CN111574773A - Flame-retardant master batch and preparation method thereof - Google Patents

Flame-retardant master batch and preparation method thereof Download PDF

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CN111574773A
CN111574773A CN202010538951.XA CN202010538951A CN111574773A CN 111574773 A CN111574773 A CN 111574773A CN 202010538951 A CN202010538951 A CN 202010538951A CN 111574773 A CN111574773 A CN 111574773A
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flame
retardant
parts
master batch
microcapsule
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陈鸿景
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Xiamen Yixingxing Plastic Raw Material Co ltd
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Xiamen Yixingxing Plastic Raw Material Co ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • B01J13/043—Drying and spraying
    • 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
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/06—Polyethene
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    • 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
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/10—Homopolymers or copolymers of propene
    • C08J2323/12—Polypropene
    • 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
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/16—Cyclodextrin; Derivatives thereof
    • 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
    • C08J2425/00—Characterised by the use 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; Derivatives of such polymers
    • C08J2425/02—Homopolymers or copolymers of hydrocarbons
    • C08J2425/04—Homopolymers or copolymers of styrene
    • C08J2425/06—Polystyrene
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2425/00—Characterised by the use 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; Derivatives of such polymers
    • C08J2425/18—Homopolymers or copolymers of aromatic monomers containing elements other than carbon and hydrogen
    • 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
    • C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • 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
    • C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
    • 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
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • 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
    • 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
    • C08K3/24—Acids; Salts thereof
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • 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
    • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477—Six-membered rings
    • C08K5/3492—Triazines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients

Abstract

The invention discloses a flame-retardant master batch and a preparation method thereof, and relates to a flame-retardant material. The technical key points of the method are that the method comprises the following components in parts by weight: 100 portions and 120 portions of carrier; 60-130 parts of halogen flame retardant; 150 portions of microcapsule flame-retardant synergist and 300 portions of microcapsule flame-retardant synergist; 0.1-3 parts of antioxidant; 3-5 parts of a lubricant; the microcapsule flame-retardant synergist comprises a core material and a wall material, wherein the weight part ratio of the core material to the wall material is 1: (4-6); the core material is one or a mixture of antimony trioxide, antimony pentoxide and sodium antimonate, the durability of the flame-retardant master batch is improved, and the microcapsule flame-retardant synergist can be uniformly dispersed in the carrier in the production process, so that the flame-retardant effect of the flame-retardant master batch is improved.

Description

Flame-retardant master batch and preparation method thereof
Technical Field
The invention relates to a flame-retardant material, in particular to a flame-retardant master batch and a preparation method thereof.
Background
With the improvement of science and technology and the improvement of the living standard of people, the high polymer materials are particularly synthesized into high polymers: such as plastics, rubber, etc., are becoming more and more important in people's lives, and their applications are showing a tendency to increase year by year. However, most organic polymer materials have flammability characteristics of different degrees in air, and flame retardant modification of the organic polymer materials for application in various industries such as military, aerospace, transportation, electric power, civil use and the like is a new problem.
At present, the ideal method for modifying the flame retardance of plastics is to add products such as flame retardants or flame-retardant master batches to improve the fireproof performance of the plastics. Among them, antimony trioxide is one of important inorganic flame retardants, which has a small flame retardant effect when used alone, but when used together with a halogen flame retardant, the antimony trioxide can greatly improve the efficacy of the halogen flame retardant, and is an indispensable synergist for the halogen flame retardant.
The invention discloses a method for preparing high-content antimony oxide master batch in Chinese patent with publication number CN102585288B, mixing unmodified antimony oxide powder with an ethanol solution containing phosphate, dispersing at high speed by a dispersion machine, transferring into a reactor with a stirring and reflux device for surface modification, filtering and drying to obtain modified antimony oxide powder; and (3) directly feeding the modified antimony oxide powder and the carrier into a double-screw extruder for extrusion granulation and screening after high-speed mixing and dispersion to obtain the high-content antimony oxide master batch.
However, most of the phosphate esters in the above method are liquid, and the molecular weight is small, the volatility is high, and the heat resistance is low, so that the flame retardant effect and the flame retardant durability of the flame retardant master batch are easily affected.
Therefore, a new solution is needed to solve the above problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the flame-retardant master batch which has the advantages of improving the durability of the flame-retardant master batch, and enabling the microcapsule flame-retardant synergist to be uniformly dispersed in a carrier in the production process so as to achieve the purpose of improving the flame-retardant effect of the flame-retardant master batch.
The second purpose of the invention is to provide a preparation method of the flame-retardant master batch, which is used for preparing the flame-retardant master batch.
In order to achieve the first purpose, the invention provides the following technical scheme:
the flame-retardant master batch comprises the following components in parts by weight: 100 portions and 120 portions of carrier; 60-130 parts of halogen flame retardant; 150 portions of microcapsule flame-retardant synergist and 300 portions of microcapsule flame-retardant synergist; 0.1-3 parts of antioxidant; 3-5 parts of a lubricant; the microcapsule flame-retardant synergist comprises a core material and a wall material, wherein the weight part ratio of the core material to the wall material is 1: (4-6); the core material is one or a mixture of more of antimony trioxide, antimony pentoxide and sodium antimonate.
By adopting the technical scheme, the microcapsule flame-retardant synergist is prepared by embedding the core material in a micro-closed capsule formed by the wall material by using a microcapsule technology, so that the core material can be effectively separated from the surrounding environment, the adverse effect of the external environment on the core material is reduced or avoided, the purpose of protecting the core material can be achieved, and the durability of the flame-retardant performance of the flame-retardant master batch is prolonged. Meanwhile, the core material can be uniformly dispersed in the carrier by forming the capsule, when the fire catches fire, the wall material is broken due to the temperature rise, the core material is contacted with the halogen flame retardant, and the core material plays an auxiliary effect on the halogen flame retardant, so that the flame retardant effect of the product is improved.
More preferably, the wall material is beta-cyclodextrin.
By adopting the technical scheme, when the material is on fire, along with the continuous rise of the temperature, when the temperature reaches 265 ℃, the beta-cyclodextrin is heated and decomposed to generate carbon dioxide, so that the halogen flame retardant is contacted with the microcapsule flame-retardant synergist and reacts, and the product and the carbon dioxide form a gas film to cover the surface of the material, thereby playing a role in isolating the material from external oxygen and thermally contacting the material, and further achieving the flame-retardant effect.
More preferably, the beta-cyclodextrin is beta-cyclodextrin produced by Jiangsu Fengyuan biotechnology limited.
More preferably, the core material also comprises 10-20 parts of sodium bicarbonate.
By adopting the technical scheme, the sodium bicarbonate is added into the core material, and is heated and decomposed along with the continuous rise of the temperature to generate carbon dioxide, so that the pressure inside the capsule is continuously increased, the capsule cracking speed is accelerated, the contact time of the core material and the halogen flame retardant is shortened, and the flame retardant effect is achieved; meanwhile, the density of the carbon dioxide is larger than that of air, the carbon dioxide can cover the product, and the insulating material is in thermal contact with external oxygen, so that the flame-retardant effect is achieved.
More preferably, the sodium bicarbonate is sodium bicarbonate sold by commerce and trade company Limited, Cincisco, Fujian province.
More preferably, the carrier is polypropylene or polyethylene.
More preferably, the carrier is polypropylene.
By adopting the technical scheme, the carrier is polypropylene, and the polypropylene has higher melt index and better fluidity, so that the coating effect on the microcapsule flame-retardant synergist is better, and the microcapsule flame-retardant synergist can be prevented from falling off from the carrier during granulation.
More preferably, the polypropylene is a polypropylene produced by chemical Limited, Wande Hubei.
More preferably, the halogen-based flame retardant is one or a mixture of more of tris (tribromophenoxy) triazine, brominated epoxy resin, brominated polystyrene, polybrominated styrene and brominated polycarbonate.
More preferably, the halogen-based flame retardant is tris (tribromophenoxy) triazine.
More preferably, the antioxidant is one or more of antioxidant 168, antioxidant 1010 and antioxidant 1076.
By adopting the technical scheme, the stability of the flame-retardant master batch in the processing process and the using process can be improved by adding the antioxidant.
Further preferably, the lubricant is one or more of polyethylene wax, stearic acid and liquid paraffin.
In order to achieve the second purpose, the invention provides the following technical scheme: a preparation method of flame-retardant master batch comprises the following steps:
s1, preparing a microcapsule flame-retardant synergist;
s11, weighing the wall material and the core material in corresponding parts by weight, wherein the ratio of the core material to the wall material in parts by weight is 1: (4-6);
s12, dissolving the wall material in water, and uniformly stirring to form an embedding solution, wherein the weight part ratio of the wall material to the water is 1: (5-7);
s13, adding core materials in corresponding parts by weight into the embedding liquid, and uniformly stirring at 33-38 ℃ and 8000-;
s14, spraying, condensing and granulating the microcapsule flame-retardant synergist solution through a centrifugal spray tower to obtain the microcapsule flame-retardant synergist;
s2, drying the carrier in a corresponding weight part at 80-120 ℃ for 2-3h to obtain a dried carrier;
s3, uniformly mixing the antioxidant, the lubricant, the halogen flame retardant, the microcapsule flame retardant synergist and the dried carrier in parts by weight to obtain a primary mixture of the flame retardant master batch;
and S4, putting the obtained mixture into a double-screw extruder for extrusion granulation to obtain the flame-retardant master batch.
By adopting the technical scheme, the microcapsule flame-retardant synergist is firstly prepared, and the core material can be uniformly dispersed in the carrier through the microcapsule flame-retardant synergist, so that the influence on the flame-retardant effect of the flame-retardant master batch caused by nonuniform distribution of the core material is avoided.
In summary, compared with the prior art, the invention has the following beneficial effects:
(1) the microcapsule flame-retardant synergist is prepared by embedding a core material in a micro-closed capsule formed by a wall material by using a microcapsule technology, so that the core material can be effectively separated from the surrounding environment, the adverse effect of the external environment on the core material is reduced or avoided, the purpose of protecting the core material can be achieved, and the durability of the flame-retardant performance of the flame-retardant master batch is prolonged;
(2) the core material can be uniformly dispersed in the carrier by forming the capsule, when the fire catches fire, the wall material is broken due to the temperature rise, the core material is contacted with the halogen flame retardant, and the core material has an auxiliary effect on the halogen flame retardant, so that the flame retardant effect of the product is improved;
(3) sodium bicarbonate is added into the core material, and is heated and decomposed along with the continuous rise of the temperature to generate carbon dioxide, so that the pressure inside the capsule is continuously increased, the capsule cracking speed is accelerated, the contact time of the core material and the halogen flame retardant is shortened, and the flame retardant effect is achieved; meanwhile, the density of the carbon dioxide is larger than that of air, the carbon dioxide can cover the product, and the insulating material is in thermal contact with external oxygen, so that the flame-retardant effect is achieved.
Detailed Description
The present invention will be described in detail with reference to the following examples.
The following examples and comparative examples were made from the following raw materials:
the polypropylene is produced by chemical industry limited company Wande Hubei;
the polyethylene is produced by Hubei Nuo Ke technology, Inc.;
the beta-cyclodextrin is produced by Jiangsu Fengyuan biotechnology limited company;
the sodium bicarbonate is sold by commerce and trade company Limited of Jinheng, Fujian province.
Example 1: a preparation method of flame-retardant master batch comprises the following steps:
s1, preparing a microcapsule flame-retardant synergist;
s11, weighing beta-cyclodextrin and antimony trioxide, wherein the weight part ratio of the antimony trioxide to the beta-cyclodextrin is 1: 4;
s12, dissolving beta-cyclodextrin in water, and uniformly stirring to form an embedding solution, wherein the weight part ratio of the beta-cyclodextrin to the water is 1: 5;
s13, adding antimony trioxide into the embedding liquid, and uniformly stirring at 33 ℃ and 10000r/min to obtain a microcapsule flame-retardant synergist solution;
s14, spraying, condensing and granulating the microcapsule flame-retardant synergist solution through a centrifugal spray tower to obtain the microcapsule flame-retardant synergist;
s2, drying 100 parts of polypropylene at 80 ℃ for 3 hours to obtain dried polypropylene;
s3, uniformly mixing 0.1 part of antioxidant 168, 3 parts of polyethylene wax, 60 parts of tris (tribromophenoxy) triazine, 150 parts of microcapsule flame-retardant synergist and dried polypropylene to obtain a primary mixture of flame-retardant master batches;
and S4, putting the obtained mixture into a double-screw extruder for extrusion granulation to obtain the flame-retardant master batch.
Example 2: a preparation method of flame-retardant master batch comprises the following steps:
s1, preparing a microcapsule flame-retardant synergist;
s11, weighing beta-cyclodextrin and antimony trioxide, wherein the weight part ratio of the antimony trioxide to the beta-cyclodextrin is 1: 5;
s12, dissolving beta-cyclodextrin in water, and uniformly stirring to form an embedding solution, wherein the weight part ratio of the beta-cyclodextrin to the water is 1: 6;
s13, adding antimony trioxide into the embedding liquid, and uniformly stirring at 33 ℃ and 10000r/min to obtain a microcapsule flame-retardant synergist solution;
s14, spraying, condensing and granulating the microcapsule flame-retardant synergist solution through a centrifugal spray tower to obtain the microcapsule flame-retardant synergist;
s2, drying 110 parts of polypropylene at 80 ℃ for 3h to obtain dried polypropylene;
s3, uniformly mixing 1.5 parts of antioxidant 168, 4 parts of polyethylene wax, 95 parts of tris (tribromophenoxy) triazine, 225 parts of microcapsule flame-retardant synergist and dried polypropylene to obtain a primary mixture of flame-retardant master batches;
and S4, putting the obtained mixture into a double-screw extruder for extrusion granulation to obtain the flame-retardant master batch.
Example 3: a preparation method of flame-retardant master batch comprises the following steps:
s1, preparing a microcapsule flame-retardant synergist;
s11, weighing beta-cyclodextrin and antimony trioxide, wherein the weight part ratio of the antimony trioxide to the beta-cyclodextrin is 1: 6;
s12, dissolving beta-cyclodextrin in water, and uniformly stirring to form an embedding solution, wherein the weight part ratio of the beta-cyclodextrin to the water is 1: 7;
s13, adding antimony trioxide into the embedding liquid, and uniformly stirring at 33 ℃ and 10000r/min to obtain a microcapsule flame-retardant synergist solution;
s14, spraying, condensing and granulating the microcapsule flame-retardant synergist solution through a centrifugal spray tower to obtain the microcapsule flame-retardant synergist;
s2, drying 120 parts of polypropylene at 80 ℃ for 3 hours to obtain dried polypropylene;
s3, uniformly mixing 3 parts of antioxidant 168, 5 parts of polyethylene wax, 130 parts of tris (tribromophenoxy) triazine, 300 parts of microcapsule flame-retardant synergist and dried polypropylene to obtain a primary mixture of flame-retardant master batches;
and S4, putting the obtained mixture into a double-screw extruder for extrusion granulation to obtain the flame-retardant master batch.
Example 4: a preparation method of flame-retardant master batch comprises the following steps:
s1, preparing a microcapsule flame-retardant synergist;
s11, weighing beta-cyclodextrin and antimony trioxide, wherein the weight part ratio of the antimony trioxide to the beta-cyclodextrin is 1: 6;
s12, dissolving beta-cyclodextrin in water, and uniformly stirring to form an embedding solution, wherein the weight part ratio of the beta-cyclodextrin to the water is 1: 7;
s13, adding antimony trioxide into the embedding liquid, and uniformly stirring at 35 ℃ and 9000r/min to obtain a microcapsule flame-retardant synergist solution;
s14, spraying, condensing and granulating the microcapsule flame-retardant synergist solution through a centrifugal spray tower to obtain the microcapsule flame-retardant synergist;
s2, drying 120 parts of polypropylene at 100 ℃ for 2.5 hours to obtain dried polypropylene;
s3, uniformly mixing 3 parts of antioxidant 168, 5 parts of polyethylene wax, 130 parts of tris (tribromophenoxy) triazine, 300 parts of microcapsule flame-retardant synergist and dried polypropylene to obtain a primary mixture of flame-retardant master batches;
and S4, putting the obtained mixture into a double-screw extruder for extrusion granulation to obtain the flame-retardant master batch.
Example 5: a preparation method of flame-retardant master batch comprises the following steps:
s1, preparing a microcapsule flame-retardant synergist;
s11, weighing beta-cyclodextrin and antimony trioxide, wherein the weight part ratio of the antimony trioxide to the beta-cyclodextrin is 1: 6;
s12, dissolving beta-cyclodextrin in water, and uniformly stirring to form an embedding solution, wherein the weight part ratio of the beta-cyclodextrin to the water is 1: 7;
s13, adding antimony trioxide into the embedding liquid, and uniformly stirring at 38 ℃ and 8000r/min to obtain a microcapsule flame-retardant synergist solution;
s14, spraying, condensing and granulating the microcapsule flame-retardant synergist solution through a centrifugal spray tower to obtain the microcapsule flame-retardant synergist;
s2, drying 120 parts of polypropylene at 120 ℃ for 2h to obtain dried polypropylene;
s3, uniformly mixing 3 parts of antioxidant 168, 5 parts of polyethylene wax, 130 parts of tris (tribromophenoxy) triazine, 300 parts of microcapsule flame-retardant synergist and dried polypropylene to obtain a primary mixture of flame-retardant master batches;
and S4, putting the obtained mixture into a double-screw extruder for extrusion granulation to obtain the flame-retardant master batch.
Example 6: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
in step S13, 10 parts of sodium bicarbonate was also added.
Example 7: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
in step S13, 15 parts of sodium bicarbonate was also added.
Example 8: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
in step S13, 20 parts of sodium bicarbonate was also added.
Example 9: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
polypropylene was replaced by equal parts by weight of polyethylene.
Example 10: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
replacing antimony trioxide with antimony pentoxide in equal parts by weight.
Example 11: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
replacing antimony trioxide by sodium antimonate with equal parts by weight.
Example 12: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
replacing antimony trioxide with a mixture of equal parts by weight of antimony trioxide and antimony pentoxide, wherein the weight ratio of the antimony trioxide to the antimony pentoxide is 1: 1.
Example 13: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
replacing antimony trioxide with a mixture of antimony trioxide and sodium antimonate in equal parts by weight, wherein the weight ratio of the antimony trioxide to the sodium antimonate is 1: 1.
Example 14: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
replacing antimony trioxide with a mixture of sodium antimonate and antimony pentoxide in equal parts by weight, wherein the weight ratio of the sodium antimonate to the antimony pentoxide is 1: 1.
Example 15: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
the tris (tribromophenoxy) triazine is replaced by brominated epoxy resin with equal parts by weight.
Example 16: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
the tris (tribromophenoxy) triazine is replaced by brominated polystyrene with equal parts by weight.
Example 17: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
the tris (tribromophenoxy) triazine is replaced by poly brominated styrene with equal parts by weight.
Example 18: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
the tris (tribromophenoxy) triazine is replaced by a mixture of tris (tribromophenoxy) triazine and brominated epoxy resin with equal parts by weight, wherein the weight ratio of the tris (tribromophenoxy) triazine to the brominated epoxy resin is 1: 1.
Example 19: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
the tris (tribromophenoxy) triazine is replaced by a mixture of brominated polystyrene, polybrominated styrene and brominated polycarbonate with equal parts by weight, wherein the weight ratio of the brominated polystyrene to the polybrominated styrene to the brominated polycarbonate is 1:1: 1.
Example 20: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
replacing the antioxidant 168 with the antioxidant 1010 in parts by weight.
Example 21: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
replacing the antioxidant 168 with antioxidant 1076 in parts by weight.
Example 22: the preparation method of the flame-retardant master batch is different from the embodiment 5 in that:
replacing the antioxidant 168 with a mixture of the antioxidant 168, the antioxidant 1010 and the antioxidant 1076 in parts by weight, wherein the weight ratio of the antioxidant 168 to the antioxidant 1010 to the antioxidant 1076 is 1:1: 1.
Example 23: in other embodiments, the flame-retardant master batch can also be prepared by the preparation method of the flame-retardant master batch of embodiments 1-4 and 4-22.
Comparative example 1: a flame-retardant master batch is prepared by the following steps:
s1, drying 120 parts of polypropylene at 120 ℃ for 2h to obtain dried polypropylene;
s2, uniformly mixing 3 parts of antioxidant 168, 5 parts of polyethylene wax, 130 parts of tris (tribromophenoxy) triazine, 300 parts of microcapsule flame-retardant synergist and dried polypropylene to obtain a primary mixture of flame-retardant master batches;
and S3, putting the obtained mixture into a double-screw extruder for extrusion granulation to obtain the flame-retardant master batch.
Performance test
The flame retardant performance tests of examples 1-23 and comparative example 1 were carried out according to the flame retardant UL94 standard, wherein examples 1-23 all meet the UL-94 standard V-0 requirement, and comparative example 1 meets the UL-94 standard V-2 requirement.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.

Claims (8)

1. The flame-retardant master batch is characterized by comprising the following components in parts by weight:
100 portions and 120 portions of carrier;
60-130 parts of halogen flame retardant;
150 portions of microcapsule flame-retardant synergist and 300 portions of microcapsule flame-retardant synergist;
0.1-3 parts of antioxidant;
3-5 parts of a lubricant;
the microcapsule flame-retardant synergist comprises a core material and a wall material, wherein the weight part ratio of the core material to the wall material is 1: (4-6);
the core material is one or a mixture of more of antimony trioxide, antimony pentoxide and sodium antimonate.
2. The flame retardant masterbatch according to claim 1, wherein said wall material is β -cyclodextrin.
3. The flame retardant masterbatch according to claim 1, wherein the core material further comprises 10-20 parts of sodium bicarbonate.
4. The flame retardant masterbatch according to claim 1, wherein said carrier is polypropylene or polyethylene.
5. The flame retardant masterbatch according to claim 1, wherein said halogen-based flame retardant is one or more selected from the group consisting of tris (tribromophenoxy) triazine, brominated epoxy resins, brominated polystyrene, polybrominated styrene, and brominated polycarbonate.
6. The flame-retardant masterbatch according to claim 1, wherein the antioxidant is one or more of antioxidant 168, antioxidant 1010 or antioxidant 1076.
7. The flame retardant masterbatch according to claim 1, wherein said lubricant is one or more selected from the group consisting of polyethylene wax, stearic acid and liquid paraffin.
8. The preparation method of the flame-retardant master batch is characterized by comprising the following steps:
s1, preparing a microcapsule flame-retardant synergist;
s11, weighing the wall material and the core material in corresponding parts by weight, wherein the ratio of the core material to the wall material in parts by weight is 1: (4-6);
s12, dissolving the wall material in water, and uniformly stirring to form an embedding solution, wherein the weight part ratio of the wall material to the water is 1: (5-7);
s13, adding core materials in corresponding parts by weight into the embedding liquid, and uniformly stirring at 33-38 ℃ and 8000-;
s14, spraying, condensing and granulating the microcapsule flame-retardant synergist solution through a centrifugal spray tower to obtain the microcapsule flame-retardant synergist;
s2, drying the carrier in a corresponding weight part at 80-120 ℃ for 2-3h to obtain a dried carrier;
s3, uniformly mixing the antioxidant, the lubricant, the halogen flame retardant, the microcapsule flame retardant synergist and the dried carrier in parts by weight to obtain a primary mixture of the flame retardant master batch;
and S4, putting the obtained mixture into a double-screw extruder for extrusion granulation to obtain the flame-retardant master batch.
CN202010538951.XA 2020-06-13 2020-06-13 Flame-retardant master batch and preparation method thereof Pending CN111574773A (en)

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Application publication date: 20200825