阅读说明：本技术 一种新型复合阻燃剂及其制备方法 (Novel composite flame retardant and preparation method thereof ) 是由 张海燕 张顺华 胡慧敏 胡荣军 于 2020-06-29 设计创作，主要内容包括：本发明公开了一种新型复合阻燃剂及其制备方法,是在微乳液中制备层状有机改性的水滑石,将其与磷氮系阻燃剂混合均匀,制得新型符合阻燃剂。本发明的方法操作简单、易行,易于工业化生产,实现了无机阻燃剂水滑石与磷氮系阻燃剂复合阻燃剂体系。与纯磷氮系阻燃材料相比,本发明的复合阻燃剂有优良阻燃性能,同时抑烟效果显著,符合无卤、低烟、环保的阻燃要求。(The invention discloses a novel composite flame retardant and a preparation method thereof, which is to prepare layered organic modified hydrotalcite in microemulsion and uniformly mix the layered organic modified hydrotalcite with a phosphorus-nitrogen flame retardant to prepare the novel composite flame retardant. The method has simple and easy operation and easy industrial production, and realizes the composite flame retardant system of the inorganic flame retardant hydrotalcite and the phosphorus-nitrogen flame retardant. Compared with pure phosphorus-nitrogen flame retardant materials, the composite flame retardant disclosed by the invention has excellent flame retardant performance, is remarkable in smoke suppression effect, and meets the flame retardant requirements of no halogen, low smoke and environmental protection.)

1. A novel composite flame retardant and a preparation method thereof are characterized in that:

(1) preparation of layered hydrotalcite

Adding 10-30g of surfactant, 400ml of H2O and 600g of octane in 300-400ml of flask, dropwise adding 30-50 wt% of alkaline solution to adjust the pH value to 8.0-12.0, uniformly stirring, adding divalent metal ion salt and trivalent metal ion salt, controlling the molar ratio of the divalent metal ion to the trivalent metal ion to be 1:1-5:1, simultaneously controlling the pH value to be =8.0-12.0 by using the alkaline solution, heating to the temperature of 100-150 ℃, reacting for 12-24h, centrifugally washing and drying the product to obtain the organic modified hydrotalcite;

(2) preparation of novel composite flame retardant

Adding 10-30 parts of phosphorus-nitrogen flame retardant and 5-10 parts of layered hydrotalcite into a solvent, wherein the solvent is a mixed solvent of hydrocarbons, ketone compounds and ester compounds, the ratio of the solvent is 1:3-1:5, uniformly stirring, and grinding for 2-5h to obtain the novel flame retardant.

2. The novel composite flame retardant and the preparation method thereof according to claim 1, characterized in that: the divalent metal ions are Mg2+, Ca2+, Sr2+, Ba2+, Fe2+, Zn2+, Cu2+, Ti2+, Sn2+, Cr2+, Pb2+, Co2+ or/and Ni2+, and the trivalent metal ions are Al3+, Fe3+, Co3+, Mn3+, V3+, Ti3+, Cr3+, Bi3+, Ce3+, Pr3+, In3+ or/and W3 +.

3. The novel composite flame retardant and the preparation method thereof according to claim 1, characterized in that: the surfactant is an anionic surfactant and is selected from sodium N-lauroyl glutamate, potassium nonylphenol ether (EO =10) phosphate monoester salt, potassium N-hexadecanol-octadecanol phosphate, lauryl phosphate monoester triethanolamine, potassium lauryl alcohol ether phosphate monoester and lauryl phosphate monoester potassium.

4. The novel composite flame retardant and the preparation method thereof according to claim 2, characterized in that: the phosphorus-nitrogen flame retardant is selected from melamine polyphosphate, a mixture of melamine polyphosphate and resorcinol bis (diphenyl phosphate) and a mixture of melamine polyphosphate and aluminum diethylphosphinate.

Technical Field

The invention relates to the technical field of flame retardants, and mainly relates to a novel composite flame retardant and a preparation method thereof.

Background

The hydrotalcite as the inorganic flame retardant has the advantages of low price, no toxicity and no stimulation, and has better compatibility with the polymer matrix after being modified. And at high temperature, hydrotalcite filled in the polymer can lose interlayer water and hydroxyl on the laminate to dehydrate and emit in a water vapor form, decompose to release water and CO2 gas, absorb a large amount of heat and dilute the concentration of oxygen, thereby reducing the temperature of the combustion surface of the polymer, preventing the further degradation of the polymer and playing a role in flame retardance. The special layered structure of the layered hydrotalcite enables the layered hydrotalcite to have larger surface area and surface adsorption active center, can adsorb harmful gas, particularly acid gas, and thus has double functions of flame retardance and smoke suppression.

The phosphorus-nitrogen flame retardant has the advantages of environmental protection and excellent flame retardant property, the hydrotalcite has the advantages of smoke suppression and matrix mechanical stability maintenance, the composite flame retardant is prepared by combining the advantages of the phosphorus-nitrogen flame retardant and the hydrotalcite, the synergistic effect of the phosphorus-nitrogen flame retardant and the hydrotalcite is exerted, and the composite flame retardant has important industrial value.

SUMMARY OF THE PATENT FOR INVENTION

The invention aims to provide a novel composite flame retardant and a preparation method thereof.

In order to achieve the above object, the present invention provides the following technical solutions:

(1) preparation of layered hydrotalcite

Adding 20g of surfactant, 300-400ml of H2O and 400-600g of octane into a flask, dropwise adding 30-50 wt% of alkaline solution to adjust the pH value to 8.0-12.0, uniformly stirring, adding divalent metal ion salt and trivalent metal ion salt, controlling the molar ratio of the divalent metal ion to the trivalent metal ion to be 2:1-5:1, simultaneously controlling the pH value to be =8.0-12.0 by using the alkaline solution, heating to 100-150 ℃, reacting for 12-24h, centrifuging, washing and drying the product to obtain the organic modified hydrotalcite.

(2) Preparation of novel composite flame retardant

Adding 5-10 parts of layered hydrotalcite into a solvent containing 10-30 parts of phosphorus-nitrogen flame retardant, wherein the solvent is a mixed solvent of hydrocarbons, ketone compounds and ester compounds, and the ratio of the solvent to the solvent is 1:3-1: 5. Grinding for 2-5h after uniformly stirring, and volatilizing the solvent at 125 ℃ to obtain the novel composite flame retardant.

The preparation method of the material for the layered hydrotalcite is characterized by comprising the following steps: the anionic surfactant is selected from sodium N-lauroyl glutamate, potassium nonylphenol ether (EO =10) phosphate monoester salt, potassium N-hexadecanol-octadecanol phosphate, triethanolamine dodecyl phosphate monoester, potassium lauryl alcohol ether phosphate monoester and potassium dodecyl phosphate monoester.

The preparation method of the novel composite flame retardant is characterized by comprising the following steps: the hydrocarbon solvent is selected from toluene, xylene, cyclohexane, hexane and octane, the ketone compound is selected from acetone, butanone and pentanedione, and the ester compound is selected from ethyl acetate, propyl acetate and butyl acetate.

The invention has the following beneficial effects:

the novel composite flame retardant generates a large amount of inert gas when meeting high temperature, structural water with equivalent amount in the structure is discharged to deoxidize organic matters into carbon, a carbon layer is formed on the surface of a product, the fire source is effectively blocked, the oxygen concentration around the fire source is reduced, and the purpose of blocking the fire source is achieved. Compared with pure phosphorus-nitrogen flame retardant materials, the composite flame retardant disclosed by the invention has excellent flame retardant performance, is remarkable in smoke suppression effect, and meets the flame retardant requirements of no halogen, low smoke and environmental protection.

Detailed Description

The technical solution of the present invention will be further specifically described below by way of specific examples. The practice of the invention is not limited to the following examples, and any variations and/or modifications made thereto are intended to fall within the scope of the invention.