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Compound halogen-free flame retardant system for TPE based on dialkyl dithiophosphinate and its application

A technology of dialkyl dithiophosphinate and system, applied in the field of halogen-free flame-retardant TPE, which can solve the problems of low mechanical strength, poor flame retardancy, material appearance and color of TPE materials, etc.

Active Publication Date: 2019-08-20
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sometimes in order to reduce the amount of inorganic hydroxide added, red phosphorus synergy is also used, but the application of red phosphorus will have problems with the appearance and color of the material, and the combustion of red phosphorus is likely to produce toxic gases such as phosphine and a large amount of smoke. So this is not the best solution either
For the flame retardant system of high polymerization degree ammonium polyphosphate (APP), it belongs to an intumescent flame retardant system. Due to its strong flame retardancy, its addition amount is greatly reduced compared with the inorganic hydroxide system, but APP is due to its Due to the hydrophilic nature of the surface, it is still incompatible with the matrix material, so the mechanical strength of the flame-retardant TPE material of the APP system is still very low. What is even more fatal is that due to the presence of ammonium ions, APP is easy to absorb moisture. After a period of time, TPE products The presence of water droplets on the surface will greatly reduce the insulation performance of the material, which will bring safety hazards. Secondly, the incompatibility between the APP system and the base material will migrate obviously from the inside of the material to the surface. As time goes by, the content of the internal flame retardant will be reduced, and the flame retardant performance of the material will decrease or even disappear.
[0005] In general, the main defects of the flame retardant system currently applied to TPE materials are: poor flame retardancy, easy migration, easy moisture absorption, and poor compatibility with the base TPE material.

Method used

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  • Compound halogen-free flame retardant system for TPE based on dialkyl dithiophosphinate and its application
  • Compound halogen-free flame retardant system for TPE based on dialkyl dithiophosphinate and its application
  • Compound halogen-free flame retardant system for TPE based on dialkyl dithiophosphinate and its application

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0049] Preparation of Aluminum Diisobutyldithiophosphite

[0050] 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.

[0051] After testing, the initial decomposition temperature of the product is 350°C, and its solubility in water is 0.02%;

Embodiment 1

[0054] (1) Compounding and surface treatment of halogen-free flame retardant system

[0055] Each material was ground in a ball mill with an average particle size of about 5 μm and a maximum particle size of 40 μm. Add aluminum diisobutyldithiophosphite, pentaerythritol and melamine that have been weighed in advance according to the proportion in the kneader, start stirring, and turn on the heating unit to raise the temperature of the material to 110°C and keep it for 30 minutes to remove the moisture in the material , and then add 2% aluminate based on the total weight of the material, and mix and treat for 20 minutes to obtain a well-mixed and surface-treated compound flame retardant system.

[0056] (2) Characterization of compound flame retardant system

[0057] Samples were taken for TGA test to obtain the temperature at which the weight loss of the compound flame retardant system was 2% and 5%, and the temperature at which the maximum decomposition rate was obtained on ...

Embodiment 2

[0067] The implementation process is the same as that of Example 1, except that the char-forming agent of the flame retardant system is selected from Saike. The materials and proportions of each compound flame retardant system in the examples are shown in Table 1, and the characterization results of thermal weight loss are shown in Table 1. The performance test results of the composite materials obtained by applying the compound flame retardant system to TPE are shown in Table 1.

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Abstract

The invention discloses a compound halogen-free flame retardant system for TPE, electric wires and cables based on dialkylphosphorodithiloate. The compound halogen-free flame retardant system is prepared from the following raw materials in percentage by weight: 30 to 50 percent of the dialkylphosphorodithiloate, 20 to 30 percent of charring agent and 20 to 40 percent of nitrogen source-containingcompound. The structural formula of the dialkylphosphorodithiloate is shown as the following formula (I); in the formula, R1 and R2 are separately selected from linear alkyl or branched alkyl; M is selected from Mg, Ca, Al, Sb, Sn, Ge, Ti, Fe, Zr, Zn, Ce, Bi, Sr, Mn, Li, Na, K, H or NH4; m is 1 to 4. The novel halogen-free flame retardant system has the characteristics of high flame retardance, migration resistance, no moisture absorption, compatibility with a matrix TPE material and the like and can be applied to the TPE; the prepared halogen-free flame retardant TPE material is used as an insulating material in the fields of high-end electronic consumer goods such as the electric wires and the cables and electrical appliances. (The formula is shown in the description).

Description

technical field [0001] The invention relates to the technical field of halogen-free flame-retardant TPE, in particular to a compound halogen-free flame-retardant system for TPE based on dialkyl dithiophosphinate and its application. Background technique [0002] Thermoplastic elastomer (TPE) based on SEBS, its basic composition includes SEBS, white oil and thermoplastic resin, etc., is a kind of polymer alloy material with general plastic processing performance, but the product has similar cross-linked rubber performance. The double bond in the molecular structure of SEBS is saturated, so it has anti-aging characteristics; the composition does not contain halogen, it is safe and non-toxic, good stability, soft texture, beautiful appearance, comfortable hand feeling, good resilience and strong moisture resistance Slidability; thermoplastic elastomers are also different from ordinary rubber, rubber cannot be recycled after cross-linking, and thermoplastic elastomers are recycl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5398C08K5/053C08K5/3492C08K9/04C08K13/06C08L53/02C08L91/06C08L23/12
Inventor 雷华文韵豪李金忠
Owner ZHEJIANG UNIV