CN103083136B - Bacterial cellulose liquid absorbing material of sandwich structure and preparation method of bacterial cellulose liquid absorbing material - Google Patents
Bacterial cellulose liquid absorbing material of sandwich structure and preparation method of bacterial cellulose liquid absorbing material Download PDFInfo
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- CN103083136B CN103083136B CN201210575842.0A CN201210575842A CN103083136B CN 103083136 B CN103083136 B CN 103083136B CN 201210575842 A CN201210575842 A CN 201210575842A CN 103083136 B CN103083136 B CN 103083136B
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Abstract
The invention relate to bacterial cellulose liquid absorbing material of a sandwich structure and a preparation method of the bacterial cellulose liquid absorbing material. The bacterial cellulose liquid absorbing material of the sandwich structure is prepared by the steps such as culture expansion cultivation, stationary culture and postprocessing, and composed of three bacterial cellulose membranes which are tightly combined, the three bacterial cellulose membranes comprise an upper ultra absorbing layer, a lower ultra absorbing layer and a liquid storing layer in the middle. Tight combination refers to that cellulose microfiber of the upper ultra absorbing layer and the lower ultra absorbing layer are combined with cellulose microfiber of the liquid storing layer by intermolecular and intermolecular hydrogen bonding in bi-1, 4-glucan chain to form a molecular layer, layers are combined by intermolecular and intermolecular hydrogen bonding, obvious physical layering does not exist, and structural continuity is good. Prepared liquid absorbing material has good liquid absorbing performance, water binding capacity, biocompatibility and mechanical performance. The bacterial cellulose liquid absorbing material of the sandwich structure is simple and quick in preparation process, green and environmental-friendly, short in cultivation period, low in cost, and applied to the fields such as medicine, personal care and daily-used mechanical industry.
Description
Technical field
The present invention relates to Bacterial cellulose liquid-absorbent material of a kind of liquid-absorbent material and preparation method thereof, particularly a kind of sandwich structure and preparation method thereof.
Background technology
At present, liquid-absorbent material has a wide range of applications in a lot of fields.As: the hemostatic material in bio-medical field, can control blood oozing from the wound surface, guarantee that surgical field of view is clear, improve operation efficiency; The dressing of absorbing wound exudate, can extend the service time of dressing on exudative wound, reduces treatment cost, effectively shortens the healing time of wound; For the liquid-absorbent material of personal nursing, can be applied to diaper, temper trousers, sanitary towel, underwear, binder etc. for incontinence, clean, comfortable Personal hygiene environment is provided.
Liquid-absorbent material requirements material has the ability of good absorption liquid, conventionally uses the good macromolecular material of hydrophilic.And along with social progress, the raising of people's quality of the life, has higher requirement to liquid-absorbent material.Require liquid-absorbent material to there is better liquid-absorbent, biocompatibility, comfortableness and mechanical property.
Bacterial cellulose (Bacterial Cellulose also claims micro organism cellulose) is a kind of nano-fiber material.It is using bacterial cell inside as biosynthesis reactor, glucose micromolecule allosteric process through series of complex under enzyme catalysis is finally passed through to β-1,4-glycosidic bond is extruded in conjunction with forming the catalytic site that β-Isosorbide-5-Nitrae-Fructus Vitis viniferae sugar chain is pne cell by antibacterial.β-Isosorbide-5-Nitrae-Fructus Vitis viniferae sugar chain is and intermolecular hydrogen bonding effect interior by molecule each other, progressively, hierarchically forms lipopolysaccharide layer, tactoid, cellulose fento the final cellulose that forms.This series of extracellular (Extracellular) forming process is called as " cellulosic self assembly ".The process that this unique microorganism participates in has just given Bacterial cellulose good physicochemical property
Bacteria cellulose material has ultra-fine tridimensional network; Good moisture absorption, moisturizing and permeability; The retentiveness of superelevation and wet strength; High-tensile and elastic modelling quantity etc.Large quantity research shows that bacteria cellulose material has in good body, biocompatibility in vitro, add shape Modulatory character that it is excellent and shape maintains make its in construct, vitro tissue engineering scaffold material has advantageous advantage.The industries such as food, medicine, weaving, papermaking, chemical industry, oil recovery, ore dressing are applied at present.Along with updating of fermentation technology, output and the production capacity of Bacterial cellulose are improved gradually, and cost reduces gradually.The liquid-absorbent material of preparing with Bacterial cellulose can be widely used in each fields such as medicine, personal nursing, daily-use chemical industry.
Summary of the invention
The Bacterial cellulose liquid-absorbent material of a kind of sandwich structure of the present invention, be to close bacteria cellulose film closely by three-layered node to form, described three-layered node closes bacteria cellulose film closely and comprises super layer and the lower super reserve liquid layer of inhaling layer and mediating inhaled; Described combination closely refers to that the cellulose microfibril of described super suction layer and the cellulose microfibril of described reserve liquid layer are by β-1, in molecule in 4-Fructus Vitis viniferae sugar chain, be combined with intermolecular hydrogen bonding, form molecular layer, also be combined with intermolecular hydrogen bonding by molecule between layers, without obvious physical layering; The elementary cell of composition Bacterial cellulose is not single β-1,4-Fructus Vitis viniferae sugar chain, but pre-microfibril (premicrofibril), it is made up of β-Isosorbide-5-Nitrae-Fructus Vitis viniferae sugar chain, every 9 β-1,4-Fructus Vitis viniferae sugar chain is parallel to each other, and by being combined with intermolecular hydrogen bonding in molecule, is left hand triple helical shape, be the ultimate unit of composition microfibril (microfibril), diameter is 1.5nm.Microfibril (microfibril) diameter is 3.5nm, between fento and fento, is combined with intermolecular hydrogen bonding by molecule, and β-Isosorbide-5-Nitrae-Fructus Vitis viniferae sugar chain is parallel arrangement, forms cellulose I type crystalline texture.
The wherein said super content of cellulose of inhaling in layer and lower super suction layer is 0.7 × 10
-2～1.0 × 10
-2g/cm
3, the content of cellulose in described reserve liquid layer is 0.2 × 10
-2～0.5 × 10
-2g/cm
3.
As preferred technical scheme:
The Bacterial cellulose liquid-absorbent material of a kind of sandwich structure as above, described bacteria cellulose film is to be left standstill under condition of culture by strain, consumption sugar source, with synthetic β-Isosorbide-5-Nitrae-Fructus Vitis viniferae sugar chain in cell and extrude cells in vitro.Article 3～4, β-1,4-Fructus Vitis viniferae sugar chain is by forming lipopolysaccharide layer with intermolecular hydrogen bonding effect in molecule, 4～5 lipopolysaccharide layers are by forming the tactoid of diameter in 1.5nm left and right with intermolecular hydrogen bonding in molecule, 3～5 tactoids are by forming the cellulose microfibril of diameter in 3.5nm left and right with intermolecular hydrogen bonding in molecule, many microfibrils are by forming cellulose tow with intermolecular hydrogen bonding effect in molecule, and many tow are by forming cellulose silk ribbon with intermolecular hydrogen bonding effect in molecule.Bacterium cell, at culture fluid surface disordered motion, ruptures even if cell generation division can not affect cellulose silk ribbon yet.Be interweaved by the cellulose microfibril forming with intermolecular hydrogen bonding in molecule by β-Isosorbide-5-Nitrae-Fructus Vitis viniferae sugar chain, pass through each other to interact with intermolecular hydrogen bonding in molecule, finally form similar and bacteria cellulose film nonwoven fabric construct at liquid level.
The thickness of the Bacterial cellulose liquid-absorbent material of sandwich structure as above is 9～16mm, and the wherein said super thickness of inhaling layer and lower super suction layer is 3～4mm, and the thickness of described reserve liquid layer is 3～8mm.
The present invention also provides a kind of preparation method of Bacterial cellulose liquid-absorbent material of sandwich structure, comprises the following steps:
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 2～5, peptone 0.05 ~ 0.5, yeast extract 0.05 ~ 0.5, citric acid 0.05 ~ 0.5, sodium hydrogen phosphate 0.05 ~ 0.5, potassium dihydrogen phosphate 0.05 ~ 0.5, surplus is water;
The pH of fermentation culture is 4.0～6.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is 2 × 10
5～2 × 10
7individual/ml.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 28～32 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent in the upper and lower part of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1～2 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2～3 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, keeps carrier of oxygen volume concentrations in 10～1% scopes simultaneously; Reach 0.5～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 3～6 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 1～2 day, pressurization makes the air pressure contacting with Bacterial cellulose upper surface within the scope of 1.1～1.5 normal atmospheres, improves oxygen concentration to 50% simultaneously; Until Bacterial cellulose film thickness rises to 3～4mm;
Reserve liquid layer formation stages 1～3 day, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 10～15% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～8mm;
Upper super suction layer formation stages 1～2 day, pressurization makes the air pressure contacting with Bacterial cellulose upper surface within the scope of 1.1～1.5 normal atmospheres, improve oxygen concentration to 50% simultaneously, until Bacterial cellulose film thickness is while rising to 9～12mm, taken out, must be possessed the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1～10wt%, boil and keep 2～10 hours, with pure water clean to pH be 7.0, by Bacterial cellulose thin film after treatment lyophilization or the processing of part setting-out, be the Bacterial cellulose liquid-absorbent material of sandwich structure again.
The preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure as above, after described high pressure steam sterilization, ultraviolet irradiation refers to that above-mentioned fermentation culture is placed in high-pressure sterilizing pot to 121 ℃ of sterilization treatment to be taken out after 30 minutes and be placed in irradiation under uviol lamp and be cooled to room temperature.
Strain as above refers to can the cellulosic microorganism of biosynthesis, comprising: acetobacter xylinum, produce one or more in acetobacter, acetify bacillus, Acetobacter pasteurianus, glucose bacillus, Agrobacterium, root nodule bacteria, sarcina, Pseudomonas cepacia, Pseudomonas cocovenenans or campylobacter jejuni.
The preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure as above, described logical pure oxygen refers to medical oxygen is passed in above-mentioned culture fluid with the speed of 1L/min, and maintains 30 minutes; Described inoculation refers to the inoculating loop after sterilizing and hooks up and be stored in right amount the strain in test tube at 4 ℃, and is transferred in above-mentioned fermentation culture; Described spreading cultivation refers to the shaking table at 28～32 ℃ of the fermentation culture after access strain cultivated 8～24 hours.
The preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure as above, described moment pressurization, continuous pressure and the three kinds of forms of interim pressurization of being pressurised into.
The preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure as above, the pressurization of described moment refers in 30 minutes and internal tank air pressure is promoted in 1.1～1.5 barometric pressure range, maximum is no more than 1.5 atmospheric pressure; Described continuous pressure refers to the air that is 0.1389～2.083% to charged pressure percent in container per hour, and radix is 1 normal atmosphere, until container inner air pressure is no longer to increase pressure within the scope of 1.1～1.5 normal atmospheres time; The pressurization of described stage refers to the every 12 hours air that are 1.67～25% to charged pressure percent in container, and radix is 1 normal atmosphere equally, until container inner air pressure is no longer to increase pressure within the scope of 1.1～1.5 normal atmospheres time.
The preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure as above, described raising oxygen concentration is moment oxygen supplement, increases continuously and three kinds of modes of interim increase;
Described moment oxygen supplement refers to: in 30 minutes, oxygen partial pressure is promoted to 50%;
Described increasing continuously refers to: oxygen concentration increase by 48.61～166.67% per hour, and radix is 10～15%, until oxygen concentration no longer increases while being 50%;
Described stage increase refers to: every 12 hours of oxygen concentration increases by 583.3～2000%, until oxygen concentration no longer increases while reaching 50%.
The preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure as above, the preparation method of the Bacterial cellulose liquid-absorbent material of described a kind of sandwich structure, it is characterized in that, described reduction air pressure refers to: the air pressure contacting with bacteria cellulose film upper surface in by container in 30 minutes is reduced to 1 normal atmosphere; Described reduction oxygen concentration refers to: in 30 minutes by container in oxygen concentration be reduced in 10～15% scopes.
Bacterial cellulose possesses its unique physics, chemistry and engineering properties as a kind of novel natural water gel: ultra-fine network structure; High-tensile and elastic modelling quantity; High-hydrophilic, good ventilative, water suction, water permeability, and have outstanding retentiveness and high wet strength.The microfibril bundle diameter of Bacterial cellulose is 3～4nm, and the cellosilk bandwidth being connected into by microfiber bundle is 70～80nm, and length is 1～9 μ m, is the thinnest current natural fiber.
Bacterial cellulose liquid-absorbent material of a kind of sandwich structure of this patent invention and preparation method thereof, in cultivation process, by controlling the air pressure and the oxygen concentration that contact with Bacterial cellulose thin film, obtain a kind of by upper super layer, the lower super reserve liquid layer of inhaling layer and mediating inhaled, in conjunction with the Bacterial cellulose liquid-absorbent material of the sandwich structure closely forming.This liquid-absorbent material has good liquid-absorbent, retentiveness, comfortableness, biocompatibility and mechanical property, preparation process is simple and quick, environmental protection, and cultivation cycle is short, with low cost, can be applied to each fields such as medicine, personal nursing, daily-use chemical industry.
Beneficial effect:
With prior art first than, the invention has the beneficial effects as follows:
(1) Bacterial cellulose liquid-absorbent material of a kind of sandwich structure and preparation method thereof, preparation process is continuous, super suction between layer and reserve liquid layer by nanometer microfibril by being combined with intermolecular hydrogen bonding in molecule.Make cellulose microfibril that β-Isosorbide-5-Nitrae-Fructus Vitis viniferae sugar chain forms by be combined with intermolecular hydrogen bonding in molecule and the process of crystalline forming in, spontaneous, form the fine and close structure to the gradual change of loosening in an orderly manner.Combination degree is darker, is not only confined to material surface.
(2) a Bacterial cellulose liquid-absorbent material for sandwich structure, without obvious physical layering, structural continuity is good; The super layer of inhaling changes and makes material possess good mechanical performance with the interior structure gradient existing of reserve liquid layer.
(3) Bacterial cellulose liquid-absorbent material of a kind of sandwich structure and preparation method thereof, on prior art basis, by increasing the air pressure contacting with Bacterial cellulose thin film in cultivation process, make the inner aerobic of Bacterial cellulose thin film district area change; Simultaneously accurate controlled pressure, does not make Bacterial cellulose thin film sink.Improve in prior art and only relied on raising oxygen partial pressure to construct the single technique of density structure, also solved the defect that too high the caused cellulose growth rate of oxygen partial pressure slows down simultaneously.
(4) Bacterial cellulose liquid-absorbent material of a kind of sandwich structure and preparation method thereof, there is good fluid absorbent and water retention property, by controlling reserve liquid layer and upper and lower super thickness and thickness proportion of inhaling layer in liquid-absorbent material, can effectively regulate the maximum absorption, liquid absorption of liquid absorbent material, effective soak time etc.
(5) Bacterial cellulose liquid-absorbent material of a kind of sandwich structure and preparation method thereof, preparation process is simple and quick, environmental protection, cultivation cycle is short, with low cost, can be applied to each fields such as medicine, personal nursing, daily-use chemical industry.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
The Bacterial cellulose liquid-absorbent material of a kind of sandwich structure of the present invention, be to close bacteria cellulose film closely by three-layered node to form, described three-layered node closes bacteria cellulose film closely and comprises super layer and the lower super reserve liquid layer of inhaling layer and mediating inhaled; Described combination closely refers to that the cellulose microfibril of described super suction layer and the cellulose microfibril of described reserve liquid layer are by β-1, in molecule in 4-Fructus Vitis viniferae sugar chain, be combined with intermolecular hydrogen bonding, form molecular layer, also be combined with intermolecular hydrogen bonding by molecule between layers, without obvious physical layering; The elementary cell of composition Bacterial cellulose is not single β-1,4-Fructus Vitis viniferae sugar chain, but pre-microfibril (premicrofibril), it is made up of β-Isosorbide-5-Nitrae-Fructus Vitis viniferae sugar chain, every 9 β-1,4-Fructus Vitis viniferae sugar chain is parallel to each other, and by being combined with intermolecular hydrogen bonding in molecule, is left hand triple helical shape, be the ultimate unit of composition microfibril (microfibril), diameter is 1.5nm.Microfibril (microfibril) diameter is 3.5nm, between fento and fento, is combined with intermolecular hydrogen bonding by molecule, and β-Isosorbide-5-Nitrae-Fructus Vitis viniferae sugar chain is parallel arrangement, forms cellulose I type crystalline texture.
The wherein said super layer of inhaling is 0.7 × 10 with the lower super content of cellulose of inhaling in layer
-2～1.0 × 10
-2g/cm
3, the content of cellulose in described reserve liquid layer is 0.2 × 10
-2～0.5 × 10
-2g/cm
3.
Described bacteria cellulose film is by strain consumption sugar source, and eccrine fiber element microfibril is by being combined formation with intermolecular hydrogen bonding in molecule.
The thickness of the Bacterial cellulose liquid-absorbent material of described sandwich structure is 9～16mm, and the wherein said super thickness of inhaling layer and lower super suction layer is 3～4mm, and the thickness of described reserve liquid layer is 3～8mm.
Embodiment 1
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 2, and peptone 0.05, yeast extract 0.05, citric acid 0.01, sodium hydrogen phosphate 0.02, potassium dihydrogen phosphate 0.01, surplus is water;
The pH of fermentation culture is 4.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is 2 × 10
5.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 28 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 10% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 3 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 1 day, pressurization makes the air pressure contacting with Bacterial cellulose upper surface within the scope of 1.1～1.5 normal atmospheres, improves oxygen concentration to 50% simultaneously; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 1 day, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 10～15% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 1 day, pressurization makes the air pressure contacting with Bacterial cellulose upper surface within the scope of 1.1～1.5 normal atmospheres, improve in oxygen concentration to 50% scope simultaneously, until Bacterial cellulose film thickness is while rising to 9～16mm, taken out, must be possessed the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1wt%, boil and keep 10 hours, with pure water clean to pH be 7.0, by Bacterial cellulose thin film after treatment lyophilization, be the Bacterial cellulose liquid-absorbent material of sandwich structure again.
Embodiment 2
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 5, and peptone 0.5, yeast extract 0.5, citric acid 0.1, sodium hydrogen phosphate 0.2, potassium dihydrogen phosphate 0.1, surplus is water;
The pH of fermentation culture is 6.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is 2 × 10
7.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 32 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 2 days Bacterial cellulose growth inducing phases: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 3 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 15% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 8 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 3 days, pressurization makes the air pressure contacting with Bacterial cellulose upper surface within the scope of 1.5 normal atmospheres, improves oxygen concentration to 50% simultaneously; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 2 days, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 15% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 3 days, pressurization makes the air pressure contacting with Bacterial cellulose upper surface within the scope of 1.5 normal atmospheres, improve in oxygen concentration to 50% scope simultaneously, until Bacterial cellulose film thickness is while rising to 9～16mm, taken out, must be possessed the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 10wt%, boil and keep 2 hours, with pure water clean to pH be 7.0, by Bacterial cellulose thin film after treatment lyophilization, be the Bacterial cellulose liquid-absorbent material of sandwich structure again.
Embodiment 3
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 3, and peptone 0.3, yeast extract 0.3, citric acid 0.05, sodium hydrogen phosphate 0.1, potassium dihydrogen phosphate 0.05, surplus is water;
The pH of fermentation culture is 5.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is 2 × 10
7.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 30 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 12.5% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 6 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 2 days, pressurization makes the air pressure contacting with Bacterial cellulose upper surface within the scope of 1.3 normal atmospheres, improves oxygen concentration to 50% simultaneously; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 2 days, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 12.5% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 2 days, pressurization makes the air pressure contacting with Bacterial cellulose upper surface within the scope of 1.3 normal atmospheres, improve in oxygen concentration to 50% scope simultaneously, until Bacterial cellulose film thickness is while rising to 9～16mm, taken out, must be possessed the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 2wt%, boil and keep 4 hours, with pure water clean to pH be 7.0, by Bacterial cellulose thin film after treatment lyophilization, be the Bacterial cellulose liquid-absorbent material of sandwich structure again.
Embodiment 4
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 5, and peptone 0.5, yeast extract 0.5, citric acid 0.1, sodium hydrogen phosphate 0.2, potassium dihydrogen phosphate 0.1, surplus is water;
The pH of fermentation culture is 5.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is 2 × 10
7.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 30 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 10% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 8 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 3 days, moment pressurization, in 30 minutes, make the air pressure contacting with Bacterial cellulose upper surface be promoted to 1.1 normal atmospheres, moment oxygen supplement simultaneously, makes the oxygen concentration contacting with Bacterial cellulose upper surface be increased to 50% in 30 minutes; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 2 days, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 10～15% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 3 days, moment pressurization, in 30 minutes, make the air pressure contacting with Bacterial cellulose upper surface be promoted to 1.1 normal atmospheres, moment oxygen supplement simultaneously, makes the oxygen concentration contacting with Bacterial cellulose upper surface be increased to 50% in 30 minutes; Until Bacterial cellulose film thickness while rising to 9～16mm, is taken out, must possess the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1wt%, boil and keep 2 hours, with pure water clean to pH be 7.0, by Bacterial cellulose thin film after treatment lyophilization, be the Bacterial cellulose liquid-absorbent material of sandwich structure again.
Embodiment 5
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 5, and peptone 0.5, yeast extract 0.5, citric acid 0.1, sodium hydrogen phosphate 0.2, potassium dihydrogen phosphate 0.1, surplus is water;
The pH of fermentation culture is 5.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is 2 × 10
7.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 30 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 10% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 8 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 3 days, moment pressurization, in 30 minutes, make the air pressure contacting with Bacterial cellulose upper surface be promoted to 1.5 normal atmospheres, moment oxygen supplement simultaneously, makes the oxygen concentration contacting with Bacterial cellulose upper surface be increased to 50% in 30 minutes; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 2 days, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 10～15% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 3 days, moment pressurization, in 30 minutes, make the air pressure contacting with Bacterial cellulose upper surface be promoted to 1.5 normal atmospheres, moment oxygen supplement simultaneously, makes the oxygen concentration contacting with Bacterial cellulose upper surface be increased to 50% in 30 minutes; Until Bacterial cellulose film thickness while rising to 9～16mm, is taken out, must possess the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1wt%, boil and keep 2 hours, with pure water clean to pH be 7.0, by Bacterial cellulose thin film after treatment lyophilization, be the Bacterial cellulose liquid-absorbent material of sandwich structure again.
Embodiment 6
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 5, and peptone 0.5, yeast extract 0.5, citric acid 0.1, sodium hydrogen phosphate 0.2, potassium dihydrogen phosphate 0.1, surplus is water;
The pH of fermentation culture is 5.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is at 2 × 107/mL.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 30 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 10% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 8 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 3 days, continuous pressure, the air that is 0.1389% to charged pressure percent in container per hour, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is 1.1 normal atmospheres, increase continuously oxygen concentration, increase by 48.61% per hour simultaneously, radix is 10%, until oxygen concentration no longer increases while being 50%; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 2 days, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 10% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 3 days, continuous pressure, the air that is 0.1389% to charged pressure percent in container per hour, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is 1.1 normal atmospheres, increase continuously oxygen concentration, increase by 48.61% per hour simultaneously, radix is 10%, until oxygen concentration no longer increases while being 50%; Until Bacterial cellulose film thickness while rising to 9～16mm, is taken out, must possess the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1wt%, boil and keep 2 hours, with pure water clean to pH be 7.0, again Bacterial cellulose film portion setting-out after treatment is processed to solid content be 80%, be the Bacterial cellulose liquid-absorbent material of sandwich structure.
Embodiment 7
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 5, and peptone 0.5, yeast extract 0.5, citric acid 0.1, sodium hydrogen phosphate 0.2, potassium dihydrogen phosphate 0.1, surplus is water;
The pH of fermentation culture is 5.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is at 2 × 107/mL.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 30 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 10% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 8 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 3 days, continuous pressure, the air that is 2.083% to charged pressure percent in container per hour, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is 1.5 normal atmospheres, increase continuously oxygen concentration, increase by 166.67% per hour simultaneously, radix is 10%, until oxygen concentration no longer increases while being 50%; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 2 days, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 10% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 3 days, continuous pressure, the air that is 2.083% to charged pressure percent in container per hour, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is 1.5 normal atmospheres, increase continuously oxygen concentration, increase by 166.67% per hour simultaneously, radix is 10%, until oxygen concentration no longer increases while being 50%; Until Bacterial cellulose film thickness while rising to 9～16mm, is taken out, must possess the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1wt%, boil and keep 2 hours, with pure water clean to pH be 7.0, again Bacterial cellulose film portion setting-out after treatment is processed to solid content be 70%, be the Bacterial cellulose liquid-absorbent material of sandwich structure.
Embodiment 8
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 5, and peptone 0.5, yeast extract 0.5, citric acid 0.1, sodium hydrogen phosphate 0.2, potassium dihydrogen phosphate 0.1, surplus is water;
The pH of fermentation culture is 5.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is 2 × 10
7individual/mL.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 30 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 10% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 8 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 3 days, continuous pressure, the air that is 1% to charged pressure percent in container per hour, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is 1.3 normal atmospheres, increase continuously oxygen concentration, increase by 100% per hour simultaneously, radix is 10%, until oxygen concentration no longer increases while being 50%; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 2 days, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 10% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 3 days, continuous pressure, the air that is 1% to charged pressure percent in container per hour, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is 1.3 normal atmospheres, increase continuously oxygen concentration, increase by 100% per hour simultaneously, radix is 10%, until oxygen concentration no longer increases while being 50%; Until Bacterial cellulose film thickness while rising to 9～16mm, is taken out, must possess the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1wt%, boil and keep 2 hours, with pure water clean to pH be 7.0, again Bacterial cellulose film portion setting-out after treatment is processed to solid content be 60%, be the Bacterial cellulose liquid-absorbent material of sandwich structure.
Embodiment 9
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 5, and peptone 0.5, yeast extract 0.5, citric acid 0.1, sodium hydrogen phosphate 0.2, potassium dihydrogen phosphate 0.1, surplus is water;
The pH of fermentation culture is 5.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is at 2 × 107/mL.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 30 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 10% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 8 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 3 days, interim pressurization, the every 12 hours air that are 1.67% to charged pressure percent in container, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is no longer pressurizeed while being 1.1 normal atmospheres, simultaneously the interim oxygen concentration that increases, increases by 583.3% in every 12 hours, until oxygen concentration no longer increases while reaching 50%; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 2 days, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 10% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 3 days, interim pressurization, the every 12 hours air that are 1.67% to charged pressure percent in container, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is no longer pressurizeed while being 1.1 normal atmospheres, the interim oxygen concentration that increases simultaneously, within every 12 hours, increase by 583.3%, until oxygen concentration no longer increases while reaching 50%, until Bacterial cellulose film thickness is while rising to 9～16mm, taken out, must be possessed the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1wt%, boil and keep 2 hours, with pure water clean to pH be 7.0, again Bacterial cellulose film portion setting-out after treatment is processed to solid content be 50%, be the Bacterial cellulose liquid-absorbent material of sandwich structure.
Embodiment 10
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 5, and peptone 0.5, yeast extract 0.5, citric acid 0.1, sodium hydrogen phosphate 0.2, potassium dihydrogen phosphate 0.1, surplus is water;
The pH of fermentation culture is 5.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is 2 × 10
7individual/mL.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 30 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 10% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 8 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 3 days, interim pressurization, the every 12 hours air that are 25% to charged pressure percent in container, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is no longer pressurizeed while being 1.5 normal atmospheres, simultaneously the interim oxygen concentration that increases, increases by 2000% in every 12 hours, until oxygen concentration no longer increases while reaching 50%; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 2 days, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 10% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 3 days, interim pressurization, the every 12 hours air that are 25% to charged pressure percent in container, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is no longer pressurizeed while being 1.5 normal atmospheres, the interim oxygen concentration that increases simultaneously, within every 12 hours, increase by 2000%, until oxygen concentration no longer increases while reaching 50%, until Bacterial cellulose film thickness is while rising to 9～16mm, taken out, must be possessed the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1wt%, boil and keep 2 hours, with pure water clean to pH be 7.0, again Bacterial cellulose film portion setting-out after treatment is processed to solid content be 30%, be the Bacterial cellulose liquid-absorbent material of sandwich structure.
Embodiment 11
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 5, and peptone 0.5, yeast extract 0.5, citric acid 0.1, sodium hydrogen phosphate 0.2, potassium dihydrogen phosphate 0.1, surplus is water;
The pH of fermentation culture is 5.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is 2 × 10
7individual/mL.
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 30 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent of the levels of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2 days: controlling with bacteria cellulose film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 10% scope simultaneously; Reach 0.5mm～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 8 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 3 days, interim pressurization, the every 12 hours air that are 15% to charged pressure percent in container, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is no longer pressurizeed while being 1.3 normal atmospheres, simultaneously the interim oxygen concentration that increases, increases by 1000% in every 12 hours, until oxygen concentration no longer increases while reaching 50%; Until Bacterial cellulose film thickness rises to 3mm～4mm;
Reserve liquid layer formation stages 2 days, reduces air pressure to 1 normal atmosphere that air pressure contacts bacteria cellulose film upper surface, reduces in oxygen concentration to 10% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 3 days, interim pressurization, the every 12 hours air that are 15% to charged pressure percent in container, radix is 1 normal atmosphere, until the air pressure contacting with Bacterial cellulose upper surface is no longer pressurizeed while being 1.3 normal atmospheres, the interim oxygen concentration that increases simultaneously, within every 12 hours, increase by 1000%, until oxygen concentration no longer increases while reaching 50%, until Bacterial cellulose film thickness is while rising to 9～16mm, taken out, must be possessed the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1wt%, boil and keep 2 hours, with pure water clean to pH be 7.0, again Bacterial cellulose film portion setting-out after treatment is processed to solid content be 10%, be the Bacterial cellulose liquid-absorbent material of sandwich structure.
Claims (10)
1. the Bacterial cellulose liquid-absorbent material of a sandwich structure, it is characterized in that: the Bacterial cellulose liquid-absorbent material of described sandwich structure is to close bacteria cellulose film closely by three-layered node to form, it is upper super layer and the lower super reserve liquid layer of inhaling layer and mediating inhaled that described three-layered node closes bacteria cellulose film closely; Described combination closely refers to that the described super layer of inhaling passes through β-1 with the cellulose microfibril of lower super suction layer and the cellulose microfibril of described reserve liquid layer, in molecule in 4-Fructus Vitis viniferae sugar chain, be combined with intermolecular hydrogen bonding, form molecular layer, also be combined with intermolecular hydrogen bonding by molecule between layers, without obvious physical layering;
The wherein said super content of cellulose of inhaling in layer and lower super suction layer is 0.7 × 10
-2～1.0 × 10
-2g/cm
3, the content of cellulose in described reserve liquid layer is 0.2 × 10
-2～0.5 × 10
-2g/cm
3.
2. the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure according to claim 1, is characterized in that, described bacteria cellulose film is by strain consumption sugar source, and eccrine fiber element microfibril is by being combined formation with intermolecular hydrogen bonding in molecule.
3. the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure according to claim 2, it is characterized in that, described strain refers to can the cellulosic microorganism of biosynthesis, comprising: acetobacter xylinum, produce one or more in acetobacter, acetify bacillus, Acetobacter pasteurianus, glucose bacillus, Agrobacterium, root nodule bacteria, sarcina, Pseudomonas cepacia, Pseudomonas cocovenenans or campylobacter jejuni.
4. the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure according to claim 1, it is characterized in that, the thickness of the Bacterial cellulose liquid-absorbent material of described sandwich structure is 9～16mm, the wherein said super thickness of inhaling layer and lower super suction layer is 3～4mm, and the thickness of described reserve liquid layer is 3～8mm.
5. the preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure as claimed in claim 1, is characterized in that comprising the following steps:
1) allotment of fermentation culture;
Fermentation culture fluid component, is calculated in mass percent, and unit is wt%: glucose, fructose, sucrose or mannitol 2～5, peptone 0.05～0.5, yeast extract 0.05～0.5, citric acid 0.05～0.5, sodium hydrogen phosphate 0.05～0.5, potassium dihydrogen phosphate 0.05～0.5, surplus is water;
The pH of fermentation culture is 4.0～6.0;
After said components is mixed after high pressure steam sterilization ultraviolet irradiation be cooled to room temperature, logical pure oxygen, obtains fermentation culture;
2) strain spreads cultivation;
Described fermentation culture is inoculated and spread cultivation; Degree spreads cultivation: bacterium cell number is 2 × 10
5～2 × 10
7individual/ml;
3) leave standstill and cultivate;
Bacterium liquid after spreading cultivation is transferred in the culture vessel that fermentation culture is housed, is positioned in constant incubator, 28～32 ℃ leave standstill cultivation;
Realize the sandwich structure of the loose and high retentiveness of the fine and close and high liquid-absorbent in the upper and lower part of Bacterial cellulose thin film, mid portion by adjusted stepwise culture fluid top air entirety air pressure and oxygen partial pressure;
A. 1～2 day Bacterial cellulose growth inducing phase: controlling the air pressure contacting with fermentation culture liquid level is 1 normal atmosphere, until the oxygen expenditure dissolving in culture fluid is totally floated afterwards upper liquid level by antibacterial, there is the translucent Bacterial cellulose thin film of one deck in liquid level;
B. Bacterial cellulose fast growing period 2～3 days: controlling Bacterial cellulose thin film upper surface air pressure is 1 normal atmosphere, regulates carrier of oxygen volume concentrations in 10～15% scopes simultaneously; Reach 0.5～1.5mm to Bacterial cellulose film thickness;
C. the steady trophophase of Bacterial cellulose 3～8 days:
Steadily trophophase divides three phases successively:
Lower super suction layer formation stages 1～3 day, pressurization makes the air pressure contacting with Bacterial cellulose thin film upper surface within the scope of 1.1～1.5 normal atmospheres, improves oxygen concentration to 50% simultaneously; Until Bacterial cellulose film thickness rises to 3～4mm;
Reserve liquid layer formation stages 1～2 day, reduces air pressure to 1 normal atmosphere that air pressure contacts Bacterial cellulose thin film upper surface, reduces in oxygen concentration to 10～15% scope simultaneously; Until Bacterial cellulose film thickness rises to 6～12mm;
Upper super suction layer formation stages 1～3 day, pressurization makes the air pressure contacting with Bacterial cellulose thin film upper surface within the scope of 1.1～1.5 normal atmospheres, improve oxygen concentration to 50% simultaneously, until Bacterial cellulose film thickness is while rising to 9～12mm, taken out, must be possessed the Bacterial cellulose thin film of sandwich structure;
4) post processing;
After standing cultivation finishes, the above-mentioned Bacterial cellulose thin film that possesses density structure is dipped in the sodium hydroxide solution that concentration is 1～10wt%, boil and keep 2～10 hours, with pure water clean to pH be 7.0, by Bacterial cellulose thin film after treatment lyophilization or the processing of part setting-out, be the Bacterial cellulose liquid-absorbent material of sandwich structure again.
6. the preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure according to claim 5, it is characterized in that, after described high pressure steam sterilization, ultraviolet irradiation refers to that described fermentation culture is placed in high-pressure sterilizing pot to 121 ℃ of sterilization treatment to be taken out after 30 minutes and be placed in irradiation under uviol lamp and be cooled to room temperature.
7. the preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure according to claim 5, is characterized in that, described logical pure oxygen refers to medical oxygen is passed in above-mentioned culture fluid with the speed of 1L/min, and maintains 30 minutes; Described inoculation refers to the inoculating loop after sterilizing and hooks up and be stored in right amount the strain in test tube at 4 ℃, and is transferred in above-mentioned fermentation culture; Described spreading cultivation refers to the shaking table at 28～32 ℃ of the fermentation culture after access strain cultivated 8～24 hours.
8. the preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure according to claim 5, is characterized in that, described moment pressurization, continuous pressure and the three kinds of forms of interim pressurization of being pressurised into; Described raising oxygen concentration is moment oxygen supplement, increases continuously and three kinds of modes of interim increase.
9. the preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure according to claim 8, it is characterized in that, described moment pressurization refers to: in 30 minutes, internal tank air pressure is promoted in 1.1～1.5 barometric pressure range, maximum is no more than 1.5 atmospheric pressure; Described continuous pressure refers to: the air that is 0.1389～2.083% to charged pressure percent in container per hour, and radix is 1 normal atmosphere, until container inner air pressure is no longer to increase pressure within the scope of 1.1～1.5 normal atmospheres time; The pressurization of described stage refers to: the every 12 hours air that are 1.67～25% to charged pressure percent in container, and radix is 1 normal atmosphere equally, until container inner air pressure is no longer to increase pressure within the scope of 1.1～1.5 normal atmospheres time;
Described moment oxygen supplement refers to: in 30 minutes, oxygen partial pressure is promoted to 50%;
Described increasing continuously refers to: oxygen concentration increase by 48.61～166.67% per hour, and radix is 10～15%, until oxygen concentration no longer increases while being 50%;
Described stage increase refers to: every 12 hours of oxygen concentration increases by 583.3～2000%, until oxygen concentration no longer increases while reaching 50%.
10. the preparation method of the Bacterial cellulose liquid-absorbent material of a kind of sandwich structure according to claim 5, it is characterized in that, described reduction air pressure refers to: the air pressure contacting with Bacterial cellulose thin film upper surface in by container in 30 minutes is reduced to 1 normal atmosphere; Described reduction oxygen concentration refers to: in 30 minutes by container in oxygen concentration be reduced in 10～15% scopes.
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| US10682257B2 (en) | 2015-07-29 | 2020-06-16 | Evophancie Biotech Ltd | Biological fiber composite dressing |
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| PL381388A1 (en) * | 2006-12-24 | 2008-07-07 | Politechnika Łódzka | Biomaterial of microbiological cellulose for internal use, production method of biomaterial and application of bomaterial of microbiological cellulose in surgery of soft tissues |
| JP5470572B2 (en) * | 2007-07-19 | 2014-04-16 | 憲司 中村 | Sheet for impregnation and wet sheet product using the same |
| TWI408232B (en) * | 2010-05-24 | 2013-09-11 | Nympheas Internationalcorp | Bacterial cellulose film, and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101509025A (en) * | 2009-03-20 | 2009-08-19 | 武汉科技学院 | Method of preparing bacteria cellulose composite material |
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| JP特开2009-24274A 2009.02.05 |
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