CN107629226A - A kind of carragheen/methylcellulose blend film and preparation method thereof - Google Patents
A kind of carragheen/methylcellulose blend film and preparation method thereof Download PDFInfo
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- CN107629226A CN107629226A CN201710861509.9A CN201710861509A CN107629226A CN 107629226 A CN107629226 A CN 107629226A CN 201710861509 A CN201710861509 A CN 201710861509A CN 107629226 A CN107629226 A CN 107629226A
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- carragheen
- methylcellulose
- eucheuma
- polyalcohol
- blend film
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Abstract
It is the invention discloses a kind of carragheen/methylcellulose blend film and preparation method thereof, the step of preparation method：S1：Carragheen is extracted from Eucheuma；S2：The carragheen that step S1 is obtained is dissolved in secondary water with methylcellulose, polyalcohol, and 1h 3h are stirred at a temperature of 70 DEG C 90 DEG C, obtain the blended liquid of carragheen, methylcellulose and polyalcohol；S3：The blended liquid solidification plastic film mulch of carragheen, methylcellulose and polyalcohol prepared by step S2；S4：By cured film prepared by step S3 polar micromolecules solvent rinse, naturally dry afterwards.By carragheen made from this method/methylcellulose blend film, it can not only meet recyclability, biodegradability and bio-compatibility, and with higher tensile strength and maximum pyrolysis rate temperature.
Description
Technical field
The present invention relates to a kind of polymeric material field, more particularly, to a kind of carragheen/methylcellulose blend film
And preparation method thereof.
Background technology
It is used for packaging for foodstuff in the market and the plastic products of preservation field depends on fossil feedstock, due to oil
Non-renewable and petroleum chemicals the non-biodegradable of resource, " white pollution " problem brought therewith can not be ignored, it would be highly desirable to
Find a kind of degradable, reproducible substitute and make packaging material, and carragheen provides as a kind of reproducible marine organisms
Source has obtained the extensive concern of domestic and foreign scholars.Carragheen is a kind of polysaccharide vegetable colloid extracted from red algae category Eucheuma,
There is recyclability, biodegradability and bio-compatibility, be widely used in food industry, chemical industry at present
And in the field such as biochemistry, medical science.
The content of the invention
It is an object of the invention to provide a kind of carragheen/methylcellulose blend film and preparation method thereof, party's legal system
The blend film obtained also has more excellent power in addition to possessing the advantages that recyclability, biodegradability and bio-compatibility
Learn performance and heat resistance.
To achieve the above object, technical scheme is as follows：
It is a kind of that the method that carragheen prepares carragheen/methylcellulose blend film is extracted from Eucheuma, it is characterised in that
Comprise the following steps：
S1：Carragheen is extracted from Eucheuma：Alkali, Eucheuma and secondary water are mixed, in -90 DEG C of temperature 70 C, ultrasound
Frequency is that 60%-80% reacts 90min-120min, filters to obtain filter residue afterwards, then filter residue is dissolved in into secondary water, and PH is into for regulation
Property, 80 DEG C of -100 DEG C of constant temperature stir 2h-4h, filter to get filtrate while hot, filtrate is freezed, then drying and dehydrating, obtain carragheen
Powdered product；
Wherein, the dosage of alkali, Eucheuma and secondary water is in parts by mass：Alkali：2-4 parts, Eucheuma：4 parts, secondary water
80-120 parts；
The alkali is one or two kinds of combinations of sodium hydroxide or potassium hydroxide；
S2：The carragheen that step S1 is obtained is dissolved in secondary water with methylcellulose, polyalcohol, at 70 DEG C -90 DEG C
At a temperature of stir 1h-3h, obtain the blended liquid of carragheen, methylcellulose and polyalcohol；
Wherein, the mass fraction of carragheen is 2%-4% in blended liquid, and the mass fraction of polyalcohol is 0.5%-2%, first
The mass fraction of base cellulose is 0.3%-2.7%, and the mass fraction of secondary water is 91.3%-97.2%；
Described polyalcohol is one or two kinds of combinations of polyethylene glycol or glycerine；
S3：The blended liquid solidification plastic film mulch of carragheen, methylcellulose and polyalcohol prepared by step S2；
S4：By cured film prepared by step S3 polar micromolecules solvent rinse, naturally dry afterwards.
Preferably, in step S2, the mass ratio of the carragheen and the methylcellulose is 6:1-4.
Preferably, in step S2, described polyalcohol uses polyethylene glycol and glycerine mass ratio as 1:1 mixed liquor.
Preferably, in step S2, the molecular weight of the polyethylene glycol is 300-1000.
Preferably, in step S2, the molecular weight of the polyethylene glycol is 400.
Preferably, in step S1, the reaction temperature used is 75 DEG C, supersonic frequency 70%.
Preferably, in step S2, the mass ratio of carragheen, methylcellulose and polyalcohol is 3:1:1.
Preferably, in step S3, the process of the plastic film mulch solidification is to solidify using the tape casting plastic film mulch and at 30 DEG C -60 DEG C
24h-48h。
Preferably, in step S4, described polar micromolecules solution is ethanol or water or ethyl acetate.
A kind of carragheen/methylcellulose blend film, it is characterised in that including the OK a karaoke club that mass fraction is 30%-83%
The polyalcohol that the methylcellulose and mass fraction that glue, mass fraction are 5%-52% are 7%-46%.
Preferably, the tensile strength of the carragheen/methylcellulose blend film is 22.6MPa-25.6MPa, maximum heat
It is 246 DEG C -254 DEG C to solve rate temperature.
It can be seen from the above technical proposal that the present invention cost-effective and environmentally friendly, is passed through by extracting carragheen from Eucheuma
By the use of methylcellulose as enhancing item, the mechanical properties such as the tensile strength of blend film are improved, by using polyalcohol conduct
Item is plasticized, enhances the pliability of blend film, reduces the moisture-vapor transmission coefficient of film.
Brief description of the drawings
Fig. 1 is a kind of flow chart of the preparation method of carragheen/methylcellulose blend film of the present invention；
Fig. 2 is the mechanism of action schematic diagram between carragheen, methylcellulose and polyalcohol.
Embodiment
Below in conjunction with the accompanying drawings, the embodiment of the present invention is described in further detail.
As shown in figure 1, extracting from Eucheuma carragheen the invention discloses one kind, to prepare carragheen/methylcellulose common
The method of mixed film, comprises the following steps：
S1：Carragheen is extracted from Eucheuma：Alkali, Eucheuma and secondary water are mixed, in -90 DEG C of temperature 70 C, ultrasound
Frequency is that 60%-80% reacts 90min-120min, filters to obtain filter residue afterwards, and filter residue is dissolved in into secondary water, regulation PH to neutrality,
80 DEG C of -100 DEG C of constant temperature stir 2h-4h, filter to get filtrate while hot, filtrate is freezed, then drying and dehydrating, obtain carragheen powder
Product.Wherein, the dosage of alkali, Eucheuma and secondary water is in parts by mass：Alkali：2-4 parts, Eucheuma：4 parts, secondary water 80-
120 parts.Alkali can be one or two kinds of combinations of sodium hydroxide or potassium hydroxide.The purpose of ultrasound is used as stirring and makes kylin
The lipid connected between carragheen and other molecules in dish or half lipid matter decompose, while protect the original of carragheen as far as possible
There is structure not to be destroyed, and improve the purity of carragheen, avoid occurring during subsequently preparing film insoluble matter causes should
The problems such as power defect, performance are bad, quality is uneven.
Alkali prioritizing selection is sodium hydroxide, and supersonic frequency prioritizing selection 70%, ultrasonic temperature prioritizing selection is 75 DEG C.
S2：The carragheen that step S1 is obtained is with methylcellulose, polynary alcohol and water in certain proportion at 70 DEG C -90 DEG C
At a temperature of be stirred, a length of 1h-3h during stirring, obtain the blended liquid of carragheen, methylcellulose and polyalcohol.Wherein,
The mass fraction of carragheen is 2%-4% in blended liquid, and the mass fraction of polyalcohol is 0.5%-2%, the matter of methylcellulose
Amount fraction is 0.3%-2.7%, and the mass fraction of secondary water is 91.3%-97.2%.Polyalcohol can be polyethylene glycol or third
One or two kinds of combinations of triol.
In this process, carrageenan molecule can form three-dimensional netted double-spiral structure during film forming is condensed, more
The addition of first alcohol and the mechanism of action of carrageenan molecule are：The molecular weight of polyalcohol is smaller, carrageenan molecule condense to be formed it is double
It can be interspersed among carrageenan molecule double-spiral structure during helical structure, the hydroxyl in polyalcohol and carrageenan molecule hydroxyl
Hydrogen bond is formed between base, is weakened between carrageenan molecule, the interaction force of intramolecular in itself, softens its rigid structure, it is soft
Toughness is more preferable, so as to improve its elongation rate of tensile failure；The addition of methylcellulose and the mechanism of action of carrageenan molecule are：Big point
The methylcellulose of subchain is cross-linked to form graft copolymer with carrageenan molecule, reduce to a certain extent in OK a karaoke club plastic structure because
Coulomb repulsion caused by sulfate group institute is negatively charged, it is close to each other to be advantageous to more carragheen chains, so as to produce spiral
Cohesion, be advantageous to improve blending film strength.The effect schematic diagram of above-mentioned mechanism is as shown in Figure 2.
S3：The blended liquid solidification plastic film mulch of carragheen, methylcellulose and polyalcohol prepared by step S2.Preferably, adopt
With the tape casting plastic film mulch, and solidify 24h-48h at 30 DEG C -60 DEG C.Due to carragheen, methylcellulose mix with polyalcohol it is more equal
Even, so the film quality after solidification is more uniform, performance is preferable.
S4：By cured film prepared by step S3 polar micromolecules solvent rinse, naturally dry, finally gives card afterwards
Draw glue/methylcellulose blend film.Preferably, polar micromolecules solvent can be ethanol or water or ethyl acetate.
Carragheen/methylcellulose the blending prepared using above-mentioned carragheen/methylcellulose blending membrane preparation method
Film, gained film appearance water white transparency, there is good mechanical property, translucency and environmentally friendly.
With reference to specific embodiment, the invention will be further described.
Embodiment 1
20g Eucheumas and 10g sodium hydroxides and 500mL secondary waters are poured into 1000mL conical flask and sealed, is put
It is 70% in supersonic frequency, ultrasonic temperature is 2h in 75 DEG C of Ultrasound Instruments, filtering, then filter residue is placed in beaker and adds 500mL
Secondary water, regulation PH to neutrality, then 90 DEG C of constant temperature stirring 2h, filter, filtrate are freeze-dried, obtain carragheen product while hot
9.4g；By 3g carragheens, 1g methylcellulose and 1.5g polyalcohols, (mass ratio of polyethylene glycol and glycerine is 1:1, wherein poly-
The molecular weight of ethylene glycol is placed in constant temperature stirring 2h at 90 DEG C 400) to be mixed in 150mL secondary waters, and rear constant temperature, which is stood, to be defoamed；Will
Mixed liquor is poured on glass Slab, using the tape casting plastic film mulch, solidifies 36h at 40 DEG C, and the blend film after solidification is placed in into second
Itd is proposed after being rinsed in alcohol, naturally dry.
Obtained carragheen/methylcellulose blending film outward appearance is colorless and transparent film, and its technical indicator is as follows：
Tensile strength：25.6MPa
Elongation at break：85.3%
Light transmittance：97.5% (500nm wavelength)
The temperature of maximum pyrolysis rate：254℃
Embodiment 2
20g Eucheumas and 10g sodium hydroxides and 500mL secondary waters are poured into 1000mL conical flask and sealed, is put
It is 70% in supersonic frequency, ultrasonic temperature is 2h in 75 DEG C of Ultrasound Instruments, filtering, then filter residue is placed in beaker and adds 500mL
Secondary water, regulation PH to neutrality, then 90 DEG C of constant temperature stirring 2h, filter, filtrate are freeze-dried, obtain carragheen product while hot
9.4g；Change methylcellulose dosage, by 3g carragheens, 0.75g methylcellulose and 1.5g polyalcohols (polyethylene glycol and the third three
The mass ratio of alcohol is 1:1, the wherein molecular weight of polyethylene glycol is placed in constant temperature at 90 DEG C and stirred 400) to be mixed in 150mL secondary waters
2h is mixed, rear constant temperature stands defoaming；Mixed liquor is poured on glass Slab, using the tape casting plastic film mulch, solidifies 36h at 40 DEG C,
Blend film after solidification is placed in ethanol after rinsing and proposed, naturally dry.
Obtained carragheen/methylcellulose blending film outward appearance is colorless and transparent film, and its technical indicator is as follows：
Tensile strength：22.6MPa
Elongation at break：105.3%
Light transmittance：94.6% (500nm wavelength)
The temperature of maximum pyrolysis rate：246℃
Embodiment 3
20g Eucheumas and 10g sodium hydroxides and 500mL secondary waters are poured into 1000mL conical flask and sealed, is put
It is 70% in supersonic frequency, ultrasonic temperature is 2h in 75 DEG C of Ultrasound Instruments, filtering, then filter residue is placed in beaker and adds 500mL
Secondary water, regulation PH to neutrality, then 90 DEG C of constant temperature stirring 2h, filter, filtrate are freeze-dried, obtain carragheen product while hot
9.4g；Methylcellulose is not added, (mass ratio of polyethylene glycol and glycerine is 1 by 3g carragheens and 1.5g polyalcohols:1, its
The molecular weight of middle polyethylene glycol is placed in constant temperature stirring 2h at 90 DEG C 400) to be mixed in 150mL secondary waters, and rear constant temperature, which is stood, to disappear
Bubble；Mixed liquor is poured on glass Slab, using the tape casting plastic film mulch, solidifies 36h at 40 DEG C, the blend film after solidification is put
Itd is proposed after being rinsed in ethanol, naturally dry.
Obtained carragheen/methylcellulose blending film outward appearance is colorless and transparent film, and its technical indicator is as follows：
Tensile strength：15.7MPa
Elongation at break：84.6%
Light transmittance：96.6% (500nm wavelength)
The temperature of maximum pyrolysis rate：215℃
For more intuitively relatively more resulting carragheen/methylcellulose blending film properties, table 1 is referred to.
Table 1：Carragheen made from different technology conditions/methylcellulose blend film technical indicator compares
It can see from above-mentioned table 1：The addition of methylcellulose clearly enhances OK a karaoke club glued membrane in embodiment 1, embodiment 2
Tensile strength, and it is seen that in embodiment 1 carragheen/methylcellulose blend film showed in These parameters it is excellent
It is different, therefore the reaction condition of embodiment 1 is optimal conditions, i.e. the mass ratio of carragheen, methylcellulose and polyalcohol is optimal to be
6:2:3。
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (10)
1. the preparation method of a kind of carragheen/methylcellulose blend film, it is characterised in that comprise the following steps：
S1：Carragheen is extracted from Eucheuma：Alkali, Eucheuma and secondary water are mixed, in -90 DEG C of temperature 70 C, supersonic frequency
90min-120min is reacted for 60%-80%, filters to obtain filter residue afterwards, then filter residue is dissolved in secondary water, regulation PH to neutrality, 80
DEG C of -100 DEG C constant temperature stirring 2h-4h, filter to get filtrate, filtrate are freezed, then drying and dehydrating, obtain the production of carragheen powder while hot
Thing；
Wherein, the dosage of alkali, Eucheuma and secondary water is in parts by mass：Alkali：2-4 parts, Eucheuma：4 parts, secondary water 80-120
Part；
The alkali is one or two kinds of combinations of sodium hydroxide or potassium hydroxide；
S2：The carragheen that step S1 is obtained is dissolved in secondary water with methylcellulose, polyalcohol, in 70 DEG C -90 DEG C of temperature
The lower stirring 1h-3h of degree, obtains the blended liquid of carragheen, methylcellulose and polyalcohol；
Wherein, the mass fraction of carragheen is 2%-4% in blended liquid, and the mass fraction of polyalcohol is 0.5%-2%, and methyl is fine
The mass fraction of dimension element is 0.3%-2.7%, and the mass fraction of secondary water is 91.3%-97.2%；
Described polyalcohol is one or two kinds of combinations of polyethylene glycol or glycerine；
S3：The blended liquid solidification plastic film mulch of carragheen, methylcellulose and polyalcohol prepared by step S2；
S4：By cured film prepared by step S3 polar micromolecules solvent rinse, naturally dry afterwards.
2. one kind according to claim 1 extracts carragheen from Eucheuma and prepares carragheen/methylcellulose blend film
Method, it is characterised in that in step S2, the mass ratio of the carragheen and the methylcellulose is 6:1-4.
3. one kind according to claim 1 extracts carragheen from Eucheuma and prepares carragheen/methylcellulose blend film
Method, it is characterised in that in step S2, described polyalcohol uses polyethylene glycol and glycerine mass ratio as 1:1 mixing
Liquid.
4. one kind according to claim 1 or 3 extracts carragheen from Eucheuma and prepares carragheen/methylcellulose blending
The method of film, it is characterised in that in step S2, the molecular weight of the polyethylene glycol is 300-1000.
5. one kind according to claim 1 extracts carragheen from Eucheuma and prepares carragheen/methylcellulose blend film
Method, it is characterised in that in step S1, the reaction temperature used is 75 DEG C, supersonic frequency 70%.
6. one kind according to claim 1 extracts carragheen from Eucheuma and prepares carragheen/methylcellulose blend film
Method, it is characterised in that in step S2, the mass ratio of carragheen, methylcellulose and polyalcohol is 3:1:1.
7. one kind according to claim 1 extracts carragheen from Eucheuma and prepares carragheen/methylcellulose blend film
Method, it is characterised in that in step S3, the process of plastic film mulch solidification is using the tape casting plastic film mulch and at 30 DEG C -60 DEG C
Solidify 24h-48h.
8. one kind according to claim 1 extracts carragheen from Eucheuma and prepares carragheen/methylcellulose blend film
Method, it is characterised in that in step S4, described polar micromolecules solution is ethanol or water or ethyl acetate.
A kind of 9. carragheen/methylcellulose blend film, it is characterised in that including mass fraction be 30%-83% carragheen,
The polyalcohol that the methylcellulose and mass fraction that mass fraction is 5%-52% are 7%-46%.
A kind of 10. carragheen/methylcellulose blend film according to claim 9, it is characterised in that the carragheen/
The tensile strength of methylcellulose blend film is 22.6MPa-25.6MPa, and maximum pyrolysis rate temperature is 246 DEG C -254 DEG C.
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| CN201710861509.9A CN107629226A (en) | 2017-09-21 | 2017-09-21 | A kind of carragheen/methylcellulose blend film and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020174234A1 (en) * | 2019-02-26 | 2020-09-03 | Solublue Ltd | Biodegradable composition |
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2017
- 2017-09-21 CN CN201710861509.9A patent/CN107629226A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020174234A1 (en) * | 2019-02-26 | 2020-09-03 | Solublue Ltd | Biodegradable composition |
| CN113840875A (en) * | 2019-02-26 | 2021-12-24 | 索卢蓝有限公司 | Biodegradable compositions |
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