CN103194027B - 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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- CN103194027B CN103194027B CN201310106144.0A CN201310106144A CN103194027B CN 103194027 B CN103194027 B CN 103194027B CN 201310106144 A CN201310106144 A CN 201310106144A CN 103194027 B CN103194027 B CN 103194027B
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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
Prior art is prepared the method that hinders luminescent material and is mainly contained 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 that Photoresist is added and in substrate resin, reaches resistance light effect, conventional carbon black, titanium dioxide etc. are Photoresist, and Photoresist products made thereby color is single, is difficult to meet people to product appearance esthetic requirement.
Summary of the invention
The present invention will solve the prior art preparation resistance luminescent material single problem of Photoresist kind used, and a kind of preparation method of nano-cellulose/xylogen light blocking film is provided.
A preparation method for nano-cellulose/xylogen light blocking film, is prepared according to the following steps:
One, under agitation condition, raw alkaline lignin is dissolved in sodium hydroxide solution, the more centrifugal insolubles of removing, get supernatant liquor, after vacuum-drying, obtain the alkali lignin of purification, wherein the concentration of sodium hydroxide solution is 0.1mol/L;
Two, adopt alkali pre-treatment sulfuric acid solution legal system for nano-cellulose, obtaining nano-cellulose diameter is the cellulose Ⅱ type nano-cellulose water-sol that 10nm～20nm, length are 145nm～155nm;
Three, alkali lignin prepared by step 1, the nano-cellulose water-sol prepared by step 2, 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%, in the nano-cellulose water-sol, the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 0.5%～10%, the total mass ratio of the quality of glycerine and alkali lignin and polyvinyl alcohol is 10%, the total mass ratio of the cumulative volume of the nano-cellulose water-sol and deionized water and alkali lignin and polyvinyl alcohol is 200mL: 10g,
Four, blend step 3 being obtained is the stirred in water bath 2.8h～3.2h of 88 DEG C～92 DEG C in temperature, supersound process 8min～15min again, then under vacuum condition, remove bubble, obtain film forming liquid, by film forming liquid plastic film mulch on smooth polyfluortetraethylene plate, use 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 using xylogen as Photoresist, good biocompatibility, preparation technology is simple, easy to operate, cost is low, good stability, increase light blocking film color, changed the single present situation of resistance luminescent material color.20%～30% alkali lignin scope composite membrane has good ultraviolet-resistant effect, is close to and reaches full obstruct.
The present invention is for the preparation of nano-cellulose/xylogen light blocking film.
Brief description of the drawings
Fig. 1 is that contrast experiment's one mass concentration is respectively 1%, 5%, 10%, 15% and 30% alkali lignin solution and carries out the test curve figure to ultraviolet-visible transmittance, 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 nano-cellulose/xylogen light blocking film of preparing of embodiment mono-, the mass ratio that wherein curve " a " is alkali lignin and polyvinyl alcohol is the tensile strength curve of nano-cellulose/xylogen light blocking film of preparing of 2:8, curve " b " is the tensile strength curve of pure PVA film, and the mass ratio that curve " c " is alkali lignin and polyvinyl alcohol is the tensile strength curve of nano-cellulose/xylogen light blocking film of preparing of 3:7;
Fig. 3 is the elongation at break graphic representation of nano-cellulose/xylogen light blocking film of preparing of embodiment mono-, the mass ratio that wherein curve " a " is alkali lignin and polyvinyl alcohol is the extension at break rate curve of nano-cellulose/xylogen light blocking film of preparing of 2:8, curve " b " is the extension at break rate curve of pure PVA film, and the mass ratio that curve " c " is alkali lignin and polyvinyl alcohol is the extension at break rate curve of nano-cellulose/xylogen light blocking film of preparing of 3:7;
Fig. 4 is the ultraviolet-visible light transmittance curve figure of nano-cellulose/xylogen light blocking film (mass ratio of alkali lignin and polyvinyl alcohol is 2:8) of preparing of embodiment mono-, 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, curve " g " is the ultraviolet-visible light transmittance curve of pure PVA film,
Fig. 5 is the ultraviolet-visible light transmittance curve figure of nano-cellulose/xylogen light blocking film (mass ratio of alkali lignin and polyvinyl alcohol is 3:7) of preparing of embodiment mono-, 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, 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/xylogen of present embodiment light blocking film, is prepared according to the following steps:
One, under agitation condition, raw alkaline lignin is dissolved in sodium hydroxide solution, the more centrifugal insolubles of removing, get supernatant liquor, after vacuum-drying, obtain the alkali lignin of purification, wherein the concentration of sodium hydroxide solution is 0.1mol/L;
Two, adopt alkali pre-treatment sulfuric acid solution legal system for nano-cellulose, obtaining nano-cellulose diameter is the cellulose Ⅱ type nano-cellulose water-sol that 10nm～20nm, length are 145nm～155nm;
Three, alkali lignin prepared by step 1, the nano-cellulose water-sol prepared by step 2, 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%, in the nano-cellulose water-sol, the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 0.5%～10%, the total mass ratio of the quality of glycerine and alkali lignin and polyvinyl alcohol is 10%, the total mass ratio of the cumulative volume of the nano-cellulose water-sol and deionized water and alkali lignin and polyvinyl alcohol is 200mL: 10g,
Four, blend step 3 being obtained is the stirred in water bath 2.8h～3.2h of 88 DEG C～92 DEG C in temperature, supersound process 8min～15min again, then under vacuum condition, remove bubble, obtain film forming liquid, by film forming liquid plastic film mulch on smooth polyfluortetraethylene plate, use 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 is prepared nano-cellulose/xylogen light blocking film using xylogen as Photoresist, good biocompatibility, preparation technology is simple, easy to operate, cost is low, good stability, increase light blocking film color, changed the single present situation of resistance luminescent material color.20%～30% alkali lignin scope composite membrane has good ultraviolet-resistant effect, is close to and reaches full obstruct.
Embodiment two: present embodiment is different from embodiment one: in step 1,50g raw alkaline lignin is dissolved in the sodium hydroxide solution that 1000mL concentration is 0.1mol/L.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one: in step 2, the concentration of the nano-cellulose water-sol is 7.744g/L.Other is identical with embodiment one.
Embodiment four: present embodiment is different from embodiment one: in step 3, in the nano-cellulose water-sol, the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 0.6%～8%.Other is identical with embodiment one.
Embodiment five: present embodiment is different from one of embodiment one to four: in step 3, in the nano-cellulose water-sol, the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 1%.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from embodiment one: the stirred in water bath 3h that in step 4 in temperature is 90 DEG C.Other is identical with embodiment one.
Embodiment seven: present embodiment is different from embodiment one: supersound process 9min～12min in step 4.Other is identical with embodiment one.
Embodiment eight: present embodiment is different from one of embodiment one to seven: supersound process 10min in step 4.Other is identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from embodiment one: be at room temperature dried 24h in step 4.Other is identical with embodiment one.
Embodiment ten: present embodiment is different from embodiment one: in step 4, the thickness of nano-cellulose/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:
Contrast experiment one:
Mass concentration is respectively to 1%, 5%, 10%, 15% and 30% alkali lignin solution and carries out the test to ultraviolet-visible transmittance, as shown in Figure 1, wherein curve a represents 1% to test result, curve b represents 5%, curve c represents 10%, curve d represents 15%, curve e represents 30%.
Embodiment mono-:
The preparation method of the present embodiment nano-cellulose/xylogen light blocking film, is prepared according to the following steps:
One, under agitation condition, 50g raw alkaline lignin is dissolved in the sodium hydroxide solution that 1000mL concentration is 0.1mol/L, the more centrifugal insolubles of removing, supernatant liquor got, after vacuum-drying, obtain the alkali lignin of purifying, wherein the concentration of sodium hydroxide solution is 0.1mol/L;
Two, adopt alkali pre-treatment sulfuric acid solution legal system for nano-cellulose, obtaining nano-cellulose diameter is the cellulose Ⅱ type nano-cellulose water-sol that 10nm～20nm, length are 150nm;
Three, the alkali lignin (Alkali lignin) of being prepared by step 1, the nano-cellulose water-sol (NCC), polyvinyl alcohol (PVA), deionized water (water), polyacrylamide (PAM) and glycerine (Glycerin) prepared by step 2, according to the proportioning blend of table 1, obtain blend;
Four, blend step 3 being obtained is the stirred in water bath 3h of 90 DEG C in temperature, supersound process 10min again, then under vacuum condition, remove bubble, obtain film forming liquid, by film forming liquid plastic film mulch on smooth polyfluortetraethylene plate, use scraper plate drawout, at room temperature dry 24h, obtains nano-cellulose/xylogen light blocking film.
In above-mentioned steps two, the concentration of the nano-cellulose water-sol is 7.744g/L.
The mechanical experimental results of nano-cellulose/xylogen light blocking film prepared by the present embodiment is as shown in table 2.
The tensile strength curve figure of nano-cellulose/xylogen light blocking film prepared by the present embodiment as shown in Figure 2, the mass ratio that wherein curve " a " is alkali lignin and polyvinyl alcohol is the tensile strength curve of nano-cellulose/xylogen light blocking film of preparing of 2:8, curve " b " is the tensile strength curve of pure PVA film, and the mass ratio that curve " c " is alkali lignin and polyvinyl alcohol is the tensile strength curve of nano-cellulose/xylogen light blocking film of preparing of 3:7.
The elongation at break graphic representation of nano-cellulose/xylogen light blocking film prepared by the present embodiment as shown in Figure 3, the mass ratio that wherein curve " a " is alkali lignin and polyvinyl alcohol is the extension at break rate curve of nano-cellulose/xylogen light blocking film of preparing of 2:8, curve " b " is the extension at break rate curve of pure PVA film, and the mass ratio that curve " c " is alkali lignin and polyvinyl alcohol is the extension at break rate curve of nano-cellulose/xylogen light blocking film of preparing of 3:7.
The ultraviolet-visible light transmittance curve figure of nano-cellulose/xylogen light blocking film (mass ratio of alkali lignin and polyvinyl alcohol is 2:8) prepared by the present embodiment 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, curve " g " is the ultraviolet-visible light transmittance curve of pure PVA film.
The ultraviolet-visible light transmittance curve figure of nano-cellulose/xylogen light blocking film (mass ratio of alkali lignin and polyvinyl alcohol is 3:7) prepared by the present embodiment 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, curve " g " is the ultraviolet-visible light transmittance curve of pure PVA film.
Table 1 proportioning raw materials
Table 2 mechanical property
From the alkali lignin solution of known 15%～30% concentration of Fig. 1～Fig. 5, the light wave of 200nm～800nm wavelength is had to good absorption and inhibition.In the time that alkali lignin content reduces, near-ultraviolet light and royal purple light are had to good absorption and iris action equally.If select 20% alkali lignin, tensile strength and elongation at break can improve.Intensity may approach pure PVA film, keep resistance photosensitiveness preferably, but resistance photosensitiveness should have certain decline simultaneously.As can be seen from Figure 2, nano-cellulose concentration is significantly improved to the tensile strength of 20% and 30% alkali lignin filling film lower than 2% time, in the time that being 1%, addition reaches maximum value, wherein the purer PVA film of the tensile strength of 20% alkali lignin filled composite film has improved 29.22%, 30% alkali lignin filled composite film 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 and all can make the elongation at break of film decrease, but still have 133.5% at 1%NCC and 20% alkali lignin elongation at break; From Fig. 4 and Fig. 5,20%～30% alkali lignin scope composite membrane has good ultraviolet-resistant effect, is close to and reaches full obstruct.
Claims (10)
1. a preparation method for nano-cellulose/xylogen light blocking film, is characterized in that being prepared a kind of preparation method of nano-cellulose/xylogen light blocking film according to the following steps:
One, under agitation condition, raw alkaline lignin is dissolved in sodium hydroxide solution, the more centrifugal insolubles of removing, get supernatant liquor, after vacuum-drying, obtain the alkali lignin of purification, wherein the concentration of sodium hydroxide solution is 0.1mol/L;
Two, adopt alkali pre-treatment sulfuric acid solution legal system for nano-cellulose, obtaining nano-cellulose diameter is the cellulose Ⅱ type nano-cellulose water-sol that 10nm～20nm, length are 145nm～155nm;
Three, alkali lignin prepared by step 1, the nano-cellulose water-sol prepared by step 2, 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%, in the nano-cellulose water-sol, the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 0.5%～10%, the total mass ratio of the quality of glycerine and alkali lignin and polyvinyl alcohol is 10%, the total mass ratio of the cumulative volume of the nano-cellulose water-sol and deionized water and alkali lignin and polyvinyl alcohol is 200mL: 10g,
Four, blend step 3 being obtained is the stirred in water bath 2.8h～3.2h of 88 DEG C～92 DEG C in temperature, supersound process 8min～15min again, then under vacuum condition, remove bubble, obtain film forming liquid, by film forming liquid plastic film mulch on smooth polyfluortetraethylene plate, use 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/xylogen light blocking film according to claim 1, is characterized in that in step 1,50g raw alkaline lignin being dissolved in the sodium hydroxide solution that 1000mL concentration is 0.1mol/L.
3. the preparation method of a kind of nano-cellulose/xylogen light blocking film according to claim 1, the concentration that it is characterized in that the nano-cellulose water-sol in step 2 is 7.744g/L.
4. the preparation method of a kind of nano-cellulose/xylogen light blocking film according to claim 1, is characterized in that in step 3 that in the nano-cellulose water-sol, the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 0.6%～8%.
5. the preparation method of a kind of nano-cellulose/xylogen light blocking film according to claim 4, is characterized in that in step 3 that in the nano-cellulose water-sol, the total mass ratio of the quality of nano-cellulose and alkali lignin and polyvinyl alcohol is 1%.
6. the preparation method of a kind of nano-cellulose/xylogen light blocking film according to claim 1, is characterized in that in step 4 being the stirred in water bath 3h of 90 DEG C in temperature.
7. the preparation method of a kind of nano-cellulose/xylogen light blocking film according to claim 1, is characterized in that supersound process 9min～12min in step 4.
8. the preparation method of a kind of nano-cellulose/xylogen light blocking film according to claim 7, is characterized in that supersound process 10min in step 4.
9. the preparation method of a kind of nano-cellulose/xylogen light blocking film according to claim 1, is characterized in that in step 4 at room temperature dry 24h.
10. the preparation method of a kind of nano-cellulose/xylogen light blocking film according to claim 1, the thickness that it is characterized in that nano-cellulose/xylogen light blocking film in step 4 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 |
| CN104497341B (en) * | 2015-01-08 | 2017-05-31 | 江南大学 | A kind of preparation method of photo crosslinked polyethylene alcohol/lignin PVA/lignin composite membranes |
| 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 |
| CN116693880A (en) * | 2023-06-28 | 2023-09-05 | 浙江科技学院 | Lignin modification treatment method and preparation method of cellulose composite membrane |
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