CN109294175B - A kind of flame-proof abrasion-resistant PBT composite - Google Patents
A kind of flame-proof abrasion-resistant PBT composite Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- 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
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- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
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- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
Composed of the following components by weight the present invention relates to a kind of flame-proof abrasion-resistant PBT composite: PBT is 80 parts -100 parts；Wear resistant filler is 8 parts -12 parts；Fire retardant is 16 parts -20 parts；Synergistic flame retardant is 5 parts -7 parts；Antioxidant is 0.1 part -0.5 part；Wear resistant filler is modified MgO/TiO2.A kind of novel wear resistant filler MgO/TiO has been made in the application2, this compounded mix embodies addition, gives full play to its wear-resisting property, significantly improves the wear-resisting property of PET composite material；PET composite material flame retardant property and wear-resisting property in the application is all very excellent, compensates for the deficiency of current material, has very big promotional value.
Description
Technical field
The invention belongs to technical field of polymer materials, particularly relate to a kind of flame-proof abrasion-resistant PBT composite.
Background technique
Polybutylene terephthalate (PBT) (PBT) is a kind of widely applied macromolecule polyester resin, and PBT has good
The advantages that fatigue durability, preferable heat resistance, excellent dimensional stability, but its flame retardant property, wear-resisting property are general.?
Some specific application fields have the requirement of flame retardant property, wear-resisting property to PBT, and common PBT composite, which is unable to satisfy, to be wanted
It asks.
In response to this, a kind of PBT composite has been made in the technical program innovation, its flame retardant property, wearability
Can be all very excellent, this material not yet sees report so far, this has the application of extension PBT composite very important
Realistic meaning.
Summary of the invention
The object of the present invention is to provide a kind of flame-proof abrasion-resistant PBT composites, to solve existing PBT composite fire-retardant
Not the problem of performance and wear-resisting property are not able to satisfy particular demands in some aspects.
The present invention is achieved by the following technical solutions:
A kind of flame-proof abrasion-resistant PBT composite, composed of the following components by weight:
The wear resistant filler is modified MgO/TiO2。
The preparation method of the wear resistant filler, comprising the following steps:
(1) a certain amount of Polyprenol, bis- (triethanolamine) metatitanic acid diisopropyl esters, isopropanol, deionized water are weighed, is added
Enter into reaction vessels, 8-10h is stirred to react under room temperature, forms solution A；
(2) a certain amount of tert-butyl alcohol magnesium, solution A are weighed, is added into reaction vessels, is stirred to react 10-12h under room temperature,
Ultrasonic disperse 2-4h, obtains solution；.
(3) weigh a certain amount of Polyprenol, bis- (triethanolamine) metatitanic acid diisopropyl esters, isopropanol, ammonium acid fluoride,
Deionized water is added into reaction vessels, and 8-10h is stirred to react under room temperature, forms solution C；
(4) a certain amount of solution C, positive butyl titanate are weighed, is added into reaction vessels, is stirred to react 8-10h under room temperature,
Ultrasonic disperse 1-3h, obtains solution D；
(5) a certain amount of solution B, solution D, ammonium hydroxide are weighed, 6-8h is stirred to react under room temperature, ultrasonic disperse 4-6h is obtained molten
Liquid E；
(6) solution E is added to autoclave, 6-8h is reacted under conditions of 220-260 DEG C, 4-6MPa, both it is modified
MgO/TiO2 particle；
(7) by the modified MgO/TiO2 particle drying of gained, grinding crosses 600 meshes, both obtains wear resistant filler.
The quality of Polyprenol, bis- (triethanolamine) metatitanic acid diisopropyl esters, isopropanol, deionized water in step (1)
Than for (10-16): (6-10): (80-100): (160-180).
The mass ratio of tert-butyl alcohol magnesium, solution A in step (2) is (60-80): (100-120).
Polyprenol, bis- (triethanolamine) metatitanic acid diisopropyl esters, isopropanol, ammonium acid fluoride in step (3), go from
The mass ratio of sub- water is (12-18): (8-10): (60-80): (6-10): (140-180).
The mass ratio of solution C, positive butyl titanate in step (4) is (120-160): (70-90).
The mass ratio of solution B, solution D, ammonium hydroxide in step (5) is (30-50): (60-80): (10-16).
The fire retardant is melamine polyphosphate.
The synergistic flame retardant is anhydrous ammonium phosphomolybdate crystal.
The antioxidant is three (2,4- di-t-butyl) phenyl-phosphites, four [β-(3,5- di-tert-butyl-hydroxy phenyl)
Propionic acid] pentaerythritol ester or 1,3,5- trimethyls -2,4, one of 6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene or several
The mixing of kind.
The beneficial effects of the present invention are:
1, a kind of novel wear resistant filler MgO/TiO has been made in the application2, this compounded mix embodies addition, makes
Its wear-resisting property is given full play to, and the wear-resisting property of PET composite material is significantly improved.
2, the application uses synergistic flame retardant of the anhydrous ammonium phosphomolybdate crystal as melamine polyphosphate, and mechanism is such as
Under: anhydrous ammonium phosphomolybdate crystal can move in the layer of charcoal on PET composite material surface, can also be promoted by thermogenetic molybdic acid
Char forming ability, and the generation of smog is prevented to a certain extent, play the role of fire retarding synergist.
3, the PET composite material flame retardant property in the application and wear-resisting property are all very excellent, compensate for current material not
Foot has very big promotional value.
Specific embodiment
Carry out the technical solution that the present invention will be described in detail by the following examples, embodiment below is merely exemplary, only
It can be used to explanation and illustration technical solution of the present invention, and be not to be construed as the limitation to technical solution of the present invention.
The application provides a kind of flame-proof abrasion-resistant PBT composite, composed of the following components by weight:
The wear resistant filler is modified MgO/TiO2。
The preparation method of the wear resistant filler, comprising the following steps:
(1) a certain amount of Polyprenol, bis- (triethanolamine) metatitanic acid diisopropyl esters, isopropanol, deionized water are weighed, is added
Enter into reaction vessels, 8-10h is stirred to react under room temperature, forms solution A；Polyprenol, bis- (triethanolamine) metatitanic acids two are different
Propyl ester, isopropanol, deionized water mass ratio be (10-16): (6-10): (80-100): (160-180).
(2) a certain amount of tert-butyl alcohol magnesium, solution A are weighed, is added into reaction vessels, is stirred to react 10-12h under room temperature,
Ultrasonic disperse 2-4h, obtains solution；Tert-butyl alcohol magnesium, solution A mass ratio be (60-80): (100-120).
(3) weigh a certain amount of Polyprenol, bis- (triethanolamine) metatitanic acid diisopropyl esters, isopropanol, ammonium acid fluoride,
Deionized water is added into reaction vessels, and 8-10h is stirred to react under room temperature, forms solution C；Polyprenol, bis- (three ethyl alcohol
Amine) metatitanic acid diisopropyl ester, isopropanol, ammonium acid fluoride, deionized water mass ratio be (12-18): (8-10): (60-80):
(6-10): (140-180).
(4) a certain amount of solution C, positive butyl titanate are weighed, is added into reaction vessels, is stirred to react 8-10h under room temperature,
Ultrasonic disperse 1-3h, obtains solution D；Solution C, positive butyl titanate mass ratio be (120-160): (70-90).
(5) a certain amount of solution B, solution D, ammonium hydroxide are weighed, 6-8h is stirred to react under room temperature, ultrasonic disperse 4-6h is obtained molten
Liquid E；Solution B, solution D, ammonium hydroxide mass ratio be (30-50): (60-80): (10-16).
(6) solution E is added to autoclave, 6-8h is reacted under conditions of 220-260 DEG C, 4-6MPa, both it is modified
MgO/TiO2 particle.
(7) by the modified MgO/TiO2 particle drying of gained, grinding crosses 600 meshes, both obtains wear resistant filler.
The fire retardant is melamine polyphosphate.
The synergistic flame retardant is anhydrous ammonium phosphomolybdate crystal.
Antioxidant is three (2,4- di-t-butyl) phenyl-phosphites (abbreviation Irganox168), the four [β-of BASF AG
(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (abbreviation Irganox1010) or 1,3,5- trimethyls -2,4,
The mixing of one or more of 6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene (abbreviation Irganox1330).
A kind of preparation method of flame-proof abrasion-resistant PBT composite, comprising the following steps:
(1) 80 parts -100 parts of PBT, 8 parts of -12 parts of wear resistant fillers, 16 parts of -20 parts of melamine polyphosphates, 5 are weighed
- 7 parts of anhydrous ammonium phosphomolybdate crystal of part, 0.1 part of -0.5 part of antioxidant are mixed and stirred for uniformly, obtaining mixture；
(2) by mixture obtained in step (1) from extruder extruding pelletization to get to PBT composite.
The step (2) specifically: mixture obtained in step (1) is put into the hopper of double screw extruder and squeezed
It is granulated out to get PBT composite is arrived, wherein the double screw extruder includes six humidity provinces sequentially arranged, a Qu Wen
200~220 DEG C of degree, two 240~260 DEG C of area's temperature, three 240~260 DEG C of area's temperature, four 240~260 DEG C of area's temperature, five Qu Wen
240~260 DEG C of degree, six 240~260 DEG C of area's temperature, 240~260 DEG C of head temperature, 200~280r/min of screw speed.
Raw material used in embodiments herein is as follows:
PBT (model 2002U), Polyplastics；Polyprenol, Shijiazhuang Hai Sen Chemical Co., Ltd.；Bis- (three ethyl alcohol
Amine) metatitanic acid diisopropyl ester, Hangzhou Jesse card Chemical Co., Ltd.；Isopropanol, the extra large Chemical Co., Ltd. in Jiangsu million；Tert-butyl alcohol magnesium,
The Shandong chemical inc Kai Yue；Ammonium acid fluoride, Wuhan sea Dehua work Development Co., Ltd；Positive butyl titanate, Nanjing
You Pu Chemical Co., Ltd.；Ammonium hydroxide, Anhui Bao Qun Chemical Co., Ltd.；Melamine polyphosphate, special science and technology is moistened in Heilungkiang to be had
Limit company；Anhydrous ammonium phosphomolybdate crystal, Henan Jia Yuan chemical products Co., Ltd；Antioxidant (model Irganox168,
Irganox1010, Irganox1330), Switzerland's Ciba.
Test equipment used herein is as follows:
ZSK30 type double screw extruder, German W&P company；JL-1000 type tensile testing machine, the wide just experiment instrument in Guangzhou
The production of device company；HTL900-T-5B type injection (mo(u)lding) machine, the production of Hai Tai plastics machinery Co., Ltd；XCJ-500 type shock-testing
Machine, the production of Chengde testing machine factory；QT-1196 type tester for elongation, Dongguan City Gao Tai detecting instrument Co., Ltd；QD-GJS-
B12K type high-speed mixer, Beijing perseverance Order instrument and meter Co., Ltd.
Embodiment 1
(1) weigh 80 parts of PBT, 8 parts of wear resistant fillers, 16 parts of melamine polyphosphates, 5 parts of anhydrous ammonium phosphomolybdate crystal,
0.1 part of Irganox168 is mixed and stirred for uniformly, obtaining mixture；
(2) by mixture obtained in step (1) from extruder extruding pelletization to get to PBT composite P1.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 200 DEG C of area's temperature, two 240 DEG C of area's temperature,
Three 240 DEG C of area's temperature, four 240 DEG C of area's temperature, five 240 DEG C of area's temperature, six 240 DEG C of area's temperature, 240 DEG C of head temperature, screw rod turns
Fast 200r/min.
Embodiment 2
(1) 100 parts of PBT, 12 parts of wear resistant fillers, 20 parts of melamine polyphosphates, 7 parts of anhydrous ammonium phosphomolybdates crystalline substances are weighed
Body, 0.1 part of Irganox168,0.2 part of Irganox1010,0.2 part of Irganox1330 are mixed and stirred for uniformly, being mixed
Material；
(2) by mixture obtained in step (1) from extruder extruding pelletization to get to PBT composite P2.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 220 DEG C of area's temperature, two 260 DEG C of area's temperature,
Three 260 DEG C of area's temperature, four 260 DEG C of area's temperature, five 260 DEG C of area's temperature, six 260 DEG C of area's temperature, 260 DEG C of head temperature, screw rod turns
Fast 280r/min.
Embodiment 3
(1) 90 parts of PBT, 10 parts of wear resistant fillers, 18 parts of melamine polyphosphates, 6 parts of anhydrous ammonium phosphomolybdates crystalline substances are weighed
Body, 0.1 part of Irganox168,0.2 part of Irganox1010 are mixed and stirred for uniformly, obtaining mixture；
(2) by mixture obtained in step (1) from extruder extruding pelletization to get to PBT composite P3.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 210 DEG C of area's temperature, two 250 DEG C of area's temperature,
Three 250 DEG C of area's temperature, four 250 DEG C of area's temperature, five 250 DEG C of area's temperature, six 250 DEG C of area's temperature, 250 DEG C of head temperature, screw rod turns
Fast 240r/min.
Embodiment 4
(1) 85 parts of PBT, 11 parts of wear resistant fillers, 19 parts of melamine polyphosphates, 7 parts of anhydrous ammonium phosphomolybdates crystalline substances are weighed
Body, 0.1 part of Irganox1010,0.2 part of Irganox1330 are mixed and stirred for uniformly, obtaining mixture；
(2) by mixture obtained in step (1) from extruder extruding pelletization to get to PBT composite P4.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 205 DEG C of area's temperature, two 245 DEG C of area's temperature,
Three 245 DEG C of area's temperature, four 245 DEG C of area's temperature, five 245 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, screw rod turns
Fast 230r/min.
Embodiment 5
(1) 95 parts of PBT, 10 parts of wear resistant fillers, 17 parts of melamine polyphosphates, 5 parts of anhydrous ammonium phosphomolybdates crystalline substances are weighed
Body, 0.1 part of Irganox1010,0.1 part of Irganox168 are mixed and stirred for uniformly, obtaining mixture；
(2) by mixture obtained in step (1) from extruder extruding pelletization to get to PBT composite P5.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 205 DEG C of area's temperature, two 255 DEG C of area's temperature,
Three 255 DEG C of area's temperature, four 255 DEG C of area's temperature, five 255 DEG C of area's temperature, six 255 DEG C of area's temperature, 255 DEG C of head temperature, screw rod turns
Fast 245r/min.
Comparative example 1
(1) 80 parts of PBT, 0.1 part of Irganox1010,0.2 part of Irganox168 is weighed to be mixed and stirred for uniformly, being mixed
Close material；
(2) by mixture obtained in step (1) from extruder extruding pelletization to get to PBT composite D1.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 205 DEG C of area's temperature, two 255 DEG C of area's temperature,
Three 255 DEG C of area's temperature, four 255 DEG C of area's temperature, five 255 DEG C of area's temperature, six 255 DEG C of area's temperature, 255 DEG C of head temperature, screw rod turns
Fast 245r/min.
Batten test is made with injection molding machine in PBT composite prepared by above-described embodiment 1-5 and comparative example 1, tests number
According to being as follows:
It can also be seen that the flame retardant property of embodiment 1-5, wear-resisting property will be better than comparative example 1 from table.This is for expanding
The application field for opening up PBT composite, has very important significance.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And deformation, the scope of the present invention are extremely equally limited by appended claims.
Claims (9)
1. a kind of flame-proof abrasion-resistant PBT composite, which is characterized in that composed of the following components by weight:
The wear resistant filler is modified MgO/TiO2；
The preparation method of the wear resistant filler, comprising the following steps:
(1) a certain amount of Polyprenol, bis- (triethanolamine) metatitanic acid diisopropyl esters, isopropanol, deionized water are weighed, is added extremely
In reaction vessels, it is stirred to react 8-10h under room temperature, forms solution A；
(2) a certain amount of tert-butyl alcohol magnesium, solution A are weighed, is added into reaction vessels, 10-12h is stirred to react under room temperature, ultrasound
Disperse 2-4h, obtains solution B；
(3) weigh a certain amount of Polyprenol, bis- (triethanolamine) metatitanic acid diisopropyl esters, isopropanol, ammonium acid fluoride, go from
Sub- water is added into reaction vessels, and 8-10h is stirred to react under room temperature, forms solution C；
(4) a certain amount of solution C, positive butyl titanate are weighed, is added into reaction vessels, 8-10h is stirred to react under room temperature, ultrasound
Disperse 1-3h, obtains solution D；
(5) a certain amount of solution B, solution D, ammonium hydroxide are weighed, 6-8h is stirred to react under room temperature, ultrasonic disperse 4-6h obtains solution E；
(6) solution E is added to autoclave, reacts 6-8h under conditions of 220-260 DEG C, 4-6MPa to get modified MgO/
TiO2 particle；
(7) by the modified MgO/TiO2 particle drying of gained, grinding crosses 600 meshes to get wear resistant filler.
2. flame-proof abrasion-resistant PBT composite according to claim 1, which is characterized in that the polyisoamylene in step (1)
Alcohol, bis- (triethanolamine) metatitanic acid diisopropyl esters, isopropanol, deionized water mass ratio be (10-16): (6-10): (80-100):
(160-180)。
3. flame-proof abrasion-resistant PBT composite according to claim 1, which is characterized in that tert-butyl alcohol magnesium in step (2),
The mass ratio of solution A is (60-80): (100-120).
4. flame-proof abrasion-resistant PBT composite according to claim 1, which is characterized in that the polyisoamylene in step (3)
Alcohol, bis- (triethanolamine) metatitanic acid diisopropyl esters, isopropanol, ammonium acid fluoride, deionized water mass ratio be (12-18): (8-
10): (60-80): (6-10): (140-180).
5. flame-proof abrasion-resistant PBT composite according to claim 1, which is characterized in that solution C, titanic in step (4)
The mass ratio of acid butyl ester is (120-160): (70-90).
6. flame-proof abrasion-resistant PBT composite according to claim 1, which is characterized in that solution B, solution in step (5)
D, the mass ratio of ammonium hydroxide is (30-50): (60-80): (10-16).
7. flame-proof abrasion-resistant PBT composite according to claim 1, which is characterized in that the fire retardant is melamine
Quadrafos.
8. flame-proof abrasion-resistant PBT composite according to claim 1, which is characterized in that the synergistic flame retardant is anhydrous
Ammonium phosphomolybdate crystal.
9. flame-proof abrasion-resistant PBT composite according to claim 1, which is characterized in that the antioxidant is three (2,4- bis-
Tert-butyl) phenyl-phosphite, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters or 1,3,5- front threes
Base -2,4, the mixing of one or more of 6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene.
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| CN103756266A (en) * | 2013-12-20 | 2014-04-30 | 南通开普乐工程塑料有限公司 | Flame retardant glass fiber reinforced PBT (Polybutylene Terephthalate) composite material and preparation method thereof |
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| CN109294175A (en) | 2019-02-01 |
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