CN108912325A - A kind of preparation method of antibacterial PA66 composite material - Google Patents
A kind of preparation method of antibacterial PA66 composite material Download PDFInfo
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- CN108912325A CN108912325A CN201810791475.5A CN201810791475A CN108912325A CN 108912325 A CN108912325 A CN 108912325A CN 201810791475 A CN201810791475 A CN 201810791475A CN 108912325 A CN108912325 A CN 108912325A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
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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
- C08K3/08—Metals
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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
- C08K3/08—Metals
- C08K2003/085—Copper
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to a kind of preparation methods of antibacterial PA66 composite material, are mixed by copper nitrate solution with ammonium hydroxide;It added N-methyl pyrrolidones and emulsifier fat alcohol polyethylene ether carries out ultrasonic disperse, while being continually fed into nitrogen, sodium borohydride is added;Reaction in product and PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydride reaction kettle is obtained into PA66 composite material.A kind of antimicrobial nano copper/PA66 material having been synthesized in this technology, the stability of nanometer copper particle can be improved using PA66 to the coating function of nano silver particles, extended the application range of antibacterial PA66 material, there is very big promotional value.
Description
Technical field
The invention belongs to technical field of polymer materials, particularly relate to a kind of preparation method of antibacterial PA66 composite material.
Background technique
For polyamide 66 (PA66) as common thermoplastic, application is very extensive.But with the development of science and technology,
Some specific fields, people have the requirement of anti-microbial property to PA66 material, and which greatly limits PA66 composite materials at these
Application on specific area.
The technical program has innovatively synthesized a kind of preparation method of antibacterial PA66 composite material, this method so far there is not yet
In report, this has very real meaning for the application range of extension PA66 composite material.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of antibacterial PA66 composite material, to solve PA66 certain specific
The problem of application in field is restricted.
The present invention is achieved by the following technical solutions:
A kind of preparation method of antibacterial PA66 composite material, includes the following steps:
(1) a certain amount of copper nitrate solution, ammonium hydroxide are weighed, the two is mixed to get solution A;
(2) N-methyl pyrrolidones was added in solution A and emulsifier fat alcohol polyethylene ether carries out ultrasonic disperse 2-
4h, while it being continually fed into nitrogen, it is warming up to 60-80 DEG C of reaction 1-3h, sodium borohydride is added and reacts 2-4h, obtains solution B;
(3) a certain amount of PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydride, solution B and deionized water are weighed;
By PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydrides, solution B are put into reaction kettle, are stirring evenly and then adding into deionization
Water is again stirring for uniformly;
(4) boosting is started to warm up after closed kettle cover, when temperature in the kettle is up to 210 DEG C, when pressure reaches 2.0MPa, heat-insulation pressure keeping
1-3h;
(5) pressure and temperature in kettle is adjusted, is 265 DEG C by temperature in the kettle heating, pressure is reduced to normal pressure, heat-insulation pressure keeping 2-
4h;
(6) stop heating, be passed through inert gas N2, start blowing when temperature in the kettle is lower than 150 DEG C and obtain PA66 composite wood
Material.
Copper nitrate solution and ammonium hydroxide mass ratio in step (1) are (20-30):(40-60).
Solution A in step (2), the mass ratio for crossing N-methyl pyrrolidones, fat alcohol polyethylene ether and sodium borohydride are
(60-80):(30-50):(1-3):(2-4).
The quality of PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydride, solution B in step (3) and deionized water
Than for (80-100):(0.1-0.3):(0.3-0.5):(10-16):(100-120).
The beneficial effects of the invention are as follows:
1, a kind of antimicrobial nano copper/PA66 material has been synthesized in this technology, has been made using cladding of the PA66 to nano silver particles
With the stability of nanometer copper particle can be improved.
2, a kind of antimicrobial nano copper/PA66 material made from this technology, has no document and patent report before, extends anti-
The application range of bacterium PA66 material 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.
Raw material used in each embodiment of the application is as follows:
Copper nitrate solution, Guangzhou Wei Long Chemical Co., Ltd.;Ammonium hydroxide, Taixing Su Cheng Chemical Co., Ltd.;Cross N-methyl pyrrole
Pyrrolidone, Zhejiang Cixi Sai Side Environmental Protection Technology Co., Ltd;Fat alcohol polyethylene ether, the prosperous Landtek skill in Xingtai;PA66 salt, flat-top
Shan Shenma engineering plastics Co., Ltd;Concentrated phosphoric acid, Shenyang is from Chemical Co., Ltd. of section;3,3,4,4- bibenzene tetracarboxylic dianhydrides, it is real
Room is tested to provide for oneself;Sodium borohydride, the good Chemical Co., Ltd. in Zhengzhou hundred.
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.
Embodiment 1
(1) 200g copper nitrate solution, 400g ammonium hydroxide are weighed, the two is mixed to get solution A.
(2) 300g is added in 600g solution A and crosses N-methyl pyrrolidones and the progress of 10g emulsifier fat alcohol polyethylene ether
Ultrasonic disperse 2h, while it being continually fed into nitrogen, 60 DEG C of reaction 1h are warming up to, 20g sodium borohydride is added and reacts 2h, obtains solution B.
(3) 800gPA66 salt, 1g concentrated phosphoric acid, 3g3,3,4,4- bibenzene tetracarboxylic dianhydride, 100g solution B, 1.0kg is weighed to go
Ionized water.By PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydrides, solution B are put into reaction kettle, after mixing evenly plus
Enter deionized water, is again stirring for uniformly.
(4) boosting is started to warm up after closed kettle cover, when temperature in the kettle is up to 210 DEG C, when pressure reaches 2.0MPa, heat-insulation pressure keeping
1h。
(5) pressure and temperature in kettle is adjusted, is 265 DEG C by temperature in the kettle heating, pressure is reduced to normal pressure, heat-insulation pressure keeping
2h。
(6) stop heating, be passed through inert gas N2, start blowing when temperature in the kettle is lower than 150 DEG C and obtain Nanometer Copper/PA66
Material P1.
Embodiment 2
(1) 300g copper nitrate solution, 600g ammonium hydroxide are weighed, the two is mixed to get solution A.
(2) 500g is added in 800g solution A and crosses N-methyl pyrrolidones and the progress of 30g emulsifier fat alcohol polyethylene ether
Ultrasonic disperse 4h, while it being continually fed into nitrogen, 80 DEG C of reaction 3h are warming up to, 40g sodium borohydride is added and reacts 4h, obtains solution B.
(3) 1.0kgPA66 salt, 3g concentrated phosphoric acid, 5g3,3,4,4- bibenzene tetracarboxylic dianhydride, 160g solution B, 1.2kg are weighed
Deionized water.By PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydrides, solution B are put into reaction kettle, after mixing evenly
Deionized water is added, is again stirring for uniformly.
(4) boosting is started to warm up after closed kettle cover, when temperature in the kettle is up to 210 DEG C, when pressure reaches 2.0MPa, heat-insulation pressure keeping
3h。
(5) pressure and pressure in kettle are adjusted, is 265 DEG C by temperature in the kettle heating, pressure is reduced to normal pressure, heat-insulation pressure keeping
4h。
(6) stop heating, be passed through inert gas N2, start blowing when temperature in the kettle is lower than 150 DEG C and obtain Nanometer Copper/PA66
Material P2.
Embodiment 3
(1) 250g copper nitrate solution, 500g ammonium hydroxide are weighed, the two is mixed to get solution A.
(2) 400g is added in 700g solution A and crosses N-methyl pyrrolidones and the progress of 20g emulsifier fat alcohol polyethylene ether
Ultrasonic disperse 3h, while it being continually fed into nitrogen, 70 DEG C of reaction 2h are warming up to, 40g sodium borohydride is added and reacts 3h, obtains solution B.
(3) 900gPA66 salt, 2g concentrated phosphoric acid, 4g3,3,4,4- bibenzene tetracarboxylic dianhydride, 130g solution B, 1.1kg is weighed to go
Ionized water.By PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydrides, solution B are put into reaction kettle, after mixing evenly plus
Enter deionized water, is again stirring for uniformly.
(4) boosting is started to warm up after closed kettle cover, when temperature in the kettle is up to 210 DEG C, when pressure reaches 2.0MPa, heat-insulation pressure keeping
2h。
(5) pressure and temperature in kettle is adjusted, is 265 DEG C by temperature in the kettle heating, pressure is reduced to normal pressure, heat-insulation pressure keeping
3h。
(6) stop heating, be passed through inert gas N2, start blowing when temperature in the kettle is lower than 150 DEG C and obtain Nanometer Copper/PA66
Material P3.
Embodiment 4
(1) 240g copper nitrate solution, 440g ammonium hydroxide are weighed, the two is mixed to get solution A.
(2) 320g is added in 770g solution A and crosses N-methyl pyrrolidones and the progress of 15g emulsifier fat alcohol polyethylene ether
Ultrasonic disperse 2h, while it being continually fed into nitrogen, 65 DEG C of reaction 1h are warming up to, 28g sodium borohydride is added and reacts 2h, obtains solution B.
(3) 880gPA66 salt, 2g concentrated phosphoric acid, 4g3,3,4,4- bibenzene tetracarboxylic dianhydride, 120g solution B, 1.2kg is weighed to go
Ionized water.By PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydrides, solution B are put into reaction kettle, after mixing evenly plus
Enter deionized water, is again stirring for uniformly.
(4) boosting is started to warm up after closed kettle cover, when temperature in the kettle is up to 210 DEG C, when pressure reaches 2.0MPa, heat-insulation pressure keeping
3h。
(5) pressure and temperature in kettle is adjusted, is 265 DEG C by temperature in the kettle heating, pressure is reduced to normal pressure, heat-insulation pressure keeping
2h。
(6) stop heating, be passed through inert gas N2, start blowing when temperature in the kettle is lower than 150 DEG C and obtain Nanometer Copper/PA66
Material P4.
Embodiment 5
(1) 260g copper nitrate solution, 460g ammonium hydroxide are weighed, the two is mixed to get solution A.
(2) 420g is added in 620g solution A and crosses N-methyl pyrrolidones and the progress of 24g emulsifier fat alcohol polyethylene ether
Ultrasonic disperse 2h, while it being continually fed into nitrogen, 65 DEG C of reaction 1h are warming up to, 35g sodium borohydride is added and reacts 4h, obtains solution B.
(3) 990gPA66 salt, 2g concentrated phosphoric acid, 4g3,3,4,4- bibenzene tetracarboxylic dianhydride, 150g solution B, 1.2kg is weighed to go
Ionized water.By PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydrides, solution B are put into reaction kettle, after mixing evenly plus
Enter deionized water, is again stirring for uniformly.
(4) boosting is started to warm up after closed kettle cover, when temperature in the kettle is up to 210 DEG C, when pressure reaches 2.0MPa, heat-insulation pressure keeping
1h。
(5) pressure and temperature in kettle is adjusted, is 265 DEG C by temperature in the kettle heating, pressure is reduced to normal pressure, heat-insulation pressure keeping
4h。
(6) stop heating, be passed through inert gas N2, start blowing when temperature in the kettle is lower than 150 DEG C and obtain Nanometer Copper/PA66
Material P5.
Comparative example 1
(1) 65 parts of PA66,0.1 part of Irganox1010,0.2 part of Irganox168 is weighed to be mixed and stirred for uniformly, being mixed
Close material;
(2) by mixture extruding pelletization obtained in step (1) to get arrive PA66 composite material D1.
Wherein each area's temperature of double screw extruder and screw speed are respectively:One 215 DEG C of area's temperature, two 265 DEG C of area's temperature,
Three 265 DEG C of area's temperature, four 265 DEG C of area's temperature, five 265 DEG C of area's temperature, six 265 DEG C of area's temperature, 265 DEG C of head temperature;Screw rod turns
Fast 255r/min.
Performance test:
Batten test is made with injection molding machine in PA66 composite material prepared by above-described embodiment 1-5 and comparative example 1, tests number
According to such as following table:
It can also be seen that the anti-microbial property of embodiment 1-5 will be better than comparative example 1 from table, this is compound for extension PA66
The application field of material, 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 (4)
1. a kind of preparation method of antibacterial PA66 composite material, which is characterized in that include the following steps:
(1) a certain amount of copper nitrate solution, ammonium hydroxide are weighed, the two is mixed to get solution A;
(2) N-methyl pyrrolidones was added in solution A and emulsifier fat alcohol polyethylene ether carries out ultrasonic disperse 2-4h, together
When be continually fed into nitrogen, be warming up to 60-80 DEG C of reaction 1-3h, sodium borohydride be added and reacts 2-4h, obtains solution B;
(3) a certain amount of PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydride, solution B and deionized water are weighed;It will
PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydrides, solution B are put into reaction kettle, are stirring evenly and then adding into deionization
Water is again stirring for uniformly;
(4) boosting is started to warm up after closed kettle cover, when temperature in the kettle is up to 210 DEG C, when pressure reaches 2.0MPa, heat-insulation pressure keeping 1-
3h;
(5) pressure and temperature in kettle is adjusted, is 265 DEG C by temperature in the kettle heating, pressure is reduced to normal pressure, heat-insulation pressure keeping 2-4h;
(6) stop heating, be passed through inert gas N2, start blowing when temperature in the kettle is lower than 150 DEG C and obtain PA66 composite material.
2. the preparation method of antibacterial PA66 composite material according to claim 1, which is characterized in that the nitre in step (1)
Sour copper solution and ammonium hydroxide mass ratio are (20-30):(40-60).
3. the preparation method of antibacterial PA66 composite material according to claim 1, which is characterized in that molten in step (2)
Liquid A, the mass ratio for crossing N-methyl pyrrolidones, fat alcohol polyethylene ether and sodium borohydride are (60-80):(30-50):(1-3):
(2-4)。
4. the preparation method of antibacterial PA66 composite material according to claim 1, which is characterized in that in step (3)
PA66 salt, concentrated phosphoric acid, 3,3,4,4- bibenzene tetracarboxylic dianhydride, solution B and deionized water mass ratio be (80-100):(0.1-
0.3):(0.3-0.5):(10-16):(100-120).
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111560170A (en) * | 2019-02-14 | 2020-08-21 | 上海凯赛生物技术股份有限公司 | Antibacterial polyamide and preparation method and application thereof |
CN113273580A (en) * | 2021-06-07 | 2021-08-20 | 广东顾纳凯材料科技有限公司 | Antibacterial agent and preparation method thereof, antibacterial polyolefin composite material and preparation method thereof |
CN113501997A (en) * | 2021-07-22 | 2021-10-15 | 安徽江淮汽车集团股份有限公司 | Preparation method and application of antibacterial agent |
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CN113273580A (en) * | 2021-06-07 | 2021-08-20 | 广东顾纳凯材料科技有限公司 | Antibacterial agent and preparation method thereof, antibacterial polyolefin composite material and preparation method thereof |
CN113501997A (en) * | 2021-07-22 | 2021-10-15 | 安徽江淮汽车集团股份有限公司 | Preparation method and application of antibacterial agent |
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Application publication date: 20181130 |