CN109161172A - A kind of low VOC antibacterial PBT composite and preparation method thereof - Google Patents
A kind of low VOC antibacterial PBT composite and preparation method thereof Download PDFInfo
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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
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract
The present invention relates to a kind of low VOC antibacterial PBT composites and preparation method thereof, are made of the component of following parts by weight: PBT is 60 parts -80 parts;Antibacterial agent is 4 parts -6 parts;It is 8 parts -10 parts that VOC, which improves master batch,;Antioxidant is 0.1 part -0.5 part;The antibacterial agent is that coral reef carries Ag+The antibacterial agent of type.Using -2 pyrrolidones of 1- methyl as stabilizer, 2- hydroxyl ethyl mercaptan is reducing agent, Ag+With -2 pyrrolidones of 1- methyl formed complex by stable dispersion in a solvent, Ag+Zeroth order is reduced to from positive monovalence by 2- hydroxyl ethyl mercaptan, and is constantly gathered under the synergistic effect of -2 pyrrolidones of 1- methyl on " core " on coral reef surface, the stone that grows into coral reef carries Ag+The antibacterial agent of type.
Description
Technical field
The invention belongs to technical field of polymer materials, a kind of low VOC antibacterial PBT composite and its preparation are particularly related to
Method.
Background technique
Polybutylene terephthalate (PBT) (PBT) is a kind of important thermoplastic material, is widely used in automobile, household electric
The fields such as device, mechanical fitting, office appliance and Communication Equipment.PBT material have it is light, nontoxic, odorless, good water absorption etc. is excellent
Point.In some specific material application fields, not only there is the requirement of anti-microbial property to PBT material, also has to VOC performance very high
Requirement, common PBT material can no longer meet this requirement.
Given this reason, the technical program innovation are made that a kind of anti-microbial property is excellent, and VOC PBT of good performance is compound
Material, this material not yet see report so far, this there is very important reality to anticipate the application of extension PBT composite
Justice.
Summary of the invention
The object of the present invention is to provide a kind of low VOC antibacterial PBT composites and preparation method thereof, to solve existing PBT
The anti-microbial property of material is not able to satisfy the problem of demand of some aspects.
The present invention is achieved by the following technical solutions:
A kind of low VOC antibacterial PBT composite, is made of the component of following parts by weight:
The antibacterial agent is that coral reef carries Ag+The antibacterial agent of type.
The antibacterial agent, specific preparation process is as follows:
(1) a certain amount of coral reef, the concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 16-20h under room temperature, must change
Property coral reef A;
(2) modified coral reef A is placed in Muffle furnace, heating reaction 10-14h, obtains modified coral in 500-700 DEG C
Reef B;
(3) a certain amount of modified coral reef B, deionized water, Klorvess Liquid are weighed, is stirred to react 6- at 30-40 DEG C
8h is washed so dry that be modified coral reef C;
(4) weigh a certain amount of modified coral reef C, deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl,
Silver nitrate solution is stirred to react 10-16h under room temperature, is filtered, washed, dries to obtain modified coral reef D;
(5) it will be modified the coral reef D dry 12-16h at 60-80 DEG C in a vacuum drying oven, roasted at 200-280 DEG C
6-10h is burnt, cooling grinding crosses 500 meshes, both obtains antibacterial agent.
The mass ratio of coral reef and the concentrated sulfuric acid in step (1) is (20-30): (120-160).
The mass ratio of modification coral reef B, deionized water and Klorvess Liquid in step (3) are (40-60): (180-
240): (6-8).
Modification coral reef C, deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl and nitric acid in step (4)
The mass ratio of silver-colored solution is (30-50);(120-160): (6-12): (3-5): (4-8).
The VOC improves master batch, and specific preparation process is as follows:
(1) weigh 60 parts of -80 parts of PBT, 6 parts of -12 parts of crushed crude pearlites, 4 parts of -8 parts of 4A type molecular sieves, 0.1 part -0.5 part it is anti-
Oxygen agent, 0.1 part of -0.3 part of oleamide are mixed and stirred for uniformly, obtaining mixture;
(2) by mixture obtained in step (1) from extruder extruding pelletization to get to VOC improve master batch.
Antioxidant described in step (1) is three (2,4- di-t-butyl) phenyl-phosphites, four [β-(3,5- di-t-butyl -4-
Hydroxy phenyl) propionic acid] pentaerythritol ester mixture, and mass ratio be 1:1.
Double screw extruder described in step (2) includes six humidity provinces sequentially arranged, 200~220 DEG C of area's temperature,
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, 200~280r/min of screw speed.
A kind of preparation method of low VOC antibacterial PBT composite, comprising the following steps:
(1) weigh 60 parts -80 parts of PBT, 4 parts of -6 parts of antibacterial agents, 8 parts of -10 parts of VOC improve master batches, 0.1 part -0.5 part it is anti-
Oxygen agent;
(2) by mixture extruding pelletization obtained in step (1) to get arrive PBT composite.
Double screw extruder in the step (2) includes six humidity provinces sequentially arranged, area's temperature 200~220
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, 200~280r/min of screw speed.
The beneficial effects of the present invention are:
1, using -2 pyrrolidones of 1- methyl as stabilizer, 2- hydroxyl ethyl mercaptan is reducing agent, Ag+With -2 pyrrolidines of 1- methyl
Ketone formed complex by stable dispersion in a solvent, Ag+Zeroth order is reduced to from positive monovalence by 2- hydroxyl ethyl mercaptan, and in 1- first
On " core " for constantly gathering coral reef surface under the synergistic effect of -2 pyrrolidones of base, the stone that grows into coral reef carries Ag+Type
Antibacterial agent.
2, the technical program improves master batch using a kind of VOC, it substantially improves the VOC performance of PBT composite.
3, PBT composite made from the technical program, anti-microbial property is excellent, and VOC is functional, has very big popularization
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.
Raw material used in the application name embodiment is as follows:
PBT (model 2002U), Polyplastics;Coral reef, the Lingshou wing reach mineral products processing factory;The concentrated sulfuric acid, Zouping day deer
Chemical Co., Ltd.;Deionized water, hundred Aurion of Beijing win Science and Technology Ltd.;Klorvess Liquid, Jiaozhuo dimension connection fine chemistry industry;2-
Hydroxyl ethyl mercaptan, Shanghai Jia Chen Chemical Co., Ltd.;- 2 pyrrolidones of 1- methyl, Shanghai Bang Jing Industrial Co., Ltd.;Silver nitrate
Solution, chemical products Co., Ltd among Zhengzhou hundred million;Crushed crude pearlite, Yishui, Shandong Yimeng perlite factory;4A type molecular sieve, Luoyang
Build imperial micro-nano new material;Oleamide, Haimen Zhong Teng Chemical Co., Ltd.;Antioxidant (model Irganox168,
Irganox1010, Irganox1330), Switzerland's Ciba.
Test equipment used in each embodiment of the application 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;101A-1 type digital display Electric heat oven, the holy glad science in Shanghai
Instrument Ltd..
The application provides a kind of low VOC antibacterial PBT composite, is made of the component of following parts by weight:
The antibacterial agent is that coral reef carries Ag+The antibacterial agent of type.
The antibacterial agent, specific preparation process is as follows:
(1) a certain amount of coral reef, the concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 16-20h under room temperature, must change
Property coral reef A;The mass ratio of coral reef and the concentrated sulfuric acid is (20-30): (120-160).
(2) modified coral reef A is placed in Muffle furnace, heating reaction 10-14h, obtains modified coral in 500-700 DEG C
Reef B;
(3) a certain amount of modified coral reef B, deionized water, Klorvess Liquid are weighed, is stirred to react 6- at 30-40 DEG C
8h is washed so dry that be modified coral reef C;The mass ratio of modified coral reef B, deionized water and Klorvess Liquid are (40-
60): (180-240): (6-8).
(4) weigh a certain amount of modified coral reef C, deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl,
Silver nitrate solution is stirred to react 10-16h under room temperature, is filtered, washed, dries to obtain modified coral reef D;Modified coral reef C,
Deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl and silver nitrate solution mass ratio be (30-50);(120-
160): (6-12): (3-5): (4-8).
(5) it will be modified the coral reef D dry 12-16h at 60-80 DEG C in a vacuum drying oven, roasted at 200-280 DEG C
6-10h is burnt, cooling grinding crosses 500 meshes, both obtains antibacterial agent.
The VOC improves master batch, and specific preparation process is as follows:
(1) weigh 60 parts of -80 parts of PBT, 6 parts of -12 parts of crushed crude pearlites, 4 parts of -8 parts of 4A type molecular sieves, 0.1 part -0.5 part it is anti-
Oxygen agent, 0.1 part of -0.3 part of oleamide are mixed and stirred for uniformly, obtaining mixture;
(2) by mixture obtained in step (1) from extruder extruding pelletization to get to VOC improve master batch.
Antioxidant in step (1) is three (2,4- di-t-butyl) phenyl-phosphites (abbreviation of BASF AG
) and four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters (abbreviation Irganox1010) Irganox168
Mixture, and mass ratio is 1:1.
Double screw extruder described in step (2) includes six humidity provinces sequentially arranged, 200~220 DEG C of area's temperature,
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, 200~280r/min of screw speed.
A kind of preparation method of low VOC antibacterial PBT composite, comprising the following steps:
(1) weigh 60 parts -80 parts of PBT, 4 parts of -6 parts of antibacterial agents, 8 parts of -10 parts of VOC improve master batches, 0.1 part -0.5 part it is anti-
Oxygen agent;
(2) by mixture extruding pelletization obtained in step (1) to get arrive PBT composite.
Double screw extruder in the step (2) includes six humidity provinces sequentially arranged, area's temperature 200~220
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, 200~280r/min of screw speed.
Embodiment 1
(1) 60 parts of PBT, 4 parts of antibacterial agents, 8 parts of VOC modified master batch, 0.1 part of Irganox1010 are weighed;
(2) by mixture extruding pelletization obtained in step (1) to get arrive PBT composite P1.
Wherein each area's temperature of double screw extruder and screw speed are respectively;One 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) 80 parts of PBT, 6 parts of antibacterial agents, 10 parts of VOC modified master batch, 0.2 part of Irganox1010,0.2 part are weighed
Irganox1330,0.1 part of Irganox168;
(2) by mixture extruding pelletization obtained in step (1) to get arrive PBT composite P2.
Wherein each area's temperature of double screw extruder and screw speed are respectively;One 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) 70 parts of PBT, 5 parts of antibacterial agents, 9 parts of VOC modified master batch, 0.2 part of Irganox1010,0.1 part are weighed
Irganox1330;
(2) by mixture extruding pelletization obtained in step (1) to get arrive PBT composite P3.
Wherein each area's temperature of double screw extruder and screw speed are respectively;One 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) 75 parts of PBT, 6 parts of antibacterial agents, 10 parts of VOC modified master batch, 0.2 part of Irganox1010,0.2 part are weighed
Irganox168;
(2) by mixture extruding pelletization obtained in step (1) to get arrive PBT composite P4.
Wherein each area's temperature of double screw extruder and screw speed are respectively;One 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) 65 parts of PBT, 6 parts of antibacterial agents, 9 parts of VOC modified master batch, 0.3 part of Irganox1010,0.1 part are weighed
Irganox1330;
(2) by mixture extruding pelletization obtained in step (1) to get arrive PBT composite P5.
Wherein each area's temperature of double screw extruder and screw speed are respectively;One 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) 70 parts of PBT, 0.3 part of Irganox1010,0.1 part of Irganox1330 is weighed to be mixed and stirred for uniformly, being mixed
Close material;
(2) by mixture extruding pelletization obtained in step (1) to get arrive PBT composite D1.
Wherein each area's temperature of double screw extruder and screw speed are respectively;One 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.
Performance test:
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:
As can be seen from the table, the anti-microbial property of embodiment 1-5, VOC performance will be better than comparative example 1.This illustrates we
The PBT of case will be good than the anti-microbial property of common PBT composite, VOC performance.
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 (10)
1. a kind of low VOC antibacterial PBT composite, which is characterized in that be made of the component of following parts by weight:
The antibacterial agent is that coral reef carries Ag+The antibacterial agent of type.
2. low VOC antibacterial PBT composite according to claim 1, which is characterized in that the antibacterial agent, it is specific to prepare
Steps are as follows:
(1) a certain amount of coral reef, the concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 16-20h under room temperature, obtain modified coral
Coral reef A;
(2) modified coral reef A is placed in Muffle furnace, heating reaction 10-14h, obtains modified coral reef in 500-700 DEG C
B;
(3) a certain amount of modified coral reef B, deionized water, Klorvess Liquid are weighed, 6-8h is stirred to react at 30-40 DEG C, washes
It washs so dry that be modified coral reef C;
(4) a certain amount of modified coral reef C, deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl, nitric acid are weighed
Silver-colored solution is stirred to react 10-16h under room temperature, is filtered, washed, dries to obtain modified coral reef D;
(5) it will be modified the coral reef D dry 12-16h at 60-80 DEG C in a vacuum drying oven, roast 6- at 200-280 DEG C
10h, cooling grinding, crosses 500 meshes, both obtains antibacterial agent.
3. low VOC antibacterial PBT composite according to claim 2, which is characterized in that the coral reef in step (1)
Mass ratio with the concentrated sulfuric acid is (20-30): (120-160).
4. low VOC antibacterial PBT composite according to claim 2, which is characterized in that the modification coral in step (3)
The mass ratio of reef B, deionized water and Klorvess Liquid are (40-60): (180-240): (6-8).
5. low VOC antibacterial PBT composite according to claim 2, which is characterized in that the modification coral in step (4)
Reef C, deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl and silver nitrate solution mass ratio be (30-50);
(120-160): (6-12): (3-5): (4-8).
6. low VOC antibacterial PBT composite according to claim 1, which is characterized in that the VOC improves master batch, specifically
Preparation step is as follows:
(1) weigh 60 parts of -80 parts of PBT, 6 parts of -12 parts of crushed crude pearlites, 4 parts of -8 parts of 4A type molecular sieves, 0.1 part of -0.5 part of antioxidant,
0.1 part of -0.3 part of oleamide is mixed and stirred for uniformly, obtaining mixture;
(2) by mixture obtained in step (1) from extruder extruding pelletization to get to VOC improve master batch.
7. low VOC antibacterial PBT composite according to claim 6, which is characterized in that antioxidant described in step (1)
For three (2,4- di-t-butyl) phenyl-phosphites, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters
Mixture, and mass ratio is 1:1.
8. low VOC antibacterial PBT composite according to claim 6, which is characterized in that twin-screw described in step (2)
Extruder includes six humidity provinces sequentially arranged, 200~220 DEG C of area's temperature, two 240~260 DEG C of area's temperature, three area's temperature
240~260 DEG C, 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, head temperature
240~260 DEG C, 200~280r/min of screw speed.
9. a kind of preparation method of low VOC antibacterial PBT composite, which comprises the following steps:
(1) 60 parts -80 parts of PBT, 4 parts of -6 parts of antibacterial agents, 8 parts of -10 parts of VOC are weighed and improves master batch, 0.1 part of -0.5 part of antioxygen
Agent;
(2) by mixture extruding pelletization obtained in step (1) to get arrive PBT composite.
10. the preparation method of low VOC antibacterial PBT composite according to claim 9, which is characterized in that the step
(2) double screw extruder in includes six humidity provinces sequentially arranged, 200~220 DEG C of area's temperature, and two area's temperature 240~
260 DEG C, 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 area's temperature 240~
260 DEG C, 240~260 DEG C of head temperature, 200~280r/min of screw speed.
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CN101300981A (en) * | 2008-05-15 | 2008-11-12 | 兰州大学 | Nano silver-carrying concave-convex stick anti-bacteria agent and preparation thereof |
CN103044861A (en) * | 2011-10-14 | 2013-04-17 | 合肥杰事杰新材料股份有限公司 | Antibacterial polybutylene terephthalate composition and preparation method thereof |
CN107400343A (en) * | 2017-09-15 | 2017-11-28 | 安徽江淮汽车集团股份有限公司 | A kind of fire-retardant scratch-resistant PBT composite and preparation method thereof |
CN107698876A (en) * | 2017-09-26 | 2018-02-16 | 武汉金发科技有限公司 | A kind of modified polypropene VOC extractants and its preparation method and application |
CN107936604A (en) * | 2017-12-04 | 2018-04-20 | 王文广 | One kind removes VOC masterbatch |
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CN101300981A (en) * | 2008-05-15 | 2008-11-12 | 兰州大学 | Nano silver-carrying concave-convex stick anti-bacteria agent and preparation thereof |
CN103044861A (en) * | 2011-10-14 | 2013-04-17 | 合肥杰事杰新材料股份有限公司 | Antibacterial polybutylene terephthalate composition and preparation method thereof |
CN107400343A (en) * | 2017-09-15 | 2017-11-28 | 安徽江淮汽车集团股份有限公司 | A kind of fire-retardant scratch-resistant PBT composite and preparation method thereof |
CN107698876A (en) * | 2017-09-26 | 2018-02-16 | 武汉金发科技有限公司 | A kind of modified polypropene VOC extractants and its preparation method and application |
CN107936604A (en) * | 2017-12-04 | 2018-04-20 | 王文广 | One kind removes VOC masterbatch |
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