CN103387689A - Method for preparing nanocellulose fiber optical transparent membrane material from peanut hulls - Google Patents
Method for preparing nanocellulose fiber optical transparent membrane material from peanut hulls Download PDFInfo
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Abstract
The invention discloses a method for preparing a nanocellulose fiber optical transparent membrane material from peanut hulls. The method comprises pretreatment, chemical treatment and mechanical treatment, wherein the pretreatment comprises the step of extracting resin, wax, fat and ether insoluble matters as well as tannins and pigments contained in the raw material by a benzene-alcohol extraction method, wherein the chemical treatment is to remove non-fiber components, hemicellulose and lignin in biomass fibers to obtain purified cellulose, and the mechanical treatment is to carry out nanocrystallization of the fibers by virtue of grinding, ultrasonics and homogenization, thereby obtaining the nanocellulose fibers. The method provided by the invention has the following advantages that in consideration of the facts that the forest area of China is limited and the peanut hull resources are rich but most wasted, the peanut hull cellulose is selected as the raw material and the nanocellulose optical transparent membrane with excellent properties can be prepared by extracting and dissolving the peanut hull cellulose, and therefore, the method has great practical significance and wide development prospect for rational utilization of the peanut hull resources and sustainable development of natural resources.
Description
Technical field
What the present invention relates to is to utilize Pericarppium arachidis hypogaeae to prepare the method for nano-cellulose fiber optical clear mould material.
Background technology
Mierocrystalline cellulose is one of natural macromolecular material the abundantest on the earth, and recyclability makes it have good performance and application widely.China's Pericarppium arachidis hypogaeae year approximately 5000 * 10
3Ton, contain a large amount of crude fibres, xylogen, hemicellulose, soluble-carbohydrate etc. in its dry-matter.
The source of the available natural cellulose of tradition is mainly timber, cotton stalk etc., but the increase day by day of the finiteness of China's timber resources and social demand has formed striking contrast, and many timber resources need import.And China is Peanut big producing country, and the gross annual output amount reaches more than 1,450 ten thousand tons, accounts for 42% of Gross World Product, approximately produces 4,500,000 tons of Pericarppium arachidis hypogaeaes every year.Contain the natural high molecular substances such as a large amount of Mierocrystalline celluloses, xylogen, hemicellulose in Pericarppium arachidis hypogaeae.At present, Pericarppium arachidis hypogaeae is except small part is used as feed, and major part is thrown away and burns, and causes significant wastage and the environmental pollution of resource.Be applied to industrial production and not only can improve the added value of agricultural-food if can extract the Mierocrystalline cellulose of high-quality from Pericarppium arachidis hypogaeae, the application that makes resource is reasonably optimizing more, and can reduce the demand pressure to cotton, fiber crops, timber, saves petroleum resources.
Impact owing to containing the performance of the meetings such as fatty compounds, phenolic compound to the film that makes in Pericarppium arachidis hypogaeae,, so first adopt benzene and dehydrated alcohol to carry out extracting to it, remove these materials.Secondly, utilize chemical treatment method to remove successively xylogen and hemicellulose in Pericarppium arachidis hypogaeae, reservation Mierocrystalline cellulose as much as possible.
Summary of the invention
What the present invention proposed is to utilize Pericarppium arachidis hypogaeae to prepare the method for nano-cellulose fiber optical clear mould material, its objective is utilization ratio but very low Pericarppium arachidis hypogaeae be raw material, isolate from Pericarppium arachidis hypogaeae and have the cellulose nano-fibrous of high length-diameter ratio in conjunction with the method for mechanical treatment by chemical treatment.
Technical solution of the present invention: utilize Pericarppium arachidis hypogaeae to prepare the method for nano-cellulose fiber optical clear mould material, comprise pre-treatment, chemical treatment and mechanical treatment, wherein pre-treatment is to adopt the method for Benzene-ethanol extraction to extract contained resin, wax, fat and some ether insolubless in raw material, tannin and pigment out; Chemical treatment is that hemicellulose, xylogen, obtain purifying cellulose in order to remove the non-fibre composition in biomass fiber; Mechanical treatment is to utilize to grind, and ultrasonic, homogeneous, with the fiber nanometer, obtains nano level cellulosic fibre.
Positively effect of the present invention: compared with prior art,
(1) the present invention utilizes chemical treatment to prepare the cellulose nano-fibrous of high length-diameter ratio in conjunction with the method for mechanical treatment from peanut hull meal, and be made into the mould material with optical transparence, prove that by ultraviolet spectrophotometer and mechanical test not only the transparency reaches 78% left and right, and tensile property has also surpassed 100MPa.
(2) utilize mechanical processing method to the solution that makes grind, ultrasonic, centrifugal, homogeneous, make the method for its nanometer simple and feasible, can promote the professional etiquette modelling of going forward side by side and produce.
(3) utilize peanut hull meal to be starting material, adopt chemical treatment to prepare the cellulose nano-fibrous of high length-diameter ratio in conjunction with the method for mechanical treatment.Simultaneously, the peanut hull meal nanofiber has presented three-dimensional space net structure.
(4) compared and only ground, grind+ultrasonic, grind+ultrasonic+centrifugal, grind+ultrasonic+mechanical property and the optical property of homogeneous, grinding+ultrasonic+homogeneous+centrifugal five kinds of different mechanical treatment mode gained films, result shows, along with the increase of grinding number of times, Young's modulus and elongation at break all are greatly improved, and tensile strength is without obvious change; After further ultrasonic and centrifugal, Young's modulus and tensile strength are improved, and elongation at break is without obvious change; Further after homogeneous, Young's modulus does not almost change, and tensile strength and elongation at break obviously increase.Simultaneously, along with the increase of grinding number of times, the transmittance that is the 600nm place at wavelength increases gradually; After further ultrasonic and centrifugal, transmittance has obvious growth before; After homogeneous, transmittance is better.
(5) along with the increase of grinding number of times, transmittance increases gradually, after grinding, most of fiber size reaches nano level,, less than 1/10th of visible wavelength, grinds number of times more, the size of fiber is meticulousr, so its visible light transmissivity improves.
(6) through ultrasonic and centrifugal after, transmitance is significantly improved, after supersound process, the size of nanofiber is meticulousr, more is conducive to seeing through of visible light, visible light transmissivity more only grinds to compare and improves.Centrifugal can be with macro nanometer fiber precipitation, further meticulous nanofiber is kept, thereby further improves the perviousness of visible light, so its visible light transmissivity is more ultrasonic compares and improve.
(7) after homogeneous, transmitance is further improved again, because after further homogeneous, the size of nanofiber is not only meticulousr, and more even, light transmission rate can have been had more raising.And centrifugal can be with macro nanometer fiber precipitation, further meticulous nanofiber is kept, thereby further improves the perviousness of visible light, thus its visible light transmissivity than isotropic phase than improving again.
(8) sample through grinding can become homodisperse suspension, and after further carrying out supersound process, fiber solution still presents suspended state, and there is no to occur very large change.After centrifugal, large-sized nanofiber is precipitated, remaining small size nanofiber supernatant liquor.And after further carrying out high-pressure homogeneous processing again, the suspension of nanofiber becomes more transparent.
(9) along with the increase of grinding number of times, Young's modulus and elongation at break all are greatly improved, and tensile strength is without obvious change; After further ultrasonic and centrifugal, Young's modulus and tensile strength are improved, and elongation at break is without obvious change; Further after homogeneous, Young's modulus does not almost change, and tensile strength and elongation at break obviously increase.
(10) along with the increase of grinding number of times, the transmittance that is the 600nm place at wavelength increases gradually; After further ultrasonic and centrifugal, transmittance has obvious growth before; After homogeneous, transmittance is better.
Description of drawings
Fig. 1 is the procedure chart of acid treatment number of times on the impact of experiment.
Fig. 2 is the procedure chart of acid treatment number of times on the impact of experiment.
Fig. 3 is the procedure chart of milled processed number of times on the impact of experiment.
Fig. 4 is the procedure chart of grinding, grinding+ultrasonic, grinding+ultrasonic+centrifugal impact on experiment.
Fig. 5 be grind+ultrasonic, grindings+ultrasonic+homogeneous, grinding+ultrasonic+homogeneous+centrifugal is on the procedure chart of the impact of testing.
Fig. 6 is the peanut hull meal FTIR figure after peanut hull meal and chemical treatment that is untreated.
Fig. 7 grinds+the transmittance figure of ultrasonic, grinding+ultrasonic+homogeneous, grinding+ultrasonic+homogeneous+centrifugal gained film.
Embodiment
A kind of method of utilizing Pericarppium arachidis hypogaeae to prepare nano-cellulose fiber optical clear mould material, comprise pre-treatment, chemical treatment and mechanical treatment, wherein pre-treatment is to adopt the method for Benzene-ethanol extraction to extract contained resin, wax, fat and some ether insolubless in raw material, tannin and pigment out; Chemical treatment is that hemicellulose, xylogen, obtain purifying cellulose in order to remove the non-fibre composition in biomass fiber; Mechanical treatment is to utilize to grind, and ultrasonic, homogeneous, with the fiber nanometer, obtains nano level cellulosic fibre.
Described pre-treatment, be the living peanut that will buy from the market, after the Semen arachidis hypogaeae of peeling off, Pericarppium arachidis hypogaeae cleaned with distilled water, puts into the baking oven oven dry more than 24 hours, dries by the fire to the over dry state, Pericarppium arachidis hypogaeae clayed into power standby with the plant pulverizer after oven dry.Utilize standard inspection sieve to filter out 50-80 purpose peanut hull meal, store for future use under room temperature.
Described pre-treatment specifically accurately takes 3 ± 0.2g, claim accurate to 0.0001g, the sample of having got ready, simultaneously separately take sample and measure moisture by GB/T2677.2, wrap with the qualitative filter paper of the benzene alcoholic solution extracting 1 ~ 2h of the part by weight mixing of 2 ︰ 1 with the dehydrated alcohol of benzene and 95%, with line, tie in order to avoid spill; Put in Soxhlet extractor, add the benzene alcoholic solution of the required use of 300ml to make over its overflow level, and add 20ml, load onto cold wink device, connect extractor, be placed in the water-bath of 85 ~ 90 ℃; Open water coolant, it is that the per hour circulation in Soxhlet extractor is no less than 4 times that the adjusting well heater makes its organic solvent boiling speed, so extracting 6h; After extracting is complete, mention condenser, finding has the paper hair in extractum, should Extract be filtered in weighing bottle by filter paper, then use bottle and filter paper at the bottom of 10 ~ 20ml benzene alcoholic solution gradation rinsing; Take out the paper bag that fills sample with clip from extractor, then condenser is connected with extractor again, till being evaporated at the bottom of extracting the extract in bottle and being 30ml, with this, reclaim a part of organic solvent.Take off end bottle, clean in the baking oven of inserting 105 ± 2 ℃ and weigh or take off end bottle after baking 5h, its content is moved into and dried in the weighing bottle of constant weight, and bottle 3 ~ 4 times at the bottom of the organic solvent rinsing of using with a small amount of extracting, washing lotion also should be inclined in people's weighing bottle, weighing bottle is placed in water-bath, and heating is to boil off unnecessary solvent; Clean finally weighing bottle and deploy people's baking oven outward, weigh after 105 ± 2 ℃ of baking 5h; Take out content, with soaked in absolute ethyl alcohol and put into the baking oven dry for standby.
Described chemical treatment comprises 1) the peanut hull meal 10g that accurately takes extracting is placed in the 600ml beaker; 2) add 500ml distilled water, 4.5g Textone and 4ml Glacial acetic acid to mix, in the situation that temperature is 75 ℃, put into heat collecting type magnetic force heating stirrer processing 6 times, process 1h at every turn; Because reacting by heating can be emitted chlorine, so at the beaker mouth, add the sealing of one deck preservative film; 3) process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; This process is in order to remove xylogen, to obtain holocellulose; 4) the holocellulose sample is put into the 600ml beaker, take 10g potassium hydroxide, add 500ml distilled water and be made into 2% solution, in the situation that temperature is 90 ℃, put into heat collecting type magnetic force heating stirrer processing 2 times, process 2h at every turn; Process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; This process is in order to remove hemicellulose; Peanut hull meal Mierocrystalline cellulose after processing is put into after baking oven baking 48h to take out weigh; Described Textone is characterized in that: Textone has bleaching action and with lignin reaction, produces organochlorine compound under acidic conditions.
Described mechanical treatment is that the peanut hull meal Mierocrystalline cellulose after chemical treatment is made into mass concentration is 0.1% solution, being placed in shredder grinds respectively 5 times, 10 times, 20 times, 30 times, upper millstone and lower millstone close contact in process of lapping, rotating speed is 1500rpm, can obtain cellulose nano-fibrous suspension; Suspension vacuum filter membrane after a part is ground, another part carries out respectively ultrasonic, high-pressure homogeneous, centrifugal treating, then vacuum filter membrane.
Described potassium hydroxide: basic hydrolysis has saponification to the ester bond of intermolecular cross-linking xylan, hemicellulose and other components.Along with the porosity of the minimizing cellulosic material of ester bond increases, rare potassium hydroxide solution is processed raw material and can be made it to swell, and increases internal surface and reduces the polymerization degree and degree of crystallinity, the associative key between xylogen and sugar is separated, the division lignin structure.Alkaline purification is mainly to remove hemicellulose.
The acidic solution that chlorinated lignin in described chemical treatment forms when only some can be dissolved in chlorination, the chlorinated lignin of some indissoluble need to dissolve in alkali.
When carrying out chemical treatment, owing to having removed most xylogen, hemicellulose and impurity, the variation of color has occurred in solution.Solution after mechanical treatment is as clear as crystal, presents light blue.
Described mechanical treatment is in the Pericarppium arachidis hypogaeae fibre stuff, because most of base matter removes, make the interfibrous reactive force of peanut hull meal decrease than raw material, but still exist certain hydrogen bond action between fiber, many nanofibers still are wrapped in fibrous inside in bunch mode of shape aggregate.Need fiber is applied certain reactive force for this reason, nanofiber is separated realizing from the peanut hull meal fiber, adopting grinding, homogeneous, the mechanical treatment such as ultrasonic, centrifugal is method relatively more commonly used at present.
Described milled processed is to utilize between mill shearing force that close contact produces to destroy to include cellulose nano-fibrous cell wall structure, and then nanofiber is separated from the peanut hull meal fiber a kind of mechanical means.The distribution of fiber diameters that milled processed obtains is even, is interweaved between fiber and reticulates tangled structure, and have higher degree of crystallinity.
Described supersound process is worked as cellulosic fibre/water termination and is subject to hyperacoustic used time of doing, and is far from it with the cavitation in pure water liquid in cavitation at the interface.Because the asymmetry of near interface can make bubble deform, more flat near cellulosic fibre one side, produce the microjet of rapid movement while making collapse, and with the speed directive cellulosic fibre/water termination greater than 100m/s, and then make the cellulosic fibre surface localized attack occur and degrade.Little solid particulate under the ordering about of turbulent flow and shockwave, can make solids produce at a high speed and collide.The microjet shockwave that ultrasonic cavitation produces will play machinery and open fine effect, and nanofiber is separated from lignocellulose fiber.
Described high-pressure homogeneous processing is to be placed in high pressure homogenizer by the aqueous suspension with the Pericarppium arachidis hypogaeae fibre stuff, hole effect and high speed impact power by the formation of homogenizing valve rapid decompression, the Pericarppium arachidis hypogaeae Mierocrystalline cellulose is produced strong shearing action, and then diameter is opened fibre at micron-sized cellulosic fibre machinery make nano level cellulosic fibre.Homogenization treatment not only can reach cellulosic fibre machinery and open fine effect, can also fiber is dispersed in its aqueous solution.To grind for this reason or supersound process after the fiber that obtains carry out high-pressure homogeneous processing, not only cellulose fibril further can be become more meticulous, can also improve degree of scatter and the homogenization degree of nanofibrils in the aqueous solution.
Embodiment 1
(1) accurately take extracting peanut hull meal 10g later and put into the 600ml beaker, add 500ml distilled water; (2) take 4.5g Textone and measure the 4ml glacial acetic acid, in the situation that being 75 ℃, temperature puts into heat collecting type magnetic force heating stirrer processing 6 times, each 1h that processes, because reacting by heating can be emitted chlorine, so at the beaker mouth, add the sealing of one deck preservative film, process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; (3) take 10g potassium hydroxide, add 500ml distilled water and be made into 2% solution, in the situation that temperature is 90 ℃, put into heat collecting type magnetic force heating stirrer processing 2 times, each 2h that processes, process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; (4) the peanut hull meal Mierocrystalline cellulose after chemical treatment is made into 1% solution and grinds 30 vacuum filter membranes, obtain nano level cellulosic fibre.
Embodiment 2: the impact of Fig. 2 acid treatment number of times on experiment
(1) accurately take extracting peanut hull meal 10g later and put into the 600ml beaker, add 500ml distilled water; (2) take 4.5g Textone and measure the 4ml glacial acetic acid, in the situation that being 75 ℃, temperature puts into heat collecting type magnetic force heating stirrer processing 7 times, each 1h that processes, because reacting by heating can be emitted chlorine, so at the beaker mouth, add the sealing of one deck preservative film, process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; (3) take 10g potassium hydroxide, add 500ml distilled water and be made into 2% solution,, process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; (4) the peanut hull meal Mierocrystalline cellulose after chemical treatment is made into 1% solution and grinds 30 vacuum filter membranes, obtain nano level cellulosic fibre.
Embodiment 3
(1) accurately take extracting peanut hull meal 10g later and put into the 600ml beaker, add 500ml distilled water; (2) take 4.5g Textone and measure the 4ml glacial acetic acid, in the situation that being 75 ℃, temperature puts into heat collecting type magnetic force heating stirrer processing 7 times, each 1h that processes, because reacting by heating can be emitted chlorine, so at the beaker mouth, add the sealing of one deck preservative film, process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; (3) take 10g potassium hydroxide, add 500ml distilled water and be made into 2% solution, in the situation that temperature is 90 ℃, put into heat collecting type magnetic force heating stirrer processing 2 times, each 2h that processes, process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; (4) the peanut hull meal Mierocrystalline cellulose after chemical treatment is made into 1% solution and grinds 30 vacuum filter membranes, obtain nano level cellulosic fibre.
Embodiment 4
(1) accurately take extracting peanut hull meal 10g later and put into the 600ml beaker, add 500ml distilled water; (2) take 4.5g Textone and measure the 4ml glacial acetic acid, in the situation that being 75 ℃, temperature puts into heat collecting type magnetic force heating stirrer processing 7 times, each 1h that processes, because reacting by heating can be emitted chlorine, so at the beaker mouth, add the sealing of one deck preservative film, process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; (3) take 10g sodium hydroxide, add 500ml distilled water and be made into 2% solution, in the situation that temperature is 90 ℃, put into heat collecting type magnetic force heating stirrer processing 2 times, process 2h at every turn.Process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; (4) the peanut hull meal Mierocrystalline cellulose after chemical treatment is made into 1% solution and grinds 30 vacuum filter membranes, obtain nano level cellulosic fibre; (5) acid treatment number of times, tensile strength, Young's modulus through sodium-hydroxide treatment and potassium hydroxide treatment gained film are all similar, elongation at break is that sodium hydroxide is 8.3%, potassium hydroxide is 10.3%, obvious difference is arranged, this is because sodium hydroxide is highly basic, will be significantly better than potassium hydroxide to the fine ability of opening of fiber, but cross strong sodium hydroxide and can make again elongated fiber yarn fracture, affect its performance, can draw in conjunction with foregoing, potassium hydroxide treatment is better than sodium-hydroxide treatment.So selecting potassium hydroxide is final alkaline purification scheme; (6) when wavelength is 600nm, acid treatment 7 times is obviously good, same than the light transmission of 6 gained films of acid treatment, and potassium hydroxide treatment is better than the light transmission of sodium-hydroxide treatment gained film, can reach a conclusion thus, the film of acid treatment 7 times and potassium hydroxide treatment gained is better.So selecting acid treatment 7 times and potassium hydroxide treatment is final chemical treatment scheme; (7) aspect transparency, when wavelength was 600nm, acid treatment 7 times was obviously good, same than the light transmission of 6 gained films of acid treatment, and potassium hydroxide treatment is better than the light transmission of sodium-hydroxide treatment gained film.
Embodiment 5: milled processed number of times impact such as Fig. 3 on experiment
It is 0.1% solution that the sample that chemical treatment is good is made into mass concentration, is placed in shredder and grinds respectively 5 times, 10 times, 20 times, 30 times, and in process of lapping, upper millstone and lower millstone close contact, can obtain cellulose nano-fibrous suspension.
Embodiment 6
The preparation of cellulose nano-fibrous membrane: first put one deck qualitative filter paper in the Büchner funnel of 9cm, then put again an organic filter membrane of micropore, get the 500g mass concentration and be 0.1% sample and pour into wherein, open vacuum pump solution is carried out vacuum filtration, Mierocrystalline cellulose is piled up uniformly and is formed wet fiber element film.Be clipped in the middle of two organic filter membranes of micropore after wet fiber element film is taken out, dry 72h under 60 ℃ of conditions, apply the approximately pressure of 15KPa simultaneously, obtains translucent cellulose nano-fibrous film after taking-up.
Embodiment 7: Fig. 4 grinds, grinds+ultrasonic, grinds+ultrasonic+centrifugal impact on experiment
Get a part after suspension agitation after grinding is even and carry out the vacuum filtration film forming, the remaining ultrasonic 40min of a part, solution generation demixing phenomenon after standing a couple of days, get ultrasonic rear supernatant liquor vacuum filtration film forming, gets centrifugal clear liquid vacuum filtration film forming after the centrifugal 15min of throw out.
Embodiment 8: Fig. 5 grinding+ultrasonic, grinding+ultrasonic+homogeneous, grinding+ultrasonic+homogeneous+centrifugal impact on experiment
Get a part after suspension agitation after grinding is even and carry out the vacuum filtration film forming, a remaining part is ultrasonic 40min first, then homogeneous 5 times in high pressure homogenizer, get supernatant liquor and carry out the vacuum filtration film forming after standing a couple of days, gets centrifugal clear liquid vacuum filtration film forming after the centrifugal 15min of throw out.
Embodiment 9: Fig. 6 peanut hull meal FTIR figure after peanut hull meal and chemical treatment that is untreated
As can be seen from Figure 6, after chemical treatment, a series of variation has occurred in the chemical composition of peanut hull meal.Mainly comprise the absorption peak (1737cm that characterizes hemicellulose polyxylose chromophoric group C=O stretching vibration in the starting material of peanut hull meal
-1), characterize O-CH in xylogen
3Absorption peak (the 1430cm of formation vibration
-1) and the absorption peak (1640cm of phenyl ring stretching vibration
-1) and the absorption peak (3370cm that characterizes Mierocrystalline cellulose OH-stretching vibration
-1), the absorption peak (2890cm of CH-stretching vibration
-1), C-O stretching vibration absorption peak (1060cm
-1) and the absorption peak (900cm of anomeric carbon C1-H vibration
-1).After chemical treatment, characterize the absorption peak (1737cm of hemicellulose polyxylose chromophoric group C=O stretching vibration
-1) the basic disappearance, show that the hemicellulose in the peanut hull meal has effectively been removed in the alkaline purification under high temperature.Simultaneously, after acid treatment, characterize O-CH in xylogen
3Absorption peak (the 1430cm of formation vibration
-1) and phenyl ring on the absorption peak (1508cm of C=C stretching vibration
-1) be close to disappearance, show that xylogen removed by major part.And the absorption peak (3370cm of sign Mierocrystalline cellulose OH-stretching vibration
-1), the absorption peak (2890cm of CH-stretching vibration
-1), C-O stretching vibration absorption peak (1060cm
-1) and the absorption peak (900cm of anomeric carbon C1-H vibration
-1) have and manifest in whole collection of illustrative plates, show that the chemical treatment to peanut hull meal does not destroy Mierocrystalline cellulose when removing hemicellulose and xylogen; The cellulose nano-fibrous sample of gained, further homogeneous and centrifugal after, it is as clear as crystal that cellulose nano-fibrous sample becomes gradually.
Embodiment 10
With ultraviolet-visible pectrophotometer (U-4100, Hitachi, Japan), analyze the transparency of peanut hull meal cellulose nano-fibrous membrane, selecting and measuring wavelength region is 380-780nm, the optical property of the film of gained such as Figure 10: can find out, along with the increase of grinding number of times, transmittance increases gradually; Through ultrasonic and centrifugal after, transmitance also obviously improves; After high-pressure homogeneous, transmitance is further improved again; Centrifugal can be with macro nanometer fiber precipitation, further meticulous nanofiber is kept, thereby further improves the perviousness of visible light, so its visible light transmissivity is more ultrasonic compares and improve.
Above-mentioned embodiment is exemplary, is content for a better understanding of the present invention, should not be understood as limiting the scope of the invention, so long as the improvement of doing according to technical solution of the present invention all falls into protection scope of the present invention.
Claims (5)
1. utilize Pericarppium arachidis hypogaeae to prepare the method for nano-cellulose fiber optical clear mould material, it is characterized in that the method comprises pre-treatment, chemical treatment and mechanical treatment, wherein pre-treatment is to adopt the method for Benzene-ethanol extraction to extract contained resin, wax, fat and some ether insolubless in raw material, tannin and pigment out; Chemical treatment is that hemicellulose, xylogen, obtain purifying cellulose in order to remove the non-fibre composition in biomass fiber; Mechanical treatment is to utilize to grind, and ultrasonic, homogeneous, with the fiber nanometer, obtains nano level cellulosic fibre.
2. the described method of utilizing Pericarppium arachidis hypogaeae to prepare nano-cellulose fiber optical clear mould material according to claim 1, it is characterized in that described pre-treatment, it is the living peanut that will buy from the market, peel off and Pericarppium arachidis hypogaeae is cleaned with distilled water after Semen arachidis hypogaeae, put into the baking oven oven dry more than 24 hours, dry by the fire to the over dry state, Pericarppium arachidis hypogaeae is clayed into power standby with the plant pulverizer after oven dry; Utilize standard inspection sieve to filter out 50-80 purpose peanut hull meal, store for future use under room temperature.
3. the described method of utilizing Pericarppium arachidis hypogaeae to prepare nano-cellulose fiber optical clear mould material according to claim 1, it is characterized in that described pre-treatment, specifically accurately take 3 ± 0.2g, claim accurate to 0.0001g, the sample of having got ready, simultaneously separately take sample and measure moisture by GB/T2677.2, with the dehydrated alcohol of benzene and 95%, with the qualitative filter paper of the organic solvent extracting 1 ~ 2h of the part by weight mixing of 2 ︰ 1, wrap, with line, tie in order to avoid spill; Put in Soxhlet extractor, with the benzene of 200ml, the benzene alcoholic solution that the dehydrated alcohol of 100ml is mixed with 300ml makes over its overflow level, and adds 20ml, loads onto cold wink device, connects extractor, is placed in the water-bath of 85 ~ 90 ℃; Open water coolant, regulate well heater and make the boiling of benzene alcoholic solution, speed is that the per hour circulation in Soxhlet extractor is no less than 4 times, so extracting 6h; After extracting is complete, mention condenser, finding has the paper hair in extractum, should Extract be filtered in weighing bottle by filter paper, then use bottle and filter paper at the bottom of a small amount of benzene alcoholic solution gradation rinsing; Take out the paper bag that fills sample with clip from extractor, then condenser is connected with extractor again, till being evaporated at the bottom of extracting the extract in bottle and being 30ml, with this, reclaim a part of benzene alcoholic solution; Take off end bottle, clean in the baking oven of inserting 105 ± 2 ℃ and weigh or take off end bottle after baking 5h, its content is moved into and dried in the weighing bottle of constant weight, and with bottle at the bottom of the rinsing of 10 ~ 20ml benzene alcoholic solution 3 ~ 4 times, washing lotion also should be inclined in people's weighing bottle, weighing bottle is placed in water-bath, and heating is to boil off unnecessary solvent; Clean finally the weighing bottle outside and insert baking oven, weigh after 105 ± 2 ℃ of baking 5h of temperature; Take out content, with soaked in absolute ethyl alcohol and put into the baking oven oven dry more than 24 hours, dry by the fire to dry for standby in the over dry state.
4. the described method of utilizing Pericarppium arachidis hypogaeae to prepare nano-cellulose fiber optical clear mould material according to claim 1, is characterized in that described chemical treatment comprises 1) the peanut hull meal 10g that accurately takes extracting is placed in the 600ml beaker; 2) add 500ml distilled water, 4.5g Textone and 4ml Glacial acetic acid to mix, in the situation that temperature is 75 ℃, put into heat collecting type magnetic force heating stirrer processing 6 times, process 1h at every turn; Because reacting by heating can be emitted chlorine, so at the beaker mouth, add the sealing of one deck preservative film; 3) process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; This process is in order to remove xylogen, to obtain holocellulose; 4) the holocellulose sample is put into the 600ml beaker, take 10g potassium hydroxide, add 500ml distilled water and be made into 2% solution, in the situation that temperature is 90 ℃, put into heat collecting type magnetic force heating stirrer processing 2 times, process 2h at every turn; Process later and filter with Büchner funnel, and with distilled water, repeatedly clean residue, until solution is neutrality; This process is in order to remove hemicellulose; Peanut hull meal Mierocrystalline cellulose after processing is put into after baking oven baking 48h to take out weigh; Described Textone is bleaching action to be arranged and with lignin reaction, produce organochlorine compound under acidic conditions.
5. the described method of utilizing Pericarppium arachidis hypogaeae to prepare nano-cellulose fiber optical clear mould material according to claim 1, it is characterized in that described mechanical treatment, that the peanut hull meal Mierocrystalline cellulose after chemical treatment is made into mass concentration is 0.1% solution, being placed in shredder grinds respectively 5 times, 10 times, 20 times, 30 times, upper millstone and lower millstone close contact in process of lapping, rotating speed is 1500rpm, can obtain cellulose nano-fibrous suspension; Suspension vacuum filter membrane after a part is ground, another part carries out respectively ultrasonic, high-pressure homogeneous, centrifugal treating, then vacuum filter membrane.
Priority Applications (1)
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| CN103821021A (en) * | 2014-02-27 | 2014-05-28 | 中国科学院金属研究所 | Nano cellulose extracted from shuck of xanthoceras sorbifolia and extraction method |
| CN104311675A (en) * | 2014-10-08 | 2015-01-28 | 王天黎 | Method for preparing submicron or nanometer cellulose by mechanical force |
| CN104963228A (en) * | 2015-07-16 | 2015-10-07 | 吉林大学 | Method for preparing nano cellulose by utilizing sunflower seed husks |
| CN106480765A (en) * | 2016-10-19 | 2017-03-08 | 天津中智科技发展有限公司 | A kind of preparation method of Lignum seu Ramulus Cunninghamiae Lanceolatae nanofiber |
| CN106978651A (en) * | 2015-11-18 | 2017-07-25 | 大村塗料株式会社 | The manufacture method of biological nano fiber |
| CN108912230A (en) * | 2018-06-13 | 2018-11-30 | 浙江工业大学之江学院 | It is a kind of cellulose nano-fibrous and preparation method thereof |
| CN108976303A (en) * | 2018-07-05 | 2018-12-11 | 东华大学 | A kind of method that solid acid catalysis sand milling prepares cellulose nano microcrystalline |
| CN109750547A (en) * | 2019-03-07 | 2019-05-14 | 德宏州制糖工业研究所 | A method of nano-cellulose is prepared using sugaring by-product bagasse |
| CN112725917A (en) * | 2020-12-28 | 2021-04-30 | 海南华创槟榔研究院 | Preparation method of areca seed cellulose nanofibrils |
| CN113583631A (en) * | 2021-09-14 | 2021-11-02 | 山东科技大学 | Calcium alginate self-adaptive microcapsule for packaging dust suppressant, preparation method thereof and bio-based dust suppression material |
| CN113731186A (en) * | 2021-08-23 | 2021-12-03 | 广西大学 | Preparation method of metal nanoparticle/lignocellulose-based functionalized filter membrane for treating wastewater |
| CN113955323A (en) * | 2021-12-03 | 2022-01-21 | 辽宁大学 | Peanut leaf fiber/fibroin composite membrane and preparation method and application thereof |
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| CN114975848A (en) * | 2022-05-27 | 2022-08-30 | 南京林业大学 | Preparation method of flexible self-supporting anode of nanocellulose and water-based zinc ion battery |
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| CN103821021A (en) * | 2014-02-27 | 2014-05-28 | 中国科学院金属研究所 | Nano cellulose extracted from shuck of xanthoceras sorbifolia and extraction method |
| CN103821021B (en) * | 2014-02-27 | 2016-01-20 | 中国科学院金属研究所 | A kind of nano-cellulose from shinyleaf yellowhorn fruit shell extraction and extracting method thereof |
| CN104311675A (en) * | 2014-10-08 | 2015-01-28 | 王天黎 | Method for preparing submicron or nanometer cellulose by mechanical force |
| CN104963228A (en) * | 2015-07-16 | 2015-10-07 | 吉林大学 | Method for preparing nano cellulose by utilizing sunflower seed husks |
| CN106978651A (en) * | 2015-11-18 | 2017-07-25 | 大村塗料株式会社 | The manufacture method of biological nano fiber |
| CN106480765A (en) * | 2016-10-19 | 2017-03-08 | 天津中智科技发展有限公司 | A kind of preparation method of Lignum seu Ramulus Cunninghamiae Lanceolatae nanofiber |
| CN106480765B (en) * | 2016-10-19 | 2018-05-04 | 天津中智科技发展有限公司 | A kind of preparation method of China fir nanofiber |
| CN108912230A (en) * | 2018-06-13 | 2018-11-30 | 浙江工业大学之江学院 | It is a kind of cellulose nano-fibrous and preparation method thereof |
| CN108976303A (en) * | 2018-07-05 | 2018-12-11 | 东华大学 | A kind of method that solid acid catalysis sand milling prepares cellulose nano microcrystalline |
| CN109750547A (en) * | 2019-03-07 | 2019-05-14 | 德宏州制糖工业研究所 | A method of nano-cellulose is prepared using sugaring by-product bagasse |
| CN112725917A (en) * | 2020-12-28 | 2021-04-30 | 海南华创槟榔研究院 | Preparation method of areca seed cellulose nanofibrils |
| CN112725917B (en) * | 2020-12-28 | 2023-07-04 | 海南华创槟榔研究院 | Preparation method of betel nut seed cellulose nanofibrils |
| CN113580415B (en) * | 2021-08-02 | 2023-05-09 | 浙江省林业科学研究院 | Solution suspension device and method for preparing bamboo fiber glass fiber net preform |
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| CN113583631B (en) * | 2021-09-14 | 2024-03-08 | 山东科技大学 | Self-adaptive calcium alginate microcapsule for encapsulating dust suppressant, preparation method of self-adaptive calcium alginate microcapsule and bio-based dust suppressant material |
| CN113955323A (en) * | 2021-12-03 | 2022-01-21 | 辽宁大学 | Peanut leaf fiber/fibroin composite membrane and preparation method and application thereof |
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| CN114392770A (en) * | 2022-02-08 | 2022-04-26 | 浙江农林大学 | Preparation method of cellulose-based photocatalytic material with weak photocatalytic performance |
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| CN114975848A (en) * | 2022-05-27 | 2022-08-30 | 南京林业大学 | Preparation method of flexible self-supporting anode of nanocellulose and water-based zinc ion battery |
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