CN105567760A - Preparation method of bacterial cellulose composite modified film - Google Patents

Preparation method of bacterial cellulose composite modified film Download PDF

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CN105567760A
CN105567760A CN201610020682.1A CN201610020682A CN105567760A CN 105567760 A CN105567760 A CN 105567760A CN 201610020682 A CN201610020682 A CN 201610020682A CN 105567760 A CN105567760 A CN 105567760A
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solution
preparation
composite modified
fermented liquid
film
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滕平
袁英皓
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SHANDONG BEINUO MEDICAL BIOLOGY TECHNOLOGY Co Ltd
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    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02Cellulose; Modified cellulose

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  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
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Abstract

The invention discloses a preparation method of a bacterial cellulose composite modified film and belongs to the technical field of biological medicine materials and preparation thereof. The preparation method includes the following steps that a solid medium is inoculated with acetobacter xylinum, the acetobacter xylinum is activated after being cultured, a seed solution medium solution is inoculated with the activated acetobacter xylinum, shaking culture is conducted at the temperature of 28-30 DEG C and the rotating speed of 120 r/min for 12 h, and a seed solution is obtained; a fermentation solution is inoculated with the seed solution, the mixture is placed in a 30 DEG C constant temperature culture box to be cultured for 7-8 d, and a gel film is generated on the surface of the fermentation solution; after being taken out, the gel film is completely flushed with deionized water, then immersed in a NaOH solution, and flushed with deionized water till the pH value of the water is 6.5 to 7.5, and the gel bacterial cellulose composite modified film is obtained. By the adoption of an in-situ fermentation method, bacterial cellulose, alginic acid and crosslinking hydroxypropyl starch are compounded, and high mechanical strength is achieved. The service time of a dressing can be prolonged, and the antibacterial performance of the dressing can be improved.

Description

The preparation method of the composite modified film of a kind of bacteria cellulose
Technical field
The present invention relates to biological medicine material and preparing technical field thereof, particularly the preparation method of the composite modified film of a kind of bacteria cellulose.
Background technology
Bacteria cellulose is a kind of novel biomaterial, there is good bioaffinity, biocompatibility, biodegradability, biological fitness and without anaphylaxis, and high retentiveness and degree of crystallinity, good nanofiber network, high tension force and intensity, the premium propertiess such as especially good mechanical tenacity, its applied research on medical material receives the concern of people day by day.
In order to improve the performance of bacteria cellulose further in the actual use procedure of bacteria cellulose, often obtain bacteria cellulose composite material with other materials compound.The present invention adopts in-situ fermentation method, make bacteria cellulose and Lalgine and cross-linked hydroxypropylated starch in-situ fermentation compound, fermentation produces gel film, dry to obtained gel Lalgine/bacteria cellulose/cross-linked hydroxypropylated starch composite film heat, then after being placed in 20 DEG C of freezing 24h of refrigerator, with the dry 24h of vacuum freeze drier, obtain Lalgine/composite modified film of bacteria cellulose/cross-linked hydroxypropylated starch.
Summary of the invention
The present invention relates to the preparation method providing the composite modified film of a kind of bacteria cellulose, the method is simple, safety non-toxic, can be widely used in biomedicine field.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for the composite modified film of bacteria cellulose, comprises the following steps:
(1) choosing acetobacter xylinum receives on solid medium, put into 30 DEG C of constant incubators, cultivation 3 ~ 5d wild Oryza species grows new thalline and is activation bacterium, then activation bacterium is received in seed liquor culture medium solution, 28 DEG C ~ 30 DEG C, 120r/min shaking culture 12h, obtain seed liquor;
(2) get fermented liquid substratum, regulator solution pH value is 5.8 ~ 6.2, and high pressure steam sterilization 20min ~ 30min at 121 DEG C, is cooled to 30 DEG C, obtains fermented liquid; The aqueous solution (W/V) that described fermented liquid substratum is made into by following ingredients: glucose 1.0 ~ 3.0%, sucrose 2.0 ~ 3.0%, corn steep liquor 1.5 ~ 2.5%, ammonium sulfate 0.2 ~ 0.5%, potassium primary phosphate 0.1 ~ 0.4%, magnesium sulfate 0.01 ~ 0.05%, Lalgine 0.5 ~ 1.0%, cross-linked hydroxypropylated starch 0.5 ~ 1.0%;
(3) be that 6.0 ~ 8.0% inoculum sizes access seed liquor in fermented liquid by volume, the constant incubator then putting into 30 DEG C cultivates 7 ~ 8d, and fermented liquid surface produces gel film;
(4) clean with deionized water rinsing after taking out gel film, then at 80 DEG C ~ 90 DEG C, soak l ~ 2h with 1 ~ 2%NaOH solution, then be 6.5 ~ 7.5 with deionized water rinsing to water pH value, obtain the composite modified film of gel bacteria cellulose.
Wherein, preferably, the solid medium described in step (1) is (w/v): glucose 3.0 ~ 5.0%, peptone 0.5 ~ 1.0%, agar 1.0 ~ 2.5%, Sodium phosphate dibasic 0.15 ~ 0.30%, citric acid 0.1 ~ 0.2%, magnesium sulfate 0.02 ~ 0.03%.
Wherein, preferably, the seed liquor substratum described in step (1) is (w/v): glucose 2.0 ~ 3.0%, corn steep liquor 0.5 ~ 1.0%, ammonium sulfate 0.5 ~ 1.0%, potassium primary phosphate 0.1 ~ 0.5%, magnesium sulfate 0.02 ~ 0.05%.
Beneficial effect of the present invention:
1) adopt in-situ fermentation method, by bacteria cellulose and Lalgine and cross-linked hydroxypropylated starch compound, the composite modified film of obtained bacteria cellulose, as medical dressing, has higher mechanical strength; The duration of service of dressing can be extended, improve the resistance bacterium performance of dressing.
2) present invention process is simple, easy to operate, and environmental protection, the low casting product realizing being prepared by it of production cost can large-scale practical application.
3) modified bacteria cellulose composite membrane tensile strength and moisture absorption intensity obviously raise, and what expand product utilizes scope.
Embodiment
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
A preparation method for the composite modified film of bacteria cellulose, comprises the following steps:
(1) choosing acetobacter xylinum receives on solid medium, put into 30 DEG C of constant incubators, cultivation 3 ~ 5d wild Oryza species grows new thalline and is activation bacterium, then activation bacterium is received in seed liquor culture medium solution, 28 DEG C ~ 30 DEG C, 120r/min shaking culture 12h, obtain seed liquor;
(2) get fermented liquid substratum, regulator solution pH value is 5.8 ~ 6.2, and high pressure steam sterilization 20min ~ 30min at 121 DEG C, is cooled to 30 DEG C, obtains fermented liquid; The aqueous solution (W/V) that described fermented liquid substratum is made into by following ingredients: glucose 1.0 ~ 3.0%, sucrose 2.0 ~ 3.0%, corn steep liquor 1.5 ~ 2.5%, ammonium sulfate 0.2 ~ 0.5%, potassium primary phosphate 0.1 ~ 0.4%, magnesium sulfate 0.01 ~ 0.05%, Lalgine 0.5 ~ 1.0%, cross-linked hydroxypropylated starch 0.5 ~ 1.0%;
(3) be that 6.0 ~ 8.0% inoculum sizes access seed liquor in fermented liquid by volume, the constant incubator then putting into 30 DEG C cultivates 7 ~ 8d, and fermented liquid surface produces gel film;
(4) clean with deionized water rinsing after taking out gel film, then at 80 DEG C ~ 90 DEG C, soak l ~ 2h with 1 ~ 2%NaOH solution, then be 6.5 ~ 7.5 with deionized water rinsing to water pH value, obtain the composite modified film of gel bacteria cellulose.
Embodiment 1
(1) glucose 3.0g is taken, peptone 0.5g, agar 1.0g, Sodium phosphate dibasic 0.15g, citric acid 0.1 and magnesium sulfate 0.02g are mixed with the 100ml aqueous solution, adjust ph is 5.8, high pressure steam sterilization 20min-30min at 121 DEG C, while hot the nutrient solution of bacterium of having gone out is poured in sterilized culture dish, namely solid plate substratum is obtained after nutrient solution cooled and solidified, the bacterial classification acetobacter xylinum (AcetobacterxylinumNUST4.2) of preservation in refrigerator is received on solid plate substratum, put into 30 DEG C of constant incubators, cultivation 3d rear plate substratum grows new thalline and is activation bacterium.
Take glucose 2.0g, corn steep liquor 0.5g, ammonium sulfate 0.5g, potassium primary phosphate 0.1g and magnesium sulfate 0.02g is mixed with the 100ml aqueous solution, and adjust ph is 5.8-6.2, high pressure steam sterilization 20min at 121 DEG C, be cooled to 30 DEG C, again the bacterial classification activated is received in seed liquor culture medium solution, 28 DEG C, 120r/min shaking culture 12h, obtain seed liquor.
(2) glucose 1.0g is taken, sucrose 2.0g, corn steep liquor 1.5g, ammonium sulfate 0.2g, potassium primary phosphate 0.1g, magnesium sulfate 0.01g, Lalgine 0.5g and cross-linked hydroxypropylated starch 0.5g is mixed with the 100ml aqueous solution, and adjust ph is 5.8, high pressure steam sterilization 20min at 121 DEG C, be cooled to 30 DEG C, obtain fermented liquid.
(3) measuring 6ml seed liquor joins in fermented liquid, and the constant incubator then putting into 30 DEG C cultivates 7d, and fermented liquid surface produces gel film.
(4) clean with deionized water rinsing after taking out gel film, then at 80 DEG C, soak lh with 1%NaOH solution, then be 7.0 with deionized water rinsing to water pH value, obtain gel Lalgine/bacteria cellulose/cross-linked hydroxypropylated starch modified membrane.
Embodiment 2
(1) glucose 4.0g is taken, peptone 0.8g, agar 1.8g, Sodium phosphate dibasic 0.20g, citric acid 0.15g and magnesium sulfate 0.02g is mixed with the 100ml aqueous solution, adjust ph is 6.0, high pressure steam sterilization 25min at 121 DEG C, while hot the nutrient solution of bacterium of having gone out is poured in sterilized culture dish, namely solid plate substratum is obtained after nutrient solution cooled and solidified, the bacterial classification acetobacter xylinum AcetobacterxylinumNUST4.2 of preservation in refrigerator is received on solid plate substratum, put into 30 DEG C of constant incubators, cultivation 4d rear plate substratum grows new thalline and is activation bacterium.
Take glucose 2.5g, corn steep liquor 0.8g, ammonium sulfate 0.8g, potassium primary phosphate 0.3g and magnesium sulfate 0.03g is mixed with the 100ml aqueous solution, and adjust ph is 6.0, high pressure steam sterilization 25min at 121 DEG C, be cooled to 30 DEG C, again the bacterial classification activated is received in seed liquor culture medium solution, 30 DEG C, 120r/min shaking culture 12h, obtain seed liquor.
(2) glucose 2.0g is taken, sucrose 2.5g, corn steep liquor 2.0g, ammonium sulfate 0.3g, potassium primary phosphate 0.3g, magnesium sulfate 0.03g, Lalgine 0.8g and cross-linked hydroxypropylated starch 0.8g is mixed with the 100ml aqueous solution, and adjust ph is 6.0, high pressure steam sterilization 25min at 121 DEG C, be cooled to 30 DEG C, obtain fermented liquid.
(3) measuring 7ml seed liquor joins in fermented liquid, and the constant incubator then putting into 30 DEG C cultivates 8d, and fermented liquid surface produces gel film.
(4) clean with deionized water rinsing after taking out gel film, then at 90 DEG C, soak 2h with 2%NaOH solution, then be 6.5 with deionized water rinsing to water pH value, obtain gel Lalgine/bacteria cellulose/cross-linked hydroxypropylated starch modified membrane.
Embodiment 3
(1) glucose 5.0g is taken, peptone 1.0g, agar 2.5g, Sodium phosphate dibasic 0.30g, citric acid 0.20g and magnesium sulfate 0.03g is mixed with the 100ml aqueous solution, adjust ph is 6.2, high pressure steam sterilization 30min at 121 DEG C, while hot the nutrient solution of bacterium of having gone out is poured in sterilized culture dish, namely solid plate substratum is obtained after nutrient solution cooled and solidified, the bacterial classification acetobacter xylinum AcetobacterxylinumNUST4.2 of preservation in refrigerator is received on solid plate substratum, put into 28 DEG C of constant incubators, cultivation 5d rear plate substratum grows new thalline and is activation bacterium.
Take glucose 3.0g, corn steep liquor 1.0g, ammonium sulfate 1.0g, potassium primary phosphate 0.5g and magnesium sulfate 0.05g is mixed with the 100ml aqueous solution, and adjust ph is 6.2, high pressure steam sterilization 30min at 121 DEG C, be cooled to 30 DEG C, again the bacterial classification activated is received in seed liquor culture medium solution, 30 DEG C, 120r/min shaking culture 12h, obtain seed liquor.
(2) glucose 3.0g is taken, sucrose 3.0g, corn steep liquor 2.5g, ammonium sulfate 0.5g, potassium primary phosphate 0.4g, magnesium sulfate 0.05g, Lalgine 1.0g and cross-linked hydroxypropylated starch 1.0g is mixed with the 100ml aqueous solution, and adjust ph is 6.2, high pressure steam sterilization 30min at 121 DEG C, be cooled to 30 DEG C, obtain fermented liquid.
(3) measuring 8ml seed liquor joins in fermented liquid, and the constant incubator then putting into 30 DEG C cultivates 7d, and fermented liquid surface produces gel film.
(4) clean with deionized water rinsing after taking out gel film, then at 90 DEG C, soak 2h with 2%NaOH solution, then be 7.5 with deionized water rinsing to water pH value, obtain gel Lalgine/bacteria cellulose/cross-linked hydroxypropylated starch modified membrane.
The bacteria cellulose composite modified film obtained to above-described embodiment carries out performance test.
Film is cut into the sample of 20mm*40mm, utilizes thickness gauge to record thickness of sample H, utilize universal material testing instrument to record ultimate strength F and extension at break L, corresponding breaking tenacity and elongation at break.
Thickness mm Ultimate strength N Extension at break mm Breaking tenacity N/mm 2 Elongation at break %
Embodiment 1 0.323 1.963 1.221 1.215 4.07
Embodiment 2 0.356 2.120 1.218 1.190 4.06
Embodiment 3 0.410 2.590 1.250 1.263 4.16
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (3)

1. a preparation method for the composite modified film of bacteria cellulose, is characterized in that, comprise the following steps:
(1) choosing acetobacter xylinum receives on solid medium, put into 30 DEG C of constant incubators, cultivation 3 ~ 5d wild Oryza species grows new thalline and is activation bacterium, then activation bacterium is received in seed liquor culture medium solution, 28 DEG C ~ 30 DEG C, 120r/min shaking culture 12h, obtain seed liquor;
(2) get fermented liquid substratum, regulator solution pH value is 5.8 ~ 6.2, and high pressure steam sterilization 20min ~ 30min at 121 DEG C, is cooled to 30 DEG C, obtains fermented liquid; The aqueous solution (W/V) that described fermented liquid substratum is made into by following ingredients: glucose 1.0 ~ 3.0%, sucrose 2.0 ~ 3.0%, corn steep liquor 1.5 ~ 2.5%, ammonium sulfate 0.2 ~ 0.5%, potassium primary phosphate 0.1 ~ 0.4%, magnesium sulfate 0.01 ~ 0.05%, Lalgine 0.5 ~ 1.0%, cross-linked hydroxypropylated starch 0.5 ~ 1.0%;
(3) be that 6.0 ~ 8.0% inoculum sizes access seed liquor in fermented liquid by volume, the constant incubator then putting into 30 DEG C cultivates 7 ~ 8d, and fermented liquid surface produces gel film;
(4) clean with deionized water rinsing after taking out gel film, then at 80 DEG C ~ 90 DEG C, soak l ~ 2h with 1 ~ 2%NaOH solution, then be 6.5 ~ 7.5 with deionized water rinsing to water pH value, obtain the composite modified film of gel bacteria cellulose.
2. the preparation method of the composite modified film of a kind of bacteria cellulose according to claim 1, it is characterized in that: the solid medium described in step (1) is (w/v): glucose 3.0 ~ 5.0%, peptone 0.5 ~ 1.0%, agar 1.0 ~ 2.5%, Sodium phosphate dibasic 0.15 ~ 0.30%, citric acid 0.1 ~ 0.2%, magnesium sulfate 0.02 ~ 0.03%.
3. the preparation method of the composite modified film of a kind of bacteria cellulose according to claim 1, it is characterized in that: the seed liquor substratum described in step (1) is (w/v): glucose 2.0 ~ 3.0%, corn steep liquor 0.5 ~ 1.0%, ammonium sulfate 0.5 ~ 1.0%, potassium primary phosphate 0.1 ~ 0.5%, magnesium sulfate 0.02 ~ 0.05%.
CN201610020682.1A 2016-01-13 2016-01-13 Preparation method of bacterial cellulose composite modified film Pending CN105567760A (en)

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Publication number Priority date Publication date Assignee Title
CN106755180A (en) * 2016-12-09 2017-05-31 浙江理工大学 A kind of method that utilization bacterium static fermentation prepares bio-modification bacteria cellulose NF membrane
CN108570156A (en) * 2018-03-28 2018-09-25 华南理工大学 Vegetables taste bacteria cellulose-base edible condiment packaging film and its preparation method and application
CN108676194A (en) * 2018-04-08 2018-10-19 北京林业大学 A kind of complex polysaccharide hydrogel and its biology in situ synthetic method
CN108951144A (en) * 2018-08-07 2018-12-07 苏州市天翱特种织绣有限公司 A kind of preparation method of the modified moisture-inhibiting wool fabric of bacteria cellulose
CN109182187A (en) * 2018-09-20 2019-01-11 天津科技大学 A method of utilizing glucose mass transfer in agar measurement Bacterial Cellulose in Fermentation Condition
CN109223727A (en) * 2018-10-11 2019-01-18 天津科技大学 A kind of production method of bacteria cellulose Capsules
CN111378209A (en) * 2020-04-20 2020-07-07 上海交通大学 Preparation method of biodegradable packaging film
CN114410709A (en) * 2022-01-20 2022-04-29 上海即索实业有限公司 High-strength bacterial cellulose composite material and preparation method thereof
CN114796009A (en) * 2021-01-21 2022-07-29 华东师范大学 Method for rapidly producing bacterial cellulose facial mask

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106755180A (en) * 2016-12-09 2017-05-31 浙江理工大学 A kind of method that utilization bacterium static fermentation prepares bio-modification bacteria cellulose NF membrane
CN108570156A (en) * 2018-03-28 2018-09-25 华南理工大学 Vegetables taste bacteria cellulose-base edible condiment packaging film and its preparation method and application
CN108570156B (en) * 2018-03-28 2020-11-24 华南理工大学 Vegetable-flavor bacterial cellulose-based edible seasoning packaging film and preparation method and application thereof
CN108676194A (en) * 2018-04-08 2018-10-19 北京林业大学 A kind of complex polysaccharide hydrogel and its biology in situ synthetic method
CN108676194B (en) * 2018-04-08 2020-12-15 北京林业大学 Composite polysaccharide hydrogel and in-situ biosynthesis method thereof
CN108951144B (en) * 2018-08-07 2021-09-21 上海衡逸服饰科技有限责任公司 Preparation method of bacterial cellulose modified moisture-permeable wool fabric
CN108951144A (en) * 2018-08-07 2018-12-07 苏州市天翱特种织绣有限公司 A kind of preparation method of the modified moisture-inhibiting wool fabric of bacteria cellulose
CN109182187A (en) * 2018-09-20 2019-01-11 天津科技大学 A method of utilizing glucose mass transfer in agar measurement Bacterial Cellulose in Fermentation Condition
CN109223727A (en) * 2018-10-11 2019-01-18 天津科技大学 A kind of production method of bacteria cellulose Capsules
CN111378209A (en) * 2020-04-20 2020-07-07 上海交通大学 Preparation method of biodegradable packaging film
CN111378209B (en) * 2020-04-20 2021-05-07 上海交通大学 Preparation method of biodegradable packaging film
CN114796009A (en) * 2021-01-21 2022-07-29 华东师范大学 Method for rapidly producing bacterial cellulose facial mask
CN114410709A (en) * 2022-01-20 2022-04-29 上海即索实业有限公司 High-strength bacterial cellulose composite material and preparation method thereof
CN114410709B (en) * 2022-01-20 2024-04-26 上海即索实业有限公司 High-strength bacterial cellulose composite material and preparation method thereof

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Application publication date: 20160511