CN109232917A - A kind of CO2The preparation method of indicator type colour developing nanofiber hydrogel - Google Patents
A kind of CO2The preparation method of indicator type colour developing nanofiber hydrogel Download PDFInfo
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- CN109232917A CN109232917A CN201810962065.2A CN201810962065A CN109232917A CN 109232917 A CN109232917 A CN 109232917A CN 201810962065 A CN201810962065 A CN 201810962065A CN 109232917 A CN109232917 A CN 109232917A
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- cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/783—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour for analysing gases
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/04—Oxycellulose; Hydrocellulose
Abstract
The invention discloses a kind of CO2The preparation method of indicator type colour developing nanofiber hydrogel, this method includes following operating procedure: (1) being by weight ratio that 100:0.08:0.52 is mixed by nano-cellulose colloid, TEMPO and NaBr, 0.4~4 part of NaClO solution is added after dilution, regulation system pH value is 10, keeping reaction temperature is 25 DEG C, it is washed after reaction, obtain oxidation nanometer cellulose；(2) by treated, oxidation nanometer cellulose is concentrated into the oxidation nanometer cellulose suspension that solid content is 1~5%, liquor zinci chloridi is added dropwise at the top of suspension, standing forms nanofiber hydrogel；(3) pigment powder is dissolved in the ethanol solution that volumetric concentration is 70%, agitated, ultrasonic treatment is configured to CO2Nanofiber hydrogel is immersed in CO by indicator solution2Colour developing nanofiber hydrogel is obtained in indicator solution, after taking-up.The product that the method for the present invention obtains has sensitive CO2It is indicative, it is with a wide range of applications in food freshness intelligent packaging field.
Description
Technical field
It is specifically a kind of to indicate CO the invention belongs to Food Packaging technology field2It is characterized eating for showing for gas
The CO of product freshness2The preparation method of indicator type colour developing nanofiber hydrogel.
Background technique
Freshness is one of the underlying attribute for determining food quality, since consumer is to the need of health and high quality food
It asks and is continuously increased, control food quality receives great attention.Freshness instruction card is come into being, its working principle is that food exists
The certain gases generated during saving can generate color reaction with particular agent, so that indicator changes, consumption
Person can be appreciated that the quality and freshness of product without dismantling packaging bag i.e., reach the function of actively showing product information.
Carbon dioxide is the main metabolites in certain micro-organisms growth course, and the appearance of carbon dioxide means food
The decline of quality, therefore, detecting amount of carbon dioxide in food packaging can be used as freshness indicator type intelligent packaging differentiation food
One of freshness index.Carbon dioxide gas is sour gas, and the simple and easy method detected to it is the variation for detecting pH value,
By the change of pH indicator color, can reflect indirectly environment amount of carbon dioxide in packing number, and then judge food product
Matter.
Hydrogel is a kind of new functional macromolecule material with three-dimensional structure.Hydrogel is high with its water content,
It is swollen rapid, soft, and has the advantages such as elasticity and excellent biocompatibility as rubber, nowadays just in production and living
Every field be extensively studied and apply.In addition, hydrogel there are controllable physical and chemical properties, improvement can be passed through
Preparation method and raw material prepare the hydrogel with higher intensity and more preferable performance, therefore the application of hydrogel is also increasingly wider
It is general.
In recent years, nano cellulose material has become the hot topic of sustainable Material Field, and nano-cellulose source is wide
It is general, have many advantages, such as environment friendly, it is cheap, be easily obtained, be renewable, and have relatively good mechanical performance.Nanometer
Cellulose surface carboxylic group can occur coupling with certain metal ions and generate hydrogel.But it has not yet to see advantageous
It is combined with modified nano-cellulose with indicator compound to prepare the CO for showing food freshness2Indicator type is aobvious
The relevant report of color nanofiber hydrogel.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of CO2The preparation of indicator type colour developing nanofiber hydrogel
Method, the colour developing nanofiber hydrogel that this method obtains can compare delicately indicative for environments CO2Concentration can be examined immediately
Measure CO inside food packaging2Whether concentration is exceeded, monitors food freshness.
The present invention solves above-mentioned technical problem with following technical solution:
A kind of CO of the present invention2The preparation method of indicator type colour developing nanofiber hydrogel, including following operating procedure:
(1) prepare oxidation nanometer cellulose: following raw material is prepared by weight, weigh 100 parts of nano-cellulose colloids,
0.08 part 2,2,6,6- tetramethyl piperidine -1- oxide (TEMPO) powder and 0.52 part of NaBr powder are uniformly mixed at room temperature
And being diluted to solid content with distilled water is 1%, is added the NaClO solution that 0.4~4 part of effective chlorine density is 112g/l, then with dense
The hydrochloric acid solution regulation system pH value that degree is 0.5mol/L is to 10, and keeping reaction temperature is 25 DEG C, system pH in reaction process
It reduces always, so that the pH value of system is maintained 10 by the way that the sodium hydroxide solution that concentration is 0.5mol/L is added dropwise, until system pH
Value maintain 10 it is constant when, into system be added 10 parts of dehydrated alcohols, make reaction terminate；Subsequent high speed centrifugation washing, until upper
HNO is added dropwise in clear liquid3And AgNO3Until solution flocculent deposit does not occur, oxidation nanometer cellulose is obtained；
(2) nanofiber hydrogel is prepared: by oxidation nanometer cellulose made from step (1), using solvent evaporated method
It is concentrated into the oxidation nanometer cellulose suspension that solid content is 1~5%, is 2mol/L chlorine by concentration without stirring
Change zinc solution to be added dropwise at the top of oxidation nanometer cellulose suspension, form hydrogel after standing 48h, then uses deionization water logging
Soaked gel 3 times 5 minutes every time, obtains nanofiber hydrogel；
(3) CO is prepared2Indicator type colour developing nanofiber hydrogel: methyl red powder and Bromothymol blue powder are pressed
Mass ratio is that 3:2 is mixed, and mixed-powder is dissolved in the ethanol solution that volumetric concentration is 70%, magnetic agitation 1h under room temperature,
Ultrasonic treatment 10min is carried out, the CO that mixed-powder concentration is 0.03~0.3% is prepared2Indicator solution；It is received what step (2) obtained
Rice cellulose aquagel is immersed in CO210h in indicator solution obtains CO after taking-up2Indicator type colour developing nanofiber hydrogel.
In step (1), the nano-cellulose colloid is bleached softwood wood-fibred, bleaching broad-leaved wood fiber or drift by raw material
White sugarcane fiber use mechanical milling method be prepared mass concentration for 5%, 2~20nm of nano-cellulose diameter, length 0.1~
100 μm of nano-cellulose colloid.
The method of the present invention, using zinc chloride as couplant, prepares nanofiber using oxidation nanometer cellulose as hydrogel substrate
Hydrogel, the mixed liquor with Bromothymol blue and methyl red are CO2Indicator solution, preparation is combined with hydrogel has CO2Refer to
Show the colour developing nanofiber hydrogel of function；Prepared colour developing nanofiber hydrogel is to CO2Characteristic gas has very
Good instruction sensibility, can effectively detect food freshness in real time.
Compared with prior art, the invention has the advantages that are as follows:
1) it uses nano-cellulose as gel bodies phase in preparation process of the present invention, assigns colour developing nano-cellulose water-setting
Glue certain form and mechanical strength, at the same itself again be biodegradable material, meet sustainable development viewpoint, at the same also with
The development trend of cellulose resource higher value application is consistent.
2) present invention uses carrier of the nano-cellulose gel as indicator, by nano-cellulose gel and CO2Concentration
Detection food freshness instruction is ingenious to be combined together, and compared with other preparation methods, nano-cellulose gel has biggish
Specific surface area, more stable to the load fixation of indicator, gel color change gradient is more obvious, and consumer more intuitively feels
By food freshness, there is scientific and convenience.
3) carrier that the method for the present invention uses nanofiber hydrogel to indicate as carbon dioxide, can make volatility two
Carbonoxide is combined well with indicator compound, improves colour developing sensibility, to realize the quick inspection to food freshness
It surveys.
4) preparation method of the present invention is simple, good mechanical performance, changes colour sensitive；Using nano-cellulose as supporting body,
Develop the color nanofiber hydrogel high mechanical strength, reusable, has very extensive application prospect.
Detailed description of the invention
Fig. 1 is the corresponding CO of the embodiment of the present invention 12Indicator type develops the color nanofiber hydrogel in different CO2Water-setting under concentration
The color of glue.With CO2The color of the increase of concentration, colour developing nanofiber hydrogel becomes light yellow from light green color, then becomes
For red, significant color indicative character is shown.Work as CO2When concentration reaches 1.3mg/ml, the color of hydrogel is by light green color
Become light yellow, visually can obviously distinguish the variation of its color.
Specific embodiment
Method of the invention is illustrated below by specific embodiment, it is not to limit that the present embodiment, which is narrative,
Property, this does not limit the scope of protection of the present invention.
Embodiment 1:
A kind of CO2The preparation process of indicator type colour developing nanofiber hydrogel is as follows:
(1) preparation of oxidation nanometer cellulose:
To bleach sugarcane fiber as raw material, use mechanical milling method be prepared mass concentration for 5%, 2~20nm of diameter,
0.1~100 μm of length of nano-cellulose colloid.
Weigh 100 parts of (by weight, similarly hereinafter) nano-cellulose colloids, 0.08 part 2,2,6,6- tetramethyl piperidine -1- oxygen
Compound (TEMPO) powder and 0.52 part of NaBr powder, being uniformly mixed at room temperature and being diluted to solid content with distilled water is 1%, is added
Enter 2 parts of effective chlorine densities be 112g/l NaClO solution, then with concentration be 0.5mol/L hydrochloric acid solution regulation system pH value extremely
10, keeping reaction temperature is 25 DEG C, and system pH reduces always in reaction process, by the way that the hydrogen-oxygen that concentration is 0.5mol/L is added dropwise
Change sodium solution so that the pH value of system is maintained 10, until system pH maintain 10 it is constant when, into system be added 10 parts it is anhydrous
Ethyl alcohol terminates reaction；Subsequent high speed centrifugation washing, until HNO is added dropwise in supernatant3And AgNO3Solution does not occur flocculent deposit
Only, oxidation nanometer cellulose is obtained；
(2) preparation of nanofiber hydrogel:
By oxidation nanometer cellulose made from step (1), uses solvent evaporated method to be concentrated into solid content and received for 3% oxidation
Concentration is without stirring that 2mol/L liquor zinci chloridi is added dropwise to oxidation nanometer cellulose by rice cellulose suspension
At the top of suspension, hydrogel is formed after standing 48h, is then impregnated hydrogel 3 times, 5 minutes every time, is received using deionized water
Rice cellulose aquagel；
(3)CO2The preparation of indicator type colour developing nanofiber hydrogel:
With Bromothymol blue powder in mass ratio it is that 3:2 is mixed by methyl red powder, mixed-powder is dissolved in body
The ethanol solution that concentration is 70% is accumulated, magnetic agitation 1h under room temperature carries out ultrasonic treatment 10min, prepares mixed-powder concentration and is
0.03% CO2Indicator solution；The nanofiber hydrogel that step (2) obtains is immersed in CO210h in indicator solution, after taking-up
To CO2Indicator type colour developing nanofiber hydrogel.
CO prepared by this example2Indicator type develops the color nanofiber hydrogel to CO2Characteristic gas has instruction well
Sensibility can effectively detect food freshness in real time.When being placed in food packaging, with CO2The increase of concentration, colour developing
The color of nanofiber hydrogel becomes light yellow from light green color, then becomes red, shows significant color indicative character.
Work as CO2When concentration reaches 1.3mg/ml, the color of hydrogel becomes light yellow from light green color, visually can obviously distinguish its color
Variation.
Embodiment 2:
A kind of CO2The preparation process of indicator type colour developing nanofiber hydrogel is as follows:
(1) preparation of oxidation nanometer cellulose:
Using bleached softwood wood-fibred as raw material, use mechanical milling method be prepared mass concentration for 5%, diameter 2~
20nm, 0.1~100 μm of length of nano-cellulose colloid.
Weigh 100 parts of (by weight, similarly hereinafter) nano-cellulose colloids, 0.08 part 2,2,6,6- tetramethyl piperidine -1- oxygen
Compound (TEMPO) powder and 0.52 part of NaBr powder, being uniformly mixed at room temperature and being diluted to solid content with distilled water is 1%, is added
Enter the NaClO solution that 0.4 part of effective chlorine density is 112g/l, then the hydrochloric acid solution regulation system pH value for being 0.5mol/L with concentration
To 10, keeping reaction temperature is 25 DEG C, and system pH reduces always in reaction process, by the way that the hydrogen that concentration is 0.5mol/L is added dropwise
Sodium hydroxide solution makes the pH value of system maintain 10, until system pH maintain 10 it is constant when, into system be added 10 parts of nothings
Water-ethanol terminates reaction；Subsequent high speed centrifugation washing, until HNO is added dropwise in supernatant3And AgNO3There is not flocculent deposit in solution
Until, obtain oxidation nanometer cellulose；
(2) preparation of nanofiber hydrogel:
By oxidation nanometer cellulose made from step (1), uses solvent evaporated method to be concentrated into solid content and received for 1% oxidation
Concentration is without stirring that 2mol/L liquor zinci chloridi is added dropwise to oxidation nanometer cellulose by rice cellulose suspension
At the top of suspension, hydrogel is formed after standing 48h, is then impregnated hydrogel 3 times, 5 minutes every time, is received using deionized water
Rice cellulose aquagel；
(3)CO2The preparation of indicator type colour developing nanofiber hydrogel:
With Bromothymol blue powder in mass ratio it is that 3:2 is mixed by methyl red powder, mixed-powder is dissolved in body
The ethanol solution that concentration is 70% is accumulated, magnetic agitation 1h under room temperature carries out ultrasonic treatment 10min, prepares mixed-powder concentration and is
0.1% CO2Indicator solution；The nanofiber hydrogel that step (2) obtains is immersed in CO210h in indicator solution, after taking-up
To CO2Indicator type colour developing nanofiber hydrogel.
CO prepared by this example2Indicator type develops the color nanofiber hydrogel to CO2Characteristic gas has instruction well
Sensibility can effectively detect food freshness in real time.When being placed in food packaging, with CO2The increase of concentration, colour developing
The color of nanofiber hydrogel becomes light yellow from light green color, then becomes red, shows significant color indicative character.
Work as CO2When concentration reaches 1.9mg/ml, the color of hydrogel becomes light yellow from light green color, visually can obviously distinguish its color
Variation.
Embodiment 3:
A kind of CO2The preparation process of indicator type colour developing nanofiber hydrogel is as follows:
(1) preparation of oxidation nanometer cellulose:
To bleach broad-leaved wood fiber as raw material, use mechanical milling method be prepared mass concentration for 5%, diameter 2~
20nm, 0.1~100 μm of length of nano-cellulose colloid.
Weigh 100 parts of (by weight, similarly hereinafter) nano-cellulose colloids, 0.08 part 2,2,6,6- tetramethyl piperidine -1- oxygen
Compound (TEMPO) powder and 0.52 part of NaBr powder, being uniformly mixed at room temperature and being diluted to solid content with distilled water is 1%, is added
Enter 4 parts of effective chlorine densities be 112g/l NaClO solution, then with concentration be 0.5mol/L hydrochloric acid solution regulation system pH value extremely
10, keeping reaction temperature is 25 DEG C, and system pH reduces always in reaction process, by the way that the hydrogen-oxygen that concentration is 0.5mol/L is added dropwise
Change sodium solution so that the pH value of system is maintained 10, until system pH maintain 10 it is constant when, into system be added 10 parts it is anhydrous
Ethyl alcohol terminates reaction；Subsequent high speed centrifugation washing, until HNO is added dropwise in supernatant3And AgNO3Solution does not occur flocculent deposit
Only, oxidation nanometer cellulose is obtained；
(2) preparation of nanofiber hydrogel:
By oxidation nanometer cellulose made from step (1), uses solvent evaporated method to be concentrated into solid content and received for 5% oxidation
Concentration is without stirring that 2mol/L liquor zinci chloridi is added dropwise to oxidation nanometer cellulose by rice cellulose suspension
At the top of suspension, hydrogel is formed after standing 48h, is then impregnated hydrogel 3 times, 5 minutes every time, is received using deionized water
Rice cellulose aquagel；
(3)CO2The preparation of indicator type colour developing nanofiber hydrogel:
With Bromothymol blue powder in mass ratio it is that 3:2 is mixed by methyl red powder, mixed-powder is dissolved in body
The ethanol solution that concentration is 70% is accumulated, magnetic agitation 1h under room temperature carries out ultrasonic treatment 10min, prepares mixed-powder concentration and is
0.3% CO2Indicator solution；The nanofiber hydrogel that step (2) obtains is immersed in CO210h in indicator solution, after taking-up
To CO2Indicator type colour developing nanofiber hydrogel.
CO prepared by this example2Indicator type develops the color nanofiber hydrogel to CO2Characteristic gas has instruction well
Sensibility can effectively detect food freshness in real time.When being placed in food packaging, with CO2The increase of concentration, colour developing
The color of nanofiber hydrogel becomes light yellow from light green color, then becomes red, shows significant color indicative character.
Work as CO2When concentration reaches 2.6mg/ml, the color of hydrogel becomes light yellow from light green color, visually can obviously distinguish its color
Variation.
Claims (2)
1. a kind of CO2The preparation method of indicator type colour developing nanofiber hydrogel, which is characterized in that it includes following operation step
It is rapid:
(1) prepare oxidation nanometer cellulose: following raw material is prepared by weight, weighs 100 parts of nano-cellulose colloids, 0.08 part
2,2,6,6- tetramethyl piperidine -1- oxide (TEMPO) powder and 0.52 part of NaBr powder, at room temperature be uniformly mixed and with steaming
It is 1% that distilled water, which is diluted to solid content, and 0.4~4 part of effective chlorine density is added and is the NaClO solution of 112g/l, then is with concentration
For the hydrochloric acid solution regulation system pH value of 0.5mol/L to 10, keeping reaction temperature is 25 DEG C, and system pH is always in reaction process
It reduces, so that the pH value of system is maintained 10 by the way that the sodium hydroxide solution that concentration is 0.5mol/L is added dropwise, until system pH is tieed up
It holds when 10 is constant, 10 parts of dehydrated alcohols is added into system, terminate reaction；Subsequent high speed centrifugation washing, until supernatant
HNO is added dropwise3And AgNO3Until solution flocculent deposit does not occur, oxidation nanometer cellulose is obtained；
(2) it prepares nanofiber hydrogel: oxidation nanometer cellulose made from step (1) is concentrated using solvent evaporated method
Concentration is without stirring 2mol/L zinc chloride by the oxidation nanometer cellulose suspension for being 1~5% to solid content
Solution is added dropwise at the top of oxidation nanometer cellulose suspension, forms hydrogel after standing 48h, then uses deionized water soaking water
Gel 3 times, 5 minutes every time, obtain nanofiber hydrogel；
(3) CO is prepared2Indicator type colour developing nanofiber hydrogel: methyl red powder and Bromothymol blue powder are pressed into quality
Than being mixed for 3:2, mixed-powder is dissolved in the ethanol solution that volumetric concentration is 70%, magnetic agitation 1h under room temperature is carried out
It is ultrasonically treated 10min, prepares the CO that mixed-powder concentration is 0.03~0.3%2Indicator solution；The Nanowire that step (2) is obtained
Dimension hydrogel is immersed in CO210h in indicator solution obtains CO after taking-up2Indicator type colour developing nanofiber hydrogel.
2. CO according to claim 12The preparation method of indicator type colour developing nanofiber hydrogel, which is characterized in that step
(1) in, the nano-cellulose colloid is that bleached softwood wood-fibred, bleaching broad-leaved wood fiber or bleaching sugarcane fiber are adopted by raw material
It is 5%, 2~20nm of nano-cellulose diameter, 0.1~100 μm of length of nanometer that mass concentration, which is prepared, with mechanical milling method
Cellulose colloid.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110251690A (en) * | 2019-06-28 | 2019-09-20 | 常州市第二人民医院 | A kind of nerve dyeing nanogel and its preparation method and application |
| CN110527442A (en) * | 2019-07-26 | 2019-12-03 | 广西大学 | A kind of preparation method of food freshness indicator type environmental protection adhesive label |
| CN110823882A (en) * | 2019-12-05 | 2020-02-21 | 吉林农业大学 | Antifreezing gel state indicating material, application and preparation method thereof |
| CN112852001A (en) * | 2021-01-08 | 2021-05-28 | 天津科技大学 | Preparation method of nano-cellulose ammonia gas induction aerogel |
| CN113402734A (en) * | 2021-06-17 | 2021-09-17 | 东北农业大学 | Preparation method and application of hydrogel for indicating freshness of chilled meat |
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| CN106345426A (en) * | 2016-10-14 | 2017-01-25 | 北京化工大学 | Method for preparing nanocellulose for efficiently adsorbing heavy metal ions from natural fallen leaves |
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| CN101851295A (en) * | 2010-06-30 | 2010-10-06 | 东北林业大学 | Preparation method of homogenized fine nano-cellulose fiber |
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| CN110251690A (en) * | 2019-06-28 | 2019-09-20 | 常州市第二人民医院 | A kind of nerve dyeing nanogel and its preparation method and application |
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| CN110823882A (en) * | 2019-12-05 | 2020-02-21 | 吉林农业大学 | Antifreezing gel state indicating material, application and preparation method thereof |
| CN112852001A (en) * | 2021-01-08 | 2021-05-28 | 天津科技大学 | Preparation method of nano-cellulose ammonia gas induction aerogel |
| CN113402734A (en) * | 2021-06-17 | 2021-09-17 | 东北农业大学 | Preparation method and application of hydrogel for indicating freshness of chilled meat |
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Application publication date: 20190118 |