CN103146008B - Preparation method of alkali lignin-starch film - Google Patents
Preparation method of alkali lignin-starch film Download PDFInfo
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- CN103146008B CN103146008B CN201310106027.4A CN201310106027A CN103146008B CN 103146008 B CN103146008 B CN 103146008B CN 201310106027 A CN201310106027 A CN 201310106027A CN 103146008 B CN103146008 B CN 103146008B
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Abstract
The invention discloses a preparation method of an alkali lignin-starch film, and relates to the preparation method of alkali lignin-starch film. The problem of phase separation in blend film caused by low molecular weight in the film machining process in the existing method is solved. The method comprises the following steps: preparing starch pasting liquor; preparing film-forming liquor; cooling the film-forming liquor to room temperature, defoaming in vacuum, pouring the film-forming liquor on a stainless steel board in tiling and casting, drying, standing at room temperature, and uncovering film to obtain the alkali lignin-starch film. The preparation method disclosed by the invention can be applied to the filed of agriculture gardening, fruit and vegetable package, and daily-used chemicals.
Description
Technical field
The present invention relates to a kind of preparation method of alkali lignin-starch film.
Background technology
Since the eighties in last century, researchist invests research and development treated starch film and starch and Biodegradable high-molecular compound blend film by attention.Chiellini etc. to some biodegradable polyester materials such as poly-hydroxy alkyl ester, poly(lactic acid), the application of polycaprolactam in starch-based material are studied, result of study shows, these materials not only have biodegradability and biocompatibility, and its mechanical property is also fine.But the use cost of these polymkeric substance is higher, be unfavorable for the industrialization of material.Funke etc., for making starting material cheap and easy to get, start from agricultural-food, to find applicable natural high moleculer eompound, as Mierocrystalline cellulose, xylogen, pectin, chitin and protein etc., and research and development totally biodegradable type starch basement membrane.In these natural high moleculer eompounds, xylogen is as the main byproduct of paper industry and emerging biomass fuel ethanol industry, and its resource utilization and higher value application are the focuses that researchist pays close attention to for a long time always.
The < < Chemical Modification that Baumberger published in 2002, Properties, and Usage of Lignin > > (Thomas Q.Hu, Kluwer Academic/plenum Publishers, New York, 2002, the chapter 1 of writing 1-20.) " Starch-lignin films ", preparation method to starch-lignin membrane, thermodynamic property, the interaction mechanism of starch and xylogen and starch-lignin blend potential application foreground etc. are summarized, in literary composition, propose, now widely used small molecules softening agent glycerine is in the film course of processing, in the blended liquid that existence causes because molecular weight is low, phenomenon of phase separation occurs.
Summary of the invention
The present invention will solve existing method in the film course of processing, has the problem being separated in the blend film causing because molecular weight is low, and a kind of preparation method of alkali lignin-starch film is provided.
The preparation method of a kind of alkali lignin-starch film of the present invention, by following steps, undertaken: the W-Gum aqueous solution that is one, 1%～10% by W-Gum and water mixed preparing quality percentage composition, then warming while stirring to 95 ℃, and keep 15～25min, obtain starch pasting liquid; Two, in the dextrin obtaining to step 1, adding methylolation alkali lignin, quality percentage composition is 50% glutaraldehyde and glycerine, is cooled to 20～90 ℃, and reaction 1～5h, obtains preparation liquid; Three, preparation liquid step 2 being obtained is cooled to room temperature, then vacuum defoamation, tiling curtain coating, then be placed in the thermostatic drying chamber of 70 ℃, keep 1～2h, then take out, standing 8～12h at room temperature, take off film, obtain alkali lignin-starch film, complete the preparation method of alkali lignin-starch film; Wherein in step 1, in W-Gum and step 2, the mass ratio of methylolation alkali lignin is 1: (0.2～1), in step 1, in W-Gum and step 2, quality percentage composition is that the mass volume ratio of 50% glutaraldehyde is 1g: (0.1～1) mL, in step 1, in W-Gum and step 2, the mass volume ratio of glycerine is 1g: (0.5～2) mL.
The present invention utilizes crosslinking reaction to improve starch and the consistency of alkali lignin in matrix material, and by introduce methylol functional group in alkali lignin molecule, make the water-intake rate of composite film material surpass three times of mould material that starch and alkali lignin simple blend obtain, contrast with blend film, alkali lignin-starch film of the present invention is homogeneous, soft, in water, soak after 24h, the shape of mould material does not obviously change, and material is still very even, do not have bubble to form; Utilize scanning electron microscope to observe the surface of mould material and section microscopic appearance, find that in mould material, group partition inter-capacitive is good, do not have obvious phenomenon of phase separation to occur,
Therefore can be used as moisture retention mould material is applied to the fields such as agriculture and garden, vegetable and fruit packaging, household chemicals.
Accompanying drawing explanation
Fig. 1 is the SEM photo on alkali lignin-starch film surface of test 1 preparation;
Fig. 2 is the SEM photo of alkali lignin-starch film section of test 1 preparation.
Embodiment
Embodiment one: the preparation method of a kind of alkali lignin-starch film of present embodiment, by following steps, undertaken: the W-Gum aqueous solution that is one, 1%～10% by W-Gum and water mixed preparing quality percentage composition, then warming while stirring to 95 ℃, and keep 15～25min, obtain starch pasting liquid; Two, in the dextrin obtaining to step 1, adding methylolation alkali lignin, quality percentage composition is 50% glutaraldehyde and glycerine, is cooled to 20～90 ℃, and reaction 1～5h, obtains preparation liquid; Three, preparation liquid step 2 being obtained is cooled to room temperature, then vacuum defoamation, tiling curtain coating, then be placed in the thermostatic drying chamber of 70 ℃, keep 1～2h, then take out, standing 8～12h at room temperature, take off film, obtain alkali lignin-starch film, complete the preparation method of alkali lignin-starch film; Wherein in step 1, in W-Gum and step 2, the mass ratio of methylolation alkali lignin is 1: (0.2～1), in step 1, in W-Gum and step 2, quality percentage composition is that the mass volume ratio of 50% glutaraldehyde is 1g: (0.1～1) mL, in step 1, in W-Gum and step 2, the mass volume ratio of glycerine is 1g: (0.5～2) mL.
Present embodiment utilizes crosslinking reaction to improve starch and the consistency of alkali lignin in matrix material, and by introduce methylol functional group in alkali lignin molecule, make the water-intake rate of composite film material surpass three times of mould material that starch and alkali lignin simple blend obtain, contrast with blend film, the alkali lignin-starch film of present embodiment is homogeneous, soft, in water, soak after 24h, the shape of mould material does not obviously change, and material is still very even, do not have bubble to form; Utilize scanning electron microscope to observe the surface of mould material and section microscopic appearance, find that in mould material, group partition inter-capacitive is good, do not have obvious phenomenon of phase separation to occur, therefore can be used as moisture retention mould material is applied to the fields such as agriculture and garden, vegetable and fruit packaging, household chemicals.
Embodiment two: present embodiment is different from embodiment one is the W-Gum aqueous solution that is 3%～7% by W-Gum and water mixed preparing quality percentage composition in step 1.Other steps and parameter are identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two is the W-Gum aqueous solution that is 5% by W-Gum and water mixed preparing quality percentage composition in step 1.Other steps and parameter are identical with embodiment one or two.
Embodiment four: what present embodiment was different from one of embodiment one to three is that step 1 is warming up to 95 ℃ in 40min.Other steps and parameter are identical with one of embodiment one to three.
Embodiment five: what present embodiment was different from one of embodiment one to four is to be cooled to 50 ℃ in step 2.Other steps and parameter are identical with one of embodiment one to four.
Embodiment six: what present embodiment was different from one of embodiment one to five is to react 2h in step 2.Other steps and parameter are identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different from one of embodiment one to six is to keep 1.5h in step 3.Other steps and parameter are identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven be in step 1 in W-Gum and step 2 the mass ratio of methylolation alkali lignin be 1: 0.7.Other steps and parameter are identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight be in step 1 in W-Gum and step 2 quality percentage composition be that the mass volume ratio of 50% glutaraldehyde is 1g: 0.1mL.Other steps and parameter are identical with one of embodiment one to eight.
Embodiment ten: present embodiment is different from one of embodiment one to nine be in step 1 in W-Gum and step 2 the mass volume ratio of glycerine be 1g: 0.8mL.Other steps and parameter are identical with one of embodiment one to nine.
By following verification experimental verification beneficial effect of the present invention:
Test 1, this tests a kind of preparation method of alkali lignin-starch film, by following steps, undertaken: the W-Gum aqueous solution that is one, 5% by W-Gum and water mixed preparing quality percentage composition, then warming while stirring to 95 ℃, and keep 20min, obtain starch pasting liquid; Two, in the dextrin obtaining to step 1, adding methylolation alkali lignin, quality percentage composition is 50% glutaraldehyde and glycerine, is cooled to 50 ℃, and reaction 2h, obtains preparation liquid; Three, preparation liquid step 2 being obtained is cooled to room temperature, then vacuum defoamation, again preparation liquid is poured on to the curtain coating that tiles on stainless steel plate, then the stainless steel plate with preparation liquid is placed in to the thermostatic drying chamber of 70 ℃, keeps 1.5h, then take out, standing 10h at room temperature, take off film, obtain alkali lignin-starch film, complete the preparation method of alkali lignin-starch film; Wherein in step 1, in W-Gum and step 2, the mass ratio of methylolation alkali lignin is 1: 0.7, in step 1, in W-Gum and step 2, quality percentage composition is that the mass volume ratio of 50% glutaraldehyde is 1g: 0.1mL, and in step 1, in W-Gum and step 2, the mass volume ratio of glycerine is 1g: 0.8mL.
The water-intake rate of the alkali lignin-starch film of this test preparation is 146.3%, alkali lignin-the starch film of this test preparation is carried out to TG and DSC test, test result shows, alkali lignin-starch film is stable 90 ℃ of following thermal characteristicss, utilize scanning electron microscope to observe the surface of alkali lignin-starch film and section microscopic appearance, result as depicted in figs. 1 and 2, from Fig. 1 and Fig. 2, in the alkali lignin-starch film of this test preparation, group partition inter-capacitive is good, do not have obvious phenomenon of phase separation to occur, alkali lignin-starch film is carried out to Mechanics Performance Testing according to GB13022-91, alkali lignin-starch film elongation at break of this test preparation is 62.54%, existing xylogen-starch blending film elongation at break is 21.52%, water-intake rate is 35.6%, compare with existing xylogen-starch blending film, alkali lignin-starch film elongation at break of this test preparation increases and water-intake rate improves, therefore the flexibility of the alkali lignin-starch film of this test preparation is good, good toughness and water-intake rate are high, can be used as moisture retention mould material and be applied to agriculture and garden, vegetable and fruit packaging, the fields such as household chemicals.
Claims (1)
1. the preparation method of an alkali lignin-starch film, the preparation method who it is characterized in that alkali lignin-starch film is undertaken by following steps: the W-Gum aqueous solution that is one, 5% by W-Gum and water mixed preparing quality percentage composition, then warming while stirring to 95 ℃, and keep 20min, obtain starch pasting liquid; Two, in the dextrin obtaining to step 1, adding methylolation alkali lignin, quality percentage composition is 50% glutaraldehyde and glycerine, is cooled to 50 ℃, and reaction 2h, obtains preparation liquid; Three, preparation liquid step 2 being obtained is cooled to room temperature, then vacuum defoamation, again preparation liquid is poured on to the curtain coating that tiles on stainless steel plate, then the stainless steel plate with preparation liquid is placed in to the thermostatic drying chamber of 70 ℃, keeps 1.5h, then take out, standing 10h at room temperature, take off film, obtain alkali lignin-starch film, complete the preparation method of alkali lignin-starch film; Wherein in step 1, in W-Gum and step 2, the mass ratio of methylolation alkali lignin is 1:0.7, in step 1, in W-Gum and step 2, quality percentage composition is that the mass volume ratio of 50% glutaraldehyde is 1g:0.1mL, and in step 1, in W-Gum and step 2, the mass volume ratio of glycerine is 1g:0.8mL.
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| CN104292483A (en) * | 2013-07-19 | 2015-01-21 | 东北林业大学 | Preparation of alkali lignin/PVA light insulation blend membrane |
| CN104877200A (en) * | 2015-04-30 | 2015-09-02 | 南京大学 | Lignin-starch composite styrene-butadiene rubber material and preparation method thereof |
| CN107964113A (en) * | 2017-08-15 | 2018-04-27 | 安徽华猫软包装有限公司 | A kind of production method of microwave packaging bag |
| CN109939569A (en) * | 2019-04-12 | 2019-06-28 | 南京林业大学 | The resource utilization method of lignin in a kind of formic acid pulping waste liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102268145A (en) * | 2011-08-22 | 2011-12-07 | 东北林业大学 | Starch-lignin membrane and preparation method thereof |
| CN102337138A (en) * | 2011-05-27 | 2012-02-01 | 刘长福 | Biodegradable liquid mulch film produced from papermaking waste liquid, and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102337138A (en) * | 2011-05-27 | 2012-02-01 | 刘长福 | Biodegradable liquid mulch film produced from papermaking waste liquid, and production method thereof |
| CN102268145A (en) * | 2011-08-22 | 2011-12-07 | 东北林业大学 | Starch-lignin membrane and preparation method thereof |
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