CN106832517A - A kind of nano-meter flame retardantses master batch and preparation method thereof - Google Patents
A kind of nano-meter flame retardantses master batch and preparation method thereof Download PDFInfo
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- CN106832517A CN106832517A CN201710026313.8A CN201710026313A CN106832517A CN 106832517 A CN106832517 A CN 106832517A CN 201710026313 A CN201710026313 A CN 201710026313A CN 106832517 A CN106832517 A CN 106832517A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
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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
- C08K3/02—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
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
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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
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
Abstract
The present invention discloses a kind of nano-meter flame retardantses master batch and preparation method thereof, and preparation method specifically includes following steps：(1) sodium-based montmorillonite is pressed 1:The mass ratio of (8 10) is added in running water, and high-speed stirred is to uniform；(2) after placing 72 80 hours to the liquid obtained by step (1), taking supernatant liquid carries out being heated to 75 90 DEG C, adds modifying agent to layering；(3) solid suspension of the layering for obtaining step (2) is separated, and is taken supernatant liquid and is added 12 parts of organic silicon solvent, is stirred；(4) take red phosphorus to be dried at 100 DEG C, add polyethylene, stirring adds 23 parts of organic silicon solvent, continues to stir；(5) by step (3) gained emulsion drying, take in 10 20 parts of additions step (4), add antioxidant, continue to stir；(6) by single screw rod extrusion moulding, as nano-meter flame retardantses master batch.The good flame retardation effect of nano-meter flame retardantses master batch of the present invention, in subsequent production composite, can reduce the addition of fire retardant, so as to reduce influence of the fire retardant to Material Physics mechanical property.
Description
Technical field
The present invention relates to nano-meter flame retardantses master-batch techniques field, more particularly to a kind of nano-meter flame retardantses master batch and its preparation side
Method.
Background technology
With the development of Polymer Technology, the synthetic material of excellent performance starts to enter into the every field of national economy.By
Combustible is mostly in macromolecular material, and substantial amounts of toxic and harmful can be discharged during burning, therefore, to height
It is one, following macromolecule modified field important topic that molecular material is carried out flame-retardant modified.Fire retardant, also known as fireproof agent, fire-proofing chemical
Or incombustible agent, it is a kind of for lifting material flame resistance, prevent material from being ignited and suppress the auxiliary agent of flame propagation；It is mainly used
In fire-retardant synthesis macromolecular material and natural macromolecular material (including plastics, fiber, rubber, coating etc.).It is added with fire-retardant
The material of agent is difficult to be ignited compared with the material without fire retardant, and can in a fire suppress flame transmission and poisonous and harmful
The diffusion of gas, substantially reduces the danger of fire, it is ensured that the use that the product such as various plastics, rubber can be safer.
At present, conventional fire retardant mainly has inorganic combustion inhibitor and a phosphorus-nitrogen expansion type fire retardant, and inorganic combustion inhibitor by
In the poor compatibility with vistanex, flame retarding efficiency is low, only in a large amount of fillings just with certain flame retardant effect, and this
Sample can seriously damage the mechanical property and processing characteristics of polyolefin.P-N type fire retardant generally is powder, and its fineness one
As more than 400 mesh, production and use during easily produce substantial amounts of dust pollution, very big harm is caused to health,
A certain degree of abrasion can be also caused to process equipment simultaneously.Additionally, P-N type fire retardant all has hygroscopicity stronger, thermally-stabilised
Property compatibility not high and vistanex it is poor the problems such as, cause fire proofing more sensitive to moisture, easy foaming and degraded,
The shortcoming of poor and infringement material to a certain extent the processing characteristics of fire retardant dispersiveness in resin and physical and mechanical properties.
The content of the invention
Present invention seek to address that above-mentioned mentioned technical problem, there is provided a kind of nano-meter flame retardantses master batch and its preparation side
Method.
The present invention uses following technical scheme：
Nano-meter flame retardantses master batch, including under raw material according to the mass fraction：Sodium-based montmorillonite 10-20 parts, modifying agent 5-8
Part, polyethylene 10-30 parts, red phosphorus 40-60 parts, organic silicon solvent 3-5 parts, antioxidant 0.5-1 parts.
Preferably, described modifying agent is dodecyl bromination ammonium material.
Preferably, described organic silicon solvent is the one kind in KH550, KH560, KH570.
Preferably, described antioxidant includes hindered phenol antioxygen and/or phosphite antioxidant.
It is further preferred that described antioxidant is one or more in B215, B225 and B900.
The preparation method of nano-meter flame retardantses master batch, comprises the following steps：(1) sodium-based montmorillonite is pressed 1:The quality of (8-10)
In than adding running water, high-speed stirred is to uniform；(2) after being placed 72-80 hours to the liquid obtained by step (1), upper liquid is taken
Body carries out being heated to 75-90 DEG C, adds modifying agent to layering；(3) solid suspension of the layering for obtaining step (2) is separated,
Take supernatant liquid and add 1-2 parts of organic silicon solvent, stir；(4) take red phosphorus to be dried at 100 DEG C, add polyethylene, stir
Mix, add 2-3 parts of organic silicon solvent, continue to stir；(5) by step (3) gained emulsion drying, take 10-20 parts and add step
Suddenly in (4), antioxidant is added, continues to stir；(6) by single screw rod extrusion moulding, as nano-meter flame retardantses master batch.
Nano-meter flame retardantses master batch prepared by the inventive method is applied to prepare the composite of nano-nylon 6.
The preparation process of the composite of nano-nylon 6：(1) mix：By PA6, nano-meter flame retardantses master batch, it is resistance to puncture master batch,
Compatilizer, antioxidant are well mixed in height stirs machine, are put into main spout；Glass fibre is by surveying spout；(2) by double spiral shells
Bar extrusion moulding.
The beneficial effects of the invention are as follows：Compared with prior art, the fire-retardant effect of nano-meter flame retardantses master batch of preparation of the invention
It is really good, in subsequent production composite, the addition of fire retardant can be reduced, so as to reduce fire retardant to Material Physics mechanical property
The influence of energy.Nano-meter flame retardantses master batch is applied to prepare the composite of nano-nylon 6, can be very good to be well mixed with material,
Effectively prevent powder and pellet mixes the uneven situation for causing quality of materials unstable.
Specific embodiment
Technical scheme is further illustrated below by specific embodiment.
Embodiment 1：
A kind of preparation method of nano-meter flame retardantses master batch, comprises the following steps：
(1) sodium-based montmorillonite is pressed 1:8 mass ratio is added in running water, and high-speed stirred is to uniform；
(2) after being placed 72 hours to the liquid obtained by step (1), taking supernatant liquid carries out being heated to 75 DEG C, adds modified
Agent is extremely layered；
(3) solid suspension of the layering for obtaining step (2) is separated, and is taken supernatant liquid and is added 1 part of organic silicon solvent, is stirred
Mix uniform；
(4) take red phosphorus to be dried at 100 DEG C, add polyethylene, stirring adds 2 parts of organic silicon solvent, continue to stir equal
It is even；
(5) by step (3) gained emulsion drying, take in 10 parts of additions step (4), add antioxidant, continue to stir；
(6) by single screw rod extrusion moulding, as nano-meter flame retardantses master batch.
Embodiment 2：
A kind of preparation method of nano-meter flame retardantses master batch, comprises the following steps：
(1) sodium-based montmorillonite is pressed 1:10 mass ratio is added in running water, and high-speed stirred is to uniform；
(2) after being placed 80 hours to the liquid obtained by step (1), taking supernatant liquid carries out being heated to 90 DEG C, adds modified
Agent is extremely layered；
(3) solid suspension of the layering for obtaining step (2) is separated, and is taken supernatant liquid and is added 2 parts of organic silicon solvent, is stirred
Mix uniform；
(4) take red phosphorus to be dried at 100 DEG C, add polyethylene, stirring adds 3 parts of organic silicon solvent, continue to stir equal
It is even；
(5) by step (3) gained emulsion drying, take in 20 parts of additions step (4), add antioxidant, continue to stir；
(6) by single screw rod extrusion moulding, as nano-meter flame retardantses master batch.
Embodiment 3：
A kind of preparation method of nano-meter flame retardantses master batch, comprises the following steps：
(1) sodium-based montmorillonite is pressed 1:9 mass ratio is added in running water, and high-speed stirred is to uniform；
(2) after being placed 75 hours to the liquid obtained by step (1), taking supernatant liquid carries out being heated to 80 DEG C, adds modified
Agent is extremely layered；
(3) solid suspension of the layering for obtaining step (2) is separated, and is taken supernatant liquid and is added 1 part of organic silicon solvent, is stirred
Mix uniform；
(4) take red phosphorus to be dried at 100 DEG C, add polyethylene, stirring adds 3 parts of organic silicon solvent, continue to stir equal
It is even；
(5) by step (3) gained emulsion drying, take in 15 parts of additions step (4), add antioxidant, continue to stir；
(6) by single screw rod extrusion moulding, as nano-meter flame retardantses master batch.
Embodiment 4：
A kind of preparation method of nano-meter flame retardantses master batch, comprises the following steps：
(1) sodium-based montmorillonite is pressed 1:8 mass ratio is added in running water, and high-speed stirred is to uniform；
(2) after being placed 78 hours to the liquid obtained by step (1), taking supernatant liquid carries out being heated to 83 DEG C, adds modified
Agent is extremely layered；
(3) solid suspension of the layering for obtaining step (2) is separated, and is taken supernatant liquid and is added 2 parts of organic silicon solvent, is stirred
Mix uniform；
(4) take red phosphorus to be dried at 100 DEG C, add polyethylene, stirring adds 2 parts of organic silicon solvent, continue to stir equal
It is even；
(5) by step (3) gained emulsion drying, take in 15 parts of additions step (4), add antioxidant, continue to stir；
(6) by single screw rod extrusion moulding, as nano-meter flame retardantses master batch.
Nano-meter flame retardantses master batch prepared by the above method, is applied to prepare the composite of nano-nylon 6.
The composite of nano-nylon 6, including following mass fraction raw material：20 parts of PA6,2 parts of compatilizer, 5 parts it is resistance to
Puncture master batch, 35 parts of nano flame-proof agglomerate, 30 parts of glass fibres, 0.2 part of antioxidant.
The preparation process of the composite of nano-nylon 6：(1) mix：By PA6, nano-meter flame retardantses master batch, it is resistance to puncture master batch,
Ethylene-methyl acrylate copolymer is well mixed in height stirs machine, is put into main spout；Glass fibre is by surveying spout；(2)
By parallel double-screw extrusion moulding.
Twin-screw processing temperature is：255 DEG C, the draw ratio of screw rod is 44：1.
Embodiment 5：
A kind of preparation method of nano-meter flame retardantses master batch, comprises the following steps：
(1) sodium-based montmorillonite is pressed 1:9 mass ratio is added in running water, and high-speed stirred is to uniform；
(2) after being placed 76 hours to the liquid obtained by step (1), taking supernatant liquid carries out being heated to 77 DEG C, adds modified
Agent is extremely layered；
(3) solid suspension of the layering for obtaining step (2) is separated, and is taken supernatant liquid and is added 1 part of organic silicon solvent, is stirred
Mix uniform；
(4) take red phosphorus to be dried at 100 DEG C, add polyethylene, stirring adds 3 parts of organic silicon solvent, continue to stir equal
It is even；
(5) by step (3) gained emulsion drying, take in 12 parts of additions step (4), add antioxidant, continue to stir；
(6) by single screw rod extrusion moulding, as nano-meter flame retardantses master batch.
Nano-meter flame retardantses master batch prepared by the above method, is applied to prepare the composite of nano-nylon 6.
The composite of nano-nylon 6, including following mass fraction raw material：50 parts of PA6,3 parts of compatilizer, 8 parts it is resistance to
Puncture master batch, 35 parts of nano-meter flame retardantses master batch, 35 parts of glass fibres, 0.1 part of antioxidant.
The preparation process of the composite of nano-nylon 6：(1) mix：By PA6, nano-meter flame retardantses master batch, it is resistance to puncture master batch,
Ethylene-methyl acrylate copolymer is well mixed in height stirs machine, is put into main spout；Glass fibre is by surveying spout；(2)
By parallel double-screw extrusion moulding, the temperature of melting extrusion is 205-255 DEG C, screw speed：380~420 turns/min, screw rod
Draw ratio is 40:1.
Claims (7)
1. a kind of nano-meter flame retardantses master batch, it is characterised in that including following raw material according to the mass fraction：Sodium-based montmorillonite 10-
20 parts, modifying agent 5-8 parts, polyethylene 10-30 parts, red phosphorus 40-60 parts, organic silicon solvent 3-5 parts, antioxidant 0.5-1 parts.
2. nano-meter flame retardantses master batch according to claim 1, it is characterised in that described modifying agent is dodecyl bromination
Ammonium material.
3. nano-meter flame retardantses master batch according to claim 1, it is characterised in that the organic silicon solvent be KH550,
One kind in KH560, KH570.
4. nano-meter flame retardantses master batch according to claim 1, it is characterised in that described antioxidant includes hindered phenol antioxygen
Agent and/or phosphite antioxidant.
5. nano-meter flame retardantses master batch according to claim 1, it is characterised in that described antioxidant be B215, B225 and
One or more in B900.
6. the preparation method of the nano-meter flame retardantses master batch according to any one of claim 1-5, it is characterised in that including with
Lower step：(1) sodium-based montmorillonite is pressed 1:The mass ratio of (8-10) is added in running water, and high-speed stirred is to uniform；(2) to step
(1) after the liquid obtained by is placed 72-80 hours, taking supernatant liquid carries out being heated to 75-90 DEG C, adds modifying agent to layering；(3)
The solid suspension of the layering that step (2) is obtained is separated, and is taken supernatant liquid and is added 1-2 parts of organic silicon solvent, is stirred；
(4) take red phosphorus to be dried at 100 DEG C, add polyethylene, stirring adds 2-3 parts of organic silicon solvent, continues to stir；(5) will
Step (3) gained emulsion drying, takes in 10-20 parts of addition step (4), adds antioxidant, continues to stir；(6) by single screw rod
Extrusion moulding, as nano-meter flame retardantses master batch.
7. the nano-meter flame retardantses master batch that according to claim 6 prepared by method, is applied to prepare the composite of nano-nylon 6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112852072A (en) * | 2021-03-02 | 2021-05-28 | 中国机械工业第四建设工程有限公司 | Flame-retardant polyester fiber internal reinforced PVC (polyvinyl chloride) waterproof coiled material, preparation method and system |
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Patent Citations (2)
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| CN102161794A (en) * | 2011-03-14 | 2011-08-24 | 安徽欣意电缆有限公司 | Low-smoke halogen-free flame-retardant polyethylene cable material |
| CN103881182A (en) * | 2012-12-20 | 2014-06-25 | 青岛欣展塑胶有限公司 | Flame-retardant antistatic master batch used for polyethylene tubes, and its preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112852072A (en) * | 2021-03-02 | 2021-05-28 | 中国机械工业第四建设工程有限公司 | Flame-retardant polyester fiber internal reinforced PVC (polyvinyl chloride) waterproof coiled material, preparation method and system |
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Application publication date: 20170613 |