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Preparation method for halogen-free flame retardant and flame retardant polyolefin composition thereof

A composition and polyolefin technology, applied in the preparation of halogen-free flame retardants, the field of flame retardant polyolefin compositions, can solve the problems of easy discoloration, low yield, low yield, etc., and achieve excellent physical properties, high purity, The effect of high flame retardant properties

Inactive Publication Date: 2014-08-20
KINGFA SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the problem of low yield in the preparation of existing piperazine diphosphate, and to provide a preparation method of piperazine diphosphate
[0006] Another object of the present invention is to overcome the problems of low yield and easy discoloration in the existing piperazine pyrophosphate preparation method, and provide a preparation method of piperazine pyrophosphate

Method used

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  • Preparation method for halogen-free flame retardant and flame retardant polyolefin composition thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0061] Weigh 23 kg of phosphoric acid solution and add it to 20 L of water, dissolve 8.6 kg of piperazine in 30 L of water and add it to the phosphoric acid solution through the feeding pipe, and stir for 4 hours at room temperature. Then heat up to 60°C, connect the reaction solution to the feed pump of the spray dryer with a feed pipe, then enter the spray dryer, and centrifugally spray dry at a speed of 18000r / min. The drying hot air temperature is 150°C to obtain 28.0 kg piperazine diphosphate.

Embodiment 2

[0063] Weigh 25.4kg of phosphoric acid solution and add it to 20L of water, dissolve 8.6kg of piperazine in 30L of water and add it to the phosphoric acid solution through the feeding pipe, and stir for 4 hours at room temperature. Then the temperature was raised to 60°C, and the reaction solution was connected to the feed pump of the spray dryer with a material pipe, and then entered into the spray dryer, and was centrifugally sprayed and dried at a speed of 8000r / min, and the drying hot air temperature was 160°C to obtain 27.8 kg piperazine diphosphate.

Embodiment 3

[0065] Weigh 23kg of phosphoric acid solution and add it to 20L of water, dissolve 8.6kg of piperazine in 30L of water and add it to the phosphoric acid solution through the feeding pipe, and stir for 2 hours at room temperature. Then the temperature was raised to 70°C, the reaction liquid was connected to the feed pump of the spray dryer with a feed pipe, and then entered into the spray dryer, and was centrifugally sprayed and dried at a speed of 10000r / min, and the drying hot air temperature was 140°C to obtain 27.5 kg piperazine diphosphate.

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Abstract

Belonging to the field of flame retardant preparation, the invention discloses a preparation method for a halogen-free flame retardant and a flame retardant polyolefin composition thereof. Specifically, piperazine diphosphate is prepared by reacting phosphoric acid with piperazine in proportion, and then performing spray drying treatment; and piperazine pyrophosphate is prepared by combining the preparation method of the piperazine diphosphate, and subjecting the obtained piperazine diphosphate to dehydration condensation reaction under an inert atmosphere or vacuum condition. The invention also provides the flame-retardant polyolefin composition, which comprises 100 parts by mass of polyolefin resin, 10-100 parts by mass of the piperazine pyrophosphate prepared by the method and the like. The yield of the piperazine diphosphate prepared by the method is over 95%, and the piperazine pyrophosphate has a W value represented whiteness of over 90. The flame retardant polyolefin composition has the advantages of excellent flame retardant properties, small adding amount of piperazine pyrophosphate, and excellent coloring properties, thus having terrific industrial application prospects.

Description

technical field [0001] The invention belongs to the field of flame retardant preparation, and more specifically relates to a preparation method of a halogen-free flame retardant and a flame retardant polyolefin composition thereof. Background technique [0002] The halogen-free flame retardant properties of polymer resins have been the most concerned topic in the flame retardant industry in the past ten years. In the existing flame-retardant modified polyolefins, in order to meet the requirements of non-halogenation, it is necessary to choose to add flame retardants containing phosphorus, nitrogen or their compound systems. The most commonly used phosphorus-containing flame retardants and their compositions mainly include microencapsulated red phosphorus, phosphoric acid esters, and intumescent flame-retardant systems mainly composed of ammonium polyphosphate. However, compared with the traditional bromine-antimony compound flame retardant system, these flame retardant syst...

Claims

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Application Information

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IPC IPC(8): C07D295/027C08L23/12C08K13/02C08K5/3462C08K5/3492C08K3/22C08K3/36
CPCC07D295/027C07D295/023C08L23/12C08L2201/02C08L2201/08C08L2201/22
Inventor 杨友强袁志敏姜向新陆湛泉肖鹏叶南飚
Owner KINGFA SCI & TECH CO LTD
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