic Halogen-free Flame Retardant System of Dialkyl Dithiophosphite and Organic Phosphite and Its Application

A technology of dialkyl dithiohypophosphite and organic phosphite, which is applied in the field of flame retardants, can solve the problems of material flame retardant failure, easy generation of phosphine, cost increase, etc., and achieve excellent performance

Active Publication Date: 2020-05-19
ZHEJIANG UNIV
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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 thermoplastic engineering plastics
[0006] One is that the two components will react and decompose at high temperature to a certain extent, producing a small amount of acidic substances, which will corrode the metal parts of the processing equipment, and the parts need to be replaced after a certain period of time, which will increase and reduce the cost The problem of production efficiency; the second is that there is a certain precipitation of the nitrogen-containing compound MPP. During the injection molding process of the material, after injection molding a product with a certain modulus, there will be deposits on the mold. The existence of these deposits will affect the appearance of the product. This requires shutdown to clean the mold, which will also reduce production efficiency. At the same time, this precipitation will also cause the flame retardant to migrate to the surface of the product, resulting in uneven distribution and loss of the flame retardant, which will eventually cause the flame retardant of the material to fail, posing a safety hazard; The third is that the addition amount is large, which has a great influence on the mechanical properties of the material
[0007] In general, the flame retardant systems currently used in glass fiber reinforced thermoplastic engineering plastics have problems such as color, generation of toxic gases, easy precipitation, corrosion, and reduced mechanical properties of materials. lead to increased costs, reduced efficiency, etc.

Method used

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  • Synergistic Halogen-free Flame Retardant System of Dialkyl Dithiophosphite and Organic Phosphite and Its Application
  • Synergistic Halogen-free Flame Retardant System of Dialkyl Dithiophosphite and Organic Phosphite and Its Application
  • Synergistic Halogen-free Flame Retardant System of Dialkyl Dithiophosphite and Organic Phosphite and Its Application

Examples

Experimental program
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Effect test

preparation example Construction

[0062] (1) Preparation of aluminum diisobutyl dithiophosphite

[0063] Prepare respectively 1392g of sodium diisobutyldithiophosphite aqueous solution with a concentration of 20wt% and 228g of an aluminum sulfate solution with a concentration of 30wt%, add 1500g of desalted water in the reactor, and add 75g of a sulfuric acid solution with a concentration of 25wt%, and heat up to 80 ℃, start to add diisobutyl dithiophosphite sodium aqueous solution and aluminum sulfate solution synchronously to the reaction kettle in proportion to obtain diisobutyl dithiophosphite aluminum precipitate, dropwise complete in 2 hours, keep warm for 1 hour, then filtered, washed, and dried to obtain 254g (yield 97%) of diisobutyl aluminum dithiophosphite flame retardant.

[0064] After testing, the initial decomposition temperature of the product is 350°C, and its solubility in water is 0.02%;

[0065] (2) MPP, Melapur 200, purchased from BASF;

[0066] (3) Zinc borate, Firebrake 500, purchased ...

Embodiment 1

[0075] The halogen-free flame retardant compound system is applied to glass fiber reinforced nylon, and the performance of the flame retardant is investigated according to the following steps and test methods.

[0076] (1) Mixing of halogen-free flame retardant system

[0077] Add the components of the compound flame retardant system and other additives that have been weighed in advance according to the ratio into the high-speed mixer, start high-speed stirring, and stir for 10 minutes to complete the mixing of powders and discharge.

[0078] (2) Extrusion granulation of materials

[0079] Set the temperature of each zone of the twin-screw extruder at the predetermined temperature. After the temperature is stable for 20 minutes, add nylon from the hopper, add glass fiber through the glass fiber inlet, and feed the powder mixed in step (1) through the powder feeding hole. Start the host and feeder to complete the extrusion and granulation of the material. The granulated mater...

Embodiment 2

[0092] The implementation process is the same as in Example 1, keeping the total amount of the flame retardant system constant, and adjusting the ratio of aluminum diisobutyldithiophosphite and aluminum methylphosphite. Other materials and proportioning are shown in Table 1, and the obtained material results are shown in Table 1.

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Abstract

The invention discloses a halogen-free flame-retardant system in which dialkyl mono-thiophosphate and organic phosphite are synergetic. The halogen-free flame-retardant system comprises 50%-95% of dialkyl mono-thiophosphate, 5%-40% of organic phosphite and 1%-10% of zinc-containing compound. The structural formula of the dialkyl mono-thiophosphate is shown as the formula (I) or (II), in the formula, R1 and R2 are independently selected from linear alkyl or branched alkyl, and the carbon number is 1-6; M is selected from Mg, Ca, Al, Sb, Sn, Ge, Ti, Fe, Zr, Zn, Ce, Bi, Sr, Mn, Li, Na, K, H or NH4, and m is 1-4. The halogen-free flame-retardant system has the advantages that the system is high in flame retardance and free of migration, does not corrode equipment and the like and is well adapted to a glass fiber reinforced thermoplastic engineering plastic system, and halogen-free flame-retardant glass fiber reinforced thermoplastic engineering plastic with excellent comprehensive performance is obtained.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a halogen-free flame-retardant system in which dialkyl dithiohypophosphite and organic phosphite are synergistic and its use in the preparation of halogen-free flame-retardant glass fiber reinforced thermoplastic engineering plastics Applications. Background technique [0002] Glass fiber reinforced thermoplastic engineering plastics are widely used in the field of electronic appliances because of their good rigidity and impact resistance, low warpage, high dimensional stability, good surface appearance, easy processing and recyclability. Applications in these fields require flame retardant materials, and thermoplastic 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 appli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L77/06C08L67/02C08L83/04C08K13/04C08K7/14C08K5/5398C08K3/38C08K5/5317
CPCC08K2003/387C08L67/02C08L77/06C08L2201/02C08L2201/22C08L2203/20C08L83/04C08K13/04C08K7/14C08K5/5398C08K3/38C08K3/32
Inventor 雷华文韵豪李金忠
Owner ZHEJIANG UNIV