Preparation method for reaction type nitrogen-phosphorus flame retardant

A nitrogen-phosphorus flame retardant and reactive technology, which is applied in the field of preparation of reactive nitrogen-phosphorus flame retardants, can solve problems such as the influence of material processing properties on physical and mechanical properties, achieve low processing performance and physical and mechanical properties, and avoid migration , the effect of reducing the emission of toxic and harmful gases

Active Publication Date: 2017-08-18
广州喜嘉新材料有限公司
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Problems solved by technology

[0005] Most of the nitrogen-phosphorus flame retardants currently reported are additive-type, which can play a certain role in the flame retardancy of polymer materials, but have a greater impact on the processing performance and physical and mechanical properties of materials. Synthesis and preparation of environmentally friendly and efficient nitrogen-phosphorus Composite reactive flame retardants are rarely reported

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  • Preparation method for reaction type nitrogen-phosphorus flame retardant

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preparation example Construction

[0017] refer to figure 1 , the present specific embodiment adopts following technical scheme: a kind of preparation method of reactive nitrogen phosphorus flame retardant, comprises the following steps: 1, the purification of pentaerythritol phosphate (PEPA): get 50-300gPEPA, add 200-500ml dehydrated alcohol In 80-230r / min rotation speed, heated to boiling at 70-80°C, filtered while hot, cooled, recrystallized, and vacuum-dried at 60-120°C for 25-72h to obtain purified PEPA.

[0018] 2. Activate PEPA with isocyanic acid: Take 100-300ml of anhydrous solvent in a three-necked flask, add 10-200g of diisocyanate, nitrogen protection, slowly add 10-200g of PEPA, in a 40-120℃ water bath, 80- React at 230r / min for 4-8h to obtain isocyanic acid-activated PEPA.

[0019] 3. Preparation of reactive nitrogen-phosphorus flame retardant: Weigh unsaturated fatty amine (alcohol) and add it dropwise to step 2 isocyanic acid activated PEPA. The reaction is continued for 4-10 hours, the reacti...

Embodiment 1

[0023] Example 1: Step 1. Purification of Pentaerythritol Phosphate (PEPA)

[0024] Pour 300ml of absolute ethanol into a 500ml three-neck flask, add 150g of PEPA, stir electromagnetically at a speed of 150r / min, heat the water bath until the solution boils, filter while it is hot, cool, recrystallize, and vacuum dry at 80°C for 30h to obtain purified PEPA.

[0025] Step 2. Covalently bonded isocyanate to activate PEPA

[0026] Take 150ml of anhydrous xylene in a 250ml three-neck flask, add 17.415g of toluene diisocyanate (TDI), 180r / min electromagnetic stirring, nitrogen protection, take 18.0g of PEPA and add it in 9 times, each interval of 10min, in a 70℃ water bath After reacting for 6 hours, the isocyanate-activated PEPA reaction solution was obtained for use.

[0027] Step 3. Preparation of Reactive Nitrogen-Phosphorus Flame Retardant

[0028] Weigh 5.8g of 2-propen-1-amine, and slowly add it dropwise to the activated PEPA solution obtained in step 2. The system contin...

Embodiment 2

[0031] Embodiment 2: the formula of natural rubber, by weight: 100 parts of natural rubber, 6 parts of zinc oxide, 2 parts of stearic acid, 0.5 part of antioxidant 4010NA, 3 parts of paraffin, 3 parts of sulfur, accelerator CZ0. 5 parts, accelerator DM0.8 parts, carbon black (N330) 20 parts, expandable graphite 10 parts, reactive nitrogen phosphorus flame retardant 30 parts. After plasticizing, kneading, calendering, extruding and vulcanization, flame-retardant natural rubber is obtained.

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Abstract

The invention discloses a preparation method for a reaction type nitrogen-phosphorus flame retardant and relates to the technical field of a nitrogen-phosphorus flame retardant and a preparation method thereof. The method comprises the following steps: 1) purifying pentaerythritol phosphonate (PEPA); 2) activating PEPA with isocyanic acid; and 3) preparing the reaction type nitrogen-phosphorus flame retardant: weighting unsaturated aliphatic amine (alcohol), dropwise adding into the PEPA activated with isocyanic acid in the step 2, reacting for 4-10h at the revolving speed of 80-230r / min in a water bath kettle at 40-120 DEG C, ending the reaction, washing with a xylene solvent for 2-4 times, and performing vacuum drying for 10-72h at 70-120 DEG C, thereby acquiring the reaction type nitrogen-phosphorus flame retardant. The fire retardant disclosed by the invention is mainly composed of nitrogen, phosphorus and carbon elements, has excellent thermal stability and chemical stability, is halogen-free, low-smoke, low-toxicity and environment-friendly, contains double active bonds, can be directly used as a chain extender for reacting with a monomer for compounding an anti-flaming macromolecule material, and is simple in bonding mode.

Description

technical field [0001] The invention relates to the technical field of phosphorus-nitrogen flame retardants and preparation thereof, in particular to a preparation method of a reactive nitrogen-phosphorus flame retardant. Background technique [0002] Since entering the 1950s, polymer materials have entered people's production and life, greatly enriching our daily life, among which rubber, plastic, fiber, paint, adhesive, etc. have played an irreplaceable role in other materials. role. While bringing us convenience, polymer materials also bring potential safety hazards. Polymer materials are flammable and can easily cause fires, threatening people's lives and property safety. Nowadays, many scientific researchers at home and abroad are devoted to polymer The flame retardant research of materials and the flame retardant modification of polymer materials have become one of the important research topics for scientific and technological workers. [0003] Flame retardants can b...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/5399C08L7/00C08L91/06C08K13/04C08K7/24C08K3/22C08K5/09
CPCC07F9/65748C08K5/5399C08L7/00C08L2201/02C08L91/06C08K13/04C08K7/24C08K2003/2296C08K5/09
Inventor 陆建帅蔡小梅陆合爱
Owner 广州喜嘉新材料有限公司
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