CN113698633A - Flame-retardant master batch composition with improved fluidity and preparation method thereof - Google Patents
Flame-retardant master batch composition with improved fluidity and preparation method thereof Download PDFInfo
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- CN113698633A CN113698633A CN202110935553.6A CN202110935553A CN113698633A CN 113698633 A CN113698633 A CN 113698633A CN 202110935553 A CN202110935553 A CN 202110935553A CN 113698633 A CN113698633 A CN 113698633A
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- retardant
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- flame retardant
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 64
- 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 63
- 239000000203 mixture Substances 0.000 title claims abstract description 33
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000003381 stabilizer Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 239000003607 modifier Substances 0.000 claims abstract description 12
- 230000004048 modification Effects 0.000 claims abstract description 10
- 238000012986 modification Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 9
- 239000000155 melt Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 5
- -1 polypropylene Polymers 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 18
- 238000012360 testing method Methods 0.000 claims description 14
- 239000004698 Polyethylene Substances 0.000 claims description 13
- 229920000573 polyethylene Polymers 0.000 claims description 13
- 239000003963 antioxidant agent Substances 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- 229920000642 polymer Polymers 0.000 claims description 11
- 239000004743 Polypropylene Substances 0.000 claims description 10
- 229920001155 polypropylene Polymers 0.000 claims description 10
- CGPRUXZTHGTMKW-UHFFFAOYSA-N ethene;ethyl prop-2-enoate Chemical compound C=C.CCOC(=O)C=C CGPRUXZTHGTMKW-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical group O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 7
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 229920001577 copolymer Polymers 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- QHZOMAXECYYXGP-UHFFFAOYSA-N ethene;prop-2-enoic acid Chemical compound C=C.OC(=O)C=C QHZOMAXECYYXGP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 239000012796 inorganic flame retardant Substances 0.000 claims description 2
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 2
- 238000007385 chemical modification Methods 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 13
- 230000003078 antioxidant effect Effects 0.000 description 10
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000009775 high-speed stirring Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- BZQKBFHEWDPQHD-UHFFFAOYSA-N 1,2,3,4,5-pentabromo-6-[2-(2,3,4,5,6-pentabromophenyl)ethyl]benzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1CCC1=C(Br)C(Br)=C(Br)C(Br)=C1Br BZQKBFHEWDPQHD-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- MWFNQNPDUTULBC-UHFFFAOYSA-N phosphono dihydrogen phosphate;piperazine Chemical compound C1CNCCN1.OP(O)(=O)OP(O)(O)=O MWFNQNPDUTULBC-UHFFFAOYSA-N 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000009467 reduction Effects 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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
-
- 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
- C08K3/02—Elements
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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
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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
- C08K3/2279—Oxides; Hydroxides of metals of antimony
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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
- C08K5/00—Use of organic ingredients
- C08K5/02—Halogenated hydrocarbons
- C08K5/03—Halogenated hydrocarbons aromatic, e.g. C6H5-CH2-Cl
-
- 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
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
- C08K5/3462—Six-membered rings
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- 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
- C08K5/34928—Salts
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- 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
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention relates to a flame-retardant functional master batch composition with improved fluidity, which comprises the following components, by mass, 10-15 parts of a carrier, 0.5-1 part of a stabilizer, 3-5 parts of a flow promoter, 0.5-1.5 parts of a graft modifier, 1-3 parts of a dispersing agent and 75-80 parts of a flame retardant. Firstly, modifying the fluidity of carrier components in a reaction kettle by adopting a chemical modification process; secondly, completing the premixing treatment of the flame retardant composition in a high-speed mixer; then completing the chemical grafting modification of the melt in the screw cylinder; the flame-retardant master batch with high fluidity is prepared by melting, granulating and molding. The invention obviously improves the flowing property and the dispersing property of the master batch composition with the flame-retardant function.
Description
Technical Field
The invention relates to the field of high-molecular polymer flame-retardant functional master batches and preparation thereof, in particular to a flame-retardant functional master batch composition for improving fluidity and a preparation method thereof.
Background
At present, the technical research of preparing the flame retardant powder into the high-concentration flame-retardant master batch is widely carried out. The problem of dust pollution of the flame retardant is solved by carrying out master granulation on the flame retardant, and the problems that the powder is difficult to disperse uniformly when used and has great influence on the mechanical property of a product are solved. The flame retardant improves the product stability and the production efficiency after the master batch granulation, so that the improvement of the material performance through the flame retardant master batch technology becomes necessary and trend for the development of the industry.
In the preparation technology of the flame retardant functional master batch, common-grade flame retardant master batches can be converted into high-performance valuable products through the technologies of surface particle size optimization, coating modification, nano synergism, content concentration increase and the like of powder materials. In the published patent and literature, there are many technical researches on preparing functional master batches of flame retardants, and among them, there are no researches on preparing high concentration products with concentration of more than 80%, and the addition of a large proportion of powdered flame retardants inevitably results in reduced fluidity, and even if the compatibility of the carrier and the flame retardants can be improved by coating treatment with a flame retardant coupling agent and the use of a compatibilizer carrier, the fluidity of the composition is not improved fundamentally, and especially the flame retardant master batches with content of more than 80% are at the cost of reduced fluidity. The master batch of the high-concentration flame retardant has low fluidity, large fluctuation of extrusion current, poor process stability, easy blockage of a machine head and poor product uniformity, and is a general technical problem in the industry.
Conventionally, the flow index of commercial products of polypropylene, polyethylene, EVA and POE as flame retardant carrier materials is generally lower than 30g/10min, and many documents report the flow modification technology of carrier polymers, such as high-melt-index melt-blown polypropylene materials and the like, but the technology is limited to improving the material flow and cannot give consideration to flow, carrying capacity, coating performance and toughness. The functional master batch of the flame retardant prepared by the currently disclosed technical achievements has low melt flowability, so that the using effect and the range are reduced and limited.
Disclosure of Invention
The invention aims to remarkably improve the reduction of the fluidity in the preparation of the master batch composition with the flame-retardant function and show good fluidity, compatibility and processability.
The technical scheme of the invention is as follows:
the technology completes the preparation process through three reactors. Firstly, modifying the fluidity of carrier components in a reaction kettle by a chemical modification process; secondly, completing the premixing treatment of the flame retardant through a high-speed mixer; then the chemical grafting modification of the melt is completed in a screw cylinder of a double-screw extruder. The fluidity of the master batch composition with the flame-retardant function is remarkably improved through the interaction of the high-flow modification of the carrier components in the kettle and the chemical grafting modification process of the screw cylinder, and the melt index of the product prepared by the technology is not lower than 30g/10min (190 ℃, 2.16kg load).
A flame-retardant master batch composition with improved fluidity comprises the following components, by mass, 10-15 parts of a carrier, 0.5-1 part of a stabilizer, 3-5 parts of a flow promoter, 0.5-1.5 parts of a graft modifier, 1-3 parts of a dispersing agent and 75-80 parts of a flame retardant;
preferably, the carrier comprises one or a mixture of two or more of polypropylene, polyethylene, ethylene/vinyl acetate copolymer and ethylene/octene copolymer;
the flow melt index of the carrier is not higher than 30g/10min, and the test standard is 190 ℃ and 2.16kg load;
preferably, the stabilizer is one or a compound of two or more of phosphite antioxidants;
preferably, the flow promoter is selected from at least one of ethylene/acrylic acid AC polymer, ethylene/ethyl acrylate EEA polymer, and ethylene/methyl acrylate EMA polymer;
preferably, the graft modifier is maleic anhydride;
the dispersing agent is one or two of polyethylene wax and N, N' -ethylene bis stearamide;
preferably, the flame retardant comprises a halogen flame retardant, a phosphorus-nitrogen flame retardant and an inorganic flame retardant composition, and the flame retardant accounts for not less than 75% of the mass ratio of the functional master batch;
a preparation method of a flame-retardant master batch composition with improved fluidity comprises the following steps:
(1) weighing the required components according to a preset proportion;
(2) putting the carrier component and the stabilizer component with the mass percentage of 50 percent weighed in the step (1) into a reactor in a reaction kettle, and heating and mixing for 20-25 minutes at the heating temperature of 165-215 ℃;
(3) adding the flow promoter component into the reaction kettle in the step (2), continuously stirring for 5-10 minutes at the temperature of 165-215 ℃ to obtain a fluidity modified carrier, and injecting the fluidity modified carrier component into a double-screw extruder from the middle part of a screw according to the composition proportion through a melt metering pump;
(4) putting the flame retardant component, the rest stabilizer component, the grafting modifier component and the dispersant component weighed in the step (1) into a high-speed mixer reactor to mix for 20-30 minutes; feeding the product obtained in the step from the root of the screw to a double-screw extruder according to the component proportion by a metering scale, and extruding;
preferably, the step (4) is to complete the chemical grafting modification process in a screw reactor; the flame-retardant master batch composition with the improved fluidity is prepared by plasticizing and processing equipment of a parallel double-screw extruder at the extrusion temperature of 165-215 ℃ and adopting a grinding surface air-cooling granulation forming mode.
The invention has the beneficial effects that:
1. the technology obviously improves the fluidity of the master batch composition with the flame-retardant function, the melt index of the obtained product is not lower than 30g/10min (190 ℃, 2.16kg load), and the product has high fluidity, thereby improving the compatibility and the processability;
2. the technology can give consideration to melt fluidity and the functions of containing, coating, infiltrating and toughening, improves impact toughness and dispersibility, can obviously reduce the processing difficulty of the flame-retardant master batch composition, particularly reduces the head pressure of an extruder, solves the problem of unstable current of a host, increases the stability of product preparation, and improves yield;
3. the three reactors of the reaction kettle, the high-speed mixer and the screw cylinder of the extruder are utilized to finish the process preparation, and the method has the characteristics of good process step superposition effect, stable modification technology process, good controllability and repeatability, and suitability for large-scale production.
Detailed Description
Example 1
(1) Weighing 10kg of carrier component polypropylene (model 7726H, melt index of 26g/10 min), 5kg of polyethylene (model LDPE608, melt index of 6g/10 min) and 0.5kg of stabilizer (model B215 antioxidant) into a reaction kettle, starting stirring at 165 ℃ for 25 minutes. 5kg of flow promoter (type EEA7500, type EMA1125 each 2.5 kg) were then added and stirring continued for 10 minutes. Modified support 1# was obtained. Feeding the No. 1 carrier component into a double-screw extruder from the root of a screw according to the composition proportion by a metering pump;
(2) weighing 60kg of fire retardant decabromodiphenylethane and 20kg of fire retardant antimony trioxide, putting the fire retardant antimony trioxide into a high-speed mixer, starting high-speed stirring, setting the temperature at 120 ℃, and keeping the time for 20 minutes; then adding 1.5kg of maleic anhydride as a grafting modifier, 0.5kg of a stabilizer (antioxidant with the model of B215) and 2kg of a dispersing agent (polyethylene wax); stirring is continuously kept for 10 minutes to prepare a flame retardant No. 1 of the test example. The twin-screw extruder was fed from the screw root through a side feed by a scale.
(3) By an aspect ratio of 40: 1, plasticizing and granulating by a double screw extruder with a screw diameter of 72mm, wherein the temperature of each zone is set to 165 ℃, 190 ℃, 200 ℃, 190 ℃, 180 ℃, 170 ℃ and 170 ℃, and grinding surface air cooling and granulating are adopted to prepare test example No. 1.
Example 2
(1) Weighing 6kg of carrier component polypropylene (model 7726H, melt index of 26g/10 min), 4kg of polyethylene (model LDPE608, melt index of 6g/10 min) and 0.5kg of stabilizer (model B215 antioxidant) into a reaction kettle, starting stirring at 165 ℃ for 20 minutes. 5kg of flow promoter (type EEA7500, type EMA1125 each 2.5 kg) were then added and stirring continued for 10 minutes. Modified support 2# was obtained. Feeding the No. 1 carrier component into a double-screw extruder from the root of a screw according to the composition proportion by a metering pump;
(2) weighing 60kg of fire retardant decabromodiphenylethane and 20kg of fire retardant antimony trioxide, putting the fire retardant antimony trioxide into a high-speed mixer, starting high-speed stirring, setting the temperature at 120 ℃, and keeping the time for 20 minutes; then adding 1 kg of maleic anhydride as a grafting modifier, 0.5kg of a stabilizer (an antioxidant with the model of B215) and 3kg of a dispersing agent (polyethylene wax); stirring is continuously kept for 10 minutes to prepare a flame retardant No. 2 of the test example. The twin-screw extruder was fed from the screw root through a side feed by a scale.
(3) By an aspect ratio of 40: 1, plasticizing and granulating by a double screw extruder with a screw diameter of 72mm, wherein the temperature of each zone is set to 155 ℃, 190 ℃, 200 ℃, 190 ℃, 180 ℃, 170 ℃ and 170 ℃, and grinding and air cooling granulation are adopted to prepare test example No. 2.
Example 3
(1) Weighing 10kg of carrier component polypropylene (model 7726H, melt index of 26g/10 min), 5kg of polyethylene (model LDPE608, melt index of 6g/10 min) and 0.5kg of stabilizer (model B215 antioxidant) into a reaction kettle, starting stirring at 165 ℃ for 25 minutes. 5kg of flow promoter (type EEA7500, type EMA1125 each 2.5 kg) were then added and stirring continued for 10 minutes. Modified support No. 3 example was obtained. Feeding 3# carrier components into a double-screw extruder from the root of a screw according to a formula proportion by a metering pump;
(2) weighing 74kg of flame retardant magnesium hydroxide flame retardant (with the particle size D900.3um) and 6kg of polysiloxane synergistic flame retardant, putting into a high-speed mixer, starting high-speed stirring, setting the temperature at 120 ℃, and keeping the time for 20 minutes; then adding 1.5kg of maleic anhydride as a grafting modifier, 0.5kg of a stabilizer (antioxidant with the model of B215) and 2kg of a dispersing agent (polyethylene wax); stirring is continuously kept for 10 minutes to prepare a flame retardant No. 3 of the test example. The twin-screw extruder was fed from the screw root through a side feed by a scale.
(3) By an aspect ratio of 40: 1, plasticizing and granulating by a double screw extruder with a screw diameter of 72mm, wherein the temperature of each zone is set to 155 ℃, 190 ℃, 200 ℃, 190 ℃, 180 ℃, 170 ℃ and 170 ℃, and grinding and air cooling granulation are adopted to prepare test example No. 3.
Example 4
(1) Weighing 10kg of carrier component polypropylene (model 7726H, melt index of 26g/10 min), 5kg of polyethylene (model LDPE608, melt index of 6g/10 min) and 0.5kg of stabilizer (model B215 antioxidant) into a reaction kettle, starting stirring at 165 ℃ for 20 minutes. 5kg of flow promoter (type EEA7500, type EMA1125 each 2.5 kg) were then added and stirring continued for 10 minutes. Modified support No. 4 was obtained. Feeding the 4# carrier component into a double-screw extruder from the root of the screw according to the composition proportion by a metering pump;
(2) weighing 45kg of flame retardant microencapsulated red phosphorus flame retardant (with the particle size D90 of 3 um) and 30kg of magnesium hydroxide synergistic flame retardant, putting the materials into a high-speed mixer, starting low-speed stirring, setting the temperature at 100 ℃ and keeping the time for 20 minutes; then adding 1.2kg of maleic anhydride as a grafting modifier, 0.5kg of a stabilizer (antioxidant with the type B215) and 3kg of a dispersing agent (polyethylene wax); stirring is continuously kept for 10 minutes to prepare a flame retardant No. 4 of the test example. The twin-screw extruder was fed from the screw root through a side feed by a scale.
(3) By an aspect ratio of 40: 1, plasticizing and granulating by a double screw extruder with a screw diameter of 72mm, wherein the temperature of each zone is set to 155 ℃, 190 ℃, 200 ℃, 190 ℃, 180 ℃, 170 ℃ and 170 ℃, and grinding surface air cooling and granulating are adopted to prepare test example No. 4.
Example 5
(1) Weighing 10kg of carrier component polypropylene (model 7726H, melt index of 26g/10 min), 5kg of ethylene vinyl acetate (model VA28, melt index of 3g/10 min) and 0.5kg of stabilizer (model B215 antioxidant) into a reaction kettle, starting stirring at 165 ℃ for 25 minutes. 5kg of flow promoter (type EEA7500, type EMA1125 each 2.5 kg) were then added and stirring continued for 10 minutes. Modified support No. 5 was obtained. Feeding the 5# carrier component into a double-screw extruder from the root of a screw according to the formula proportion by a metering pump;
(2) weighing 65kg of flame retardant piperazine pyrophosphate and 15kg of melamine cyanurate, putting into a high-speed mixer, starting high-speed stirring, setting the temperature at 120 ℃, and keeping the time for 20 minutes; then adding 1.5kg of maleic anhydride as a grafting modifier, 0.5kg of a stabilizer (antioxidant with the model of B215) and 2kg of a dispersing agent (polyethylene wax); stirring is continued for 10 minutes to prepare a flame retardant No. 5 of the test example. The twin-screw extruder was fed from the screw root through a side feed by a scale.
(3) By an aspect ratio of 40: 1, plasticizing and granulating by a double screw extruder with a screw diameter of 72mm, wherein the temperature of each zone is set to 155 ℃, 190 ℃, 200 ℃, 190 ℃, 180 ℃, 170 ℃ and 170 ℃, and grinding surface air cooling and granulating are adopted to prepare test example No. 5.
The test parameters of the above examples are shown in table 1.
Table 1
Comparative example
(1) Comparative examples were prepared as described in examples 1-5;
(2) the same as the technology is that: in the comparative example, 10-15 parts of carrier components, 0.5-1 part of stabilizing agent, 1-3 parts of dispersing agent and 75-80 parts of flame retardant which are consistent with the embodiment are reserved; except that the flow promoter component is removed; further, the process for preparing the modified carrier in the reactor of the reaction kettle is removed to prove the importance of the modified carrier;
(3) mixing by a high-speed mixer, grafting by a double-screw extruder, and granulating, wherein the process and parameters are the same as those in the embodiment;
(4) comparative examples 1-5 were formed and the results after testing are shown in table 2.
Selection of flow promoters
The accelerator is at least one selected from ethylene/acrylic Acid (AC) polymer, ethylene/ethyl acrylate (EEA) polymer and ethylene/methyl acrylate (EMA) polymer, and the melt strength, the impact toughness and the carrying capacity of the carrier mixture are not reduced on the premise of ensuring that the melt flowability is remarkably improved. EEA and EMA are typically used as blending components for polyethylene and polypropylene to improve impact strength and toughness and to enhance flowability. The flow promoter of the technology is selected according to the principle that the model with high melt fluidity of 50g/10min and elongation at break of more than 500 percent is selected. The method of flow promoters selected for use in the present technology is illustrated by a comparison of the following two sets of data.
The first set of data is the common model EEA and EMA.
The second set of data is the EEA and EMA selected by the present technique.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The master batch composition with the flame-retardant function is characterized by comprising, by mass, 10-15 parts of a carrier, 0.5-1 part of a stabilizer, 3-5 parts of a flow promoter, 0.5-1.5 parts of a graft modifier, 1-3 parts of a dispersing agent and 75-80 parts of a flame retardant.
2. The master batch composition with the function of improving the flowability and the flame retardance of claim 1, wherein the carrier comprises one or a mixture of two or more of polypropylene, polyethylene, ethylene/vinyl acetate copolymer and ethylene/octene copolymer;
the carrier flow melt index is not higher than 30g/10min, and the test standard is 190 ℃ and 2.16kg load.
3. The master batch composition with the flame-retardant function and the improved flowability of the claim 1, wherein the stabilizer is one or a compound of two or more of phosphite antioxidants.
4. The flame retardant functional masterbatch composition with improved flow property according to claim 1, wherein said flow promoter is at least one selected from the group consisting of ethylene/acrylic Acid (AC) polymer, ethylene/ethyl acrylate (EEA) polymer and ethylene/methyl acrylate (EMA) polymer.
5. The master batch composition with the flame retardant function and the improved fluidity of claim 1, wherein the grafting modifier is maleic anhydride;
the dispersing agent is one or two of polyethylene wax and N, N' -ethylene bis stearamide.
6. The master batch composition with the flame-retardant function and the improved flowability of the claim 1, which is characterized in that:
the flame retardant comprises a halogen flame retardant, a phosphorus-nitrogen flame retardant and an inorganic flame retardant composition, and the mass ratio of the flame retardant to the functional master batch is not less than 75%.
7. A preparation method of a flame-retardant master batch composition with improved fluidity is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing the required components according to a preset proportion;
(2) putting the carrier component and the stabilizer component with the mass percentage of 50 percent weighed in the step (1) into a reactor in a reaction kettle, and heating and mixing for 20-25 minutes at the heating temperature of 165-215 ℃;
(3) adding the flow promoter component into the reaction kettle in the step (2), continuously stirring for 5-10 minutes at the temperature of 165-215 ℃ to obtain a fluidity modified carrier, and injecting the fluidity modified carrier component into a double-screw extruder from the middle part of a screw according to the composition proportion through a melt metering pump;
(4) putting the flame retardant component, the rest stabilizer component, the grafting modifier component and the dispersant component weighed in the step (1) into a high-speed mixer reactor to mix for 20-30 minutes; the product obtained in the step is extruded from the root of the screw to a double-screw extruder according to the component proportion by a metering scale.
8. The preparation method of the flame-retardant functional master batch composition with improved fluidity according to claim 7, wherein the preparation method comprises the following steps: step (4) completing a chemical grafting modification process in a screw reactor; the flame-retardant master batch composition with the improved fluidity is prepared by plasticizing and processing equipment of a parallel double-screw extruder at the extrusion temperature of 165-215 ℃ and adopting a grinding surface air-cooling granulation forming mode.
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| CN103849056A (en) * | 2012-12-04 | 2014-06-11 | 青岛三利中德美水设备有限公司 | PE (polyethylene) flame retardant modified antistatic toughening masterbatch and preparation method thereof |
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| CN108102237A (en) * | 2017-12-14 | 2018-06-01 | 江苏万纳普新材料科技有限公司 | A kind of heat-proof combustion-resistant master batch and its manufacturing method |
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