CN108946699A - A kind of preparation method of modified fullerenes material - Google Patents

A kind of preparation method of modified fullerenes material Download PDF

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CN108946699A
CN108946699A CN201810792188.6A CN201810792188A CN108946699A CN 108946699 A CN108946699 A CN 108946699A CN 201810792188 A CN201810792188 A CN 201810792188A CN 108946699 A CN108946699 A CN 108946699A
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fullerene
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deionized water
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CN108946699B (en
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刘凯
喻春凤
吴露露
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Anhui Jianghuai Automobile Group Corp
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    • C01B32/152—Fullerenes
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
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    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K2201/017—Additives being an antistatic agent
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Abstract

The present invention relates to a kind of preparation methods of modified fullerenes material, by nano-TiO2After being handled with argon plasma, nano-TiO can be reduced2Surface can, make it easier to be uniformly dispersed, be not susceptible to agglomeration；And utilize the nano-TiO of modified fullerenes load2、La3+The antibiotic property that ABS composite material can be improved well, promotes the function of the antistatic property of PBT, is greatly improved polyolefine material antibiotic property obtained and antistatic property all, has the great significance for popularization.

Description

A kind of preparation method of modified fullerenes material
Technical field
The invention belongs to technical field of polymer materials, particularly relate to a kind of preparation method of modified fullerenes material.
Background technique
Many scholars have been caused by the antibacterial antistatic material for adding suitable antibacterial agent, prepared by antistatic agent Extensive concern, this functional material has the function of antibacterial antistatic.A kind of modified fullerenes material has been made in applicant, uses It carrys out improved polyalkene, can improve anti-microbial property, the antistatic property of polyolefin, and this fullerene-based material is not yet seen so far Report, this has very important realistic meaning for the application of extension fullerene-based material.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of modified fullerenes material, to improve the antibiotic property of polyolefin Energy, antistatic property.
The present invention is achieved by the following technical solutions:
A kind of preparation method of modified fullerenes material, comprising the following steps:
(1) a certain amount of nano-TiO is weighed2, dehydrated alcohol, by nano-TiO2It is placed in sonic oscillation 8- in dehydrated alcohol 12min；
(2) nano-TiO by step (1) after alcohol treatment2After drying, by the nano-TiO2It is put into plasma chamber, It is passed through argon plasma, 20-24min is reacted, obtains modified Nano TiO2；
(3) a certain amount of modified Nano TiO is weighed2, deionized water, LaCl3·7H2O, polyacrylamide places them into 3-5h is vibrated in ultrasonic oscillation instrument, obtains solution A；
(4) a certain amount of fullerene, ZnCl3 solution, deionized water are weighed, fullerene is pulverized, fullerene powder, ZnCl3 solution, deionized water, which are put into ultrasonic oscillation instrument, vibrates 4-6h, filtering, so dry that carry zinc fullerene；
(5) zinc fullerene will be carried to be added into solution A, addition HCl solution adjusts pH value to neutrality, stirs at 60-80 DEG C 3-5h is reacted, filters, is dry, grinding to obtain modified fullerenes.
The mass ratio of nano TiO 2 and dehydrated alcohol in step (1) is (20-30): (160-240).
Modified Nano TiO2, deionized water, LaCl in step (3)3·7H2The mass ratio of O and polyacrylamide is (40- 60): (200-240): (20-28): (10-16).
Fullerene, ZnCl3 solution in step (4) and the mass ratio of deionized water are (30-40): (8-12): (100- 160)。
The beneficial effects of the present invention are:
1, by nano-TiO2After being handled with argon plasma, nano-TiO can be reduced2Surface can, it is equal to make it easier to dispersion It is even, it is not susceptible to agglomeration.
2, the effect of modified fullerenes mainly has: the nano-TiO that 1. it is loaded2、La3+It is compound ABS can be improved well The antibiotic property of material；2. fullerene can promote the antistatic property of PBT, modified fullerenes made from this technology have both antibacterial, Anti-static function.
3, polyolefine material antibiotic property and antistatic property made from the modified fullerenes made from this technology all obtain Very big improvement, has the great significance for popularization.
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 present embodiments is as follows:
PBT (model 2002U), Polyplastics；PP (model Z30S), Maoming Petrochemical；PE (model 5070), Panjin ethylene； PA6 (model C M1017), toray；PET (model 008L), Canadian Aclo；Fullerene, Puyang Yongxin fullerene science and technology Co., Ltd, nano TiO 2, Beijing Deco island Science and Technology Ltd.；Dehydrated alcohol, Xuzhou base chemical industry forever；Deionized water, Hefei Jing Chun company；Polyacrylamide, Henan is logical to reach Environmental Protection Technology Co., Ltd long；LaCl3·7H2O, triumphant material in Jining；ZnCl3 Solution, Weifang Hengfeng chemical industry.
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.
In present embodiments, need to adjust pH value using HCl solution to neutrality, in this application, for HCl The concentration of solution, whether mass concentration or volumetric concentration adjust pH value as long as can be realized, without limiting Will not have an impact to the realization of technical solution.
Embodiment 1
(1) 200g nano-TiO is weighed2, 1.6kg dehydrated alcohol, by nano-TiO2It is placed in sonic oscillation in dehydrated alcohol 8min。
(2) after drying up, by nano-TiO2It is put into plasma chamber, is passed through argon plasma, react 20min, obtain modification Nano-TiO2。
(3) 400g modified Nano TiO is weighed2, 2.0kg deionized water, 200gLaCl3·7H2O, 100g polyacrylamide, It places them into ultrasonic oscillation instrument and vibrates 3h, obtain solution A.
(4) 300g fullerene, 80gZnCl3 solution, 1kg deionized water are weighed, fullerene is pulverized, fullerene Powder, ZnCl3 solution, deionized water, which are put into ultrasonic oscillation instrument, vibrates 4h, filtering, so dry that carry zinc fullerene.
(5) zinc fullerene will be carried to be added into solution A, addition HCl solution adjusts pH value to neutrality, is stirred to react at 60 DEG C 3h is filtered, is dry, grinding to obtain modified fullerenes P1.
Application examples 1
It takes 6 parts of P1 to be added in 94 parts of polypropylene (PP), stirs 10min through high mixer, be subsequently added into double screw extruder Middle carry out blending extrusion, obtains PP composite material X1.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 170 DEG C, the The temperature of two humidity provinces is 220 DEG C, and the temperature of third humidity province is 230 DEG C, and the temperature of the 4th humidity province is 240 DEG C, the 5th temperature The temperature for spending area is 240 DEG C, and the temperature of the 6th humidity province is 240 DEG C, and the head temperature of double screw extruder is 230 DEG C, screw rod Revolving speed is 220r/min.
Comparative example 1
94 parts of polypropylene (PP) are taken, stir 10min through high mixer, is subsequently added into double screw extruder be blended and squeeze Out, PP composite material D1 is obtained.
The anti-microbial property data of PP composite material prepared by above application examples 1 and comparative example 1 are as shown in the table:
As can be seen from the above table, the anti-microbial property of X1, antistatic property will be better than D1, this illustrates that modified fullerenes are added Afterwards, the mechanical property of PP composite material, antistatic property are more preferable.
Embodiment 2
(1) 300g nano-TiO is weighed2, 2.4kg dehydrated alcohol, by nano-TiO2It is placed in sonic oscillation in dehydrated alcohol 12min。
(2) after drying up, by nano-TiO2It is put into plasma chamber, is passed through argon plasma, react 24min, obtain modification Nano-TiO2。
(3) 600g modified Nano TiO is weighed2, 2.4kg deionized water, 280gLaCl3·7H2O, 160g polyacrylamide, It places them into ultrasonic oscillation instrument and vibrates 5h, obtain solution A.
(4) 400g fullerene, 120gZnCl3 solution, 1.6kg deionized water are weighed, fullerene is pulverized, fowler Alkene powder, ZnCl3 solution, deionized water, which are put into ultrasonic oscillation instrument, vibrates 6h, filtering, so dry that carry zinc fullerene.
(5) zinc fullerene will be carried to be added into solution A, addition HCl solution adjusts pH value to neutrality, is stirred to react at 80 DEG C 5h is filtered, is dry, grinding to obtain modified fullerenes P2.
Application examples 2
Take 6 parts of P2 to be added in 94 parts of polybutylene terephthalate (PBT)s (PBT), stir 10min through high mixer, then plus Enter and carry out blending extrusion in double screw extruder, obtains PBT composite X2.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 200 DEG C, the The temperature of two humidity provinces is 260 DEG C, and the temperature of third humidity province is 260 DEG C, and the temperature of the 4th humidity province is 260 DEG C, the 5th temperature The temperature for spending area is 260 DEG C, and the temperature of the 6th humidity province is 260 DEG C, and the head temperature of double screw extruder is 260 DEG C, screw rod Revolving speed is 300r/min.
Comparative example 2
94 parts of PBT are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain PBT composite D2.
The anti-microbial property data of PBT composite prepared by above application examples 2 and comparative example 2 are as shown in the table:
As can be seen from the above table, the anti-microbial property of X2, antistatic property will be better than D2, this illustrates that modified fullerenes are added Afterwards, the mechanical property of PBT composite, antistatic property are more preferable.
Embodiment 3
(1) 250g nano-TiO is weighed2, 200g dehydrated alcohol, by nano-TiO2It is placed in sonic oscillation in dehydrated alcohol 10min。
(2) after drying up, by nano-TiO2It is put into plasma chamber, is passed through argon plasma, react 22min, obtain modification Nano-TiO2。
(3) 500g modified Nano TiO is weighed2, 2.2kg deionized water, 240gLaCl3·7H2O, 130g polyacrylamide, It places them into ultrasonic oscillation instrument and vibrates 4h, obtain solution A.
(4) 350g fullerene, 100gZnCl3 solution, 1.3kg deionized water are weighed, fullerene is pulverized, fowler Alkene powder, ZnCl3 solution, deionized water, which are put into ultrasonic oscillation instrument, vibrates 5h, filtering, so dry that carry zinc fullerene.
(5) zinc fullerene will be carried to be added into solution A, addition HCl solution adjusts pH value to neutrality, is stirred to react at 70 DEG C 4h is filtered, is dry, grinding to obtain modified fullerenes P3.
Application examples 3
It takes 6 parts of P3 to be added in 94 parts of polyethylene (PE), stirs 10min through high mixer, be subsequently added into double screw extruder Middle carry out blending extrusion, obtains PE composite material X3.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 120 DEG C, the The temperature of two humidity provinces is 180 DEG C, and the temperature of third humidity province is 180 DEG C, and the temperature of the 4th humidity province is 180 DEG C, the 5th temperature The temperature for spending area is 180 DEG C, and the temperature of the 6th humidity province is 180 DEG C, and the head temperature of double screw extruder is 180 DEG C, screw rod Revolving speed is 300r/min.
Comparative example 3
94 parts of PE are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain PE Composite material D3.
The anti-microbial property data of PE composite material prepared by above application examples 3 and comparative example 3 are as shown in the table:
As can be seen from the above table, the anti-microbial property of X3, antistatic property will be better than D3, this illustrates that modified fullerenes are added Afterwards, the mechanical property of PE composite material, antistatic property are more preferable.
Embodiment 4
(1) 240g nano-TiO is weighed2, 2.1kg dehydrated alcohol, by nano-TiO2It is placed in sonic oscillation in dehydrated alcohol 9min。
(2) after drying up, by nano-TiO2It is put into plasma chamber, is passed through argon plasma, react 21min, obtain modification Nano-TiO2。
(3) 550g modified Nano TiO is weighed2, 2.1kg deionized water, 230gLaCl3·7H2O, 110g polyacrylamide, It places them into ultrasonic oscillation instrument and vibrates 5h, obtain solution A.
(4) 360g fullerene, 110gZnCl3 solution, 1.4kg deionized water are weighed, fullerene is pulverized, fowler Alkene powder, ZnCl3 solution, deionized water, which are put into ultrasonic oscillation instrument, vibrates 4h, filtering, so dry that carry zinc fullerene.
(5) zinc fullerene will be carried to be added into solution A, addition HCl solution adjusts pH value to neutrality, is stirred to react at 65 DEG C 3h is filtered, is dry, grinding to obtain modified fullerenes P4.
Application examples 4
It takes 6 parts of P4 to be added in 94 parts of polyamide 6s (PA6), stirs 10min through high mixer, be subsequently added into twin-screw extrusion Blending extrusion is carried out in machine, obtains PA6 composite material X4.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 230 DEG C, the The temperature of two humidity provinces is 260 DEG C, and the temperature of third humidity province is 260 DEG C, and the temperature of the 4th humidity province is 260 DEG C, the 5th temperature The temperature for spending area is 260 DEG C, and the temperature of the 6th humidity province is 260 DEG C, and the head temperature of double screw extruder is 250 DEG C, screw rod Revolving speed is 320r/min.
Comparative example 4
94 parts of PA6 are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain PA6 composite material D4.
The anti-microbial property data of PA6 composite material prepared by above application examples 4 and comparative example 4 are as shown in the table:
As can be seen from the above table, the mechanical property of X4, antistatic property will be better than D4, this illustrates that modified fullerenes are added Afterwards, the mechanical property of PA6 composite material, antistatic property are more preferable.
Embodiment 5
(1) 280g nano-TiO is weighed2, 2.1kg dehydrated alcohol, by nano-TiO2It is placed in sonic oscillation in dehydrated alcohol 8min。
(2) after drying up, by nano-TiO2It is put into plasma chamber, is passed through argon plasma, react 20min, obtain modification Nano-TiO2。
(3) 450g modified Nano TiO is weighed2, 2.2kg deionized water, 260gLaCl3·7H2O, 150g polyacrylamide, It places them into ultrasonic oscillation instrument and vibrates 3h, obtain solution A.
(4) a certain amount of fullerene, ZnCl3 solution, deionized water are weighed, fullerene is pulverized, fullerene powder, ZnCl3 solution, deionized water, which are put into ultrasonic oscillation instrument, vibrates 4h, filtering, so dry that carry zinc fullerene.
(5) zinc fullerene will be carried to be added into solution A, addition HCl solution adjusts pH value to neutrality, is stirred to react at 60 DEG C 5h is filtered, is dry, grinding to obtain modified fullerenes P5.
Application examples 5
It takes 6 parts of P4 to be added in 94 parts of PET, stirs 10min through high mixer, be subsequently added into double screw extruder and be total to It is mixed to squeeze out, obtain PET composite material X5.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 260 DEG C, the The temperature of two humidity provinces is 300 DEG C, and the temperature of third humidity province is 300 DEG C, and the temperature of the 4th humidity province is 300 DEG C, the 5th temperature The temperature for spending area is 300 DEG C, and the temperature of the 6th humidity province is 300 DEG C, and the head temperature of double screw extruder is 300 DEG C, screw rod Revolving speed is 280r/min.
Comparative example 5
94 parts of PET are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain PET composite material D5.
The anti-microbial property data of PET composite material prepared by above application examples 5 and comparative example 5 are as shown in the table:
As can be seen from the above table, the anti-microbial property of X5, antistatic property will be better than D5, this illustrates that modified fullerenes are added Afterwards, the mechanical property of PET composite material, antistatic property are more preferable.
The technical program describes a kind of preparation method of modified fullerenes, and the polyolefine material being modified with it is in antibacterial It is also improved to some extent in terms of performance, antistatic property, this has extremely important the application field of extension fullerene Meaning.
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 modified fullerenes material, which comprises the following steps:
(1) a certain amount of nano-TiO is weighed2, dehydrated alcohol, by nano-TiO2It is placed in sonic oscillation 8-12min in dehydrated alcohol；
(2) nano-TiO by step (1) after alcohol treatment2After drying, by the nano-TiO2It is put into plasma chamber, is passed through Argon plasma reacts 20-24min, obtains modified Nano TiO2；
(3) a certain amount of modified Nano TiO is weighed2, deionized water, LaCl3·7H2O, polyacrylamide places them into ultrasound 3-5h is vibrated in wave concussion instrument, obtains solution A；
(4) a certain amount of fullerene, ZnCl3 solution, deionized water are weighed, fullerene is pulverized, fullerene powder, ZnCl3 solution, deionized water, which are put into ultrasonic oscillation instrument, vibrates 4-6h, filtering, so dry that carry zinc fullerene；
(5) zinc fullerene will be carried to be added into solution A, addition HCl solution adjusts pH value to neutrality, is stirred to react at 60-80 DEG C 3-5h is filtered, is dry, grinding to obtain modified fullerenes.
2. the preparation method of modified fullerenes material according to claim 1, which is characterized in that the nanometer in step (1) The mass ratio of TiO2 and dehydrated alcohol is (20-30): (160-240).
3. the preparation method of modified fullerenes material according to claim 1, which is characterized in that the modification in step (3) Nano TiO 2, deionized water, LaCl3·7H2The mass ratio of O and polyacrylamide is (40-60): (200-240): (20-28): (10-16)。
4. the preparation method of modified fullerenes material according to claim 1, which is characterized in that the fowler in step (4) The mass ratio of alkene, ZnCl3 solution and deionized water is (30-40): (8-12): (100-160).
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CN111716841A (en) * 2020-06-10 2020-09-29 南通纺织丝绸产业技术研究院 Propylene-proof mask and preparation method thereof
CN115305708A (en) * 2022-08-03 2022-11-08 纳奇科化妆品有限公司 Preparation method of toilet cleaning wet tissue with lasting antibacterial effect
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CN111716841A (en) * 2020-06-10 2020-09-29 南通纺织丝绸产业技术研究院 Propylene-proof mask and preparation method thereof
CN115305708A (en) * 2022-08-03 2022-11-08 纳奇科化妆品有限公司 Preparation method of toilet cleaning wet tissue with lasting antibacterial effect
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CN115818700A (en) * 2022-12-12 2023-03-21 广东工业大学 Preparation method and application of fullerene nanoenzyme with surface loaded with GeO quantum dots and single ion sites
CN115818700B (en) * 2022-12-12 2023-07-04 广东工业大学 Preparation method and application of fullerene nano-enzyme with GeO quantum dots and single ion sites loaded on surface

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