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Preparation of environment-protective glass fibre flame-retardant nylon flame retardant

A glass fiber, flame retardant nylon technology, applied in the field of flame retardant preparation, can solve the problems of atmospheric environmental pollution, high price, failure to meet flame retardant requirements, etc., and achieve uniform particle size, uniform shape distribution, and smooth surface. Effect

Active Publication Date: 2009-03-04
GUANGDONG JUSHI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these flame retardants have obvious disadvantages. For example, halogen flame retardants have several disadvantages: ① Materials containing halogen flame retardants may poison people when burned in a fire; Toxic substances pollute the air environment; ③ when this type of plastic is formulated and processed, it may harm the health of workers
Red phosphorus flame retardants also have several disadvantages: ①During processing, red phosphorus generates phosphine and further leads to end products with inherent dark red or dark brown color; ②Materials containing red phosphorus flame retardants Burning in a fire will also release poisonous gas, causing poisoning
[0003] Melamine cyanurate is also widely used in the flame retardancy of nylon resin compositions, but it is used in glass fiber reinforced nylon resin compositions, which cannot meet sufficient flame retardancy requirements
However, they still have several disadvantages: ①Although they have a certain flame retardant effect, they still cannot meet the flame retardant requirements for use; ②The compatibility with nylon is not good, resulting in limited performance of glass fiber reinforced nylon resin compositions ; ③ The electrical performance of the flame retardant is poor, resulting in a low leakage trace index (CTI) of the product
The use of melamine polyphosphate in glass fiber reinforced nylon compositions can achieve a combustion rating of 94V0 (1.6mm), but its electrical performance defects and high price determine the limitations of its application range.
[0007] Patents such as US6547992, US6255371, US2004021135A1, and US2006058432A1 disclose the application of non-halogen flame retardants based on organic hypophosphite esters in glass fiber reinforced nylon, such as: the OP1311 and OP1312 series of flame retardants developed by Exolit, Germany, which are used in flame retardants. It shows excellent performance in terms of combustion, mechanics and electricity, but its very expensive price greatly limits its application range.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] First, after the kneader is preheated to 100°C, 2470g of diammonium hydrogen phosphate, 2500g of phosphorus pentoxide and 250g of urea are successively added to a 10L volumetric kneader. Then the temperature was raised to 280° C., under the state of ammonia flow (100 L / h), after reacting for 50 minutes, 500 g of dicyandiamide was added, and aging was continued for 5 hours to obtain 5440 g of modified APP.

[0037] In a 5L reaction kettle with a stirring and reflux device, add 430g of dicyandiamide and suspend it in 2500ml of pure water, raise the temperature to 80°C, keep stirring and dispersing for 30min, then slowly add 320g of 68% industrial nitric acid within 15min, and keep the temperature at 80 ℃, under the state of stirring and reflux for 1 hour to form a salt solution of dicyandiamide.

[0038] In another 10L reaction kettle with a stirring and reflux device, add 500g of the modified APP prepared above and suspend it in 1200ml of anhydrous acetone, then add 4g o...

Embodiment 2

[0040] First, after the kneader is preheated to 150°C, 2470g of diammonium hydrogen phosphate, 2900g of phosphorus pentoxide and 700g of urea are successively added to a 10L volumetric kneader, and at 100°C, pass 500L of ammonia gas and react for 60 minutes Then the temperature was raised to 290° C., under the state of ammonia flow (100 L / h), after reacting for 80 minutes, 700 g of melam was added, and the aging was continued for 11 hours to obtain 5683 g of modified APP.

[0041] In a 5L reaction kettle with a stirring and reflux device, add 650g of melam and suspend it in 2000ml of pure water, raise the temperature to 80°C, keep stirring and dispersing for 30min, then slowly add 650930% industrial hydrochloric acid within 15min, and keep the temperature at 80 ℃, under the state of stirring and reflux for 1 hour to form a salt solution of melam.

[0042]In another 10L reaction kettle with a stirring and reflux device, add 500g of the modified APP prepared above and suspend it...

Embodiment 3

[0044] First, after the kneader is preheated to 100°C, 123.5Kg of diammonium hydrogen phosphate, 132.5Kg of phosphorus pentoxide and 20Kg of urea are successively added into a 500L volumetric kneader. Minutes, then the temperature was raised to 300°C, under the state of ammonia flow (5000L / h), after reacting for 60 minutes, 25Kg of melamine was added, and the aging was continued for 8 hours to obtain 280.5Kg of modified APP.

[0045] In a 500L reactor with a stirring and reflux device, add 65Kg of melamine to suspend in 300L of pure water, raise the temperature to 80°C, keep stirring and dispersing for 30min, then slowly add 130Kg of 30% industrial hydrochloric acid within 15min, and keep the temperature at 80°C , reacted for 1 hour under the state of stirring and reflux to form a salt solution of melamine.

[0046] In another 1000L reactor with a stirring and reflux device, add 50Kg of the modified APP prepared above and suspend it in 200L of absolute ethanol, then add 0.5Kg ...

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PUM

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Abstract

The invention discloses a preparation method of a flame retardant of environment-protective fiberglass retardant nylon. At first, diammonium phosphate, phosphorus pentoxide, carbamide and a multi-amino group compound are added into a kneader according to a proportion and are reacted for 4 to 12 hours under an ammonia atmosphere to obtain modified APP; then the APP is dispersed in solvent and cation surface activator is added to carry out ion exchange reaction with cyanamide salt for 1 to 10 hours under the situations of micro-boiling and circumfluence of the solvent; after the reaction is finished, the nitrogen-phosphor flame retardant used for nylon is obtained after the reagent is cooled, filtered, washed and dried. The flame retardant prepared by the invention has more uniform chemical components, better thermal stability, more excellent compatibility with nylon as well as more excellent flame retardant performance and more reasonable price. No corrosive and poisonous compounds are generated during the use process of the flame retardant. The product prepared by the invention is mainly used as the flame retardant of fiberglass reinforced retardant nylon and fiberglass reinforced retardant polyester.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of an environment-friendly glass fiber flame retardant nylon flame retardant. Background technique [0002] At present, the flame retardants used for glass fiber reinforced nylon resin compositions on an industrial scale are mainly halogen-containing flame retardants or red phosphorus. However, these flame retardants have obvious disadvantages. For example, halogen flame retardants have several disadvantages: ① Materials containing halogen flame retardants may poison people when burned in a fire; Toxic substances pollute the atmospheric environment; ③ when this type of plastic is formulated and processed, it may harm the health of workers. Red phosphorus flame retardants also have several disadvantages: ①During processing, red phosphorus generates phosphine and further leads to end products with inherent dark red or dark brown color; ②Materials co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/52C08K5/315C08K5/3492C08L77/00C08K7/14
Inventor 周侃何燕岭陈钢
Owner GUANGDONG JUSHI CHEM CO LTD
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