CN103551126B - A kind of high adsorption also has antibacterial resistance to mould activated carbon fiber and manufacture method thereof - Google Patents
A kind of high adsorption also has antibacterial resistance to mould activated carbon fiber and manufacture method thereof Download PDFInfo
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- CN103551126B CN103551126B CN201310544709.3A CN201310544709A CN103551126B CN 103551126 B CN103551126 B CN 103551126B CN 201310544709 A CN201310544709 A CN 201310544709A CN 103551126 B CN103551126 B CN 103551126B
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Abstract
The invention belongs to antibacterial environmental protection field, particularly a kind of antibacterial active carbon fiber and manufacture method thereof.Described antibacterial active carbon fiber is a kind of polyester fiber sorbing material, deposits the composite coating of carbon and metal at porous polyester fibrous material surface.In preparation technology of the present invention, first utilize over-saturation foaming, nitrogen is entered in the free volume of polyester fiber, then by step-down and hyperthermic treatment, make the nitrogen expansion in press-in free volume, form a large amount of bubble, and fixing hole shape.Utilize magnetically controlled sputter method, carbon is deposited on fibrous material surface with the target that mixes of metal.
Description
Technical field
The invention belongs to antibacterial environmental protection field, particularly a kind of cost is low, adsorptivity is high and have carbon fiber and the manufacture method thereof of antibacterial resistance to mould activity.
Background technology
Active carbon (GAC) is a kind of porous charcoal through activation process, has extremely strong adsorption capacity, and it has century-old history in the application in the fields such as military affairs, chemical industry, environmental protection.Activated carbon fiber (being threadiness), fiber is covered with micropore, and it is higher several times to tens times in atmosphere than granular activated carbon to organic gas adsorption capacity, high 5 ~ 6 times in aqueous, fast 100 ~ 1000 times of the rate of adsorption.Industrially utilize his superpower adsorption capacity to go to reclaim organic solvent, purify air, purification water.
Activated carbon fiber is a kind of high-tech product, a few countries is only had to produce in the world, his goods can be the forms such as silk, paper, felt, cloth, traditional activated carbon fiber is because of complex process and energy consumption height is long in time limit, the market price is about 250,000/ton, be tens times of active carbon to twenties times, seriously limit its market use amount.
And due to activated carbon fiber in use, also can adsorb microorganism, filtering adsorbing material is gone mouldy, can microbial contamination be caused.
In order to overcome above-mentioned defect, the invention discloses a kind of manufacturing process simple, cost is low, has again antibacterial resistance to mould activated carbon fiber.This high-specific surface area, high added value, high-tech, oligosaprobic novel active material with carbon element have fabulous development prospect and wide application market.
Summary of the invention
Technical problem to be solved by this invention is: in prior art, and in use, the existence due to microorganism easily produces goes mouldy activated carbon fiber, and the processing cost of active-carbon fibre material is too high.
For solving this technical problem, the invention provides a kind of novel active carbon fibrous absorption material, be a kind of polyester fiber absorption filtering material, this porous polyester fibrous material surface deposits the composite coating of carbon and metal.In composite coating, material with carbon element comprises graphite, carbon dust, and metal material comprises one or more in copper, silver, zinc, titanium, manganese, nickel, aluminium.
Present invention also offers a kind of preparation method of above-mentioned polyester fiber absorption filtering material, first over-saturation foaming is adopted to prepare porous polyester fibrous material, prepared the composite coating of one deck carbon and metal again at porous polyester fiber surface by physical gas-phase deposite method, this technique can complete in same equipment.
Over-saturation foaming prepares porous polyester fibrous material, and concrete operations are,
(1) utilize room temperature pressurization, under High Pressure, make gas fully infiltrate polyester fiber, make gas enter in the free volume of polyester fiber,
Macromolecular fibre huge number, the present invention with polyester fiber (as PET, PBT, PAR, TPEE etc.) for perforate base material, wherein preferred PET, PET itself is nontoxic, tasteless, and security is good, has excellent mechanical property, high temperature resistant, cryogenic property, have good patience to oil, fat, alkali, olefin(e) acid and most of solvent, and transparency is high, there is uvioresistant ability;
Perforate gas has nitrogen, argon gas, carbon dioxide or uses two or more mist, preferred nitrogen of the present invention, and nitrogen thermodynamics, chemical property are all more stable, and nonhazardous effect, cost are low, free from environmental pollution,
In this step, high voltage control is at 6MPa-8MPa, and different pressure is different on the impact of the void density in porous fibre: pressure is larger, and fiber bubble density is larger, but requires higher to working condition, equipment etc. simultaneously,
Also there is impact pressing time to bubble density, and the time of pressurization is longer, and the hole in the fiber obtained is more, and power consumption also will be more, and general control was at 4 hours to 24 hours;
(2) rapid depressurization is to normal pressure, and then is down to negative pressure, and wherein, from high pressure drop to the time of " a negative atmospheric pressure ", control in 10min, 7-10min is comparatively suitable;
(3) in winding constant temperature oven, negative pressure (a negative atmospheric pressure) foams, and constant temperature oven temperature is 120 DEG C-160 DEG C, and foamed time is 10S-20S, and step (2), (3) can be carried out in same equipment,
Different blowing temperature has impact to porous fibre hole density, and temperature is higher, and gas expansion is faster, and the hole density in polyester fiber also presents positive correlation and improves,
Step-down and hyperthermic treatment, make the gas expansion in press-in free volume, forms a large amount of bubble, and fix hole shape in Polyester Fibers,
To sum up, by pressurizeing by room temperature, then intensification foam process can obtain foamed fibre, and bubble structure with the difference for the treatment of conditions, and is very different.When other process conditions are constant, in foamed fibre, bubble density increases along with the increase of pressure, pressing time, blowing temperature, foamed time respectively, after wherein foamed time is greater than 10s, has no significant effect bubble density.
After tap operation terminates, being operating as of composite coating is prepared by physical gas-phase deposite method, adopt vacuum coating equipment, be deposited in the top layer and hole of porous polyester fiber with the composite target material of magnetically controlled sputter method by carbon and metal, concrete technology step is: (1) porous fibre drying process; (2) upper stove; (3) inflatable body; (4) plated film; (5) stove under,
In step (3), plated film adopts magnetic-control sputtering coiling machine, and institute's inflatable body is methane, acetylene or both mists, and in step (4), volumetric flow of gas is 400 ~ 600SCCM, electric current: 6A ~ 15A.
The composite target material of carbon and metal is the compressing hybrid target of material with carbon element and metal material, and preparation technology is: by material with carbon element and metal powder, and in proportion after mixing, be pressed into bulk with cold static pressure technology, then excision forming, pressure is every square centimeter of 50-80 kilogram.The percentage by weight of carbon and metal be " 99.9% to 0.01% " to " 80% to 20% ", metal is selected from one or more in copper, silver, zinc, titanium, manganese, nickel, aluminium.
Beneficial effect of the present invention is: (1), when preparing porous polyester fibrous material, adopts nitrogen gas foaming, to people and animals without any toxic action and cost is low, free from environmental pollution; (2) on porous polyester fiber, composite target material enters into hole by activated carbon loaded, considerably increases the specific area of activated carbon, enhances its suction-operated; (3) Nanometer Copper is mixed in carbon dust, the composite obtained can be made to have long-acting antibacterial, mildew-resistant effect; (4) use the method for magnetron sputtering, the composite deposit of deposit carbon and metal, decreases environmental pollution, reduces production cost.
Preparation technology's difficult point and innovative point: preparation and magnetron sputtering plating carbon, the metal coating of porous polyester fiber complete in same equipment.1, design positive/negative-pressure system in magnetron sputtering stove, set up a silica gel ring containing electromagnetism silk at the inner close fire door position of furnace chamber, by inhaling and can meet in external pressure effect guarantee stove the impact of malleation, negative pressure in Electromagnetic Control silica gel ring.2, in stove, pass into excessive nitrogen, argon gas or titanium dioxide gas, room temperature pressurization makes gas enter in the free volume of macromolecule PET, and then step-down, constant temperature process obtain porous PET.3, in same stove, open magnetron sputtering, carbon, metal material are deposited on porous fibre.
Detailed description of the invention
Following processing step, completes in same equipment:
One, porous polyester fiber is prepared with over-saturation gas method.
The forming process of expanded material generally all will through 3 Main Stage, i.e. the immobilization of the formation of nuclei of bubbles, the expansion of bubble and bubble is shaping etc.Its concrete technology step is: (1) makes nitrogen fully infiltrate polyester PET fiber under High Pressure;
(2) rapid depressurization is to normal pressure; (3) foam in constant temperature oven.
The positive/negative-pressure system in magnetron sputtering stove is utilized (to set up a silica gel ring containing electromagnetism silk at the inner close fire door position of furnace chamber, by inhaling and can meet in external pressure effect guarantee stove the impact of malleation, negative pressure in Electromagnetic Control silica gel ring), under room temperature (25 DEG C), make nitrogen fully infiltrate polyester PET (fiber company is learned in Shanghai connection Chinesizing) fiber 12h with 8MPa pressure, negative pressure (a negative atmospheric pressure) is down to rapidly in 10min, under this negative pressure, in 160 DEG C of foaming 10s.
Two, carbon, copper coating is prepared with physical vapour deposition (PVD)-magnetically controlled sputter method.
By graphite and copper powder, after the ratio of " 90%:10% " mixes by weight percentage, be pressed into bulk with cold static pressure technology, then cut into required shape, pressure is 65 kilograms every square centimeter, obtains mixing target.
With magnetically controlled sputter method, carbon, copper mixing target coating are plated in porous polyester fiber sheath, its concrete technology step is: (1) porous fibre drying process; (2) upper stove; (3) inflatable body; (4) plated film; (5) stove under,
In step (3), plated film adopts magnetic-control sputtering coiling machine, and inflatable body is methane; In step (4), acetylene gas volume flow is 500SCCM, and electric current: 12A, initial vacuum is 7.0*10-3Pa, plated film linear speed 4m/min, and coating times is 1 ~ 2 time, and folding and unfolding power is 50N.
Table 1 embodiment measurement result
Antibacterial, fungus resistance is detected by Guangzhou institute of microbiology of the third-party institution, and antiviral detection is cooperated to carry out by Jiangsu Inst. of Fowls Science of Poultry Institute, Chinese Academy of Agricultural Science study on prevention room.
In table 1, " adsorptivity " in hurdle, refers to the absorption property to organic gas methane,
" antiviral property " data on hurdle, specifically summarize according to the content in following table and obtain
Table 2
The data of " anti-microbial property " in hurdle, test according to " GB/T20944.3-2008 succusion " and obtain, table specific as follows:
Table 3
" anti-fungi performance " refers to the anti-fungi performance to mould, records according to GB/T1741-2007.
Claims (6)
1. a preparation method for polyester fiber sorbing material, is characterized in that:
Described polyester fiber sorbing material is that porous polyester fibrous material surface deposits the composite coating of carbon and metal;
Described method is, first adopts over-saturation foaming to prepare porous polyester fibrous material, then prepares the composite coating of one deck carbon and metal at porous polyester fiber surface by physical gas-phase deposite method.
2. the preparation method of polyester fiber sorbing material as claimed in claim 1, it is characterized in that: described over-saturation foaming prepares porous polyester fibrous material, concrete operations are, (1) utilizes room temperature pressurization, under High Pressure, make gas fully infiltrate polyester fiber; (2) rapid depressurization is to normal pressure, and then is down to negative pressure; (3) constant temperature foaming.
3. the preparation method of polyester fiber sorbing material as claimed in claim 2, is characterized in that: the high pressure described in step (1) is 6MPa-8MPa; Step (2) mesohigh is down to the time controling of negative pressure in 10min; Foam in winding constant temperature oven in step (3), winding constant temperature oven temperature is 120 DEG C-160 DEG C, and foamed time is 10s-20s.
4. the preparation method of polyester fiber sorbing material as claimed in claim 1, it is characterized in that: described prepares being operating as of composite coating by physical gas-phase deposite method, adopt vacuum coating equipment, in the top layer composite target material of carbon and metal being deposited on porous polyester fiber with magnetically controlled sputter method and hole.
5. the preparation method of polyester fiber sorbing material as claimed in claim 4, is characterized in that: described magnetically controlled sputter method concrete technology step is (1) porous fibre drying process; (2) upper stove; (3) inflatable body; (4) plated film; (5) stove under, in step (3), institute's inflatable body is methane, acetylene or both mists, and in step (4), volumetric flow of gas is 400 ~ 600SCCM, and electric current is 6A ~ 15A.
6. the preparation method of polyester fiber sorbing material as claimed in claim 4, is characterized in that: in described carbon and the composite target material of metal, the percentage by weight of carbon and metal is that " 99.9%:0.01% " is to " 80%:20% ".
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5951744A (en) * | 1994-12-23 | 1999-09-14 | Alliedsignal Inc. | Multicomponent depth odor control filter and method of manufacture |
| CN102762295A (en) * | 2009-12-25 | 2012-10-31 | 伊莱克福有限公司 | Composite material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5951744A (en) * | 1994-12-23 | 1999-09-14 | Alliedsignal Inc. | Multicomponent depth odor control filter and method of manufacture |
| CN102762295A (en) * | 2009-12-25 | 2012-10-31 | 伊莱克福有限公司 | Composite material |
Non-Patent Citations (2)
| Title |
|---|
| "含载银活性炭的腈氯纶多功能纤维的制备与表征";陈晨，等;《功能材料》;20071231;第38卷(第9期);第3443页摘要，第1、2段，第2.1、3.4节 * |
| "新型多孔聚酯纤维的制备";熊春燕，等;《合成技术及应用》;20051231;第20卷(第4期);第48页第3、4段 * |
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