Intumescent flame retardant and preparation method thereof

A technology of intumescent flame retardant and ammonium poly(methylidene phosphonate), which is applied in the field of flame retardants, can solve the problems of APP flame retardants such as easy moisture return, uneven dispersion, precipitation, etc., and achieves good hydrolysis stability and thermal stability. Good, simple craftsmanship

Inactive Publication Date: 2017-11-17
青岛长荣化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the above-mentioned problems that the APP flame retardant existing in the prior art is easy to return to moisture, precipitate, and frost, and the

Method used

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  • Intumescent flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation of embodiment 1 aminotrimethylene ammonium phosphonate

[0028] It is prepared from 50% aminotrimethylene phosphonic acid and 25% industrial ammonia as raw materials. According to phosphonate PO 3 h 2 with amino NH 2 The molar ratio is 1:2.5 (aminotrimethylene phosphonic acid: ammonia=1:7.5), prepare aminotrimethylene phosphonic acid and strong ammonia water, first dilute 25% strong ammonia water to 10% (add 2 / 3 times quality of water), and then added dropwise to aminotrimethylene phosphonic acid under stirring, controlling the reaction temperature at 20-30°C, continuing to stir and react for 0.5h after the dropwise addition, heating and evaporating most of the water in the reaction mixture, and cooling to crystallize , filtered, washed, and the filtrate recovery sleeve is used to dilute concentrated ammonia water, and the filter cake is dried and crushed to obtain the ammonium trimethylene phosphonate product.

Embodiment 2

[0029] The preparation of embodiment 2 ethylenediamine tetramethylene ammonium phosphonate

[0030] It is prepared from 28% ethylenediamine tetramethylene phosphonic acid and solid ammonium bicarbonate. According to phosphonate PO 3 h 2 with amino NH 2 The molar ratio is 1:2.1 (ethylenediaminetetramethylenephosphonic acid: ammonium bicarbonate = 1:8.4), to prepare ethylenediaminetetramethylenephosphonic acid and ammonium bicarbonate, first dissolve ammonium bicarbonate in water to prepare 20% solution (add 4 times the mass of water), then add dropwise to ethylenediaminetetramethylenephosphonic acid under stirring, control the reaction temperature at 60-70°C, raise the temperature to 80-90°C after the addition and continue stirring React for 1 hour, heat to evaporate most of the water in the reaction mixture, cool to crystallize, filter, wash, and the filtrate recovery sleeve is used to prepare ammonium bicarbonate solution, the filter cake is dried and pulverized to obtain ...

Embodiment 3 2

[0031] The preparation of embodiment 3 diethylene triamine ammonium pentamethylene phosphonate

[0032] It is prepared from diethylenetriaminepentamethylenephosphonic acid with a content of 50% and solid ammonium carbonate as raw materials. According to phosphonate PO 3 h 2 with amino NH 2 The molar ratio is 1:2.2 (diethylenetriaminepentamethylenephosphonic acid: ammonium carbonate=1:5.5), prepare diethylenetriaminepentamethylenephosphonic acid and ammonium carbonate, first ammonium carbonate is dissolved in water to prepare 40 % solution (add 1.5 times the mass of water), and then add it dropwise to diethylenetriaminepentamethylenephosphonic acid under stirring, control the reaction temperature at 80-90°C, raise the temperature to 110-120°C after the addition and continue stirring React for 1.5 hours, evaporate most of the water in the reaction mixture, cool and crystallize, filter, wash, and use the filtrate recovery sleeve to prepare ammonium carbonate solution. The filt...

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Abstract

The invention relates to an intumescent flame retardant and a preparation method thereof. The intumescent flame retardant is polymethylene ammonium phosphonate which at least contains three methylammonium phosphonate groups -CH2P(O)(ONH4)2 in one molecule, and the intumescent flame retardant is prepared from polymethylene phosphonic acid and an ammonium source through a reaction, wherein the mole ratio of phosphonate groups PO3H2 to amino groups NH2 is 1:(2-2.5), a water solution is prepared from the ammonium source and water in the mass ratio being 1:(0.01-5) and dropwise added to polymethylene phosphonic acid while being stirred after complete dissolution, the reaction temperature is controlled to be 20-130 DEG C, the mixture is continuously stirred to react for 0.5-1.5 h after the water solution is dropwise added, evaporation concentration, cooling crystallization, filtration, washing, filtrate recovery for preparation of an ammonia source solution, filter cake drying and crushing are performed, and a product is obtained. The flame retardant is excellent in performance, good in stability and compatible with a polymer material, raw materials used in the preparation method are easily sourced, the cost is lower, and the process is simple, safe and environment-friendly.

Description

technical field [0001] The invention relates to an intumescent flame retardant and a preparation method thereof, belonging to the technical field of flame retardants. Background technique [0002] Traditional halogen-containing flame retardants may cause suffocation to fire victims due to the release of toxic hydrogen halide gas when burned. When the intumescent flame retardant (IFR) containing phosphorus and nitrogen burns, a carbon foam layer will be formed on the surface of the material, which has the functions of heat insulation, oxygen insulation, smoke suppression, anti-drip, etc., and has excellent flame retardancy, and Low toxicity, no corrosive gas generation, is an environmentally friendly green flame retardant. [0003] Ammonium polyphosphate (APP) is a common IFR, which has the flame retardant mechanism of acid source and gas source, with high flame retardant effect and low price. However, because APP is easily hydrolyzed into small molecules of ammonium phosph...

Claims

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Application Information

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IPC IPC(8): C08K5/5317C08L23/12C07F9/38
CPCC08K5/5317C07F9/38C08L2201/02C08L23/12
Inventor 韩忠山韩明序杨松慧
Owner 青岛长荣化工科技有限公司
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