Liquid halogen-free phosphorus-nitrogen collaboration flame retardant and preparation method thereof

A technology of synergistic flame retardant and flame retardant, applied in the fields of manufacturing tools, inorganic compound addition, textile and paper making, etc. Good application value and economic benefits, easy control and industrialization, simple preparation effect

Inactive Publication Date: 2012-07-04
QINGHAI NORMAL UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The use of flame retardant technology has been challenged by higher material requirements. The main problems in its application are: (l) the technical level of flame retardant products is low, and most products will release toxic gases at high temperatures, or after a period of application After that, the flame retardant performance is obviously reduced; (2) the flame retardant effect of flame retardant products is low, the price is high, and the mechanical properties of the material are greatly affected; (3) the applicability is poor, and different flame retardants can only be added to one or very few materials; (4) Poor designability, the same series of general flame retardant products are very single, and the application of flame retardants is also limited due to the differences in materials themselves.

Method used

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  • Liquid halogen-free phosphorus-nitrogen collaboration flame retardant and preparation method thereof
  • Liquid halogen-free phosphorus-nitrogen collaboration flame retardant and preparation method thereof
  • Liquid halogen-free phosphorus-nitrogen collaboration flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 49.8g of phosphorus oxychloride in a two-necked flask equipped with a reflux device and a tail gas absorption device. Heat it to 40°C in a constant temperature oil bath with stirring, add a funnel to the other mouth of the two-necked bottle, control the dropping rate to 10ml / min and add 10.1g of ethylene glycol dropwise. The temperature was 50°C, and the reaction was continued for one hour. Add 10.4 g of urea in small portions. After the addition is completed, raise the temperature to 80° C., add 19.6 g of urea in small portions, continue the reaction for one hour, and cool naturally. That is, a milky white transparent viscous liquid flame retardant product is obtained. The yield is 100%. The product has a boiling point of 220°C and a 1% decomposition temperature of 330°C.

[0030] Dissolve 10 g of the liquid halogen-free phosphorus nitrogen synergistic flame retardant obtained in Example 1 into 100 ml of water, soak common kraft wrapping paper in water for 10 m...

Embodiment 2

[0032] Add 70g of phosphoric acid, 10ml of cyclohexane (water removal agent) and 3ml of concentrated sulfuric acid catalyst into a two-necked flask equipped with a reflux device and a tail gas absorption device, and reflux at a constant temperature to remove water. Heat to 80° C. in a constant-temperature oil bath with stirring, and add 32.1 g of urea in small portions. After the addition was complete, the temperature was raised to 90°C, and the reaction was continued for one hour. Control the dropping rate at 7ml / min and add 50g of ethanol dropwise. After the dropwise addition is completed, keep the constant temperature at 90°C and continue the reaction for 0.2 hours. After distilling off the water-removing agent inside, cool naturally. That is, a colorless and transparent viscous liquid flame retardant product is obtained. The yield was 93%. The product has a boiling point of 200°C and a 1% decomposition temperature of 320°C.

[0033] 16g of the liquid halogen-free phosph...

Embodiment 3

[0035]Add 40g of phosphorus pentachloride in a two-necked flask equipped with a reflux device and a tail gas absorption device. Heat to 30°C in a constant temperature oil bath with stirring, add a funnel to the other port of the two-neck bottle, add 14.1 g of resorcinol in small portions, raise the temperature to 50°C, and continue the reaction for one hour. 6.2 g of propanol was added dropwise at a rate of 10 ml / min, and the reaction was continued at a constant temperature for 0.1 hour after the dropwise addition was completed. Then add 7.7 g of urea into the reactor in small amounts, and after the addition of the sample is completed, raise the temperature to 80° C., continue the reaction for one hour, and cool naturally. That is, a bright yellow transparent viscous liquid flame retardant product is obtained. The yield was 96%. The product has a boiling point of 200°C and a 1% decomposition temperature of 330°C.

[0036] 16g of the liquid halogen-free phosphorus nitrogen ...

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Abstract

The invention discloses a synthesizing method of a liquid halogen-free P-N collaboration flame retardant. A phosphorous long-chain intermediate is prepared through a condensation reaction between diamine (glycol and urea) and phosphorus source materials, then alcohol (amine and urea) are utilized to carry out end sealing, and accordingly a series of liquid halogen-free P-N collaboration flame retardants with good flame-retardant performance are synthesized. The flame retardant prepared by the method not only is low in price, low in using quantity and good in flame-retardant effect and has small influence on mechanical performance of a material, but also avoids being precipitated when being added into the material. The flame retardant can be widely applied to materials including plastics, foam materials, wood, paper and the like, has remarkable social benefits and industrial application value, and is suitable for large-scale popularization and application.

Description

[0001] technical field [0002] The invention relates to the technical field of flame retardant synthesis, in particular to a synthesis method of an organic liquid halogen-free phosphorus-nitrogen synergistic flame retardant. Background technique [0003] With the wide application and continuous development of synthetic materials, people have put forward higher requirements for flame retardant materials. In recent years, polymer materials such as plastics, rubber, and synthetic fibers and their products have developed vigorously and are widely used in industries, Agriculture, military and other aspects of the national economy, but these materials are flammable and combustible, and when burned, the heat release rate is high, the calorific value is high, the flame spreads fast, it is not easy to extinguish, and sometimes produces thick smoke and toxic gases. It causes harm to the environment and poses a huge threat to people's life safety. For this reason, all countries have ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/51C08K5/5399C08L97/02C08L69/00C08L55/02B27K3/50B27K3/52D21H21/14D21H17/63
Inventor 王建朝尹大学王书海翟博叶广
Owner QINGHAI NORMAL UNIV
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