CN103451920B - Preparation method of silver-loaded active wood carbon fiber - Google Patents
Preparation method of silver-loaded active wood carbon fiber Download PDFInfo
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- CN103451920B CN103451920B CN201310359852.5A CN201310359852A CN103451920B CN 103451920 B CN103451920 B CN 103451920B CN 201310359852 A CN201310359852 A CN 201310359852A CN 103451920 B CN103451920 B CN 103451920B
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Abstract
The invention relates to a preparation method of silver-loaded active wood carbon fiber. The preparation method comprises the steps of steeping active wood carbon fiber in a silver nitrate solution at atmospheric pressure, and performing thermal decomposition under an anaerobic condition to obtain the silver-loaded active wood carbon fiber. The silver-loaded active wood carbon fiber obtained by optimizing and regulating the silver nitrate concentration and thermal decomposition temperature through taking the active wood carbon fiber with a larger pore size structure as a raw material is low in silver ion dissolution rate only achieving 0.226% on the premise of keeping the antibacterial ratio at 100%, the safety and durability of the silver-loaded active wood carbon fiber can be increased, and energy consumption in the preparation process can also be decreased, and the process steps can be simplified.
Description
Technical field
The present invention relates to carbon fiber preparation field, specifically, relate to a kind of method of being carried the active wooden carbon fiber of silver by the preparation of normal pressure dipping silver nitrate.
Background technology
Activated carbon fiber has the specific area of abundant micropore and super large, excellent absorption property and high adsorption desorption speed, and good resistance to acids and bases and chemical stability, its product can also change form as required.Therefore, activated carbon fiber is widely used in environmental protection and medical field, such as pernicious gas absorption and purification of waste water.But activated carbon fiber, because of the adsorptivity of its excellence, also can adsorb a lot of bacterium, makes it the pollution sources becoming microorganism, affect the effect that it uses.Silver, as a kind of inorganic antiseptic efficiently, can be adsorbed by activated carbon fiber, thus give activated carbon fiber anti-microbial property.
Vacuum impregnation and vacuum decomposition preparation is adopted to carry silver-colored wooden carbon fiber in " active carbon loading silver fiber " (ten thousand happy stoves etc., University Of Tianjin's journal, the 32nd volume the 5th phase, P621, in September, 1999).Vacuum condition not only increases the complexity of technique, and the dissolution rate of silver ion is also increased, and affects its security and durability." structure of silver type antibacterial fibre of activated carbon and the research of anti-microbial property thereof " (remaining water is held under the arm, Materials Science and Engineering, 19th volume the 4th phase, P66, December calendar year 2001) in mention the activated carbon fiber obtained by low temperature drying after being dipped in silver salt solution through the sisal based activated carbon fiber of steam activation, viscose base activated carbon fiber containing AgCl or AgI.But the antibacterial effect of the silver compound activated carbon fiber of this year indissoluble is poor lower than the antibacterial effect of the activated carbon fiber, particularly silver iodide that carry argent, and silver chlorate only has when its mass fraction reaches a certain amount of, and antibiotic rate just can reach 100%.
For above-mentioned weak point, propose a kind of active wooden carbon fiber of silver that carries newly and be of great significance.
Summary of the invention
The object of this invention is to provide a kind of method of being carried the active wooden carbon fiber of silver by the preparation of normal pressure dipping silver nitrate.
In order to realize the object of the invention, the present invention adopts following technical scheme.
A preparation method for year active wooden carbon fiber of silver, by the thermal decomposition and obtaining under anaerobic after liquor argenti nitratis ophthalmicus normal pressure dipping of wooden for activity carbon fiber.
In above-mentioned preparation method, described nitrate concentration is 0.05-0.4molL
-1, preferred 0.2molL
-1; Dip time is 20-30h, preferred 24h; Described heat decomposition temperature is 150-450 DEG C, preferably 350 DEG C, time 30-100min, preferred 90min.
Wherein, the wooden carbon fiber of described activity prepares by the following method and obtains:
1) wood-curing waste is crushed to 30-80 order, mixes with phenol under catalyst action, at 150-160 DEG C, stir 2-3h, obtain liquefied substance;
2) by after liquefied substance and synthetics mix and blend 0.5-1.5h, be heated to 160-175 DEG C with 10 DEG C/h and obtain spinning solution, then insert in weaving loom, when spinning solution is heated to 110-130 DEG C, can reels off raw silk from cocoons and obtain synthetic fiber;
3) synthetic fiber being placed in volume ratio is the formaldehyde of 1:1 and the mixed liquor of hydrochloric acid, with the heating rate of 10-15 DEG C/h, is heated to 85-95 DEG C, insulation 2-4h, is down to the drying of room temperature after washing, obtains wood carbon fiber precursor;
4) wood carbon fiber precursor is heated to 800 DEG C, passes into activator, be obtained by reacting active wooden carbon fiber;
Wherein, in step 1), described phenol and waste material mass ratio are 4-6:1; Catalyst and waste material mass ratio are 0.4-0.6:1.Described catalyst is phosphoric acid or mass fraction is 36% dilute sulfuric acid; The speed stirred can adjust according to the size of inventory and reactor;
Wherein, step 2) in, described synthetics and liquefied substance mass ratio are 0.04-0.06:1; Described synthetics is hexamethylenetetramine;
Wherein, in step 4), described heating rate is 2-4 DEG C of min
-1, preferably 3 DEG C of min
-1; Described activator is steam, and passing into flow is 1.0-2.5ml/min/g, and the time of passing into is 10-90min, preferred 60min;
The wooden carbon fiber specific area of the activity that said method obtains reaches 740.50-1734.839m
2/ g;
Present invention also offers year active wooden carbon fiber of silver that above-mentioned preparation method obtains, its performance indications are as follows:
The antibiotic rate of Escherichia coli and staphylococcus aureus: 100(%)
Silver turnover rate: 0.226-2.213(%)
Specific area: 704.50-1159.434(m
2/ g)
Micropore specific area: 421.153-928.263(m
2/ g)
Total pore volume: 0.376-0.636(cm
3/ g)
Micropore volume: 0.176-0.364(cm
3/ g)
Average pore size: 0.896-1.307(nm)
The present invention take wood-curing waste as raw material, the chemical composition such as cellulose and lignin need not be extracted separately from living beings, compared with existing biomass carbon fiber (such as viscose glue base, lignin-base), simplify production technology, reduce production cost, improve the utilization rate of living beings.
The present invention adopts Soaking load silver simple substance, avoids the defect that vacuum impregnation technology in prior art etc. brings.The present invention is by optimizing activation condition, obtain compared with the wooden carbon fiber of the activity of macroporous structure, again as raw material, silver nitrate concentration, dip time, heat decomposition temperature are done and optimized and revised further, by each factor interaction, obtain carrying silver-colored wooden carbon fiber under the prerequisite keeping antibiotic rate 100%, silver ion dissolution rate is low, is only 0.226%, adds safety and the durability of product, also reduce the energy resource consumption in preparation process, Simplified flowsheet step simultaneously.
Detailed description of the invention
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
The preparation of embodiment 1 year active wooden carbon fiber of silver
After wood machining residues being ground into 30 orders, put in the middle of liquefying plant.Add the phenol of 4 times of wood powder weight and the phosphoric acid of 0.4 times of wood powder weight again, mixture is heated to 160 DEG C, insulation 2.5h.After timber liquefied matter is down to room temperature, add the hexamethylenetetramine of 4% liquefied substance weight, through 1 hour, be warmed up to 170 DEG C, synthesis spinning solution.Subsequently spinning solution is placed in spinning machine, when spinning solution is heated to 120 DEG C, receives silk with the speed receiving roll dies 100 revs/min.The fiber of synthesis being placed in volume ratio is the formaldehyde of 1:1 and the mixed liquor of hydrochloric acid, is heated to 85 DEG C with the heating rate of 10 DEG C/h, insulation 2h.Room temperature after washing to be down to is dry.The precursor taking 2.85g is placed in activation furnace; under the protection of nitrogen; will with the ramp of 3 DEG C/min to after 800 DEG C; steam is passed into while insulation; flow is 1ml/min/g; and steam evaporator is closed after 60min, make activation furnace automatically lower the temperature simultaneously, stop passing into nitrogen when temperature reaches 350 DEG C.Be 1249.511m by preparation specific area
2the wooden impregnated carbon fiber of activity of/g is in the silver nitrate concentration of 0.1mol/L in concentration, takes out dry after 24h.Be placed in nitrogen environment by the wooden carbon fiber of impregnated activity, be heated to 250 DEG C, insulation 60min, to be cooledly obtain carrying a silver-colored active wooden carbon fiber to room temperature.
The antibiotic rate carrying the active wooden carbon fiber of silver of preparation is 100%, and silver-colored turnover rate is 1.394%, specific area 976.433m
2/ g, micropore specific area is 828.115m
2/ g, total pore volume is 0.494cm
3/ g, Micropore volume is 0.327cm
3/ g, average pore size is 1.012nm.
The preparation of embodiment 2 years active wooden carbon fibers of silver
After wood machining residues being ground into 60 orders, put in the middle of liquefying plant.Add the phenol of 5 times of wood powder weight and the phosphoric acid of 0.5 times of wood powder weight again, mixture is heated to 160 DEG C, insulation 2.5h.After timber liquefied matter is down to room temperature, add the hexamethylenetetramine of liquefied substance 5% weight, through 1 hour, be warmed up to 170 DEG C, synthesis spinning solution.Subsequently spinning solution is placed in spinning machine, when spinning solution is heated to 120 DEG C, receives silk with the speed receiving roll dies 100 revs/min.The fiber of synthesis being placed in volume ratio is the formaldehyde of 1:1 and the mixed liquor of hydrochloric acid, is heated to 85 DEG C with the heating rate of 10 DEG C/h, insulation 2h.Room temperature after washing to be down to is dry.The precursor taking 4.49g is placed in activation furnace, under the protection of nitrogen, and will with the ramp of 3 DEG C/min to after 800 DEG C; steam is passed into while insulation; its flow is 1ml/min/g, and closes steam evaporator after 90min, makes activation furnace automatically lower the temperature simultaneously.Stop passing into nitrogen when temperature reaches 300 DEG C.Be 1737.839m by preparation specific area
2the wooden impregnated carbon fiber of activity of/g is in the silver nitrate concentration of 0.1mol/L in concentration, takes out dry after 24h.Be placed in nitrogen environment by the wooden carbon fiber of impregnated activity, be heated to 250 DEG C, insulation 90min, to be cooledly obtain carrying a silver-colored active wooden carbon fiber to room temperature.
The antibiotic rate carrying the active wooden carbon fiber of silver of preparation is 100%, and silver-colored turnover rate is 0.348%, specific area 1159.434m
2/ g, micropore specific area is 862.687m
2/ g, total pore volume is 0.636cm
3/ g, Micropore volume is 0.346cm
3/ g, average pore size is 1.097nm.
The preparation of embodiment 3 years active wooden carbon fibers of silver
After wood machining residues being ground into 80 orders, put in the middle of liquefying plant.Add the phenol of 5 times of wood powder weight and the sulfuric acid of 0.6 times of wood powder weight again, mixture is heated to 160 DEG C, insulation 2.5h.After timber liquefied matter is down to room temperature, add the hexamethylenetetramine of liquefied substance 6% weight, through 1 hour, be warmed up to 170 DEG C, synthesis spinning solution.Subsequently spinning solution is placed in spinning machine, when spinning solution is heated to 120 DEG C, receives silk with the speed receiving roll dies 100 revs/min.The fiber of synthesis being placed in volume ratio is the formaldehyde of 1:1 and the mixed liquor of hydrochloric acid, is heated to 85 DEG C with the heating rate of 10 DEG C/h, insulation 2h.Room temperature after washing to be down to is dry.The precursor taking 4.49g is placed in activation furnace, under the protection of nitrogen, and will with the ramp of 2 DEG C/min to after 800 DEG C; steam is passed into while insulation; its flow is 1.0ml/min/g, and closes steam evaporator after 60min, makes activation furnace automatically lower the temperature simultaneously.Stop passing into nitrogen when temperature reaches 320 DEG C.Be 1249.511m by preparation specific area
2the wooden impregnated carbon fiber of activity of/g is in the silver nitrate concentration of 0.2mol/L in concentration, takes out dry after 24h.Be placed in nitrogen environment by the wooden carbon fiber of impregnated activity, be heated to 350 DEG C, insulation 90min, to be cooledly obtain carrying a silver-colored active wooden carbon fiber to room temperature.
The antibiotic rate carrying the active wooden carbon fiber of silver of preparation is 100%, and silver-colored turnover rate is 0.226%, specific area 800.083m
2/ g, micropore specific area is 697.741m
2/ g, total pore volume is 0.376cm
3/ g, Micropore volume is 0.275cm
3/ g, average pore size is 0.941nm.
The preparation of embodiment 4 years active wooden carbon fibers of silver
After wood machining residues being ground into 60 orders, put in the middle of liquefying plant.Add the phenol of 5 times of wood powder weight and the phosphoric acid of 0.5 times of wood powder weight again, mixture is heated to 150 DEG C, insulation 2.5h.After timber liquefied matter is down to room temperature, add the hexamethylenetetramine of liquefied substance 6% weight, through 1 hour, be warmed up to 175 DEG C, synthesis spinning solution.Subsequently spinning solution is placed in spinning machine, when spinning solution is heated to 120 DEG C, receives silk with the speed receiving roll dies 100 revs/min.The fiber of synthesis being placed in volume ratio is the formaldehyde of 1:1 and the mixed liquor of hydrochloric acid, is heated to 85 DEG C with the heating rate of 10 DEG C/h, insulation 2h.Room temperature after washing to be down to is dry.The precursor taking 4.31g is placed in activation furnace, under the protection of nitrogen, and will with the ramp of 3 DEG C/min to after 800 DEG C; steam is passed into while insulation; its flow is 1.0ml/min/g, and closes steam evaporator after 60min, makes activation furnace automatically lower the temperature simultaneously.Stop passing into nitrogen when temperature reaches 350 DEG C.Be 1249.511m by preparation specific area
2the wooden impregnated carbon fiber of activity of/g is in the silver nitrate concentration of 0.1mol/L in concentration, takes out dry after 24h.Be placed in nitrogen environment by the wooden carbon fiber of impregnated activity, be heated to 350 DEG C, insulation 60min, to be cooledly obtain carrying a silver-colored active wooden carbon fiber to room temperature.
The antibiotic rate carrying the active wooden carbon fiber of silver of preparation is 100%, and silver-colored turnover rate is 1.047%, specific area 1050.483m
2/ g, micropore specific area is 770.711m
2/ g, total pore volume is 0.594cm
3/ g, Micropore volume is 0.208cm
3/ g, average pore size is 1.131nm.
The preparation of embodiment 5 years active wooden carbon fibers of silver
After wood machining residues being ground into 80 orders, put in the middle of liquefying plant.Add the phenol of 5 times of wood powder weight and the phosphoric acid of 0.6 times of wood powder weight again, mixture is heated to 160 DEG C, insulation 2.5h.After timber liquefied matter is down to room temperature, add the hexamethylenetetramine of liquefied substance 6% weight, through 1 hour, be warmed up to 170 DEG C, synthesis spinning solution.Subsequently spinning solution is placed in spinning machine, when spinning solution is heated to 120 DEG C, receives silk with the speed receiving roll dies 100 revs/min.The fiber of synthesis being placed in volume ratio is the formaldehyde of 1:1 and the mixed liquor of hydrochloric acid, is heated to 85 DEG C with the heating rate of 10 DEG C/h, insulation 2h.Room temperature after washing to be down to is dry.The precursor taking 3.0g is placed in activation furnace, under the protection of nitrogen, and will with the ramp of 2 DEG C/min to after 700 DEG C; steam is passed into while insulation; its flow is 1.0ml/min/g, and closes steam evaporator after 60min, makes activation furnace automatically lower the temperature simultaneously.Stop passing into nitrogen when temperature reaches 350 DEG C.Be 1249.511m by preparation specific area
2the wooden impregnated carbon fiber of activity of/g is in the silver nitrate concentration of 0.1mol/L in concentration, takes out dry after 24h.Be placed in nitrogen environment by the wooden carbon fiber of impregnated activity, be heated to 350 DEG C, insulation 60min, to be cooledly obtain carrying a silver-colored active wooden carbon fiber to room temperature.
The antibiotic rate carrying the active wooden carbon fiber of silver of preparation is 100%, and silver-colored turnover rate is 1.082%, specific area 1050.002m
2/ g, micropore specific area is 732.498m
2/ g, total pore volume is 0.613cm
3/ g, Micropore volume is 0.294cm
3/ g, average pore size is 1.167nm.The preparation of embodiment 6 years active wooden carbon fibers of silver
After wood machining residues being ground into 80 orders, put in the middle of liquefying plant.Add the phenol of 5 times of wood powder weight and the phosphoric acid of 0.6 times of wood powder weight again, mixture is heated to 160 DEG C, insulation 2.5h.After timber liquefied matter is down to room temperature, add the hexamethylenetetramine of liquefied substance 5% weight, through 1 hour, be warmed up to 165 DEG C, synthesis spinning solution.Subsequently spinning solution is placed in spinning machine, when spinning solution is heated to 120 DEG C, receives silk with the speed receiving roll dies 100 revs/min.The fiber of synthesis being placed in volume ratio is the formaldehyde of 1:1 and the mixed liquor of hydrochloric acid, is heated to 90 DEG C with the heating rate of 10 DEG C/h, insulation 2h.Room temperature after washing to be down to is dry.The precursor taking 4.49g is placed in activation furnace, under the protection of nitrogen, and will with the ramp of 4 DEG C/min to after 800 DEG C; steam is passed into while insulation; its flow is 1.0ml/min/g, and closes steam evaporator after 60min, makes activation furnace automatically lower the temperature simultaneously.Stop passing into nitrogen when temperature reaches 350 DEG C.Be 1262.962m by preparation specific area
2the wooden impregnated carbon fiber of activity of/g is in the silver nitrate concentration of 0.4mol/L in concentration, takes out dry after 24h.Be placed in nitrogen environment by the wooden carbon fiber of impregnated activity, be heated to 300 DEG C, insulation 70min, to be cooledly obtain carrying a silver-colored active wooden carbon fiber to room temperature.
The antibiotic rate carrying the active wooden carbon fiber of silver of preparation is 100%, and silver-colored turnover rate is 1.352%, specific area 927.038m
2/ g, micropore specific area is 837.267m
2/ g, total pore volume is 0.416cm
3/ g, Micropore volume is 0.328cm
3/ g, average pore size is 0.896nm.
Comparative example 1
Silver-colored activated carbon fiber is carried in the method preparation recorded according to " active carbon loading silver fiber " (ten thousand happy stoves etc., University Of Tianjin's journal, the 32nd volume the 5th phase, P621, in September, 1999).
After testing, the scope of bacterial restrain width and specimen finish ratio is 15 × 10
-2, after dynamically washing away 5h, silver-colored turnover rate is more than 50%, and specific area is 523.274m
2/ g.
Comparative example 2
Silver chlorate and silver iodide activated carbon fiber are carried in the method preparation recorded according to " structure of silver type antibacterial fibre of activated carbon and the research of anti-microbial property thereof " (remaining water is held under the arm, Materials Science and Engineering, the 19th volume the 4th phase, P66, December calendar year 2001).
After testing, for staphylococcus aureus, the antibiotic property of silver iodide is poor, and is just 100% to the antibiotic rate of Staphylococcus aureus when the content of silver chlorate must reach more than 11wt%, and specific area is only 670m
2/ g.
Can find out from embodiment 1-6, comparative example 1-2, what adopt preparation method of the present invention to obtain carries the active wooden carbon fiber of silver under the prerequisite keeping antibiotic rate 100%, silver ion dissolution rate is low, minimumly be only 0.226%, add safety and the durability of product, and specific area be large, absorption affinity is strong, also reduce the energy resource consumption in preparation process, Simplified flowsheet step, reduces production cost simultaneously.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (1)
1. carry a preparation method for the active wooden carbon fiber of silver, it is characterized in that, after wood machining residues being ground into 80 orders, put in the middle of liquefying plant, add the phenol of 5 times of wood powder weight and the sulfuric acid of 0.6 times of wood powder weight again, mixture is heated to 160 DEG C, insulation 2.5h; After timber liquefied matter is down to room temperature, add the hexamethylenetetramine of liquefied substance 6% weight, through 1 hour, be warmed up to 170 DEG C, synthesis spinning solution; Subsequently spinning solution is placed in spinning machine, when spinning solution is heated to 120 DEG C, receives silk with the speed receiving roll dies 100 revs/min; The fiber of synthesis being placed in volume ratio is the formaldehyde of 1:1 and the mixed liquor of hydrochloric acid, is heated to 85 DEG C with the heating rate of 10 DEG C/h, insulation 2h, and room temperature after washing to be down to is dry; The precursor taking 4.49g is placed in activation furnace, under the protection of nitrogen, will with the ramp of 2 DEG C/min to after 800 DEG C, steam is passed into while insulation, its flow is 1.0ml/min/g, and steam evaporator is closed after 60min, make activation furnace automatically lower the temperature simultaneously, stop passing into nitrogen when temperature reaches 320 DEG C;
Be 1249.511m by preparation specific area
2the wooden impregnated carbon fiber of activity of/g is in the silver nitrate concentration of 0.2mol/L in concentration, take out dry after 24h, be placed in nitrogen environment by the wooden carbon fiber of impregnated activity, be heated to 350 DEG C, insulation 90min, to be cooledly obtains carrying a silver-colored active wooden carbon fiber to room temperature.
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| CN106007625A (en) * | 2016-05-25 | 2016-10-12 | 华国平 | Method for manufacturing environment-friendly fiber cement board for constructional engineering |
| CN106003340A (en) * | 2016-05-25 | 2016-10-12 | 华国平 | Manufacturing method of energy-saving environment-friendly fiber cement board for constructional engineering |
| CN105926277A (en) * | 2016-05-31 | 2016-09-07 | 深圳市微纳集成电路与系统应用研究院 | Conductive fiber, preparation method of conductive fiber, capacitive pressure sensor and production method of capacitive pressure sensor |
| CN106758178B (en) * | 2016-12-18 | 2018-10-26 | 中南大学 | A kind of method that carbonohydrazides complexing silver nitrate prepares antibiotic fabric product |
| CN109385889B (en) * | 2018-11-08 | 2021-05-07 | 银维康新材料科技(珠海)有限公司 | Antibacterial and anti-radiation fabric |
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| CN102719935A (en) * | 2012-06-07 | 2012-10-10 | 北京林业大学 | Preparation method of active wood-based carbon fibers |
| CN103182098A (en) * | 2006-01-09 | 2013-07-03 | 逢甲大学 | Antimicrobial composition and wound coverture |
| CN103225134A (en) * | 2013-05-09 | 2013-07-31 | 张家港耐尔纳米科技有限公司 | Preparation method of silver-loaded active carbon fibers |
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| CN103182098A (en) * | 2006-01-09 | 2013-07-03 | 逢甲大学 | Antimicrobial composition and wound coverture |
| CN102719935A (en) * | 2012-06-07 | 2012-10-10 | 北京林业大学 | Preparation method of active wood-based carbon fibers |
| CN103225134A (en) * | 2013-05-09 | 2013-07-31 | 张家港耐尔纳米科技有限公司 | Preparation method of silver-loaded active carbon fibers |
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