CN109181200A - A kind of high-performance refractory AES composite material and preparation method thereof - Google Patents
A kind of high-performance refractory AES composite material and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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Abstract
Composed of the following components by weight the present invention relates to a kind of high-performance refractory AES composite material and preparation method: AES is 80 parts -100 parts；Fire-retardant compounded mix is 16 parts -18 parts；Antioxidant is 0.1 part -0.5 part；Fire-retardant compounded mix is modified paligorskite.AES composite material produced by the present invention only adds 16 parts of -18 parts of fire-retardant compounded mixs, has just achieved the effect that V-0, and it reduce the costs of fire-retardant AES, has very big promotional value.
Description
Technical field
The invention belongs to technical field of polymer materials, a kind of high-performance refractory AES composite material and its system are particularly related to
Preparation Method.
Background technique
AES is a kind of engineering plastics of high comprehensive performance, and good stability of the dimension, insulating properties is good, oil resistant, processing and forming
Performance is relatively good, but its flame retardant property is general, and which greatly limits AES composite material answering on some fire proofing fields
With.
The technical program innovation is modified AES using a kind of novel flame-retardant compounded mix, and a kind of high-performance is finally made
Fire-retardant AES composite material and preparation method thereof, pertinent literature are simultaneously not found in report, this is with very important realistic meaning.
Summary of the invention
The object of the present invention is to provide a kind of high-performance refractory AES composite materials and preparation method thereof, to solve existing skill
AES composite material in art.
The present invention is achieved by the following technical solutions:
A kind of high-performance refractory AES composite material, composed of the following components by weight:
80 parts -100 parts of AES；
16 parts -18 parts of fire-retardant compounded mix；
0.1 part -0.5 part of antioxidant；
The fire-retardant compounded mix is modified paligorskite.
The preparation method of the modified paligorskite, comprising the following steps:
1) a certain amount of palygorskite, deionized water, phosphoric acid are weighed, by palygorskite, deionized water in 60- in reaction vessels
80 DEG C of water-bath 3-5h, then phosphoric acid is slowly added dropwise, 2-4h is reacted, solution A is obtained；
(2) solution A filtered, washed, dried, ground, crossed 500 meshes and obtain modified paligorskite M1；
(3) a certain amount of modified paligorskite M1, deionized water, potassium pyrophosphate, benzyltrimethylammonium bromide are weighed, will be modified
Palygorskite, deionized water, in 70-90 DEG C of water-bath 1-3h, then add potassium pyrophosphate, benzyl trimethyl bromine in reaction vessels
Change ammonium, reacts 6-8h, obtain solution B；
(4) solution B filtered, washed, dried, ground, crossed 500 meshes and obtain modified paligorskite M2；
(5) a certain amount of modified paligorskite M2, tetraphenyl resorcinol diphosphate, zinc borate are weighed, by them in height
Fast blender is sufficiently mixed, and is stirred 40-60min, is cooled to room temperature, has both obtained fire-retardant compounded mix modified paligorskite.
The mass ratio of palygorskite, deionized water, phosphoric acid in step (1) is (60-80): (120-180): (10-20).
The mass ratio of modified paligorskite M1, deionized water, potassium pyrophosphate, benzyltrimethylammonium bromide in step (3) is
(40-60): (160-200): (1-3): (4-6).
The mass ratio of modified paligorskite M2, tetraphenyl resorcinol diphosphate, zinc borate in step (5) are (30-
50): (10-20)；(5-7).
The temperature of high-speed mixer in step (5) is 70-90 DEG C, revolving speed 240-320r/min.
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- trimethyl -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene
One of (Irganox1330) or it is a variety of.
A kind of preparation method of high-performance refractory AES composite material, includes the following steps:
(1) 80 parts -100 parts of AES, 16 parts -18 parts fire-retardant compounded mixs, 0.1 part of -0.5 part of antioxidant are weighed, mixing is simultaneously
It stirs evenly, obtains mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES composite material.
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 AES composite material is arrived, wherein the double screw extruder includes six humidity provinces sequentially arranged, area's temperature
190~210 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 area's temperature
240~260 DEG C of degree, six 240~260 DEG C of area's temperature, 240~260 DEG C of head temperature；200~260r/min of screw speed.
The medicine have the advantages that
(1) by phosphoric acid to paligorskite modified, H+Instead of Mg+, Si-O-Mg-O-Si key becomes Si-O-H key, surface
Product increases, and is conducive to palygorskite and scatter in threadiness, palygorskite is preferably dispersed in AES.
(2) benzyltrimethylammonium bromide, potassium pyrophosphate are entered between palygorskite crystal layer with suction type, increase slope thread
The interlamellar spacing of stone improves palygorskite and the compatibility of AES, to improve the mechanical property of AES composite material.
(3) AES composite material produced by the present invention only adds 16 parts of -18 parts of fire-retardant compounded mixs, has just reached V-0
Effect there is very big promotional value it reduce the cost of fire-retardant AES.
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.
Raw material used in embodiments herein is as follows:
AES (model SK50), Japanese UMG；Palygorskite, Lingshou Jiade mining industry processing factory；Phosphoric acid, the auspicious chemical industry of Linyi China are limited
Company；Potassium pyrophosphate, Hangzhou with and Chemical Co., Ltd.；Benzyltrimethylammonium bromide, Hubei Ju Sheng Science and Technology Ltd.；Four benzene
Base resorcinol diphosphate, Hangzhou great Yang Chemical Co., Ltd.；Zinc borate, granary Heng Ze chemical industry Co., Ltd., Factory；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.
The present invention provides a kind of high-performance refractory AES composite material, composed of the following components by weight:
80 parts -100 parts of AES；
16 parts -18 parts of fire-retardant compounded mix；
0.1 part -0.5 part of antioxidant；
Fire-retardant compounded mix is modified paligorskite.
The preparation method of modified paligorskite, comprising the following steps:
1) a certain amount of palygorskite, deionized water, phosphoric acid are weighed, by palygorskite, deionized water in 60- in reaction vessels
80 DEG C of water-bath 3-5h, then phosphoric acid is slowly added dropwise, 2-4h is reacted, solution A is obtained；Palygorskite, deionized water, phosphoric acid mass ratio
For (60-80): (120-180): (10-20).
(2) solution A filtered, washed, dried, ground, crossed 500 meshes and obtain modified paligorskite M1；
(3) a certain amount of modified paligorskite M1, deionized water, potassium pyrophosphate, benzyltrimethylammonium bromide are weighed, will be modified
Palygorskite, deionized water, in 70-90 DEG C of water-bath 1-3h, then add potassium pyrophosphate, benzyl trimethyl bromine in reaction vessels
Change ammonium, reacts 6-8h, obtain solution B；Modified paligorskite M1, deionized water, potassium pyrophosphate, benzyltrimethylammonium bromide mass ratio
For (40-60): (160-200): (1-3): (4-6).
(4) solution B filtered, washed, dried, ground, crossed 500 meshes and obtain modified paligorskite M2；
(5) a certain amount of modified paligorskite M2, tetraphenyl resorcinol diphosphate, zinc borate are weighed, by them in height
Fast blender is sufficiently mixed, and is stirred 40-60min, is cooled to room temperature, has both obtained fire-retardant compounded mix modified paligorskite；Modified slope
Thread stone M2, tetraphenyl resorcinol diphosphate, zinc borate mass ratio be (30-50): (10-20)；(5-7)；High-speed stirred
The temperature of machine is 70-90 DEG C, revolving speed 240-320r/min.
Antioxidant is three (2,4- di-t-butyl) phenyl-phosphites (Irganox168), four [β-(3,5- di-t-butyl -4-
Hydroxy phenyl) propionic acid] pentaerythritol ester (Irganox1010) or 1,3,5- trimethyl -2,4,6- (3,5- di-t-butyl -4- hydroxyl
Base benzyl) one of benzene (I rganox1330) or a variety of.
A kind of preparation method of high-performance refractory AES composite material, includes the following steps:
(1) 80 parts -100 parts of AES, 16 parts -18 parts fire-retardant compounded mixs, 0.1 part of -0.5 part of antioxidant are weighed, mixing is simultaneously
It stirs evenly, obtains mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES composite material.
Step (2) specifically: put into the hopper of double screw extruder to squeeze out mixture obtained in step (1) and make
Grain is to get arriving AES composite material, wherein and double screw extruder includes six humidity provinces sequentially arranged, area's temperature 190~
210 DEG C, 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 area's temperature 240~
260 DEG C, six 240~260 DEG C of area's temperature, 240~260 DEG C of head temperature；200~260r/min of screw speed.
Embodiment 1
(1) 80 parts of AES, 16 parts of fire-retardant compounded mixs, 0.1 part of Irganox1010 are weighed, is mixed and stirred for uniformly, obtaining
Mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES composite material P1.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 190 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 AES, 18 parts of fire-retardant compounded mixs, 0.1 part of Irganox168,0.2 part of Irganox1010,0.2 are weighed
Part Irganox1330 is mixed and stirred for uniformly, obtaining mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES composite material P2.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 210 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 260r/min.
Embodiment 3
(1) 90 parts of AES, 17 parts of fire-retardant compounded mixs, 0.1 part of Irganox168,0.2 part of Irganox1010 are weighed, is mixed
And stir evenly, obtain mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES composite material P3.
Wherein each area's temperature of double screw extruder and screw speed are respectively as follows: 200 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 230r/min.
Embodiment 4
(1) 95 parts of AES, 16 parts of fire-retardant compounded mixs, 0.1 part of Irganox168,0.1 part of Irganox1330 are weighed, is mixed
And stir evenly, obtain mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES composite material 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 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.
Embodiment 5
(1) 85 parts of AES, 18 parts of fire-retardant compounded mixs, 0.1 part of Irganox168,0.3 part of Irganox1330 are weighed, is mixed
And stir evenly, obtain mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES composite material 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 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 240r/min.
Comparative example 1
(1) 85 parts of AES, 0.1 part of Irganox168,0.3 part of Irganox1330 are weighed, is mixed and stirred for uniformly, being mixed
Close material；
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES composite material D1.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 190 DEG C, the
The temperature of two humidity provinces is 250 DEG C, and the temperature of third humidity province is 250 DEG C, and the temperature of the 4th humidity province is 250 DEG C, the 5th temperature
The temperature for spending area is 250 DEG C, and the temperature of the 6th humidity province is 250 DEG C, and the head temperature of double screw extruder is 250 DEG C, screw rod
Revolving speed is 220r/min.
Comparative example 2
(1) 85 parts of AES, 14 parts of APP, 4 parts of PER, 0.1 part of Irganox168,0.3 part of Irganox1330 are weighed, mixing is simultaneously
It stirs evenly, obtains mixture；
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES composite material D2.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 190 DEG C, the
The temperature of two humidity provinces is 250 DEG C, and the temperature of third humidity province is 250 DEG C, and the temperature of the 4th humidity province is 250 DEG C, the 5th temperature
The temperature for spending area is 250 DEG C, and the temperature of the 6th humidity province is 250 DEG C, and the head temperature of double screw extruder is 250 DEG C, screw rod
Revolving speed is 220r/min.
Performance test:
Batten test, test is made with injection molding machine in AES composite material prepared by above-described embodiment 1-5 and comparative example 1-2
Data are as follows:
Each embodiment of table 1 and the test of comparative example properties of product
As can be seen from the above table:
1. embodiment 1-5, compared with comparative example 1, mechanical property, flame retardant property have different degrees of raising, this explanation adds
Add the fire-retardant compounded mix in the technical program, mechanical property, the flame retardant property of AES composite material are all improved.
2. embodiment 1-5 is compared with comparative example 2 (being added to 18 parts of fire retardants), mechanical property, flame retardant property are different
The raising of degree, this illustrates the fire retardant for adding same aliquot, and the fire-retardant compounded mix flame retardant property of the technical program is more excellent, this
If also explanation wants to reach same flame retardant effect, fire-retardant filler number needed for the AES composite material of the technical program is lower, reaches
This purpose of drop.
This can satisfy the fields such as IT, communication, electronics, automobile to engineering for the application field of extension AES composite material
The requirement of part.
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 high-performance refractory AES composite material, which is characterized in that composed of the following components by weight:
80 parts -100 parts of AES；
16 parts -18 parts of fire-retardant compounded mix；
0.1 part -0.5 part of antioxidant；
The fire-retardant compounded mix is modified paligorskite.
2. high-performance refractory AES composite material according to claim 1, which is characterized in that the system of the modified paligorskite
Preparation Method, comprising the following steps:
(1) a certain amount of palygorskite, deionized water, phosphoric acid are weighed, by palygorskite, deionized water in 60-80 in reaction vessels
DEG C water-bath 3-5h, then phosphoric acid is slowly added dropwise, 2-4h is reacted, solution A is obtained；
(2) solution A filtered, washed, dried, ground, crossed 500 meshes and obtain modified paligorskite M1；
(3) a certain amount of modified paligorskite M1, deionized water, potassium pyrophosphate, benzyltrimethylammonium bromide are weighed, by modified slope thread
Stone, deionized water, in 70-90 DEG C of water-bath 1-3h, then add potassium pyrophosphate, benzyltrimethylammonium bromide in reaction vessels,
6-8h is reacted, solution B is obtained；
(4) solution B filtered, washed, dried, ground, crossed 500 meshes and obtain modified paligorskite M2；
(5) a certain amount of modified paligorskite M2, tetraphenyl resorcinol diphosphate, zinc borate are weighed, by them in high-speed stirring
The machine of mixing is sufficiently mixed, and is stirred 40-60min, is cooled to room temperature, has both obtained fire-retardant compounded mix modified paligorskite.
3. high-performance refractory AES composite material according to claim 2, which is characterized in that palygorskite in step (1),
Deionized water, phosphoric acid mass ratio be (60-80): (120-180): (10-20).
4. high-performance refractory AES composite material according to claim 2, which is characterized in that the modification slope thread in step (3)
Stone M1, deionized water, potassium pyrophosphate, benzyltrimethylammonium bromide mass ratio be (40-60): (160-200): (1-3): (4-
6)。
5. high-performance refractory AES composite material according to claim 2, which is characterized in that the modification slope thread in step (5)
Stone M2, tetraphenyl resorcinol diphosphate, zinc borate mass ratio be (30-50): (10-20)；(5-7).
6. high-performance refractory AES composite material according to claim 2, which is characterized in that the high-speed stirred in step (5)
The temperature of machine is 70-90 DEG C, revolving speed 240-320r/min.
7. high-performance refractory AES composite material according to claim 1, which is characterized in that the antioxidant is three (2,4-
Di-t-butyl) phenyl-phosphite, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters or 1,3,5- front three
One of base -2,4,6- (3,5- di-t-butyl -4- hydroxyphenylmethyl) benzene (Irganox1330) is a variety of.
8. a kind of preparation method of high-performance refractory AES composite material, which comprises the steps of:
(1) AES, 16 parts -18 parts fire-retardant compounded mixs, 0.1 part of -0.5 part of antioxidant for weighing 80 parts -100 parts, are mixed and stirred for
Uniformly, mixture is obtained；
(2) by mixture extruding pelletization obtained in step (1) to get arrive AES composite material.
9. the preparation method of high-performance refractory AES composite material according to claim 8, which is characterized in that the step
(2) specifically: mixture obtained in step (1) is put into the hopper of double screw extruder extruding pelletization to get to AES
Composite material, wherein the double screw extruder includes six humidity provinces sequentially arranged, 190~210 DEG C of area's temperature, and 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 240~260 DEG C of area's temperature, six
240~260 DEG C of area's temperature, 240~260 DEG C of head temperature；200~260r/min of screw speed.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114410058A (en) * | 2022-03-29 | 2022-04-29 | 山东祥龙新材料股份有限公司 | Flame-retardant composite material for safety helmet and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106479071A (en) * | 2016-10-21 | 2017-03-08 | 安徽江淮汽车集团股份有限公司 | A kind of fire-retardant PS composite and preparation method thereof |
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2018
- 2018-09-20 CN CN201811100603.3A patent/CN109181200A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106479071A (en) * | 2016-10-21 | 2017-03-08 | 安徽江淮汽车集团股份有限公司 | A kind of fire-retardant PS composite and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114410058A (en) * | 2022-03-29 | 2022-04-29 | 山东祥龙新材料股份有限公司 | Flame-retardant composite material for safety helmet and preparation method thereof |
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Address after: 230601 No. 99 Ziyun Road, Hefei Economic and Technological Development Zone, Anhui Province Applicant after: Anhui Jianghuai Automobile Group Limited by Share Ltd Address before: 230601 No. 669 Shixin Road, Taohua Industrial Park, Hefei City, Anhui Province Applicant before: Anhui Jianghuai Automobile Group Limited by Share Ltd |
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Application publication date: 20190111 |
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