CN103506082B - The preparation method of a kind of flax fiber/expanded graphite composite fibre sorbing material - Google Patents
The preparation method of a kind of flax fiber/expanded graphite composite fibre sorbing material Download PDFInfo
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- CN103506082B CN103506082B CN201210220109.7A CN201210220109A CN103506082B CN 103506082 B CN103506082 B CN 103506082B CN 201210220109 A CN201210220109 A CN 201210220109A CN 103506082 B CN103506082 B CN 103506082B
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Abstract
The present invention discloses the preparation method of a kind of flax fiber/expanded graphite composite fibre sorbing material, this drainage sorbing material that exceedes synthesizes composite fibre using flax fiber as base starting material and expanded graphite, uses a kind of biologically active sorbing material that the boehmite that flax fiber and expanded graphite composite fibre and main component are aluminium hydroxide manufactures.This drainage sorbing material that exceedes can produce positive charge, can adsorb electronegative microorganism and bacteriophage, reaches most microorganism and bacteriophage in adsorbed water.Particularly logical small area analysis, after low-voltage external power source, purifying water effect is better.The feature that the sorbing material that the present invention obtains has material to be easy to get, cheap, operating environment requirements is low and absorption property is high, will be used widely in medical science, veterinary science, food industry and the field such as the water relevant with microbial process and solution purification.
Description
Technical field
The invention belongs to sorbing material technical field, be specifically related to the preparation method of a kind of flax fiber/expanded graphite composite fibre sorbing material.
Background technology
Flax is the natural plant fibre that the mankind use the earliest.Apart from the history of modern existing more than 10,000 years.Flax fiber is a kind of rare natural fiber, only accounts for 1.5% of fiber total amount, due to the natural, ancient, noble of it and high-quality, have the laudatory title of " fiber queen ".By economic characteristics classification, generally there being flax of cultivating value to be divided into fiber flax, oil seed flax and Oil and Fibre Flax three major types type, fiber has higher economic worth with flax, all can processing and utilization to seed from former stem, and value of exploiting and utilizing is high.
Flax fiber is tough, soft and fine, its intensity is 1.5 times of cotton fiber, 1.6 times of spun silk, and limit count is high, and fabrics smooth is clean and tidy, the senior dress material of suitable for making; Flax fiber has that hygroscopicity is strong, rapid heat dissipation, rub resistance, high temperature resistant, nonflammable, not easily split, the particular advantages such as electric conductivity is little, dust-absorbing rate is low, bacteriostasis and health-care, suitable for making aeroplane fabric, military cloth, fire-fighting, aerospace, medical treatment and health care clothes and canvas, rotary hose, interior decoration cloth and technique sting rust product etc.; Scutching leftover bits and pieces and hards also have higher value, the short fiber after processing and numb flax, can produce mixed yarn, also can spin the pure dimity with hair, silk, cotton, chemical fibre etc.; Hards is the quality raw materials manufacturing artificial board or fine paper.
China's gross amount of water resources 2.8 tcm, occupies the 6th, the world.China's water resources ownership per capita only has 2150m3, is equivalent to 1/4 of the per capita water yield in the world.When to the year two thousand thirty, Chinese population reaches 1,600,000,000 peak, water resource only has 1760m3 per capita, will become accepted per capita lower than " short water supply " country of 1700m3 in the world.
According to China Environmental State Bulletin, in 752 emphasis sections of 2002 annual Haihe River, the Liaohe River, Huaihe River, the Yellow River, Song Hua River, the Changjiang river, the large water system monitoring of the Zhujiang River seven, I ~ III class water quality accounts for 29.5%, and IV class water quality accounts for 17.7%, and V class and bad V class water quality account for 52.8%.The monitoring of Ministry of Water Resources to 532 rivers shows, has the pollution that 436 rivers are subject in various degree, in the section, 15 major metropolitan of seven river, great river warps, has the water quality severe contamination of section, 13 cities.
What lake, the whole nation reached eutrophication water reaches 66%, and Main Lakes nitrogen and phosphorus pollution is heavier, and cause eutrophication problem to be given prominence to, blue-green algae is spread unchecked and is on the rise, and has a strong impact on the development of culture fishery and tourist industry, harm ecological environment.
Quality of groundwater also allows of no optimist.Show according to China's Evaluation of Groundwater Resources in 2003 and strategic issue research, have the groundwater resources of 63% can supply directly to drink, 17% is drinkable after suitably processing, and 8% needs just can drink after special disposal.12% is not suitable for drinking but can be used as industrial or agricultural resource of water supply, the whole nation about has the underground water pollution of half city proper serious, main contamination index comprises salinity, total hardness, nitrate, nitrite, ammonia nitrogen, iron, manganese, chloride, sulfate, fluoride, and pH value etc. are all in the trend of exceeding standard.The underground water that the whole nation about has more than 7,000 ten thousand people still drinking fluorine and exceed standard, 3.6 hundred million people in the countryside do not drink the drinking water meeting national standard.
In recent years, the Chinese government has started the improvement of drinking water pollution comprehensively.Especially by environmental protection with energy-conservationly rise to state basic policy, the improvement of drinking water, will more over a long time from now on as wherein important content, from water source, running water produces, water facilities to the purification of water tip, carry out comprehensive rebuilding and improving.
At present, flax fiber obtains development and application widely with the performance of its temperature adjustment, antiallergy, antistatic, antibacterial excellence, and the flax fiber new product of various health, environmental protection, new material constantly enter in people's life, are subject to popular favor.But the technology applied about utilizing composite fibre that flax fiber is base material to prepare the method for filtering material and the product aspect of flax fiber sorbing material have not been reported.Hydrone and bacterium are very small, and the bore hole of people cannot be seen, conveniently, generally in units of nanometer, mark its size.But under the microscope, the size of hydrone and bacterium is then far different.The diameter of single hydrone is far smaller than 1 nanometer, and the size of most of bacterium then has hundreds of nanometer.Generally microorganism and bacteriophage all can not be adsorbed to fall for the adsorbent filtering water source at present, and can only work in acidity and neutral environment.
Summary of the invention
Order of the present invention is to provide the preparation method of a kind of flax fiber/expanded graphite composite fibre sorbing material, this drainage sorbing material that exceedes synthesizes composite fibre using flax fiber as base starting material and expanded graphite, uses the boehmite manufacture that the composite fibre of flax fiber and expanded graphite and main component are aluminium hydroxide to form sorbing material.This drainage sorbing material that exceedes can produce positive charge, can adsorb electronegative microorganism and bacteriophage, reaches most microorganism and bacteriophage in adsorbed water.
For achieving the above object, the technical solution used in the present invention is as follows:
(1) flax is through degumming tech: raw ramie → infiltrate → come unstuck → strike fiber crops → wash → strike fiber crops → washing → drying → softness → drying → comb fiber crops, obtain flax fiber, for subsequent use; (Zhang Baosheng, Luwen is good, and simple analysis flax fiber comes unstuck and boiling-off of flax roving bleaching process, weaves in Heilungkiang, 04 phase in 1999)
(2) get expanded graphite in proportion and add deionized water, through sonic oscillation, form the homogeneous phase mixed liquor A of expanded graphite;
(3) after mixed liquor A being cooled to 0 DEG C, in ice-water bath, add Na0H, urea, flax fiber, stir and make mixed liquid B;
(4) deposit 1-3 hour by freezing at the temperature of-15 DEG C for mixed liquid B, then the mixed liquor of freezing state is placed on thawed at room temperature, stir 25-35 minute, obtained flax fiber and expanded graphite form homogeneous phase mixed liquor C;
(5) mixed liquor C is spurted into the H of high-speed stirred
2s0
4remove unnecessary Na0H in solution, obtain the fibrous flax fiber of hygrometric state and expanded graphite composite fibre; With deionized water rinsing composite fibre until the pH value of washing lotion reaches 7, composite fibre at room temperature dries naturally, then dries in an oven, obtains dry composite fiber;
(6) with silica suspension through Hydrothermal Synthesis process composite fibre (what grants complete, Du Haiyan, and grandson family jumps New Chemical Materials, the Hydrothermal Synthesis of inorganic nano material and deriving method thereof, 10 phases in 2007); Obtain silica tubulose covered composite yarn fiber;
(7) by the silica tubulose covered composite yarn fiber of gained and boehmite powder Homogeneous phase mixing; The mass ratio of silica tubulose covered composite yarn fiber and boehmite powder is 1/100-1/2;
(8) (mixture directly puts into the groove with pole plate, the spacing 10-20 centimetre of pole plate to carry out activation process with sinusoidal ac to mixture.Pole plate produces AC field to material producing life-stylize effect after loading alternating current between pole plate.); After activated process, the aluminium hydroxide bulky grain of non-spherical is attached to composite fiber surface, forms the sorbing material that eyelet is larger.
Expanded graphite/flax fiber weight ratio 1/10000 ~ 3/1000 described in step (2), the sonic oscillation time is 10-20 minute;
The part by weight of the Na0H, urea and the flax fiber that add in step (3) is 3:2:2, and the gross weight adding three kinds of materials accounts for 14% of the weight of mixed liquid B, and it is 10-20 minute that preparation mixed liquid B mixing time is made in described stirring.
H described in step (5)
2s0
4the concentration of solution is 3-7wt%.
Described in step (5), composite fibre at room temperature dries 2 days naturally, then dries 8-12 minute in the baking oven of 80 DEG C, obtains dry composite fiber.
Described in step (6), silica suspension concentration is 1%.
With the sinusoidal ac of 50 hertz frequencies, activation process is carried out to mixture in step (8).
Above material clamps through micropore mold, prepare various type shape filter, the above mould is cast, cup type, square, round according to the requirement of the filter type shape of required preparation, and the mould of the various shape such as sheet type, the various shape filter of required preparation can meet extensive filtering demand.
The drainage sorbing material that exceedes of the present invention synthesizes composite fibre using flax fiber as base starting material and expanded graphite, uses the boehmite manufacture that the composite fibre of flax fiber and expanded graphite and main component are aluminium hydroxide to form sorbing material.This drainage sorbing material that exceedes can produce positive charge, can adsorb electronegative microorganism and bacteriophage, reaches most microorganism and bacteriophage in adsorbed water.Particularly logical small area analysis, after low-voltage external power source, purifying water effect is better.
Flax fiber prepared by the present invention/expanded graphite composite fibre exceedes drainage sorbing material will provide one can eliminate bacterium in water fast, and can not block, and will bring a kind of simple and easy, cheap process for purifying water for social demand.Compared with current water filtration sorbing material, bioactive water filtering adsorbing material of the present invention has the advantages that material is easy to get, cheap, operating environment requirements is low and absorption property is high, will be used widely in medical science, veterinary science, food industry and the field such as the water relevant with microbial process and solution purification.The space that can develop is comparatively large, wide market.
Adopt the filter of embodiment 1, under pressure 0 .5mpa, filter the treatment effect of river as following table.
The content of other harmful substance of table 1 water sample purification front and back and removal rate (unit: mgL
-1)
Microbiological indicator test result and removal rate before and after the purification of table 2 water sample
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.
Embodiment 1
Flax is through degumming tech process: raw ramie → infiltrate → come unstuck → strike fiber crops → wash → strike fiber crops → washing → drying → softness → drying → comb fiber crops, obtain flax fiber, stand-by.Take weight 0.01g expanded graphite and put into 250mL beaker, add 100mL deionized water, sonic oscillation is after 15 minutes, form the homogeneous phase mixed liquor A of expanded graphite, the homogeneous phase mixed liquor of expanded graphite is put into refrigerator and cooled but after 0 DEG C, 6.0gNa0H is added in ice-water bath, 4.0g urea (urea), 4.0g flax fiber, stir 15 minutes, mixed liquor (containing 6wt%NaOH, 4wt%Urea, 4wt%MCC and 0.01g expanded graphite) is put into the refrigerator of-15 DEG C, cooled and stored 2 hours.Again the mixed liquor of freezing state is placed on thawed at room temperature, and stirs 30 minutes, obtained flax fiber and expanded graphite form homogeneous mixed solution, obtained flax fiber and expanded graphite homogeneous mixed solution are spurted into the H of the 5wt% of high-speed stirred
2s0
4remove unnecessary Na0H in solution, obtain the fibrous flax fiber of hygrometric state and expanded graphite composite fibre.With deionized water rinsing composite fibre until the pH value of washing lotion reaches 7, composite fibre at room temperature dries 2 days naturally, dry 10 minutes in the baking oven of 80 DEG C again, obtain dry composite fiber, be that the silica suspension of 1% is through Hydrothermal Synthesis process composite fibre by concentration, obtain silica tubulose covered composite yarn fiber, by silica tubulose covered composite yarn fiber and boehmite powder Homogeneous phase mixing, put into microporous pipe mould, with the sinusoidal ac of 50 hertz frequencies, activation process is carried out to mixture, after activated process, the aluminium hydroxide bulky grain of non-spherical is attached to composite fiber surface, forming thickness is 1 centimetre, pore-size distribution is at the flake porous filtering material of 0.01 um-30um, clamp through micropore mold, be prepared into cast filter.
Embodiment 2
Flax is through degumming tech process: raw ramie → infiltrate → come unstuck → strike fiber crops → wash → strike fiber crops → washing → drying → softness → drying → comb fiber crops, obtain flax fiber, stand-by.Take weight 0.09g expanded graphite and put into 250mL beaker, add 100mL deionized water, sonic oscillation is after 30 minutes, forms the homogeneous phase mixed liquor of expanded graphite, the homogeneous phase mixed liquor of expanded graphite put into refrigerator and cooled but after 0 DEG C, 12.0gNa0H is added in ice-water bath, 8.0g urea (urea), 8.0g flax fiber, stirs 30 minutes, mixed liquor is put into the refrigerator of-15 DEG C, cooled and stored 2 hours.Again the mixed liquor of freezing state is placed on thawed at room temperature, and stirs 40 minutes, obtained flax fiber and expanded graphite form homogeneous mixed solution, obtained flax fiber and expanded graphite homogeneous mixed solution are spurted into the H of the 5wt% of high-speed stirred
2s0
4remove unnecessary Na0H in solution, obtain the fibrous flax fiber of hygrometric state and expanded graphite composite fibre.With deionized water rinsing composite fibre until the pH value of washing lotion reaches 7, composite fibre at room temperature dries 3 days naturally, dry 10 minutes in the baking oven of 80 DEG C again, obtain dry composite fiber, be that the silica suspension of 1% is through Hydrothermal Synthesis process composite fibre by concentration, obtain silica tubulose covered composite yarn fiber, by silica tubulose covered composite yarn fiber and boehmite powder Homogeneous phase mixing, the sinusoidal ac putting into micropore cup type mould 100 hertz frequencies carries out activation process to mixture, after activated process, the aluminium hydroxide bulky grain of non-spherical is attached to composite fiber surface, forming thickness is 1 centimetre, pore-size distribution is at the flake porous filtering material of 0.01 um-30um, clamp through micropore mold, be prepared into cup type filter.
Embodiment 3
Flax is through degumming tech process: raw ramie → infiltrate → come unstuck → strike fiber crops → wash → strike fiber crops → washing → drying → softness → drying → comb fiber crops, obtain flax fiber, stand-by.Take weight 0.15g expanded graphite and put into 250mL beaker, add 100mL deionized water, sonic oscillation is after 20 minutes, forms the homogeneous phase mixed liquor of expanded graphite, the homogeneous phase mixed liquor of expanded graphite put into refrigerator and cooled but after 0 DEG C, 18.0gNa0H is added in ice-water bath, 12.0g urea (urea), 12.0g flax fiber, stirs 40 minutes, mixed liquor is put into the refrigerator of-15 DEG C, cooled and stored 2 hours.Again the mixed liquor of freezing state is placed on thawed at room temperature, and stirs 50 minutes, obtained flax fiber and expanded graphite form homogeneous mixed solution, obtained flax fiber and expanded graphite homogeneous mixed solution are spurted into the H of the 5wt% of high-speed stirred
2s0
4remove unnecessary Na0H in solution, obtain the fibrous flax fiber of hygrometric state and expanded graphite composite fibre.With deionized water rinsing composite fibre until the pH value of washing lotion reaches 7, composite fibre at room temperature dries 3 days naturally, dry 10 minutes in the baking oven of 80 DEG C again, obtain dry composite fiber, be that the silica suspension of 1% is through Hydrothermal Synthesis process composite fibre by concentration, obtain silica tubulose covered composite yarn fiber, by silica tubulose covered composite yarn fiber and boehmite powder Homogeneous phase mixing, put into microporous sheet mould, with the sinusoidal ac of 100 hertz frequencies, activation process is carried out to mixture, after activated process, the aluminium hydroxide bulky grain of non-spherical is attached to composite fiber surface, forming thickness is 1 centimetre, pore-size distribution is at the flake porous filtering material of 0.01 um-30um, clamp through micropore mold, be prepared into sheet type filter.
Claims (1)
1. a preparation method for flax fiber/expanded graphite composite fibre sorbing material, is characterized in that, comprise the steps:
(1) flax is through degumming tech: raw ramie → infiltrate → come unstuck → strike fiber crops → wash → strike fiber crops → washing → drying → softness → drying → comb fiber crops, obtain flax fiber, for subsequent use;
(2) get expanded graphite in proportion and add deionized water, through sonic oscillation, form the homogeneous phase mixed liquor A of expanded graphite;
(3) after mixed liquor A being cooled to 0 DEG C, in ice-water bath, add Na0H, urea, flax fiber, stir and make mixed liquid B; The part by weight of the Na0H added, urea and flax fiber is 3:2:2, and the gross weight adding three kinds of materials accounts for 14% of the weight of mixed liquid B, and it is 10-20 minute that preparation mixed liquid B mixing time is made in described stirring;
(4) deposit 1-3 hour by freezing at the temperature of-15 DEG C for mixed liquid B, then the mixed liquor of freezing state is placed on thawed at room temperature, stir 25-35 minute, obtained flax fiber and expanded graphite form homogeneous phase mixed liquor C;
(5) mixed liquor C is spurted into the H of high-speed stirred
2s0
4remove unnecessary Na0H in solution, obtain the fibrous flax fiber of hygrometric state and expanded graphite composite fibre; With deionized water rinsing composite fibre until the pH value of washing lotion reaches 7, composite fibre at room temperature dries naturally, then dries in an oven, obtains dry composite fiber; Described H
2s0
4the concentration of solution is 3-7wt%; Described composite fibre at room temperature dries 2 days naturally, then dries 8-12 minute in the baking oven of 80 DEG C, obtains dry composite fiber;
(6) use silica suspension through Hydrothermal Synthesis process composite fibre; Obtain silica tubulose covered composite yarn fiber; Described silica suspension concentration is 1%;
(7) by the silica tubulose covered composite yarn fiber of gained and boehmite powder Homogeneous phase mixing; The mass ratio of silica tubulose covered composite yarn fiber and boehmite powder is 1/100-1/2;
(8) with sinusoidal ac, activation process is carried out to mixture; After activated process, the aluminium hydroxide bulky grain of non-spherical is attached to composite fiber surface, forms sorbing material;
With the sinusoidal ac of 50 hertz frequencies, activation process is carried out to mixture in step (8).
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| JP2503497B2 (en) * | 1987-03-30 | 1996-06-05 | 日立化成工業株式会社 | Graphite / fiber composite material |
| US20030198659A1 (en) * | 2001-10-25 | 2003-10-23 | Hoffmann Michael P. | Fibrous pest control |
| CN2872872Y (en) * | 2006-04-03 | 2007-02-28 | 洛阳深奥科技开发有限公司 | Expansion graphite composite cigarette filter tip |
| US20090178970A1 (en) * | 2008-01-16 | 2009-07-16 | Ahlstrom Corporation | Coalescence media for separation of water-hydrocarbon emulsions |
| WO2010139816A1 (en) * | 2009-06-05 | 2010-12-09 | Desarrollos Tecnicos Mc, S.L. | Composition and use of an adsorbent material for filtering toxic components during the process of incineration and/or distillation of glycerine generated from the production of biodiesel |
| CN102174214B (en) * | 2011-03-07 | 2014-05-21 | 海南光宇生物科技有限公司 | Bacterial cellulose/graphene composite material and preparation method thereof |
| CN102489259B (en) * | 2011-11-10 | 2013-08-21 | 河南大学 | Graphene oxide/cellulose compound material as well as preparation method and application of same |
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