CN104629270A - Preparation method of long-acting antibacterial polyester material - Google Patents
Preparation method of long-acting antibacterial polyester material Download PDFInfo
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- CN104629270A CN104629270A CN201410753630.6A CN201410753630A CN104629270A CN 104629270 A CN104629270 A CN 104629270A CN 201410753630 A CN201410753630 A CN 201410753630A CN 104629270 A CN104629270 A CN 104629270A
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Abstract
The invention discloses a preparation method of a long-acting antibacterial polyester material, belongs to the field of preparation of antibacterial materials and provides a preparation method of a long-acting antibacterial polyester material which is durable and efficient in antibacterial performance. The method comprises the following steps: chemically integrating a certain quantity of polyhexamethylene biguanidine with a polyethylene glycol terephthalate (PET) substrate to prepare an antibacterial PET master batch, and adding the antibacterial PET master batch into the PET substrate to prepare PET resin which is durable and efficient in antibacterial performance. The PET resin which is durable and efficient in antibacterial performance is prepared by the method; meanwhile, the defect that the PET resin is easy to hydrolyze in the processing process can be overcome; and the long-acting antibacterial performance is given to the PET substrate.
Description
Technical field
The invention belongs to anti-biotic material preparation field.
Background technology
Harmful microorganism breeding rapidly, spreads disease, causes high risks to human body.Along with the progress of human society, people wish that more macromolecular material can have the performance of antibacterial and mouldproof, thus the protection mankind's is healthy.So far, the preparation of most of anti-biotic material still adopts and mix inorganic antibiotic metal ion in plastic substrate, and these metal ions comprise silver, copper, tin, zinc or mercury ion etc.Be that the inorganic molecules antiseptic-germicide of representative is enriched in material surface by transporting action with silver ions, produce anti-microbial effect after contacting with bacterium, along with the loss of antiseptic-germicide, its antibacterial effect is constantly decayed.In addition, evidence show, silver ions has higher toxicity to mammalian somatic cell, can destroy brain cell, liver cell and stem cell.Therefore, there is the risk of human toxicity and environmental pollution in the anti-biotic material made in this way, its more and more not accept by people, more can not be used as and the textile material of human body close contact.Antiseptic-germicide and molecular resin are linked by chemical bond, can give the performance of material long acting antibiotic, this technology represents the development trend in anti-biotic material future.Because most of resin material is chemically inert, therefore the ultimate challenge of long acting antibiotic Polymer materialspreparation is how antiseptic-germicide and resin matrix are carried out effective bonding.In former research, antiseptic-germicide is fixed on the surface of polymer materials by the method mainly through chemical bond connection, these methods generally include plasma body initiation, radiation, coating or atom transferred free radical (ATRP) etc., but there is the defects such as preparation process is loaded down with trivial details, cost is higher, side reaction is too much in these methods, and, be bonded in the antiseptic-germicide on surface of polymer material, in use lose antibacterial effect because of reasons such as wearing and tearing or chemical corrosions.
Polyethylene terephthalate (PET) has excellent physical and chemical performance, and PET is the maximum class synthon of usage quantity, is widely used in the fields such as clothes, bedding and clothing, medical textile, decoration and industry.But the easy cooperating microorganisms of textiles, under suitable conditions, microorganism breeds rapidly, easily makes skin infections, causes disease to human body.
Summary of the invention
The object of this invention is to provide and a kind of there is long acting antibiotic polyester material preparation method that is lasting, high-efficiency antimicrobial performance.
The present invention is achieved by the following technical programs: a kind of long acting antibiotic polyester material preparation method, comprises preparation three step of the preparation of polyhexamethylene Guanidinium hydrochloride-epoxy chloropropane (PHMG-e) antibacterial polymer, the preparation of PET-g-PHMG antibacterial plastic concentrate and antibacterial PET sample;
The preparation process of described polyhexamethylene Guanidinium hydrochloride-epoxy chloropropane (PHMG-e) antibacterial polymer is, be equipped with magnetic stir bar, dropping funnel, 34g polyhexamethylene Guanidinium hydrochloride (PHMG) and 28g epoxy chloropropane is added in the 500mL there-necked flask of reflux condensate device and thermometer, add 150mL dimethylformamide (DMF) solvent again, abundant stirring makes PHMG dissolve completely, then boron trifluoride diethyl etherate (0.45g) is dripped, at 60 DEG C of isothermal reaction 4h, 20.5g sodium ethylate is added again after question response thing cool to room temperature, 8h is reacted at 25 DEG C, solution is filtered, the method of underpressure distillation is adopted to remove unreacted epoxy chloropropane and DMF, obtain PHMG-e,
The preparation process of described PET-g-PHMG antibacterial plastic concentrate is, by polyethylene terephthalate (PET) vacuum-drying 24h at 130 DEG C, PET and the 9gPHMG-e getting 51g drying fully mixes (content of PHMG-e accounts for 15% of total mass), then in Haake rheometer, melt blending reaction is carried out, the processing temperature of Haake rheometer is set as 270 DEG C, blended time 5min, obtains antibacterial PET antibacterial plastic concentrate (PET-g-PHMG);
The preparation process of described antibacterial PET sample is, by pure PET and antibacterial plastic concentrate PET-g-PHMG in 130 DEG C of vacuum-drying 24h, get pre-dry pure PET and PET-g-PHMG to mix, then in Haake rheometer, carry out melt blending, obtained antimicrobial levels is the antibacterial PET sample of 0.5%.
The present invention has following beneficial effect:
Adopt the method to prepare and there is PET resin that is lasting, high-efficiency antimicrobial performance, overcome the shortcoming of PET resin facile hydrolysis in the course of processing simultaneously, give PET matrix long-term antimicrobial efficiency.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Specific embodiment: preparation process of the present invention comprises preparation three step of the preparation of polyhexamethylene Guanidinium hydrochloride-epoxy chloropropane (PHMG-e) antibacterial polymer, the preparation of PET-g-PHMG antibacterial plastic concentrate and antibacterial PET sample;
The preparation process of described polyhexamethylene Guanidinium hydrochloride-epoxy chloropropane (PHMG-e) antibacterial polymer is, be equipped with magnetic stir bar, dropping funnel, 34g polyhexamethylene Guanidinium hydrochloride (PHMG) and 28g epoxy chloropropane is added in the 500mL there-necked flask of reflux condensate device and thermometer, add 150mL dimethylformamide (DMF) solvent again, abundant stirring makes PHMG dissolve completely, then boron trifluoride diethyl etherate (0.45g) is dripped, at 60 DEG C of isothermal reaction 4h, 20.5g sodium ethylate is added again after question response thing cool to room temperature, 8h is reacted at 25 DEG C, solution is filtered, the method of underpressure distillation is adopted to remove unreacted epoxy chloropropane and DMF, obtain PHMG-e,
The preparation process of described PET-g-PHMG antibacterial plastic concentrate is, by polyethylene terephthalate (PET) vacuum-drying 24h at 130 DEG C, PET and the 9gPHMG-e getting 51g drying fully mixes (content of PHMG-e accounts for 15% of total mass), then in Haake rheometer, melt blending reaction is carried out, the processing temperature of Haake rheometer is set as 270 DEG C, blended time 5min, obtains antibacterial PET antibacterial plastic concentrate (PET-g-PHMG);
The preparation process of described antibacterial PET sample is, by pure PET and antibacterial plastic concentrate PET-g-PHMG in 130 DEG C of vacuum-drying 24h, get pre-dry pure PET and PET-g-PHMG to mix, then in Haake rheometer, carry out melt blending, obtained antimicrobial levels is the antibacterial PET sample of 0.5%.
Adopt concussion method to carry out antibacterial test to antibacterial PET sample, reach more than 99% to the bacteriostasis rate of Gram-negative and positive bacteria, adopt soxhlet extraction methods with after deionized water extracting antibacterial PET sample 48h, its bacteriostasis rate still can reach 99.77%.
Above content is the further description done the present invention in conjunction with concrete embodiment, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (1)
1. a long acting antibiotic polyester material preparation method, is characterized in that: preparation three step comprising the preparation of polyhexamethylene Guanidinium hydrochloride-epoxy chloropropane (PHMG-e) antibacterial polymer, the preparation of PET-g-PHMG antibacterial plastic concentrate and antibacterial PET sample;
The preparation process of described polyhexamethylene Guanidinium hydrochloride-epoxy chloropropane (PHMG-e) antibacterial polymer is, be equipped with magnetic stir bar, dropping funnel, 34g polyhexamethylene Guanidinium hydrochloride (PHMG) and 28g epoxy chloropropane is added in the 500mL there-necked flask of reflux condensate device and thermometer, add 150mL dimethylformamide (DMF) solvent again, abundant stirring makes PHMG dissolve completely, then boron trifluoride diethyl etherate (0.45g) is dripped, at 60 DEG C of isothermal reaction 4h, 20.5g sodium ethylate is added again after question response thing cool to room temperature, 8h is reacted at 25 DEG C, solution is filtered, the method of underpressure distillation is adopted to remove unreacted epoxy chloropropane and DMF, obtain PHMG-e,
The preparation process of described PET-g-PHMG antibacterial plastic concentrate is, by polyethylene terephthalate (PET) vacuum-drying 24h at 130 DEG C, PET and the 9gPHMG-e getting 51g drying fully mixes (content of PHMG-e accounts for 15% of total mass), then in Haake rheometer, melt blending reaction is carried out, the processing temperature of Haake rheometer is set as 270 DEG C, blended time 5min, obtains antibacterial PET antibacterial plastic concentrate (PET-g-PHMG);
The preparation process of described antibacterial PET sample is, by pure PET and antibacterial plastic concentrate PET-g-PHMG in 130 DEG C of vacuum-drying 24h, get pre-dry pure PET and PET-g-PHMG to mix, then in Haake rheometer, carry out melt blending, obtained antimicrobial levels is the antibacterial PET sample of 0.5%.
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| CN201410753630.6A CN104629270A (en) | 2014-12-10 | 2014-12-10 | Preparation method of long-acting antibacterial polyester material |
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| CN201410753630.6A CN104629270A (en) | 2014-12-10 | 2014-12-10 | Preparation method of long-acting antibacterial polyester material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107686551A (en) * | 2017-08-29 | 2018-02-13 | 东华大学 | A kind of safe and efficient permanent hydrophilic antibacterial polyester material and preparation method thereof |
| CN109503832A (en) * | 2018-10-18 | 2019-03-22 | 上海高聚生物科技有限公司 | A kind of polycyclic oxygen propyl group hexyl guanidine hydrochloride and preparation method thereof |
| CN109880319A (en) * | 2019-03-20 | 2019-06-14 | 亳州科蔚科技服务有限公司 | A kind of medical degradable high-molecular anti-bacteria composite material |
| CN113026341A (en) * | 2021-02-26 | 2021-06-25 | 石家庄学院 | Preparation method of copper-titanium coupled long-acting antibacterial polyester fiber based on efficient pretreatment process |
| CN113026361A (en) * | 2021-02-26 | 2021-06-25 | 石家庄学院 | Method and reaction device for preparing long-acting antibacterial polyester fiber by coupling poly hexamethylene hydrochloride with glutaraldehyde |
| CN116145280A (en) * | 2022-12-31 | 2023-05-23 | 诸暨市锦晨纺织有限公司 | TiO (titanium dioxide) 2 PHMG composite modified PET antibacterial fabric and preparation method thereof |
-
2014
- 2014-12-10 CN CN201410753630.6A patent/CN104629270A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107686551A (en) * | 2017-08-29 | 2018-02-13 | 东华大学 | A kind of safe and efficient permanent hydrophilic antibacterial polyester material and preparation method thereof |
| CN107686551B (en) * | 2017-08-29 | 2019-07-23 | 东华大学 | A kind of safe and efficient permanent hydrophilic antibacterial polyester material and preparation method thereof |
| CN109503832A (en) * | 2018-10-18 | 2019-03-22 | 上海高聚生物科技有限公司 | A kind of polycyclic oxygen propyl group hexyl guanidine hydrochloride and preparation method thereof |
| CN109880319A (en) * | 2019-03-20 | 2019-06-14 | 亳州科蔚科技服务有限公司 | A kind of medical degradable high-molecular anti-bacteria composite material |
| CN113026341A (en) * | 2021-02-26 | 2021-06-25 | 石家庄学院 | Preparation method of copper-titanium coupled long-acting antibacterial polyester fiber based on efficient pretreatment process |
| CN113026361A (en) * | 2021-02-26 | 2021-06-25 | 石家庄学院 | Method and reaction device for preparing long-acting antibacterial polyester fiber by coupling poly hexamethylene hydrochloride with glutaraldehyde |
| CN113026361B (en) * | 2021-02-26 | 2022-12-30 | 石家庄学院 | Method and reaction device for preparing long-acting antibacterial polyester fiber by coupling poly hexamethylene hydrochloride with glutaraldehyde |
| CN116145280A (en) * | 2022-12-31 | 2023-05-23 | 诸暨市锦晨纺织有限公司 | TiO (titanium dioxide) 2 PHMG composite modified PET antibacterial fabric and preparation method thereof |
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