CN113956533A - Polyolefin flame-retardant filler, preparation method and application - Google Patents
Polyolefin flame-retardant filler, preparation method and application Download PDFInfo
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- CN113956533A CN113956533A CN202111329151.8A CN202111329151A CN113956533A CN 113956533 A CN113956533 A CN 113956533A CN 202111329151 A CN202111329151 A CN 202111329151A CN 113956533 A CN113956533 A CN 113956533A
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- retardant filler
- flame
- magnesium hydroxide
- polyolefin
- hexadecylamine
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 60
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229920000098 polyolefin Polymers 0.000 title claims abstract description 42
- 239000000945 filler Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 5
- NFMWFGXCDDYTEG-UHFFFAOYSA-N trimagnesium;diborate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]B([O-])[O-].[O-]B([O-])[O-] NFMWFGXCDDYTEG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 42
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 38
- 239000002131 composite material Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 16
- 239000000347 magnesium hydroxide Substances 0.000 claims description 16
- 239000004743 Polypropylene Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 229920001155 polypropylene Polymers 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 14
- 239000004698 Polyethylene Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 12
- 229920000573 polyethylene Polymers 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- -1 polyethylene Polymers 0.000 claims description 11
- 229920002292 Nylon 6 Polymers 0.000 claims description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 10
- 239000004327 boric acid Substances 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 5
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052796 boron Inorganic materials 0.000 abstract description 2
- 238000003763 carbonization Methods 0.000 abstract description 2
- 238000002485 combustion reaction Methods 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 16
- 238000002156 mixing Methods 0.000 description 15
- 239000000203 mixture Substances 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
-
- 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
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/06—Polystyrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention relates to a polyolefin flame-retardant filler, a preparation method and application thereof. The hexadecylamine in the flame-retardant filler is of an organic long-chain structure, the compatibility of the flame-retardant filler and a polyolefin material in the flame-retardant filler can be improved, so that the mechanical property is improved, and the magnesium borate contains boron which can be used for realizing the synergistic flame retardance with the nitrogen element of the hexadecylamine, so that the flame-retardant property can be improved. Meanwhile, the magnesium borate can promote the carbonization of a polymer chain and increase the residual quantity of carbon after combustion, thereby improving the flame retardant property of the flame retardant.
Description
Technical Field
The invention belongs to the technical field of flame retardants, and particularly relates to a polyolefin flame-retardant filler, a preparation method and an application thereof.
Background
Polyolefins are composed primarily of carbon, ammonia, and oxygen atoms, and therefore polyolefins are generally flammable, and there are many ways to improve the flame retardant properties of polyolefins, but conventional methods have been to incorporate flame retardant fillers into polyolefins. The existing flame-retardant fillers are all conventional fillers, and have poor compatibility when being mixed with polyolefin, so that the compatibility problem needs to be solved by using a compatilizer while the flame-retardant fillers are used, and the mechanical property of the polyolefin cannot reach the optimal state of the polyolefin.
Disclosure of Invention
The invention aims to provide a polyolefin flame-retardant filler, a preparation method and application thereof, so as to solve the problems of the conventional flame-retardant filler.
In order to achieve the purpose, the method is realized by the following technical scheme:
a polyolefin flame retardant filler is magnesium hydroxide @ magnesium borate @ hexadecylamine.
Further, the mass ratio of the magnesium hydroxide @ magnesium borate to the hexadecylamine is (30-50): (14-16).
A process for the preparation of a polyolefin flame retardant filler according to any of the preceding claims, comprising the steps of:
s1, weighing magnesium hydroxide, acetone and boric acid according to a set amount, adding into a reaction vessel, stirring and reacting for 10-16h at normal temperature to prepare a solution A;
s2, filtering and washing the solution A, and drying the solution A in a vacuum drying oven at the temperature of 40-60 ℃ for 6-8h to obtain magnesium hydroxide @ magnesium borate;
s3, weighing the magnesium hydroxide @ magnesium borate, hexadecylamine and acetone according to the set amount, adding the weighed materials into a reaction vessel, stirring and reacting for 10-18h at normal temperature, washing, filtering, and drying in a vacuum drying oven for 8-10h at 50-70 ℃ to obtain the magnesium hydroxide @ magnesium borate @ hexadecylamine, namely the polyolefin flame-retardant filler.
Further, the mass ratio of magnesium hydroxide, acetone and boric acid in step S1 is (50-60): (120-160): (30-40).
Further, the mass ratio of magnesium hydroxide @ magnesium borate, hexadecylamine and acetone in step S3 is (30-50): (14-16): (160-200).
The application of the polyolefin flame-retardant filler, wherein the polyolefin flame-retardant filler is applied to the polyolefin composite material.
Further, the polyolefin is one of polyethylene, polypropylene, polystyrene, polybutylene terephthalate and polyamide 6.
The invention has the beneficial effects that:
1. the hexadecylamine is an organic long-chain structure, the compatibility of the flame-retardant filler and a polyolefin material in the application can be improved, so that the mechanical property is improved, and the magnesium borate contains boron which can be used for realizing the synergistic flame retardance with the nitrogen element of the hexadecylamine, so that the flame retardant property can be improved. Meanwhile, the magnesium borate can promote the carbonization of a polymer chain and increase the residual quantity of carbon after combustion, thereby improving the flame retardant property of the flame retardant.
2. The polyolefin flame-retardant filler can well improve the flame retardant property and the mechanical property of the polyolefin composite material, and has great popularization value.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
The raw materials used in the examples of the invention are as follows:
PBT (model 2002U), Japan treaty; PP (model Z30S), mazineb petrochemical; PE (model 5070), brocade ethylene; PA6 (model CM1017), eastern japan; PS (model 350), national joe, taiwan; magnesium hydroxide, Weifang Dakang chemical Co., Ltd; acetone, chemical Limited, Jinchuan, Jinan; boric acid, chemical ltd, denhakun; hexadecylamine, yunnan lilian bio ltd.
The test instrument used in the present invention is as follows:
model ZSK30 twin-screw extruder, W & P, Germany; an internal mixer, big lianhua korea rubber; JL-1000 type tensile testing machine, produced by Guangzhou Youcai laboratory instruments; HTL900-T-5B injection molding machine, manufactured by Haita plastics machinery, Inc.; XCJ-500 impact tester, manufactured by Chengde tester; QT-1196 tensile tester, Gaotai detection instruments, Inc. of Dongguan; QD-GJS-B12K model high-speed mixer, HengOde instruments, Beijing.
Preparation example 1
(1) Weighing 500g of magnesium hydroxide, 1.2kg of acetone and 300g of boric acid, adding into a reaction vessel, and stirring and reacting for 10 hours at normal temperature to prepare a solution A.
(2) And filtering and washing the solution A, and drying the solution A in a vacuum drying oven at 40 ℃ for 6 hours to obtain the magnesium hydroxide @ magnesium borate.
(3) Weighing 300g of magnesium hydroxide @ magnesium borate, 140g of hexadecylamine and 1.6kg of acetone, adding the mixture into a reaction vessel, stirring and reacting for 10 hours at normal temperature, washing, filtering, and drying in a vacuum drying oven for 8 hours at 50 ℃ to obtain the magnesium hydroxide @ magnesium borate @ hexadecylamine, namely the polyolefin flame-retardant filler P1.
Application example 1
And adding 20 parts of P1 into 80 Parts of Polypropylene (PP), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PP composite material X1.
Comparative example 1
80 Parts of Polypropylene (PP) is taken, stirred for 10min by a high-speed mixer and then added into a double-screw extruder for blending and extrusion, so as to obtain the PP composite material D1.
Comparative example 2
Adding 20 parts of magnesium hydroxide into 80 Parts of Polypropylene (PP), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PP composite material N1.
The performance data of the PP composites prepared in application example 1 and comparative examples 1 and 2 are shown in the following table:
as can be seen from the table above, the flame retardant property and the mechanical property of X1 are superior to those of D1 and N1, which shows that the flame retardant property and the mechanical property of PP are better after the flame retardant filler is added.
Preparation example 2
(1) 600g of magnesium hydroxide, 1.6kg of acetone and 400g of boric acid are weighed and added into a reaction vessel, and the mixture is stirred and reacted for 16 hours at normal temperature to prepare a solution A.
(2) And filtering and washing the solution A, and drying the solution A in a vacuum drying oven at 60 ℃ for 8 hours to obtain the magnesium hydroxide @ magnesium borate.
(3) Weighing 500g of magnesium hydroxide @ magnesium borate, 160g of hexadecylamine and 2.0kg of acetone, adding the mixture into a reaction vessel, stirring and reacting for 18h at normal temperature, washing, filtering, and drying in a vacuum drying oven for 10h at 70 ℃ to obtain the magnesium hydroxide @ magnesium borate @ hexadecylamine, namely the polyolefin flame-retardant filler P2.
Application example 2
And adding 20 parts of P2 into 80 parts of polybutylene terephthalate (PBT), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PBT composite material X2.
Comparative example 3
And (3) taking 80 parts of PBT, stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PBT composite material D2.
Comparative example 4
And adding 20 parts of magnesium hydroxide into 80 parts of PBT, stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PBT composite material N2.
The performance data of the PBT composites prepared in application example 2 and comparative examples 3 and 4 are shown in the following table:
as can be seen from the table above, the flame retardant property and the mechanical property of X2 are superior to those of D2 and N2, which shows that the flame retardant property and the mechanical property of PBT are better after the flame retardant filler is added.
Preparation example 3
(1) 550g of magnesium hydroxide, 1.4kg of acetone and 350g of boric acid are weighed and added into a reaction vessel, and the mixture is stirred and reacted for 13 hours at normal temperature to prepare a solution A.
(2) And filtering and washing the solution A, and drying the solution A in a vacuum drying oven at 50 ℃ for 7 hours to obtain magnesium hydroxide @ magnesium borate.
(3) Weighing 400g of magnesium hydroxide @ magnesium borate, 150g of hexadecylamine and 1.8kg of acetone, adding the mixture into a reaction vessel, stirring and reacting for 14h at normal temperature, washing, filtering, and drying in a vacuum drying oven for 9h at 60 ℃ to obtain the magnesium hydroxide @ magnesium borate @ hexadecylamine, namely the polyolefin flame-retardant filler P3.
Application example 3
And adding 20 parts of P3 into 80 parts of Polyethylene (PE), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PE composite material X3.
Comparative example 5
And (3) taking 80 parts of PE, stirring for 10min by using a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PE composite material D3.
Comparative example 6
And adding 20 parts of magnesium hydroxide into 80 parts of PE, stirring for 10min by using a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PE composite material N3.
The performance data of the PE composites prepared in application example 3 and comparative examples 5 and 6 are shown in the following table:
as can be seen from the table above, the flame retardant property and the mechanical property of X3 are superior to those of D3 and N3, which shows that the flame retardant property and the mechanical property of PE are better after the flame retardant filler is added.
Preparation example 4
(1) 580g of magnesium hydroxide, 1.28kg of acetone and 380g of boric acid are weighed and added into a reaction vessel, and the solution A is prepared after stirring and reacting for 13 hours at normal temperature.
(2) And filtering and washing the solution A, and drying the solution A in a vacuum drying oven at 45 ℃ for 7 hours to obtain magnesium hydroxide @ magnesium borate.
(3) 380g of magnesium hydroxide @ magnesium borate, 155g of hexadecylamine and 1.85kg of acetone are weighed and added into a reaction vessel, stirred and reacted for 13 hours at normal temperature, washed, filtered and dried for 9 hours in a vacuum drying oven at 55 ℃ to obtain the magnesium hydroxide @ magnesium borate @ hexadecylamine, namely the polyolefin flame-retardant filler P4.
Application example 4
And adding 20 parts of P4 into 80 parts of polyamide 6(PA6), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PA6 composite material X4.
Comparative example 7
80 parts of PA6 are taken and stirred for 10min by a high-speed mixer, and then added into a double-screw extruder for blending and extrusion to obtain the PA6 composite material D4.
Comparative example 8
Adding 20 parts of magnesium hydroxide into 80 parts of polyamide 6(PA6), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PA6 composite material N3.
The performance data for the PA6 composites prepared in application example 4 and comparative examples 7 and 8 are shown in the following table:
as can be seen from the table above, the flame retardant property and the mechanical property of X4 are superior to those of D4 and N4, which shows that the flame retardant property and the mechanical property of PA6 are better after the flame retardant filler is added.
Preparation example 5
(1) 515g of magnesium hydroxide, 1.35kg of acetone and 380g of boric acid are weighed and added into a reaction vessel, and stirred and reacted for 13 hours at normal temperature to prepare a solution A.
(2) And filtering and washing the solution A, and drying the solution A in a vacuum drying oven at 55 ℃ for 7 hours to obtain magnesium hydroxide @ magnesium borate.
(3) 380g of magnesium hydroxide @ magnesium borate, 145g of hexadecylamine and 1.75kg of acetone are weighed and added into a reaction vessel, stirred and reacted for 16h at normal temperature, washed, filtered and dried in a vacuum drying oven for 8h at 55 ℃ to obtain the magnesium hydroxide @ magnesium borate @ hexadecylamine, namely the polyolefin flame-retardant filler P5.
Application example 5
And adding 20 parts of P5 into 80 Parts of Styrene (PS), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PS composite material X5.
Comparative example 9
And (3) taking 80 parts of PS, stirring for 10min by using a high-speed mixer, and then adding the PS into a double-screw extruder for blending and extruding to obtain the PS composite material D5.
Comparative example 10
And adding 20 parts of magnesium hydroxide into 80 Parts of Styrene (PS), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PS composite material N5.
The performance data of the PS composite materials prepared in the above application example 5, comparative example 9 and comparative example 10 are shown in the following table:
as can be seen from the table above, the flame retardant property and the mechanical property of X5 are superior to those of D5 and N5, which shows that the flame retardant property and the mechanical property of PS are better after the flame retardant filler is added.
The application describes a polyolefin flame-retardant filler and a preparation method thereof, and the polyolefin material prepared by the polyolefin flame-retardant filler has a very important significance in improving the flame-retardant property to a certain extent.
The above disclosure is only for the purpose of describing several embodiments of the present application, but the present application is not limited thereto, and any variations that can be considered by those skilled in the art are intended to fall within the scope of the present application.
Claims (7)
1. The polyolefin flame-retardant filler is characterized by comprising magnesium hydroxide, magnesium borate and hexadecylamine.
2. The polyolefin flame retardant filler according to claim 1, characterized in that the mass ratio of magnesium hydroxide @ magnesium borate to hexadecylamine is (30-50): (14-16).
3. A process for the preparation of a polyolefin flame retardant filler according to any of the preceding claims 1 or 2, characterized in that it comprises the following steps:
s1, weighing magnesium hydroxide, acetone and boric acid according to a set amount, adding into a reaction vessel, stirring and reacting for 10-16h at normal temperature to prepare a solution A;
s2, filtering and washing the solution A, and drying the solution A in a vacuum drying oven at the temperature of 40-60 ℃ for 6-8h to obtain magnesium hydroxide @ magnesium borate;
s3, weighing the magnesium hydroxide @ magnesium borate, hexadecylamine and acetone according to the set amount, adding the weighed materials into a reaction vessel, stirring and reacting for 10-18h at normal temperature, washing, filtering, and drying in a vacuum drying oven for 8-10h at 50-70 ℃ to obtain the magnesium hydroxide @ magnesium borate @ hexadecylamine, namely the polyolefin flame-retardant filler.
4. The method for preparing polyolefin flame-retardant filler according to claim 3, wherein the mass ratio of magnesium hydroxide, acetone and boric acid in step S1 is (50-60): (120-160): (30-40).
5. The method for preparing a polyolefin flame retardant filler according to claim 3, wherein the mass ratio of magnesium hydroxide @ magnesium borate, hexadecylamine and acetone in step S3 is (30-50): (14-16): (160-200).
6. Use of a polyolefin flame retardant filler, characterized in that a polyolefin flame retardant filler according to any of the preceding claims 1 or 2 is used in a polyolefin composite.
7. Use of a polyolefin flame retardant filler according to claim 6, wherein the polyolefin is one of polyethylene, polypropylene, polystyrene, polybutylene terephthalate, polyamide 6.
Priority Applications (1)
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| CN102702678A (en) * | 2012-05-25 | 2012-10-03 | 厦门大学 | Halogen-free flame retardant toughened epoxy resin based composite material and preparation method thereof |
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