CN112194833A - Intumescent flame-retardant polyethylene containing organic metal complex and preparation method thereof - Google Patents
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
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Abstract
The invention discloses a flame-retardant polyethylene containing organic metal complex and its preparing method, which reduces the proportion of ammonium polyphosphate, avoids the dependence on excessive ammonium polyphosphate flame-retardant property, reduces the water-resistant property of the material, adds cyanuric chloride to improve the stability, because the chlorine atom activity of cyanuric chloride is high, the nucleophilic substitution reaction is easy to carry out, which is convenient to construct the compound with flame-retardant function, the chlorine atoms with different reaction activities can be substituted in sequence at different temperatures, which has outstanding thermal stability, improves the water-resistant property and flame-retardant property of the material, adopts macromolecular polyurethane to substitute, the polyurethane has good hydrophobicity and substrate compatibility and stable thermal property, can effectively substitute micromolecular pentaerythritol, and has obvious effect on the flame-retardant property of the material, the thermal stability of the material system is improved, and the flame retardant rate is improved.
Description
Technical Field
The invention relates to the technical field of preparation of flame-retardant polyethylene, in particular to expanded flame-retardant polyethylene containing an organic metal complex and a preparation method thereof.
Background
Polyethylene (PE) is a thermoplastic resin obtained by polymerizing ethylene. In industry, copolymers of ethylene with small amounts of alpha-olefins are also included. Polyethylene is odorless, non-toxic, feels like wax, has excellent low-temperature resistance, good chemical stability, can resist corrosion of most of acid and alkali, is insoluble in common solvents at normal temperature, has small water absorption and excellent electrical insulation, has the defect of high toxicity due to the fact that a halogen flame retardant has a good flame retardant effect, and is eliminated for use.
Disclosure of Invention
The invention aims to provide an expanded flame-retardant polyethylene containing an organic metal complex and a preparation method thereof, and aims to solve the problems that ammonium polyphosphate provided in the background art is poor in thermal stability, has high hygroscopicity, can affect the performance of a material to a certain extent, and traditional pentaerythritol and melamine can cause the weather resistance of a polymer matrix to be poor and the compatibility with the material to be poor.
In order to achieve the purpose, the invention provides the following technical scheme: an intumescent flame retardant polyethylene containing organic metal complex, wherein the intumescent flame retardant polyethylene containing organic metal complex comprises polyethylene, intumescent flame retardant and organic metal complex, and the weight percentages of the polyethylene, intumescent flame retardant and organic metal complex are as follows: 70-80% of polyethylene, 20-30% of intumescent flame retardant and 1-3% of organic metal complex, wherein the intumescent flame retardant is prepared by compounding extruded flame retardant master batches, ammonium polyphosphate and cyanuric chloride, and the flame retardant master batches, the ammonium polyphosphate and the cyanuric chloride are as follows by weight percent in the intumescent flame retardant: 40-50% of flame-retardant master batch, 5-10% of ammonium polyphosphate and 30-40% of cyanuric chloride.
Preferably, the flame-retardant master batch is formed by co-melting and extruding an acid source, a carbon source, a gas source and low-density polyethylene, wherein the weight percentage of the acid source, the carbon source, the gas source and the low-density polyethylene in the flame-retardant master batch is 5-10%, the weight percentage of the carbon source is 40-60%, the weight percentage of the gas source is 10-15%, and the weight percentage of the low-density polyethylene is 20%.
Preferably, the acid source comprises one or more of phosphoric acid, boric acid, sulfuric acid, and phosphoric acid esters.
Preferably, the carbon source comprises one or more of starch, sucrose, dextrin, polyurethane, ethylene glycol, and phenolic resin.
Preferably, the gas source comprises one or more of urea, melamine, and polyamide.
The organic metal complex comprises one or more of iron, cobalt, nickel, zinc, copper metal ions, acetylacetone, salicylaldoxime and salicylaldehyde.
A method for preparing expanded flame-retardant polyethylene containing organic metal complex, comprising the following steps:
step 1: preparing the flame-retardant master batch, namely mixing an acid source, a carbon source and an air source according to a ratio of 1: 2-4: 1, adding 20 percent of low-density polyethylene, continuously stirring uniformly, putting the mixture after stirring into a double-screw extruder for extrusion, wherein the rotating speed is 30-60 revolutions per minute, the temperature is 200-;
step 2: stability treatment, namely adding 5-15% of cyanuric chloride and 5-10% of ammonium polyphosphate into the flame-retardant master batch in the step 1, stirring at the temperature of 5-15 ℃, stirring for 30 minutes, adding 5-15% of cyanuric chloride, stirring at the temperature of 40-60 ℃, adding 5-15% of cyanuric chloride, stirring at the temperature of 80-100 ℃ for 2 hours, and drying to obtain an intumescent flame retardant after stirring is finished, wherein the drying time is 6 hours and the temperature is 50-70 ℃;
and step 3: and (3) carrying out eutectic treatment, namely adding 1-3% of the expanded flame retardant dried in the step (2) into 70-80% of the organic metal complex and polyethylene, extruding and blending by a double-screw extruder at the temperature of 160-200 ℃ at 80-100 r/min, cooling for 6-8 hours at normal temperature after extrusion, and carrying out cutting granulation.
Compared with the prior art, the invention has the beneficial effects that:
1) the invention reduces the proportion of ammonium polyphosphate, avoids relying on excessive ammonium polyphosphate flame retardant performance, thereby reducing the water resistance of the material, adds cyanuric chloride to improve the stability, is convenient to construct a compound with a flame retardant function because the chlorine atom activity of the cyanuric chloride is very high, the nucleophilic substitution reaction is easy to carry out, chlorine atoms with different reaction activities can be substituted successively at different temperatures, the purpose of molecular renewal is realized by introducing required reactants on a triazine ring by controlling the reaction temperature, the invention has outstanding thermal stability, and the water resistance and the flame retardant performance of the material are improved.
2) The polyurethane is adopted to replace the traditional pentaerythritol, the pentaerythritol is easy to react with an acid source, the performance influence on the material is large, the macromolecular polyurethane is adopted to replace the material, the polyurethane is good in hydrophobicity and compatibility with a matrix and stable in thermal performance, the micromolecular pentaerythritol can be effectively replaced, the remarkable effect is achieved on the flame retardance of the material, the thermal stability of a material system is improved, and the flame retardance is improved.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a graph showing the results of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Referring to fig. 1, the present invention provides a technical solution:
example 1:
an intumescent flame retardant polyethylene containing organic metal complex, wherein the intumescent flame retardant polyethylene containing organic metal complex comprises polyethylene, intumescent flame retardant and organic metal complex, and the weight percentages of the polyethylene, intumescent flame retardant and organic metal complex are as follows: 70% of polyethylene, 28% of intumescent flame retardant and 2% of organic metal complex, wherein the intumescent flame retardant is prepared by compounding extruded flame-retardant master batches, ammonium polyphosphate and cyanuric chloride, and the flame-retardant master batches, the ammonium polyphosphate and the cyanuric chloride are as follows in percentage by weight in the intumescent flame retardant: 50% of flame-retardant master batch, 10% of ammonium polyphosphate and 40% of cyanuric chloride.
The flame-retardant master batch is formed by co-melting and extruding an acid source, a carbon source, a gas source and low-density polyethylene, wherein the weight percentage of the acid source, the carbon source, the gas source and the low-density polyethylene in the flame-retardant master batch is 5%, the weight percentage of the carbon source is 60%, the weight percentage of the gas source is 15% and the weight percentage of the low-density polyethylene is 20%.
The acid source comprises one or more of phosphoric acid, boric acid, sulfuric acid and phosphate.
The carbon source comprises one or more of starch, cane sugar, dextrin, polyurethane, glycol and phenolic resin.
The gas source comprises one or more of urea, melamine and polyamide.
The organic metal complex comprises one or more of iron, cobalt, nickel, zinc, copper metal ions, acetylacetone, salicylaldoxime and salicylaldehyde.
A method for preparing expanded flame-retardant polyethylene containing organic metal complex, comprising the following steps:
step 1: preparing the flame-retardant master batch by mixing an acid source, a carbon source and an air source according to a ratio of 1: 2: 1, adding 20 percent of low-density polyethylene, continuously stirring uniformly, putting the mixture after stirring into a double-screw extruder, extruding at the rotating speed of 30 revolutions per minute and the temperature of 200 ℃, and granulating after extruding;
step 2: stability treatment, namely adding 20% of cyanuric chloride and 10% of ammonium polyphosphate into the flame-retardant master batch in the step 1, stirring at 5 ℃ for 30 minutes, adding 10% of cyanuric chloride, stirring at 1 hour and 40 ℃, adding 10% of cyanuric chloride, stirring at 80 ℃ for 2 hours, and drying after stirring to obtain an intumescent flame retardant, wherein the drying time is 6 hours and the temperature is 50 ℃;
and step 3: and (3) carrying out eutectic treatment, namely adding 2% of the dried intumescent flame retardant in the step (2) into an organic metal complex and 70% of polyethylene, extruding and blending by a double-screw extruder at the temperature of 160 ℃ at 80 rpm, cooling for 6 hours at normal temperature after extrusion, and cutting and granulating.
Example 2:
an intumescent flame retardant polyethylene containing organic metal complex, wherein the intumescent flame retardant polyethylene containing organic metal complex comprises polyethylene, intumescent flame retardant and organic metal complex, and the weight percentages of the polyethylene, intumescent flame retardant and organic metal complex are as follows: 75% of polyethylene, 22% of intumescent flame retardant and 3% of organic metal complex, wherein the intumescent flame retardant is prepared by compounding extruded flame-retardant master batches, ammonium polyphosphate and cyanuric chloride, and the flame-retardant master batches, the ammonium polyphosphate and the cyanuric chloride are as follows in percentage by weight in the intumescent flame retardant: 50% of flame-retardant master batch, 10% of ammonium polyphosphate and 40% of cyanuric chloride.
The flame-retardant master batch is formed by co-melting and extruding an acid source, a carbon source, a gas source and low-density polyethylene, wherein the weight percentages of the acid source, the carbon source, the gas source and the low-density polyethylene in the flame-retardant master batch are 10%, 55%, 15% and 20%.
The acid source comprises one or more of phosphoric acid, boric acid, sulfuric acid and phosphate.
The carbon source comprises one or more of starch, cane sugar, dextrin, polyurethane, glycol and phenolic resin.
The gas source comprises one or more of urea, melamine and polyamide.
The organic metal complex comprises one or more of iron, cobalt, nickel, zinc, copper metal ions, acetylacetone, salicylaldoxime and salicylaldehyde.
A method for preparing expanded flame-retardant polyethylene containing organic metal complex, comprising the following steps:
step 1: preparing the flame-retardant master batch, namely mixing an acid source, a carbon source and an air source according to a ratio of 1: 3: 1, adding 20 percent of low-density polyethylene, continuously stirring uniformly, putting the mixture after stirring into a double-screw extruder, extruding at the rotating speed of 60 revolutions per minute and the temperature of 300 ℃, and granulating after extruding;
step 2: stability treatment, namely adding 30% of cyanuric chloride and 10% of ammonium polyphosphate into the flame-retardant master batch in the step 1, stirring at 15 ℃ for 30 minutes, adding 5% of cyanuric chloride, stirring at 1 hour and 60 ℃, adding 5% of cyanuric chloride, stirring at 100 ℃ for 2 hours, and drying after stirring to obtain an intumescent flame retardant, wherein the drying time is 6 hours and the temperature is 70 ℃;
and step 3: and (3) carrying out eutectic treatment, namely adding 3% of the organic metal complex and 75% of polyethylene into the dried intumescent flame retardant in the step (2), extruding and blending by a double-screw extruder at 100 revolutions per minute and 200 ℃, cooling for 8 hours at normal temperature after extrusion, and cutting and granulating.
Example 3:
an intumescent flame retardant polyethylene containing organic metal complex, wherein the intumescent flame retardant polyethylene containing organic metal complex comprises polyethylene, intumescent flame retardant and organic metal complex, and the weight percentages of the polyethylene, intumescent flame retardant and organic metal complex are as follows: 70% of polyethylene, 29% of intumescent flame retardant and 1% of organic metal complex, wherein the intumescent flame retardant is prepared by compounding extruded flame-retardant master batches, ammonium polyphosphate and cyanuric chloride, and the flame-retardant master batches, the ammonium polyphosphate and the cyanuric chloride are as follows in percentage by weight in the intumescent flame retardant: 50% of flame-retardant master batch, 10% of ammonium polyphosphate and 40% of cyanuric chloride.
The flame-retardant master batch is formed by co-melting and extruding an acid source, a carbon source, a gas source and low-density polyethylene, wherein the weight percentage of the acid source, the carbon source, the gas source and the low-density polyethylene in the flame-retardant master batch is 5%, the weight percentage of the carbon source is 60%, the weight percentage of the gas source is 15% and the weight percentage of the low-density polyethylene is 20%.
The acid source comprises one or more of phosphoric acid, boric acid, sulfuric acid and phosphate.
The carbon source comprises one or more of starch, cane sugar, dextrin, polyurethane, glycol and phenolic resin.
The gas source comprises one or more of urea, melamine and polyamide.
The organic metal complex comprises one or more of iron, cobalt, nickel, zinc, copper metal ions, acetylacetone, salicylaldoxime and salicylaldehyde.
A method for preparing expanded flame-retardant polyethylene containing organic metal complex, comprising the following steps:
step 1: preparing the flame-retardant master batch by mixing an acid source, a carbon source and an air source according to a ratio of 1: 4: 1, adding 20 percent of low-density polyethylene, continuously stirring uniformly, putting the mixture after stirring into a double-screw extruder, extruding at the rotating speed of 50 revolutions per minute and the temperature of 300 ℃, and granulating after extruding;
step 2: stability treatment, namely adding 10% of cyanuric chloride and 10% of ammonium polyphosphate into the flame-retardant master batch in the step 1, stirring at 10 ℃ for 30 minutes, adding 15% of cyanuric chloride, stirring at 1 hour and 50 ℃, adding 15% of cyanuric chloride, stirring at 90 ℃ for 2 hours, and drying after stirring to obtain an intumescent flame retardant, wherein the drying time is 6 hours and the temperature is 60 ℃;
and step 3: and (3) carrying out eutectic treatment, namely adding 1% of the organic metal complex and 70% of polyethylene into the dried intumescent flame retardant in the step (2), extruding and blending by a double-screw extruder, cooling for 7 hours at normal temperature after extrusion at 90 revolutions per minute and 180 ℃, and cutting and granulating.
The test results according to figure 2 show that,
while there have been shown and described the fundamental principles and essential features of the invention and advantages thereof, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof; the present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. An intumescent, flame retardant polyethylene comprising an organometallic complex, characterized in that: the intumescent flame retardant polyethylene containing the organic metal complex comprises polyethylene, an intumescent flame retardant and the organic metal complex, wherein the weight percentages of the polyethylene, the intumescent flame retardant and the organic metal complex are as follows: 70-80% of polyethylene, 20-30% of intumescent flame retardant and 1-3% of organic metal complex, wherein the intumescent flame retardant is prepared by compounding extruded flame retardant master batches, ammonium polyphosphate and cyanuric chloride, and the flame retardant master batches, the ammonium polyphosphate and the cyanuric chloride are as follows by weight percent in the intumescent flame retardant: 40-50% of flame-retardant master batch, 5-10% of ammonium polyphosphate and 30-40% of cyanuric chloride.
2. The expanded flame-retardant polyethylene containing an organometallic complex according to claim 1, wherein: the flame-retardant master batch is formed by co-melting and extruding an acid source, a carbon source, a gas source and low-density polyethylene, wherein the weight percentages of the acid source, the carbon source, the gas source and the low-density polyethylene in the flame-retardant master batch are 5-10%, 40-60%, 10-15% and 20%.
3. The expanded flame-retardant polyethylene containing an organometallic complex according to claim 1, wherein: the acid source comprises one or more of phosphoric acid, boric acid, sulfuric acid and phosphate.
4. The expanded flame-retardant polyethylene containing an organometallic complex according to claim 1, wherein: the carbon source comprises one or more of starch, cane sugar, dextrin, polyurethane, glycol and phenolic resin.
5. The expanded flame-retardant polyethylene containing an organometallic complex according to claim 1, wherein: the gas source comprises one or more of urea, melamine and polyamide.
6. The expanded flame-retardant polyethylene containing an organometallic complex according to claim 1, wherein: the organic metal complex comprises one or more of iron, cobalt, nickel, zinc, copper metal ions, acetylacetone, salicylaldoxime and salicylaldehyde.
7. The method for preparing expanded flame-retardant polyethylene containing organometallic complex according to claim 1, wherein: the method comprises the following steps:
step 1: preparing the flame-retardant master batch, namely mixing an acid source, a carbon source and an air source according to a ratio of 1: 2-4: 1, adding 20 percent of low-density polyethylene, continuously stirring uniformly, putting the mixture after stirring into a double-screw extruder for extrusion, wherein the rotating speed is 30-60 revolutions per minute, the temperature is 200-;
step 2: stability treatment, namely adding 5-15% of cyanuric chloride and 5-10% of ammonium polyphosphate into the flame-retardant master batch in the step 1, stirring at the temperature of 5-15 ℃, stirring for 30 minutes, adding 5-15% of cyanuric chloride, stirring at the temperature of 40-60 ℃, adding 5-15% of cyanuric chloride, stirring at the temperature of 80-100 ℃ for 2 hours, and drying to obtain an intumescent flame retardant after stirring is finished, wherein the drying time is 6 hours and the temperature is 50-70 ℃;
and step 3: and (3) carrying out eutectic treatment, namely adding 1-3% of the expanded flame retardant dried in the step (2) into 70-80% of the organic metal complex and polyethylene, extruding and blending by a double-screw extruder at the temperature of 160-200 ℃ at 80-100 r/min, cooling for 6-8 hours at normal temperature after extrusion, and carrying out cutting granulation.
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