CN107815076A - A kind of fiber glass reinforced PBT antimony system compositional flame-retardant master batch - Google Patents
A kind of fiber glass reinforced PBT antimony system compositional flame-retardant master batch Download PDFInfo
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- CN107815076A CN107815076A CN201711137010.XA CN201711137010A CN107815076A CN 107815076 A CN107815076 A CN 107815076A CN 201711137010 A CN201711137010 A CN 201711137010A CN 107815076 A CN107815076 A CN 107815076A
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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
- 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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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
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- C08K3/2279—Oxides; Hydroxides of metals of antimony
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- C08K5/00—Use of organic ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C08K9/04—Ingredients treated with organic substances
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Abstract
The present invention discloses a kind of fiber glass reinforced PBT antimony system compositional flame-retardant master batch, and its raw material composition and mass fraction is:50~85 parts of antimony oxide;2~5 parts of coupling agent;0.5~3 part of in-lubricant;3~10 parts of external lubricant;1~5 part of toughener;10~25 parts of PBT resin.The present invention has concentration height, good flame retardation effect, easy to use and low cost and other advantages, in the production process of fiber glass reinforced PBT modified materials use will have good flame-retardant modified effect, reduction dust pollution, be advantageous to clean manufacturing.
Description
Technical field
The invention belongs to fire proofing technical field, and in particular to a kind of fiber glass reinforced PBT antimony system compositional flame-retardant master batch.
Background technology
PBT is a kind of crystal type thermoplastic polymer, and its fiberglass reinforced product has high rigidity, electrical property and dimensionally stable
Function admirable, it is widely used in automobile, field of electronics.But because PBT has inflammability, and caused by glass addition
" wick effect " cause PBT product fire resistances it is poor, it is therefore necessary to it is carried out it is flame-retardant modified could meet properties of product will
Ask.Flame-retardant PBT is carried out fire-retardant by the way of directly addition antimony oxide powder more at present, and flame retardant effect is poor, and smoke amount is big,
And due to it is scattered it is uneven it is compatible with interface it is bad cause it is compound to fiber glass reinforced PBT after the addition of the inorganic particles such as antimony oxide
The mechanical performance of material has a great influence, and seriously governs application of the antimony oxide in flame-retardant PBT plastics.For inorganic particle
In resin the problem of difficult scattered and interface compatibility difference, the mode in industry frequently with composite modified or female granulated processed is carried out
Improve.
At present, it is domestic to have developed some flame-retardant master batch containing antimony oxide, but these fire-retardant master granule majorities are to need
Add the fire-retardant master granule that halogen flame carries out Synergistic, or the master batch that simple addition antimony oxide is fabricated to, such as Chinese patent
CN201110429778.0《A kind of antimony trioxide parent particle and preparation method thereof》Disclose a kind of with nanmeter antimong trioxide, load
Body, the antimony trioxide parent particle that modified ethylene bis-fatty acid amides are raw material.Chinese patent CN200710000830.4《One kind three
Aoxidize the preparation method of two antimony master batches》Disclose a kind of with antimony oxide powder, carrier, dispersant and coupling agent are raw material,
It is modified, extrude, be granulated, sieve, the method that the process such as dry prepares antimony trioxide parent particle.
Because the individual character of fire-retardant master granule, specific aim are stronger, different resins need to use base material similar in corresponding or physical property to hinder
Fire master batch, so PBT flame-retardant master batch be difficult accomplish it is general.There is no at present in industry solve fiber glass reinforced PBT composite it is inflammable,
Impact strength is low, flame retardance element disperse it is uneven and with antimony system compositional flame-retardant master batch the problems such as resin compatible difference.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of fiber glass reinforced PBT antimony system compositional flame-retardant
Master batch, solves after fiberglass reinforced that PBT composite is inflammable, impact strength is low, flame retardance element poor dispersion and and resin compatible
The technical barriers such as difference.
For achieving the above object, the technical scheme that the present invention takes is as follows:
A kind of fiber glass reinforced PBT antimony system compositional flame-retardant master batch, it is characterised in that raw material components and mass fraction are:
50~85 parts of antimony oxide;
2~5 parts of coupling agent;
0.5~3 part of in-lubricant;
3~10 parts of external lubricant;
1~5 part of toughener;
10~25 parts of PBT vector resins.
Preferably, described antimony oxide is full cubic crystal model, and average grain diameter is in 0.8~1.8 μm, purity
99.60~99.85%, whiteness is 95~99.
Preferably, described coupling agent is one kind in silane coupler, Aluminate.
Preferably, the in-lubricant A is a kind of in zinc stearate, calcium stearate.
Preferably, the external lubricant B is one kind in chlorinated paraffin, Tissuemat E, OPE.
Preferably, the toughener is in ethylene-vinyl acetate copolymer, maleic anhydride stem grafting polyolefin copolymer
It is a kind of.
Preferably, the melt mass flow rate of the PBT vector resins is 10~150g/10min.
The present invention also provides a kind of preparation method of fiber glass reinforced PBT antimony system compositional flame-retardant master batch, it is characterised in that bag
Include following steps:
Step 1, PBT is dried:PBT vector resins are dried using hot air circulation, 120 DEG C of temperature, drying time 8h;
Step 2, surface is modified:Antimony oxide is weighed by above-mentioned mass fraction and Aluminate input homogenizer is carried out
It is modified, 110 DEG C~120 DEG C of modification temperature, stir speed (S.S.) 800rpm/min, mixing time 3h~3.5h;
Step 3, the other components of the antimony oxide being modified and above-mentioned mass fraction are put into variable ratio frequency changer to mix at a high speed
Mixed at high speed is carried out in conjunction machine, rotating speed 800rpm/min, temperature control is at 100~110 DEG C.;
Step 4, mixture is transferred into extruder to be granulated, processing temperature is 220 DEG C~280 DEG C., behaviour does mode and given birth to by master batch
The conventional method of production carries out operating screened, dry, obtained fiber glass reinforced PBT antimony system compositional flame-retardant master batch.
Advantages of the present invention:
The present invention to antimony oxide organise and answered again after coating modification using silane coupler or Aluminate
With mixing, the compatibility of compound flame retardant and resin is improved by organic modification, reduces antimony oxide surface charge and table
Face tension force, the generation of agglomeration is reduced, improve dispersiveness.
Present invention employs the inside and outside lubricant agents such as calcium stearate and OPE to carry out compounding use, improves compounding production
The processing characteristics and mobility of product, dispersiveness of the compound product in fiber glass reinforced PBT material is improved, and then improve fire-retardant master granule
Fire-retardant synergistic function.
Present invention employs the toughener such as ethylene-vinyl acetate copolymer and maleic anhydride stem grafting polyolefin copolymer to multiple
Toughness reinforcing is carried out with fire-retardant master granule, so as to the phenomenon that avoids that compound product pelletizing is frangible, granular size differs, improves compound product
Processability and impact flexibility.
It is excellent that antimony system compositional flame-retardant master batch prepared by the present invention has fire-retardant synergistic efficiency high, dispersive property is good, cost is low etc.
Point, especially suitable for the flame-retardant modified of fiber glass reinforced PBT material, the Physical Mechanical using the compound product to composite
Energy, processing characteristics and tinctorial property influence less, and can realize the clean manufacturing of down-stream enterprise.
Due to the addition of inside and outside lubricant agent and toughener, and the optimization design of formula, the scattered of fire-retardant master granule is improved
Property and the compatibility with PBT resin.Therefore the antimony system compositional flame-retardant master batch prepared using the present invention of equivalent and three oxidations two
Antimony powder body phase ratio, the fire-retardant composite of the present invention have the impact strength and extension at break of better fire resistance and Geng Gao
Rate.
Embodiment
With reference to embodiment, the present invention is further described, but does not limit the scope of the invention.
Embodiment 1:
It is according to constituent content:85 parts of antimony oxide, purity are more than 99.6%, 0.8 μm of particle diameter, 3 parts of zinc stearate,
3 parts of Tissuemat E, 5 parts of aluminate coupling agent, 2 parts of EVA, the formula that 10 parts of PBT resin.PBT resin is entered using hot air circulation
Row drying process, 120 DEG C of temperature, drying time 8h.And measure antimony oxide and Aluminate input high-speed stirring by above-mentioned formula
Mix machine and carry out antimony oxide surface modification, 110 DEG C, stir speed (S.S.) 800rpm/min, mixing time 3.5h of modification temperature.It is modified to complete
Afterwards, the other components added in dried PBT resin and formula, hot mixing, rotating speed are carried out in high-speed mixing equipment
800rpm/min, temperature control is at 110 DEG C or so.It is to be mixed uniformly after be transferred to extruder and carry out plasticizing kneading, extrusion processing temperature
Spend for 200 DEG C~230 DEG C, extruded, granulation can obtain fiber glass reinforced PBT antimony system compositional flame-retardant master batch.Then by 6 parts
The sample, which is added in 100 parts of PBT pure resins, to be well mixed, and standard batten is made with the granulation and molding process planning of routine
The detection of fire resistance, smoke suppressing and mechanical property is carried out, test result is shown in Table 1.
Embodiment 2:
It is according to constituent content:70 parts of antimony oxide, purity are more than 99.6%, 1.8 μm of particle diameter, calcium stearate 1.5
Part, 3 parts of paraffin, 3 parts of aluminate coupling agent, 3 parts of EVA, the formula that 18 parts of PBT resin.PBT resin is entered using hot air circulation
Row drying process, 120 DEG C of temperature, drying time 8h.And measure antimony oxide and Aluminate input high-speed stirring by above-mentioned formula
Mix machine and carry out antimony oxide surface modification, 120 DEG C, stir speed (S.S.) 800rpm/min, mixing time 3h of modification temperature.It is modified to complete
Afterwards, the other components added in dried PBT resin and formula, hot mixing, rotating speed are carried out in high-speed mixing equipment
800rpm/min, temperature control is at 110 DEG C or so.It is to be mixed uniformly after be transferred to extruder and carry out plasticizing kneading, extrusion processing temperature
Spend for 200 DEG C~230 DEG C, extruded, granulation can obtain fiber glass reinforced PBT antimony system compositional flame-retardant master batch.Then by 7 parts
The sample, which is added in 100 parts of PBT pure resins, to be well mixed, and standard batten is made with the granulation and molding process planning of routine
The detection of fire resistance, smoke suppressing and mechanical property is carried out, test result is shown in Table 1.
Embodiment 3:
It is according to constituent content:50 parts of antimony oxide, purity are more than 99.6%, 1.8 μm of particle diameter, zinc stearate 0.5
Part, 5 parts of Tissuemat E, 2 parts of silane coupler, 5 parts of POE-g-MAH, the formula that 25 parts of PBT resin.Using hot air circulation pair
Processing, 120 DEG C of temperature, drying time 8h is dried in PBT resin.And measure antimony oxide and Aluminate throwing by above-mentioned formula
Enter homogenizer and carry out antimony oxide surface modification, 115 DEG C, stir speed (S.S.) 800rpm/min, mixing time 3.5h of modification temperature.
After the completion of modification, the other components that add in dried PBT resin and formula carry out hot mixing in high-speed mixing equipment,
Rotating speed 800rpm/min, temperature control is at 110 DEG C or so.It is to be mixed uniformly after be transferred to extruder and carry out plasticizing kneading, extrusion plus
Work temperature is 200 DEG C~230 DEG C, and extruded, granulation can obtain fiber glass reinforced PBT antimony system compositional flame-retardant master batch.Then will
The 10 parts sample, which is added in 100 parts of PBT pure resins, to be well mixed, and mark is made with the granulation and molding process planning of routine
Quasi- batten carries out the detection of fire resistance, smoke suppressing and mechanical property, and test result is shown in Table 1.
Comparative example 1:
The pure antimony oxide powder that 5.1 parts are not surface-treated, purity are more than 99.6%, 1.8 μm of particle diameter, are added
It is added in 100 parts of PBT pure resins and is well mixed, and it is fire-retardant with conventional granulation and molding process planning the progress of standard batten to be made
The detection of performance, smoke suppressing and mechanical property, test result are shown in Table 1.
Tested according to the corresponding national standard of project, its performance test results such as following table:
Table 1:Formula composition and the performance test results
Claims (8)
1. a kind of fiber glass reinforced PBT antimony system compositional flame-retardant master batch, it is characterised in that raw material components and mass fraction are:
50~85 parts of antimony oxide;
2~5 parts of coupling agent;
0.5~3 part of in-lubricant;
3~10 parts of external lubricant;
1~5 part of toughener;
10~25 parts of PBT vector resins.
2. fiber glass reinforced PBT according to claim 1 antimony system compositional flame-retardant master batch, it is characterised in that:
Described antimony oxide is full cubic crystal model, and average grain diameter is at 0.8~1.8 μm, and purity is 99.60~99.85%, in vain
Spend for 95~99.
3. fiber glass reinforced PBT according to claim 1 antimony system compositional flame-retardant master batch, it is characterised in that:
Described coupling agent is one kind in silane coupler, Aluminate.
4. fiber glass reinforced PBT according to claim 1 antimony system compositional flame-retardant master batch, it is characterised in that:
The in-lubricant is a kind of in zinc stearate, calcium stearate.
5. fiber glass reinforced PBT according to claim 1 antimony system compositional flame-retardant master batch, it is characterised in that:
The external lubricant is one kind in chlorinated paraffin, Tissuemat E, OPE.
6. fiber glass reinforced PBT according to claim 1 antimony system compositional flame-retardant master batch, it is characterised in that:
The toughener is one kind in ethylene-vinyl acetate copolymer, maleic anhydride stem grafting polyolefin copolymer.
7. fiber glass reinforced PBT according to claim 1 antimony system compositional flame-retardant master batch, it is characterised in that:
The melt mass flow rate of the PBT vector resins is 10~150g/10min.
8. a kind of preparation method for preparing fiber glass reinforced PBT antimony system compositional flame-retardant master batch as claimed in claim 1, its feature
It is, comprises the following steps:
Step 1, PBT is dried:PBT vector resins are dried using hot air circulation, 120 DEG C of temperature, drying time 8h;
Step 2, surface is modified:Antimony oxide is weighed by above-mentioned mass fraction and Aluminate input homogenizer is changed
Property, 110 DEG C~120 DEG C of modification temperature, stir speed (S.S.) 800rpm/min, mixing time 3h~3.5h;
Step 3, the other components of the antimony oxide being modified and above-mentioned mass fraction are put into variable ratio frequency changer high-speed mixer
Middle carry out mixed at high speed, rotating speed 800rpm/min, temperature control is at 100~110 DEG C;
Step 4, mixture is transferred into extruder to be granulated, processing temperature is 220 DEG C~280 DEG C, screened, is dried, and glass is made
Strengthen PBT antimony system compositional flame-retardant master batches.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103627168A (en) * | 2013-11-13 | 2014-03-12 | 广东聚石化学股份有限公司 | Special halogen-free flame-retardant master batch for nylon and preparation method thereof |
CN103709609A (en) * | 2012-09-29 | 2014-04-09 | 青岛欣展塑胶有限公司 | Flame-retardant nanometer master batch for polyester plastic |
CN105602246A (en) * | 2016-03-04 | 2016-05-25 | 广西华锑科技有限公司 | Antimony-based compound flame-retardant masterbatch for nylon 66 and preparation method of antimony-based compound flame-retardant masterbatch |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103709609A (en) * | 2012-09-29 | 2014-04-09 | 青岛欣展塑胶有限公司 | Flame-retardant nanometer master batch for polyester plastic |
CN103627168A (en) * | 2013-11-13 | 2014-03-12 | 广东聚石化学股份有限公司 | Special halogen-free flame-retardant master batch for nylon and preparation method thereof |
CN105602246A (en) * | 2016-03-04 | 2016-05-25 | 广西华锑科技有限公司 | Antimony-based compound flame-retardant masterbatch for nylon 66 and preparation method of antimony-based compound flame-retardant masterbatch |
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Application publication date: 20180320 |