CN114891272B - Melamine formaldehyde resin microencapsulated flame retardant and preparation method thereof - Google Patents
Melamine formaldehyde resin microencapsulated flame retardant and preparation method thereof Download PDFInfo
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- CN114891272B CN114891272B CN202210380817.0A CN202210380817A CN114891272B CN 114891272 B CN114891272 B CN 114891272B CN 202210380817 A CN202210380817 A CN 202210380817A CN 114891272 B CN114891272 B CN 114891272B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/30—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with substituted triazines
- C08G12/32—Melamines
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34922—Melamine; Derivatives thereof
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a melamine formaldehyde resin microencapsulated flame retardant and a preparation method thereof. The existing flame retardant has poor compatibility with a matrix, so that the prepared composite material has poor toughness and high brittleness. The preparation method adopted by the invention comprises the following steps: 1) Ball milling hydrotalcite, melamine and diethyl aluminum hypophosphite according to a certain proportion for modification; 2) Adjusting the pH value of the melamine and formaldehyde solution by using a triethanolamine solution to obtain a prepolymer; 3) Hydrotalcite, melamine and diethyl aluminum hypophosphite are added into the prepolymer, and an acetic acid solution is used for adjusting the pH value, so that the melamine formaldehyde resin coated flame retardant microcapsule is obtained. The invention is used for preparing the melamine formaldehyde resin microcapsule flame retardant, and the melamine formaldehyde resin microcapsule hydrotalcite/melamine/diethyl aluminum hypophosphite flame retardant prepared by the method has the characteristics of excellent flame retardance and compatibility with a matrix.
Description
Technical Field
The invention belongs to the field of polymers, and in particular relates to a melamine formaldehyde resin microencapsulated flame retardant and a preparation method thereof.
Background
The flame retardant is a functional auxiliary agent for improving the flame retardant property of the polymer, and can be divided into a reactive flame retardant and an additive flame retardant. The added flame retardant is mechanically mixed with the polymer master batch directly in a physical mode, the cost of the process consumed by the mode is low, and the method for producing the polymer flame retardant material is generally adopted. The common additive flame retardant has low flame retardant efficiency when being used alone, and has poor compatibility with polymers, so that a series of problems of poor dispersion, swelling, deterioration of mechanical properties of composite materials and the like occur. Therefore, how to simultaneously improve the flame retardant efficiency of the flame retardant and reduce the influence thereof on the mechanical properties of the polymer is a hot spot of current researches.
In order to effectively improve the compatibility between the flame retardant and the polymer, a microcapsule technology of coating the flame retardant with the polymer can be adopted. The microcapsule flame retardant adopts a proper polymer material to form a layer of protective shell on the surface of the flame retardant, and the flame retardant is dispersed into a high-lipophilicity micro core-shell structure. The shell material generally has no flame retardant effect, and only improves the influence of the flame retardant on the mechanical property of the polymer, so that the selection of the components of the core flame retardant is the key of the microcapsule flame retardant to exert the flame retardant effect.
The expansion type flame retardant (IFR) is a composite flame retardant consisting of a carbon source, an acid source and an air source, and has the advantages of molten drop suppression, low toxicity, no halogen, low smoke and the like. In the combustion process of the polymer, carbon sources and acid sources are mutually combined to generate esterification reaction to form a porous carbon layer with a coking carbon structure, and gas generated by gas source combustion further expands the carbon layer and adheres to the surface of the polymer to interrupt combustion chain reaction. The Melamine (MEL) and the diethyl aluminum hypophosphite (ADP) can form the nitrogen-phosphorus intumescent flame retardant by compounding, and can exert synergistic flame retardant effect. Hydrotalcite (LDH) is an inorganic environment-friendly flame retardant, and decomposes and releases CO in the combustion process of polymers 2 、H 2 The concentration of oxygen and combustible gas is reduced by nonflammable gases such as O, and metal oxide generated by decomposition can form a compact carbon protection layer with polymer carbon residue to prevent further combustion of materials and absorb volatile substances generated during combustion.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the melamine formaldehyde resin microencapsulated flame retardant and the preparation method thereof, and the melamine formaldehyde resin microencapsulated flame retardant can effectively improve the flame retardant effect of the polymer under the condition of low addition and has less influence on the mechanical property of the composite material.
For this purpose, the invention adopts the following technical scheme: a method for preparing a melamine formaldehyde resin microencapsulated flame retardant, comprising:
step 1: putting the flame retardant A, B and the flame retardant C into an oven for drying, and then ball-milling and mixing by using a ball mill to obtain a flame retardant D;
step 2: placing melamine and formaldehyde solution into a container, stirring, regulating the pH value of the solution to 8-9 by using triethanolamine solution, heating in water bath for a period of time, and cooling to room temperature to obtain prepolymer E;
step 3: adding a flame retardant D into the prepolymer E, regulating the pH value to 5-6 by using an acetic acid solution, stirring the obtained mixture for a period of time under the heating of a water bath, and cooling to room temperature; filtering the product, washing the product to be neutral by ethanol, and drying the product to obtain the microencapsulated flame retardant F;
in the step 1, the flame retardant A component is hydrotalcite, the flame retardant B component is melamine, and the flame retardant C component is diethyl aluminum hypophosphite.
Further, the addition proportion of the flame retardant A is 10wt.% to 15wt.%.
Further, the addition proportion of the flame retardant B is 20wt.% to 30wt.%.
Further, the addition proportion of the flame retardant C is 55wt.% to 70wt.%.
Further, in the step 1, the ball milling and mixing are carried out at a rotating speed of 200-300 r/min and a ball milling time of 8-10 h.
Further, in the step 2, the mass fraction of the formaldehyde solution is 37 wt%, and the molar ratio of the formaldehyde to the melamine is 2.5-4: 1.
further, in the step 2, the mass fraction of the triethanolamine solution is 10 wt%, the water bath temperature is 65-75 ℃, the water bath heating time is 90-120 min, and the stirring rate is 100-300 r/min.
Further, in the step 3, the mass ratio of the prepolymer E to the flame retardant D is 5-8: 1.
further, in the step 3, the mass fraction of the acetic acid solution is 10wt.%, the water bath temperature is 65-75 ℃, the water bath heating time is 120-150 min, and the stirring rate is 100-300 r/min.
The invention has the beneficial effects that:
compared with the prior art, the invention synthesizes the microencapsulated flame retardant with a core-shell structure by taking hydrotalcite, melamine and diethyl aluminum phosphinate synergistic flame retardant as an inner shell and melamine formaldehyde resin as a shell material; the invention has simple process, cheap and easily obtained raw materials, is easy to realize batch continuous production in production, and has better application prospect. The melamine formaldehyde microencapsulated flame retardant obtained by the invention has good flame retardant effect and good compatibility with polymers; the low addition amount can effectively prevent or delay the combustion of the polymer on the premise of less influencing the mechanical property of the polymer.
Drawings
FIG. 1 is a schematic flow chart of the preparation method of the invention;
FIG. 2 is a scanning electron microscope image of a flame retardant prepared according to the present invention.
Detailed Description
The following detailed description of the invention further details the invention to make the technical solution of the invention easier to understand and grasp. It should be understood that the specific embodiments described herein are intended to be illustrative of only some, but not all embodiments of the invention, and that other embodiments may be made by those skilled in the art without the benefit of the inventive faculty.
Example 1
Drying 15 g of hydrotalcite, 25.5 g of melamine and 59.5 g of diethyl aluminum hypophosphite in an oven, and ball milling for 8 hours at 250r/min by using a ball mill to obtain a flame retardant D;
12.61 g melamine and 24.35 g 37wt.% formaldehyde solution were placed in a three-necked flask with slow stirring. The mixture was adjusted to a pH of 8.5 with 10wt.% triethanolamine solution. Then heating in water bath at 70 ℃ and stirring at a stirring rate of 150r/min for 90 minutes, and cooling to room temperature to obtain a prepolymer E;
6 g of flame retardant D was added to the prepolymer E described above in a mass ratio. The pH of the above mixture was adjusted to 5.5 with 10wt.% acetic acid. Then, the mixture was heated in a water bath at 70℃and stirred at a stirring rate of 150r/min for 120 minutes, and then cooled to room temperature. Filtering the product and drying to obtain the microencapsulated flame retardant F.
The resulting flame retardant F was added to acrylonitrile-butadiene-styrene copolymer (ABS) and the vertical burning performance of the composite was tested according to standard GB/T2408-2008 and the limiting oxygen index of the composite was tested according to standard GB/T2406.2-2009. At an addition amount of 30wt.% of the flame retardant F, the limiting oxygen index of the test specimen can reach 27.4% and the vertical combustion V-0 grade can be satisfied.
Example 2
Drying 10 g of hydrotalcite, 27 g of melamine and 63 g of diethyl aluminum hypophosphite in an oven, and ball milling for 8 hours at 250r/min by using a ball mill to obtain a flame retardant D;
12.61 g melamine and 24.35 g 37wt.% formaldehyde solution were placed in a three-necked flask with slow stirring. The mixture was adjusted to a pH of 8.5 with 10wt.% triethanolamine solution. Then heating in water bath at 70 ℃ and stirring at a stirring rate of 150r/min for 90 minutes, and cooling to room temperature to obtain a prepolymer E;
6 g of flame retardant D was added to the prepolymer E described above in a mass ratio. The pH of the above mixture was adjusted to 5.5 with 10wt.% acetic acid. Then, the mixture was heated in a water bath at 70℃and stirred at a stirring rate of 150r/min for 120 minutes, and then cooled to room temperature. Filtering the product and drying to obtain the microencapsulated flame retardant F.
The resulting flame retardant F was added to acrylonitrile-butadiene-styrene copolymer (ABS) and the vertical burning performance of the composite was tested according to standard GB/T2408-2008 and the limiting oxygen index of the composite was tested according to standard GB/T2406.2-2009. At an addition amount of 30wt.% of the flame retardant F, the limiting oxygen index of the test specimen can reach 27.8% and the vertical combustion V-0 grade can be satisfied.
Example 3
Drying 13 g of hydrotalcite, 37 g of melamine and 50 g of diethyl aluminum hypophosphite in an oven, and ball milling for 8 hours at 250r/min by using a ball mill to obtain a flame retardant D;
12.61 g melamine and 24.35 g 37wt.% formaldehyde solution were placed in a three-necked flask with slow stirring. The mixture was adjusted to a pH of 8.5 with 10wt.% triethanolamine solution. Then heating in water bath at 70 ℃ and stirring at a stirring rate of 150r/min for 90 minutes, and cooling to room temperature to obtain a prepolymer E;
8 g of flame retardant D was added to the prepolymer E described above in a mass ratio. The pH of the above mixture was adjusted to 5.5 with 10wt.% acetic acid. Then, the mixture was heated in a water bath at 70℃and stirred at a stirring rate of 150r/min for 120 minutes, and then cooled to room temperature. Filtering the product and drying to obtain the microencapsulated flame retardant F.
The resulting flame retardant F was added to polypropylene (PP) and the vertical burn performance of the composite was tested according to standard GB/T2408-2008 and the limiting oxygen index of the composite was tested according to standard GB/T2406.2-2009. At an addition amount of 30wt.% of the flame retardant F, the limiting oxygen index of the test specimen can reach 30.6%, and the vertical combustion V-0 grade can be satisfied.
Claims (5)
1. A method for preparing a melamine formaldehyde resin microencapsulated flame retardant, which is characterized by comprising the following steps:
step 1: putting the flame retardant A, B and the flame retardant C into an oven for drying, and then ball-milling and mixing by using a ball mill to obtain a flame retardant D;
step 2: placing melamine and formaldehyde solution into a container, stirring, regulating the pH value of the solution to 8-9 by using triethanolamine solution, heating in water bath for a period of time, and cooling to room temperature to obtain prepolymer E;
step 3: adding a flame retardant D into the prepolymer E, regulating the pH value to 5-6 by using an acetic acid solution, stirring the obtained mixture for a period of time under the heating of a water bath, and cooling to room temperature; filtering the product, washing the product to be neutral by ethanol, and drying the product to obtain the microencapsulated flame retardant F;
in the step 1, the flame retardant component A is hydrotalcite, the flame retardant component B is melamine, and the flame retardant component C is diethyl aluminum hypophosphite;
the adding proportion of the flame retardant A is 10wt.% to 15wt.%;
the adding proportion of the flame retardant B is 20wt.% to 30wt.%;
the adding proportion of the flame retardant C is 55wt.% to 70wt.%;
in the step 2, the mass fraction of the formaldehyde solution is 37 wt%, and the addition amount mole ratio of formaldehyde to melamine is 2.5-4: 1, a step of;
in the step 3, the mass ratio of the prepolymer E to the flame retardant D is 5-8: 1.
2. the method according to claim 1, wherein in step 1, the ball milling mixing is performed at a rotational speed of 200-300 r/min for a ball milling time of 8-10 hours.
3. The preparation method according to claim 1, wherein in the step 2, the mass fraction of the triethanolamine solution is 10wt.%, the water bath temperature is 65-75 ℃, the water bath heating time is 90-120 min, and the stirring rate is 100-300 r/min.
4. The preparation method according to claim 1, wherein in the step 3, the mass fraction of the acetic acid solution is 10wt.%, the water bath temperature is 65-75 ℃, the water bath heating time is 120-150 min, and the stirring rate is 100-300 r/min.
5. A melamine formaldehyde resin microencapsulated flame retardant obtainable by the process of any one of claims 1 to 4.
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