CN103194027A - Method for preparing nano-crystalline cellulose/lignin photoresist film - Google Patents
Method for preparing nano-crystalline cellulose/lignin photoresist film Download PDFInfo
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- CN103194027A CN103194027A CN2013101061440A CN201310106144A CN103194027A CN 103194027 A CN103194027 A CN 103194027A CN 2013101061440 A CN2013101061440 A CN 2013101061440A CN 201310106144 A CN201310106144 A CN 201310106144A CN 103194027 A CN103194027 A CN 103194027A
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Abstract
The invention discloses a method for preparing a nano-crystalline cellulose/lignin photoresist film. The method relates to a preparation method of a photoresist material, and aims at solving the problem of single variety of a photoresist used for preparing the photoresist material in the prior art. The method comprises the steps of 1, purifying alkali lignin; 2, preparing nano cellulose hydrosol; 3, blending; and 4, preparing the nano-crystalline cellulose/lignin photoresist film. The lignin is taken as the photoresist to prepare the nano-crystalline cellulose/lignin photoresist film. The method is good in biocompatibility, simple in preparation technology, easy to operate, low in cost and good in stability; the color of the photoresist film is increased; and the current situation of single color of the photoresist film is changed. The method disclosed by the invention is used for preparing the nano-crystalline cellulose/lignin photoresist film.
Description
Technical field
The present invention relates to hinder the preparation method of luminescent material.
Background technology
The method of prior art for preparing resistance luminescent material mainly contains two kinds: the one, by increasing the method for top coat or light blocking film, processing requirement is higher, involve great expense, less stable, another kind of is exactly Photoresist to be added reach the resistance light effect in the substrate resin, carbon black commonly used, titanium dioxide etc. are Photoresist, and Photoresist products made thereby color is single, is difficult to satisfy people to the product appearance esthetic requirement.
Summary of the invention
The present invention will solve the used single problem of Photoresist kind of prior art for preparing resistance luminescent material, and the preparation method of a kind of nano-cellulose/xylogen light blocking film is provided.
The preparation method of a kind of nano-cellulose/xylogen light blocking film is prepared according to the following steps:
One, under agitation condition, thick alkali lignin is dissolved in the sodium hydroxide solution, the centrifugal insolubles of removing is got supernatant liquor again, obtains the alkali lignin of purifying after the vacuum-drying, and wherein the concentration of sodium hydroxide solution is 0.1mol/L;
Two, adopt alkali pre-treatment sulfuric acid solution legal system to be equipped with nano-cellulose, obtaining the nano-cellulose diameter is that 10nm~20nm, length are the cellulose type nano-cellulose water-sol of 145nm~155nm;
Three, alkali lignin with the step 1 preparation, the nano-cellulose water-sol of step 2 preparation, polyvinyl alcohol, deionized water, polyacrylamide and glycerine blend, obtain blend, wherein the mass ratio of alkali lignin and polyvinyl alcohol is 2~3:8~7, the total mass ratio of the quality of polyacrylamide and alkali lignin and polyvinyl alcohol is 2%, the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 0.5%~10% in the nano-cellulose water-sol, the total mass ratio of the quality of glycerine and alkali lignin and polyvinyl alcohol is 10%, and the total mass ratio of the cumulative volume of the nano-cellulose water-sol and deionized water and alkali lignin and polyvinyl alcohol is 2:1;
Four, the blend that step 3 is obtained is stirred in water bath 2.8h~3.2h of 88 ℃~92 ℃ in temperature, supersound process 8min~15min again, under vacuum condition, remove bubble then, obtain film forming liquid, with film forming liquid plastic film mulch on smooth polyfluortetraethylene plate, use the scraper plate drawout, at room temperature dry 22h~26h obtains nano-cellulose/xylogen light blocking film.
The invention has the beneficial effects as follows: nano-cellulose and xylogen all have biological degradability, the present invention prepares nano-cellulose/xylogen light blocking film with xylogen as Photoresist, good biocompatibility, preparation technology is simple, easy to operate, cost is low, good stability, increase the light blocking film color, changed the single present situation of resistance luminescent material color.20%~30% alkali lignin scope composite membrane has ultraviolet-resistant effect preferably, is close to reach full obstruct.
The present invention is for the preparation of nano-cellulose/xylogen light blocking film.
Description of drawings
Fig. 1 carries out test curve figure to the ultraviolet-visible transmittance for contrast experiment's one mass concentration is respectively 1%, 5%, 10%, 15% and 30% alkali lignin solution, and wherein curve a represents 1%, curve b represents 5%, curve c represents 10%, curve d represents 15%, curve e represents 30%;
Fig. 2 is the tensile strength curve figure of the nano-cellulose/xylogen light blocking film of embodiment one preparation, wherein curve " a " is the tensile strength curve of the nano-cellulose/xylogen light blocking film of 2:8 preparation for the mass ratio of alkali lignin and polyvinyl alcohol, curve " b " is the tensile strength curve of pure PVA film, and curve " c " is the tensile strength curve of the nano-cellulose/xylogen light blocking film of 3:7 preparation for the mass ratio of alkali lignin and polyvinyl alcohol;
Fig. 3 is the elongation at break graphic representation of the nano-cellulose/xylogen light blocking film of embodiment one preparation, wherein curve " a " is the extension at break rate curve of the nano-cellulose/xylogen light blocking film of 2:8 preparation for the mass ratio of alkali lignin and polyvinyl alcohol, curve " b " is the extension at break rate curve of pure PVA film, and curve " c " is the extension at break rate curve of the nano-cellulose/xylogen light blocking film of 3:7 preparation for the mass ratio of alkali lignin and polyvinyl alcohol;
Fig. 4 is the ultraviolet-visible light transmittance curve figure of the nano-cellulose/xylogen light blocking film (mass ratio of alkali lignin and polyvinyl alcohol is 2:8) of embodiment one preparation, wherein curve " a " is the ultraviolet-visible light transmittance curve of numbering m-0-20, curve " b " is the ultraviolet-visible light transmittance curve of numbering m-1-20, curve " c " is the ultraviolet-visible light transmittance curve of numbering m-2-20, curve " d " is the ultraviolet-visible light transmittance curve of numbering m-3-20, curve " e " is the ultraviolet-visible light transmittance curve of numbering m-4-20, curve " f " is the ultraviolet-visible light transmittance curve of numbering m-5-20, and curve " g " is the ultraviolet-visible light transmittance curve of pure PVA film;
Fig. 5 is the ultraviolet-visible light transmittance curve figure of the nano-cellulose/xylogen light blocking film (mass ratio of alkali lignin and polyvinyl alcohol is 3:7) of embodiment one preparation, wherein curve " a " is the ultraviolet-visible light transmittance curve of numbering m-0-30, curve " b " is the ultraviolet-visible light transmittance curve of numbering m-1-30, curve " c " is the ultraviolet-visible light transmittance curve of numbering m-2-30, curve " d " is the ultraviolet-visible light transmittance curve of numbering m-3-30, curve " e " is the ultraviolet-visible light transmittance curve of numbering m-4-30, curve " f " is the ultraviolet-visible light transmittance curve of numbering m-5-30, and curve " g " is the ultraviolet-visible light transmittance curve of pure PVA film.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of a kind of nano-cellulose of present embodiment/xylogen light blocking film is prepared according to the following steps:
One, under agitation condition, thick alkali lignin is dissolved in the sodium hydroxide solution, the centrifugal insolubles of removing is got supernatant liquor again, obtains the alkali lignin of purifying after the vacuum-drying, and wherein the concentration of sodium hydroxide solution is 0.1mol/L;
Two, adopt alkali pre-treatment sulfuric acid solution legal system to be equipped with nano-cellulose, obtaining the nano-cellulose diameter is that 10nm~20nm, length are the cellulose type nano-cellulose water-sol of 145nm~155nm;
Three, alkali lignin with the step 1 preparation, the nano-cellulose water-sol of step 2 preparation, polyvinyl alcohol, deionized water, polyacrylamide and glycerine blend, obtain blend, wherein the mass ratio of alkali lignin and polyvinyl alcohol is 2~3:8~7, the total mass ratio of the quality of polyacrylamide and alkali lignin and polyvinyl alcohol is 2%, the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 0.5%~10% in the nano-cellulose water-sol, the total mass ratio of the quality of glycerine and alkali lignin and polyvinyl alcohol is 10%, and the total mass ratio of the cumulative volume of the nano-cellulose water-sol and deionized water and alkali lignin and polyvinyl alcohol is 2:1;
Four, the blend that step 3 is obtained is stirred in water bath 2.8h~3.2h of 88 ℃~92 ℃ in temperature, supersound process 8min~15min again, under vacuum condition, remove bubble then, obtain film forming liquid, with film forming liquid plastic film mulch on smooth polyfluortetraethylene plate, use the scraper plate drawout, at room temperature dry 22h~26h obtains nano-cellulose/xylogen light blocking film.
Nano-cellulose and xylogen all have biological degradability, present embodiment prepares nano-cellulose/xylogen light blocking film with xylogen as Photoresist, good biocompatibility, preparation technology is simple, easy to operate, cost is low, good stability, increase the light blocking film color, changed the single present situation of resistance luminescent material color.20%~30% alkali lignin scope composite membrane has ultraviolet-resistant effect preferably, is close to reach full obstruct.
Embodiment two: what present embodiment and embodiment one were different is: in the step 1 the thick alkali lignin of 50g is dissolved in the sodium hydroxide solution that 1000mL concentration is 0.1mol/L.Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: the concentration of the nano-cellulose water-sol is 7.744g/L in the step 2.Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is: in the step 3 in the nano-cellulose water-sol total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol be 0.6%~8%.Other is identical with embodiment one.
Embodiment five: what present embodiment was different with one of embodiment one to four is: in the step 3 in the nano-cellulose water-sol total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol be 1%.Other is identical with one of embodiment one to four.
Embodiment six: what present embodiment and embodiment one were different is: the stirred in water bath 3h that in the step 4 in temperature is 90 ℃.Other is identical with embodiment one.
Embodiment seven: what present embodiment and embodiment one were different is: supersound process 9min~12min in the step 4.Other is identical with embodiment one.
Embodiment eight: what present embodiment was different with one of embodiment one to seven is: supersound process 10min in the step 4.Other is identical with one of embodiment one to seven.
Embodiment nine: what present embodiment and embodiment one were different is: dry 24h at room temperature in the step 4.Other is identical with embodiment one.
Embodiment ten: what present embodiment and embodiment one were different is: the thickness of nano-cellulose in the step 4/xylogen light blocking film is 0.06mm~0.09mm.Other is identical with embodiment one.
Adopt following examples and contrast experiment to verify beneficial effect of the present invention:
The contrast experiment one:
Mass concentration is respectively 1%, 5%, 10%, 15% and 30% alkali lignin solution carries out test to the ultraviolet-visible transmittance, test result as shown in Figure 1, wherein curve a represents 1%, curve b represents 5%, curve c represents 10%, curve d represents 15%, curve e represents 30%.
Embodiment one:
The preparation method of present embodiment nano-cellulose/xylogen light blocking film is prepared according to the following steps:
One, under agitation condition, the thick alkali lignin of 50g is dissolved in the sodium hydroxide solution that 1000mL concentration is 0.1mol/L, and the centrifugal insolubles of removing is got supernatant liquor again, obtain the alkali lignin of purifying after the vacuum-drying, wherein the concentration of sodium hydroxide solution is 0.1mol/L;
Two, adopt alkali pre-treatment sulfuric acid solution legal system to be equipped with nano-cellulose, obtaining the nano-cellulose diameter is that 10nm~20nm, length are the cellulose type nano-cellulose water-sol of 150nm;
Three, the nano-cellulose water-sol (NCC), polyvinyl alcohol (PVA), deionized water (water), polyacrylamide (PAM) and the glycerine (Glycerin) of the alkali lignin (Alkali lignin) that step 1 is prepared, step 2 preparation obtain blend according to the proportioning blend of table 1;
Four, the blend that step 3 is obtained is 90 ℃ stirred in water bath 3h in temperature, supersound process 10min again, under vacuum condition, remove bubble then, obtain film forming liquid, with film forming liquid plastic film mulch on smooth polyfluortetraethylene plate, use the scraper plate drawout, at room temperature dry 24h obtains nano-cellulose/xylogen light blocking film.
The concentration of the nano-cellulose water-sol is 7.744g/L in the above-mentioned steps two.
The Mechanics Performance Testing result of the nano-cellulose/xylogen light blocking film of present embodiment preparation is as shown in table 2.
The tensile strength curve figure of the nano-cellulose/xylogen light blocking film of present embodiment preparation as shown in Figure 2, wherein curve " a " is the tensile strength curve of the nano-cellulose/xylogen light blocking film of 2:8 preparation for the mass ratio of alkali lignin and polyvinyl alcohol, curve " b " is the tensile strength curve of pure PVA film, and curve " c " is the tensile strength curve of the nano-cellulose/xylogen light blocking film of 3:7 preparation for the mass ratio of alkali lignin and polyvinyl alcohol.
The elongation at break graphic representation of the nano-cellulose/xylogen light blocking film of present embodiment preparation as shown in Figure 3, wherein curve " a " is the extension at break rate curve of the nano-cellulose/xylogen light blocking film of 2:8 preparation for the mass ratio of alkali lignin and polyvinyl alcohol, curve " b " is the extension at break rate curve of pure PVA film, and curve " c " is the extension at break rate curve of the nano-cellulose/xylogen light blocking film of 3:7 preparation for the mass ratio of alkali lignin and polyvinyl alcohol.
The ultraviolet-visible light transmittance curve figure of the nano-cellulose/xylogen light blocking film (mass ratio of alkali lignin and polyvinyl alcohol is 2:8) of present embodiment preparation as shown in Figure 4, wherein curve " a " is the ultraviolet-visible light transmittance curve of numbering m-0-20, curve " b " is the ultraviolet-visible light transmittance curve of numbering m-1-20, curve " c " is the ultraviolet-visible light transmittance curve of numbering m-2-20, curve " d " is the ultraviolet-visible light transmittance curve of numbering m-3-20, curve " e " is the ultraviolet-visible light transmittance curve of numbering m-4-20, curve " f " is the ultraviolet-visible light transmittance curve of numbering m-5-20, and curve " g " is the ultraviolet-visible light transmittance curve of pure PVA film.
The ultraviolet-visible light transmittance curve figure of the nano-cellulose/xylogen light blocking film (mass ratio of alkali lignin and polyvinyl alcohol is 3:7) of present embodiment preparation as shown in Figure 5, wherein curve " a " is the ultraviolet-visible light transmittance curve of numbering m-0-30, curve " b " is the ultraviolet-visible light transmittance curve of numbering m-1-30, curve " c " is the ultraviolet-visible light transmittance curve of numbering m-2-30, curve " d " is the ultraviolet-visible light transmittance curve of numbering m-3-30, curve " e " is the ultraviolet-visible light transmittance curve of numbering m-4-30, curve " f " is the ultraviolet-visible light transmittance curve of numbering m-5-30, and curve " g " is the ultraviolet-visible light transmittance curve of pure PVA film.
Table 1 proportioning raw materials
Table 2 mechanical property
From Fig. 1~Fig. 5 as can be known the alkali lignin solution of 15%~30% concentration the light wave of 200nm~800nm wavelength is had good absorption and inhibition.When alkali lignin content reduces, near-ultraviolet light and royal purple light there are good absorption and iris action equally.If select 20% alkali lignin, tensile strength and elongation at break can improve.Intensity may keep hindering preferably photosensitiveness simultaneously near pure PVA film, but the resistance photosensitiveness should have certain decline.As can be seen from Figure 2, nano-cellulose concentration is lower than 2% o'clock tensile strength to 20% and 30% alkali lignin filling film and is significantly improved, when being 1%, addition reaches maximum value, wherein the purer PVA film of tensile strength of 20% alkali lignin filling composite membrane has improved 29.22%, what 30% alkali lignin was filled composite membrane can reach 89.10% of pure PVA film toughness, but can substitute 10% material polyethylene more; As can be seen from Figure 3, add alkali lignin and NCC the elongation at break of film is decreased, but still have 133.5% at 1%NCC and 20% alkali lignin elongation at break; From Fig. 4 and Fig. 5 as can be known, 20%~30% alkali lignin scope composite membrane has ultraviolet-resistant effect preferably, is close to reach full obstruct.
Claims (10)
1. the preparation method of nano-cellulose/xylogen light blocking film is characterized in that the preparation method of a kind of nano-cellulose/xylogen light blocking film being prepared according to the following steps:
One, under agitation condition, thick alkali lignin is dissolved in the sodium hydroxide solution, the centrifugal insolubles of removing is got supernatant liquor again, obtains the alkali lignin of purifying after the vacuum-drying, and wherein the concentration of sodium hydroxide solution is 0.1mol/L;
Two, adopt alkali pre-treatment sulfuric acid solution legal system to be equipped with nano-cellulose, obtaining the nano-cellulose diameter is that 10nm~20nm, length are the cellulose type nano-cellulose water-sol of 145nm~155nm;
Three, alkali lignin with the step 1 preparation, the nano-cellulose water-sol of step 2 preparation, polyvinyl alcohol, deionized water, polyacrylamide and glycerine blend, obtain blend, wherein the mass ratio of alkali lignin and polyvinyl alcohol is 2~3:8~7, the total mass ratio of the quality of polyacrylamide and alkali lignin and polyvinyl alcohol is 2%, the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 0.5%~10% in the nano-cellulose water-sol, the total mass ratio of the quality of glycerine and alkali lignin and polyvinyl alcohol is 10%, and the total mass ratio of the cumulative volume of the nano-cellulose water-sol and deionized water and alkali lignin and polyvinyl alcohol is 2:1;
Four, the blend that step 3 is obtained is stirred in water bath 2.8h~3.2h of 88 ℃~92 ℃ in temperature, supersound process 8min~15min again, under vacuum condition, remove bubble then, obtain film forming liquid, with film forming liquid plastic film mulch on smooth polyfluortetraethylene plate, use the scraper plate drawout, at room temperature dry 22h~26h obtains nano-cellulose/xylogen light blocking film.
2. the preparation method of a kind of nano-cellulose according to claim 1/xylogen light blocking film is characterized in that in the step 1 the thick alkali lignin of 50g being dissolved in the sodium hydroxide solution that 1000mL concentration is 0.1mol/L.
3. the preparation method of a kind of nano-cellulose according to claim 1/xylogen light blocking film, the concentration that it is characterized in that the nano-cellulose water-sol in the step 2 is 7.744g/L.
4. the preparation method of a kind of nano-cellulose according to claim 1/xylogen light blocking film is characterized in that in the step 3 that the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 0.6%~8% in the nano-cellulose water-sol.
5. the preparation method of a kind of nano-cellulose according to claim 4/xylogen light blocking film is characterized in that in the step 3 that the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 1% in the nano-cellulose water-sol.
6. the preparation method of a kind of nano-cellulose according to claim 1/xylogen light blocking film is characterized in that in the step 4 in temperature being 90 ℃ stirred in water bath 3h.
7. the preparation method of a kind of nano-cellulose according to claim 1/xylogen light blocking film is characterized in that supersound process 9min~12min in the step 4.
8. the preparation method of a kind of nano-cellulose according to claim 7/xylogen light blocking film is characterized in that supersound process 10min in the step 4.
9. the preparation method of a kind of nano-cellulose according to claim 1/xylogen light blocking film is characterized in that in the step 4 dry 24h at room temperature.
10. the preparation method of a kind of nano-cellulose according to claim 1/xylogen light blocking film, the thickness that it is characterized in that nano-cellulose in the step 4/xylogen light blocking film is 0.06mm~0.09mm.
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CN103467759A (en) * | 2013-07-17 | 2013-12-25 | 东北林业大学 | Preparation method of industrial alkali lignin/polyvinyl alcohol cross-linked thin film |
CN104292483A (en) * | 2013-07-19 | 2015-01-21 | 东北林业大学 | Preparation of alkali lignin/PVA light insulation blend membrane |
CN104497341A (en) * | 2015-01-08 | 2015-04-08 | 江南大学 | Preparation method of photo-crosslinked PVA (polyvinyl alcohol)/lignin composite membrane |
CN114316294A (en) * | 2021-12-31 | 2022-04-12 | 湖北工业大学 | Partially-dissolved lignocellulose and preparation method and application of bioplastic thereof |
CN115449104A (en) * | 2022-10-11 | 2022-12-09 | 浙江理工大学 | Preparation method of high-toughness uvioresistant wood cellulose membrane |
CN116102792A (en) * | 2022-09-07 | 2023-05-12 | 中国农业大学 | Cellulose acetate film with ultraviolet shielding function, preparation method and application thereof |
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Cited By (6)
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CN114316294A (en) * | 2021-12-31 | 2022-04-12 | 湖北工业大学 | Partially-dissolved lignocellulose and preparation method and application of bioplastic thereof |
CN116102792A (en) * | 2022-09-07 | 2023-05-12 | 中国农业大学 | Cellulose acetate film with ultraviolet shielding function, preparation method and application thereof |
CN115449104A (en) * | 2022-10-11 | 2022-12-09 | 浙江理工大学 | Preparation method of high-toughness uvioresistant wood cellulose membrane |
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