CN110183728B - In-situ polymerization intumescent flame retardant, preparation raw material, preparation method and application thereof - Google Patents
In-situ polymerization intumescent flame retardant, preparation raw material, preparation method and application thereof Download PDFInfo
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- C08K3/38—Boron-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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- C08K2201/005—Additives being defined by their particle size in general
Abstract
The invention belongs to the field of flame retardants, and discloses an in-situ polymerization intumescent flame retardant, a preparation raw material, a preparation method and application thereof. The preparation method of the in-situ polymerization intumescent flame retardant comprises the following steps: s1, stirring and mixing the concentrated acid and the flake graphite at the temperature of 30-40 ℃ for 30-60 min, and then carrying out ultrasonic treatment on the obtained mixture for 20-100 min to obtain swollen flake graphite; s2, carrying out in-situ polymerization on the swollen flake graphite, a nitrogen-containing compound and a phosphorus-containing compound, carrying out solid-liquid separation on the obtained in-situ polymerization product, and washing and drying the obtained solid product to obtain intercalated graphite; and S3, uniformly mixing the intercalated graphite and the boride. The in-situ polymerization intumescent flame retardant prepared by the method has the characteristics of no halogen, environmental protection, no toxicity, high efficiency, no dripping and the like, can effectively retard flame for polyolefin, has good compatibility with polyolefin matrix, and basically has no influence on the mechanical properties of the polyolefin.
Description
Technical Field
The invention belongs to the field of flame retardants, and particularly relates to an in-situ polymerization intumescent flame retardant, a preparation raw material, a preparation method and application thereof.
Background
The flame retardant is used as a second largest global polymer material additive which is second only to a plasticizer, and is widely applied to various industries such as automobiles, household appliances, electricians and electronics, aerospace, medical health, buildings and the like at present. The consumption of the flame retardant is more than 20 million tons every year, and 80 percent of the flame retardant is halogen flame retardant. However, the halogen flame retardant has the problems of toxicity, heavy smoke, dripping, environmental protection and the like in combustion, from 2006, the european union limits the use of a plurality of halogen flame retardants, such as octabromodiphenyl ether, pentabromodiphenyl ether and the like, while other halogen flame retardants are not limited, but with the increasing severity and prominence of environmental protection problems, the halogen flame retardant will exit the history stage and replace the halogen flame retardant with non-toxic, high-efficiency, good compatibility with a substrate and moderate price.
At present, common halogen-free flame retardants include phosphorus flame retardants, nitrogen flame retardants, phosphorus-nitrogen flame retardants, and the like, but the existing halogen-free flame retardants have the problems of poor compatibility with a substrate, easy precipitation, large addition amount, easy deliquescence, and the like, and the flame retardant performance and the compatibility with the substrate still need to be further improved.
Disclosure of Invention
The invention aims to overcome the defects of poor flame retardant effect and poor compatibility with a matrix of the conventional halogen-free flame retardant, and provides an in-situ polymerization intumescent flame retardant which has good flame retardant effect, good compatibility with the matrix and basically no influence on the mechanical properties of the matrix, a preparation raw material, a preparation method and application thereof.
Specifically, the invention provides a raw material for preparing an in-situ polymerization intumescent flame retardant, wherein the raw material for preparing the in-situ polymerization intumescent flame retardant comprises the following components in percentage by weight:
preferably, the concentrated acid is selected from at least one of concentrated phosphoric acid, concentrated sulfuric acid, concentrated nitric acid and concentrated chromic acid.
Preferably, the concentration of the concentrated acid is 98 wt% or more.
Preferably, the carbon content of the flake graphite is 87 wt% or more.
Preferably, the particle size of the crystalline flake graphite is 80-100 meshes.
Preferably, the nitrogen-containing compound is an ammonium compound and/or an amide compound, and more preferably at least one selected from the group consisting of a carbamide, a polyurethane, a dicyandiamide, a melamine and a polyurea resin.
Preferably, the phosphorus-containing compound is selected from at least one of ammonium phosphate salts, phosphate esters, ammonium polyphosphate, polyphosphoric acid amides, pentaerythritol phosphate ester melamine salts, melamine polyphosphate and melamine phosphate.
Preferably, the boride is selected from at least one of zinc borate, calcium borate and aluminum borate.
The invention also provides a preparation method of the in-situ polymerization intumescent flame retardant, wherein the preparation method takes the preparation raw materials of the in-situ polymerization intumescent flame retardant as raw materials and comprises the following steps:
s1, stirring and mixing the concentrated acid and the flake graphite at the temperature of 30-40 ℃ for 30-60 min, and then carrying out ultrasonic treatment on the obtained mixture for 20-100 min to obtain swollen flake graphite;
s2, carrying out in-situ polymerization on the swollen flake graphite, the nitrogen-containing compound and the phosphorus-containing compound, carrying out solid-liquid separation on an obtained in-situ polymerization product, and washing and drying the obtained solid product to obtain intercalated graphite;
s3, uniformly mixing the intercalated graphite and the boride.
Preferably, in step S2, the in-situ polymerization conditions include a temperature of 40 to 50 ℃ and a time of 30 to 60 min.
Preferably, in step S2, the washing conditions are such that the pH of the washed product is 7-8.
Preferably, in step S2, the drying conditions include a temperature of 50 to 65 ℃ and a time of 30 to 50 min.
The invention also provides the in-situ polymerization intumescent flame retardant prepared by the method.
In addition, the invention also provides application of the in-situ polymerization intumescent flame retardant as a polyolefin flame retardant.
The preparation method comprises the steps of stirring and mixing concentrated acid and flake graphite, carrying out ultrasonic treatment, swelling and opening flake graphite sheets by utilizing the concentrated acid, adding an intercalation nitrogen-containing compound and a phosphorus-containing compound for in-situ polymerization, and finally mixing boride for compounding for synergistic flame retardance, wherein the obtained in-situ polymerization intumescent flame retardant has the characteristics of no halogen, environmental protection, no toxicity, high efficiency, no dripping and the like, can effectively retard flame for polyolefin, is good in compatibility with polyolefin matrix, and basically has no influence on the mechanical property of the polyolefin.
The flame retardant principle of the invention is that when the in-situ polymerization intumescent flame retardant is in an environment to be flame retarded at about 300 ℃, a nitrogen-containing compound and a phosphorus-containing compound adsorbed between flake graphite sheets can be heated and decomposed into gas, the flake graphite can expand by hundreds of times instantly, oxygen can be effectively isolated from entering and the escape of combustible gas can be inhibited, simultaneously, the generated nitrogen can dilute the oxygen concentration in the air and reduce the surface temperature of the material, and then boric acid ester salt can be generated by matching with boride to promote the surface carbonization of the object to be flame retarded.
Detailed Description
The type of the concentrated acid in the present invention is not particularly limited, and may be any of various existing high-concentration acid solutions capable of swelling and opening flake graphite sheets, and specific examples thereof include, but are not limited to: at least one of concentrated phosphoric acid, concentrated sulfuric acid, concentrated nitric acid and concentrated chromic acid. The concentration of the concentrated acid is preferably 98 wt% or more.
The graphite crystal of the flake graphite is scaly. The carbon content of the crystalline flake graphite is preferably more than 87 wt%, and more preferably 90-95 wt%. That is, the flake graphite is preferably medium carbon graphite, high carbon graphite, or high purity graphite. The particle size of the flake graphite is preferably 80-100 meshes.
The nitrogen-containing compound of the present invention is not particularly limited in kind, and may be any of various existing substances that can enter the flake graphite sheet as an intercalation and be decomposed into nitrogen gas by heating, for example, ammonium compounds and/or amide compounds, and specific examples thereof include, but are not limited to: at least one of a carbamide, a polyurethane, a dicyandiamide, a melamine and a polyurea resin.
In the present invention, the phosphorus-containing compound plays a role in promoting dehydration and carbon formation on the surface of the object to be flame-retarded, and performs a carbon formation reaction with a carbon source (resin) under the action of high temperature, so as to promote foaming and expansion of the molten system, isolate oxygen from the reaction of combustible gas, and further inhibit combustion, and specific examples thereof include, but are not limited to: at least one of ammonium phosphate salts, phosphoric acid esters, ammonium polyphosphate, polyphosphoric acid amides, pentaerythritol phosphoric acid ester melamine salts, melamine polyphosphate and melamine phosphate.
When the raw material used is a compound containing both nitrogen and phosphorus, the content of the raw material should be taken into account in the content of the phosphorus-containing compound.
The boride is not particularly limited in kind in the present invention, and may be at least one selected from the group consisting of zinc borate, calcium borate and aluminum borate.
The preparation method of the in-situ polymerization intumescent flame retardant provided by the invention takes the preparation raw materials of the in-situ polymerization intumescent flame retardant as raw materials and comprises the following steps:
s1, stirring and mixing the concentrated acid and the flake graphite at the temperature of 30-40 ℃ for 30-60 min, and then carrying out ultrasonic treatment on the obtained mixture for 20-100 min to obtain swollen flake graphite;
s2, carrying out in-situ polymerization on the swollen flake graphite, the nitrogen-containing compound and the phosphorus-containing compound, carrying out solid-liquid separation on an obtained in-situ polymerization product, and washing and drying the obtained solid product to obtain intercalated graphite;
s3, uniformly mixing the intercalated graphite and the boride.
The specific reaction process is as follows: the flake graphite is firstly swelled and opened under the action of concentrated acid, then a nitrogen-containing compound and a phosphorus-containing compound are added, the two substances can be used as intercalation substances to enter a flake structure of the flake graphite to form graphite oxide, strong chemical bonding can be formed through the group action between the two substances, when the flake graphite is subjected to high temperature, the compounds can be rapidly decomposed into gas to further swell the graphite, so that the flame retardant effect is achieved, and finally the mixed boride can play a synergistic flame retardant effect.
In the invention, in step S1, the ultrasonic frequency used for the ultrasonic treatment may be 20 to 50 KHz.
In the present invention, in step S2, the in-situ polymerization condition preferably includes a temperature of 40 to 50 ℃ and a time of 30 to 60 min. The solid-liquid separation method may be, for example, suction filtration, pressure filtration, or the like. The washing agent used for the washing is preferably an alkali solution, and specifically may be at least one of a sodium hydroxide solution, a potassium hydroxide solution, a sodium bicarbonate solution, a potassium bicarbonate solution, and the like. The washing time is preferably determined to ensure that the pH value of the washing product is 7-8. The drying conditions generally include a temperature of 50-65 ℃ and a time of 30-50 min.
In the present invention, in step S3, the mixing conditions generally include that the temperature may be room temperature, the stirring rate may be 80 to 130rpm, and the time may be 20 to 40 min.
The invention also provides the in-situ polymerization intumescent flame retardant prepared by the method.
In addition, the invention also provides application of the in-situ polymerization intumescent flame retardant as a polyolefin flame retardant. The polyolefin may be at least one of polypropylene, polyethylene, poly-1-butene, poly-2-butene, polybutadiene, polystyrene, and the like.
The following detailed description of embodiments of the invention is intended to be illustrative of the invention and is not to be construed as limiting the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
This example is intended to illustrate the preparation of the in-situ polymerization intumescent flame retardant provided by the present invention, wherein the amounts of the raw materials are shown in table 1, and the specific process is as follows:
s1, adding concentrated acid (concentrated phosphoric acid with the concentration of 98 wt%) and flake graphite (with the carbon content of 90 wt% and the particle size of 80-100 meshes) into a three-neck flask provided with a condenser tube, stirring and mixing for 60min at 30 ℃, and then treating the obtained mixture for 100min in ultrasonic waves with the frequency of 30KHz to obtain swollen flake graphite;
s2, pouring the swollen flake graphite into a flask containing a nitrogen-containing compound (carbamide) and a phosphorus-containing compound (melamine phosphate), stirring for 60min at 40 ℃ to complete in-situ polymerization, then carrying out suction filtration on the obtained in-situ polymerization product, washing filter residues with an alkali liquor until the pH value is 7, and drying the obtained washing product at 65 ℃ for 30min to obtain intercalated graphite;
s3, adding the intercalated graphite into boride (zinc borate), and stirring at a high speed for 30min to obtain the in-situ polymerization intumescent flame retardant.
Example 2
This example is intended to illustrate the preparation of the in-situ polymerization intumescent flame retardant provided by the present invention, wherein the amounts of the raw materials are shown in table 1, and the specific process is as follows:
s1, adding concentrated acid (concentrated sulfuric acid with the concentration of 98 wt%) and flake graphite (with the carbon content of 95 wt% and the particle size of more than 80-100 meshes) into a three-neck flask provided with a condenser tube, stirring and mixing for 30min at 40 ℃, and then treating the obtained mixture in ultrasonic waves with the frequency of 30Hz for 60min to obtain swollen flake graphite;
s2, pouring the swollen flake graphite into a flask containing a nitrogen-containing compound (polyurea resin) and a phosphorus-containing compound (orthophosphate), stirring for 30min at 50 ℃ to complete in-situ polymerization, then carrying out suction filtration on the obtained in-situ polymerization product, washing filter residues with alkali liquor until the pH value is 8, and drying the obtained washing product at 50 ℃ for 50min to obtain intercalated graphite;
s3, adding the intercalated graphite into boride (calcium borate), and stirring at a high speed for 30min to obtain the in-situ polymerization intumescent flame retardant.
Example 3
This example is intended to illustrate the preparation of the in-situ polymerization intumescent flame retardant provided by the present invention, wherein the amounts of the raw materials are shown in table 1, and the specific process is as follows:
s1, adding concentrated acid (concentrated nitric acid with the concentration of 98 wt%) and flake graphite (with the carbon content of 92 wt% and the particle size of more than 80-100 meshes) into a three-neck flask with a condenser pipe, stirring and mixing for 45min at 35 ℃, and then treating the obtained mixture in ultrasonic waves with the frequency of 50Hz for 20min to obtain swollen flake graphite;
s2, pouring the swollen flake graphite into a flask containing a nitrogen-containing compound (polyurethane) and a phosphorus-containing compound (ammonium tripolyphosphate), stirring for 45min at 45 ℃ to complete in-situ polymerization, then carrying out suction filtration on the obtained in-situ polymerization product, washing filter residues with an alkali liquor until the pH value is 7.5, and then drying the obtained washing product at 55 ℃ for 40min to obtain intercalated graphite;
s3, adding the intercalated graphite into boride (aluminum borate), and stirring at a high speed for 30min to obtain the in-situ polymerization intumescent flame retardant.
Example 4
This example is intended to illustrate the preparation of the in-situ polymerization intumescent flame retardant provided by the present invention, wherein the amounts of the raw materials are shown in table 1, and the specific process is as follows:
s1, adding concentrated acid (concentrated chromic acid with the concentration of 98 wt%) and flake graphite (with the carbon content of 90 wt% and the particle size of 80-100 meshes) into a three-neck flask with a condenser pipe, stirring and mixing for 45min at 35 ℃, and then treating the obtained mixture in ultrasonic waves with the frequency of 50Hz for 60min to obtain swollen flake graphite;
s2, pouring the swollen flake graphite into a flask containing a nitrogen-containing compound (dicyandiamide) and a phosphorus-containing compound (pentaerythritol phosphate melamine salt) and stirring for 45min at 45 ℃ to complete in-situ polymerization, then performing suction filtration on the obtained in-situ polymerization product, washing filter residues with an alkali liquor until the pH value is 7.5, and then drying the obtained washing product at 65 ℃ for 30min to obtain intercalated graphite;
s3, adding the intercalated graphite into boride (zinc borate), and stirring at a high speed for 30min to obtain the in-situ polymerization intumescent flame retardant.
Comparative example 1
An in-situ polymerization intumescent flame retardant was prepared according to the method of example 1, except that the boride and a part of the phosphorus-containing compound were replaced with the same weight part of concentrated acid, and the remaining conditions were the same as those of example 1, to obtain a reference in-situ polymerization intumescent flame retardant. The amounts of the respective substances are shown in table 1.
Comparative example 2
An in-situ polymerization intumescent flame retardant was prepared by following the procedure of example 1 except that the amounts of the respective materials were out of the range of the present invention and the remaining conditions were the same as in example 1 to obtain a reference in-situ polymerization intumescent flame retardant. The amounts of the respective substances are shown in table 1.
Comparative example 3
An in-situ polymerization intumescent flame retardant was prepared according to the method of example 1, except that the boride was replaced with the same weight part of crystalline flake graphite, and the remaining conditions were the same as those of example 1, to obtain the reference in-situ polymerization intumescent flame retardant. The amounts of the respective substances are shown in table 1.
Comparative example 4
An in-situ polymerization intumescent flame retardant was prepared by following the procedure of example 1, except that the nitrogen-containing compound was replaced with the same weight part of the phosphorus-containing compound, and the remaining conditions were the same as in example 1, to obtain a reference in-situ polymerization intumescent flame retardant. The amounts of the respective substances are shown in table 1.
TABLE 1 amount of raw materials (wt%)
Test example
The in-situ polymerization intumescent flame retardants obtained in examples 1 to 4 and the reference in-situ polymerization intumescent flame retardants obtained in comparative examples 1 to 4 were added to polypropylene (No. 7726H, pure LOI 18%, UL94V-2, notched Izod impact strength of 11.8kJ/m measured according to GB/T1843-2008 standard) at a ratio of 24 wt% and 30 wt%, respectively2) The notched izod impact strength, LOI oxygen index, and flame retardant properties of the resulting composite were tested as follows, with the results shown in table 2.
(1) Notched izod impact strength: testing according to GB/T1843-2008 standard;
(2) LOI oxygen index: testing according to GB/T2406.2-2009 standard;
(3) flame retardant property: the test was carried out according to UL94 standard, wherein the specimen thickness was 3.2 mm.
TABLE 2
As can be seen from the results in Table 2, the oxygen index (LOI) corresponding to the flame retardant addition amounts of 24 wt% and 30 wt% in examples 1 to 4 reach 28.2% to 30.7% and 29.6% to 32.1%, respectively, which are significantly higher than those of comparative examples 1 to 4, i.e., 24.4% to 26.2% and 25.5% to 27.1%; the flame retardant grades of the examples all reach V-0 grade, which is higher than V-1 grade and V-2 grade in comparative examples 1-4; meanwhile, the in-situ polymerization intumescent flame retardant provided by the invention has no influence on the notched impact strength of the cantilever beam of the polyolefin composite material.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention.
Claims (9)
1. The preparation method of the in-situ polymerization intumescent flame retardant is characterized in that the raw materials for preparing the in-situ polymerization intumescent flame retardant consist of the following components in percentage by weight:
the boride is selected from at least one of zinc borate, calcium borate and aluminum borate, and the total content of concentrated acid, phosphorus flake graphite, a nitrogen-containing compound, a phosphorus-containing compound and the boride is 100%;
the method comprises the following steps:
s1, stirring and mixing the concentrated acid and the flake graphite at the temperature of 30-40 ℃ for 30-60 min, and then carrying out ultrasonic treatment on the obtained mixture for 20-100 min to obtain swollen flake graphite;
s2, carrying out in-situ polymerization on the swollen flake graphite, the nitrogen-containing compound and the phosphorus-containing compound, carrying out solid-liquid separation on an obtained in-situ polymerization product, and washing and drying the obtained solid product to obtain intercalated graphite;
s3, uniformly mixing the intercalated graphite and the boride to obtain the in-situ polymerization intumescent flame retardant.
2. The method for preparing an in-situ polymerization intumescent flame retardant of claim 1, wherein in step S2, the in-situ polymerization conditions include a temperature of 40-50 ℃ and a time of 30-60 min; the washing condition enables the pH value of a washing product to be 7-8; the drying conditions comprise that the temperature is 50-65 ℃ and the time is 30-50 min.
3. A process of preparing an in situ polymerized intumescent flame retardant as claimed in claim 1, wherein said concentrated acid is selected from at least one of concentrated phosphoric acid, concentrated sulfuric acid, concentrated nitric acid and concentrated chromic acid; the concentration of the concentrated acid is more than 98 wt%.
4. The method for preparing in-situ polymerization intumescent flame retardant of claim 1, characterized in that the carbon content of the crystalline flake graphite is more than 87 wt%; the particle size of the crystalline flake graphite is 80-100 meshes.
5. The method of claim 1, wherein the nitrogen-containing compound is an ammonium compound and/or an amide compound.
6. Process for the preparation of in situ polymerized intumescent flame retardant according to claim 5, characterized in that said nitrogen containing compound is selected from at least one of the group consisting of carbamide, polyurethane, dicyandiamide, melamine and polyurea resins.
7. The method of claim 1, wherein the phosphorus-containing compound is at least one selected from ammonium phosphate salts, phosphate esters, ammonium polyphosphate, polyphosphoric acid amides, pentaerythritol phosphate melamine salts, melamine polyphosphate and melamine phosphate.
8. An in-situ polymerization intumescent flame retardant prepared by the method of any one of claims 1 to 7.
9. Use of the in situ polymerized intumescent flame retardant of claim 8 as a flame retardant for polyolefins.
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