CN103031356B - Method for applying peanut shells to synchronously prepare nanocellulose crystal and sugar - Google Patents

Method for applying peanut shells to synchronously prepare nanocellulose crystal and sugar Download PDF

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CN103031356B
CN103031356B CN201210552239.0A CN201210552239A CN103031356B CN 103031356 B CN103031356 B CN 103031356B CN 201210552239 A CN201210552239 A CN 201210552239A CN 103031356 B CN103031356 B CN 103031356B
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solution
arachidis hypogaeae
pericarppium arachidis
cellulose
sugar
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CN103031356A (en
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孙庆杰
熊柳
吴旻
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Qingdao Agricultural University
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Qingdao Agricultural University
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Abstract

The invention discloses a method for applying peanut shells to synchronously prepare nanocellulose crystal and sugar. The method uses the peanut shells as a raw material to extract cellulose, adopts an enzymatic hydrolysis method to prepare the nanocellulose crystal, controls the enzymolysis degree and obtains sugar liquor at the same time, belonging to the technical field of nanostructure materials. The nanocellulose crystal preparation method does not adopt an inorganic acid hydrolysis method generating a lot of waste acid and impurities but adopts the cellulose enzymatic hydrolysis method with mild process conditions and strong specificity, being green and environmentally-friendly and conforming to the national strategy of sustainable development requirements. The method uses the peanut shells as the raw material to replace high-cost raw materials such as cotton, chemical pulp or microcrystalline cellulose and the like, so that the comprehensive utilization value of the peanut shells is increase, the current situations of waste of resources and economic losses as most of the agricultural and sideline products are used as wastes or fuels are changed, and the economic and social benefits are brought while the environment is improved. A lot of sugar liquor is produced during preparation, and the purpose of making the most of things is achieved.

Description

A kind ofly apply the method for Pericarppium arachidis hypogaeae interlock system for nano cellulose crystal and sugar
Technical field
The present invention relates to the method for a kind of interlock system for nano cellulose crystal and sugar, particularly a kind of Pericarppium arachidis hypogaeae of applying prepares as prepared using enzyme hydrolysis method the method that nano cellulose crystal produces sugar simultaneously.
Background technology
China's peanut yield accounts for about 1/3 of Gross World Product, and the Pericarppium arachidis hypogaeae that only peanut produces in the course of processing is about 4,500,000 tons every year.The main component of Pericarppium arachidis hypogaeae comprises 65.7%-79.3% crude fibre and 10.6%-21.2% carbohydrate, 4%-7% protein, 1.9%-4.6% ash content, 1%-2% crude fat, 0.7% starch etc.In addition, also some medicinal ingredientss such as carotene, saponin, β-sitosterol are contained in Pericarppium arachidis hypogaeae.Pericarppium arachidis hypogaeae can extract some important industrial chemicals such as glucose, furfural, ethyl formate after suitably processing.Current Pericarppium arachidis hypogaeae, except on a small quantity for being processed into feed and for except industrial chemicals, major part is treated as waste or fuel, causing the great wasting of resources and huge financial loss, also result in comparatively serious environmental pollution simultaneously.Pericarppium arachidis hypogaeae can obtain Mierocrystalline cellulose through irenine oxidative treatment, in this, as raw material prepared by nano cellulose crystal, and also can environmental protect while bringing economic benefit and social benefit.
Mierocrystalline cellulose is that occurring in nature is the abundantest and have the natural macromolecular material of biodegradability, with β-1 by D-Glucopyranose, the linear long chain macromolecule polymkeric substance that 4 glycosidic links are formed by connecting with chair conformation, wherein two glucose form a cellobiose monomer, two ends form long-chain with other glucose molecules again, one, chain two ends are reducing ends, and another is non-reducing end.Face that resource consumes fast in the world today, under the situation of environmental degradation, put forth effort on the reproducible cellulose resource of exploitation and there is important strategic importance.But Mierocrystalline cellulose is as a kind of natural high moleculer eompound, it also exists many shortcomings in performance, and as limited strength, not resistance to chemical attack etc., and its physical aspect also limit its range of application.If but be prepared into nano material, just can optimize its performance to a certain extent, make Mierocrystalline cellulose have more wide application prospect.Nano cellulose crystal be a kind of bar-shaped, size generally between 30-100nm, can disperse to be formed the cellulose crystals of stable suspension in water.It not only has cellulosic basic structure and performance, also there is the characteristic of nano particle, as huge specific surface area, higher Young's modulus, superpower adsorptive power and high reactive behavior, the character of its character and general fibre element is therefore caused to have very big-difference.
At present, the conventional preparation method of nano cellulose crystal is mineral acid hydrolysis method, and this method can produce a large amount of spent acid and impurity, and consumes a large amount of water and power resource.And adopt cellulase hydrolysis method, not only processing condition are gentle, specificity is strong, and environmental protection, meet the requirement of National Sustainable Development Strategies.Present stage nano cellulose crystal raw materials mainly cotton, chemical pulp or Microcrystalline Cellulose, raw materials cost used is higher, and adopt Pericarppium arachidis hypogaeae preparing nano cellulose crystals can improve the comprehensive utilization value of agricultural byproducts very well, preparation also can produce a large amount of liquid glucoses simultaneously, can reach the object of making the best use of everything.
Summary of the invention
The object of the invention is to provide a kind of and apply the method for Pericarppium arachidis hypogaeae interlock system for nano cellulose crystal and sugar.
The technical solution used in the present invention is:
Apply the method for Pericarppium arachidis hypogaeae interlock system for nano cellulose crystal and sugar, described method comprises the steps:
(1) get the Pericarppium arachidis hypogaeae of certain mass, with washed with de-ionized water, remove wherein after impurity, naturally dry;
(2) agricultural byproducts after drying adopt pulverizer to pulverize, and seal and save backup after crossing 80 mesh sieves;
(3) take the Powdered Pericarppium arachidis hypogaeae pressed powder of certain mass, add the H of 4% by solid-to-liquid ratio 1:15 2o 2solution and 8% NaOH solution (V h2O2: V naOHfor 5:1), heated and stirred process 2.0h in 40 DEG C of water-baths, cooling;
(4) cold go after suspension liquid in the centrifugal 20min of 3000r/min, abandoning supernatant, dries in the loft drier after washing of precipitate to neutrality at 105 DEG C, pulverize, cross 100 mesh sieves, sealing preserve;
(5) by Pericarppium arachidis hypogaeae cellulose solution ultrasonic frequency be 40 kHz, power be 250 W under in 45 ° of C ultrasonication 3h;
(6) by this Pericarppium arachidis hypogaeae cellulose solution and the mixing of 30ml acetic acid-sodium acetate buffer solution after, and mix with the ratio of 1:6 with cellulase solution, be placed in constant temperature oscillation case enzymolysis, hydrolysis temperature is 45 ° of C, and enzymolysis time is 3 days;
(7) reaction terminates rear taking-up Pericarppium arachidis hypogaeae nano cellulose crystal mixed solution, and filtering separation removing cellulase, lyophilize obtains Pericarppium arachidis hypogaeae nano cellulose crystal, is sugar soln in remaining liq.
The invention has the advantages that the mineral acid hydrolysis method of the spent acid that the non-selected generation of the preparation method of nano cellulose crystal is a large amount of and impurity, and have employed processing condition gentleness, cellulase hydrolysis method that specificity is strong, not only environmental protection, also meets the requirement of National Sustainable Development Strategies.And select Pericarppium arachidis hypogaeae in agricultural byproducts as raw materials, instead of the starting material such as the cotton of high cost, chemical pulp or Microcrystalline Cellulose, the comprehensive utilization value of Pericarppium arachidis hypogaeae can be improved very well, most of agricultural byproducts can be changed and be treated as waste or fuel and the present situation that causes the very big wasting of resources and tremendous economic loss, while bringing economic benefit and social benefit, can be good at environmental protect.Preparation also can produce a large amount of liquid glucoses simultaneously, reaches the object of making the best use of everything.
Embodiment
Be below several specific embodiment of the present invention, further illustrate the present invention, but protection scope of the present invention be not limited only to this.
Embodiment 1
Take the Powdered Pericarppium arachidis hypogaeae pressed powder of 24g, add the H of 4% by solid-to-liquid ratio 1:15 2o 2the NaOH solution 60ml(V of solution 300ml and 8% h2O2: V naOHfor 5:1), heated and stirred process 2.0h in 40 DEG C of water-baths, cooling.Cold go after suspension liquid in the centrifugal 20min of 3000r/min, abandoning supernatant, dries in the loft drier after washing of precipitate to neutrality at 105 DEG C, pulverize, cross 100 mesh sieves, sealing preserve.The 8g Pericarppium arachidis hypogaeae cellulose powder that extracts is dissolved, ultrasonic frequency be 40 kHz, power be 250 W under in 45 ° of C ultrasonication 3h.After by this Pericarppium arachidis hypogaeae cellulose solution and the mixing of 30ml acetic acid-sodium acetate buffer solution, and mix with the ratio of 1:6 with cellulase solution, be placed in constant temperature oscillation case enzymolysis, hydrolysis temperature is 45 ° of C, and enzymolysis time is 3 days.Reaction terminates rear taking-up Pericarppium arachidis hypogaeae nano cellulose crystal mixed solution, and filtering separation removing cellulase, lyophilize obtains Pericarppium arachidis hypogaeae nano cellulose crystal, is sugar soln in remaining liq.
Embodiment 2
Take the Powdered Pericarppium arachidis hypogaeae pressed powder of 48g, add the H of 4% by solid-to-liquid ratio 1:15 2o 2the NaOH solution 60ml(V of solution 300ml and 8% h2O2: V naOHfor 5:1), heated and stirred process 2.0h in 40 DEG C of water-baths, cooling.Cold go after suspension liquid in the centrifugal 20min of 3000r/min, abandoning supernatant, dries in the loft drier after washing of precipitate to neutrality at 105 DEG C, pulverize, cross 100 mesh sieves, sealing preserve.The 16g Pericarppium arachidis hypogaeae cellulose powder that extracts is dissolved, ultrasonic frequency be 40 kHz, power be 250 W under in 45 ° of C ultrasonication 3h.After by this Pericarppium arachidis hypogaeae cellulose solution and the mixing of 30ml acetic acid-sodium acetate buffer solution, and mix with the ratio of 1:6 with cellulase solution, be placed in constant temperature oscillation case enzymolysis, hydrolysis temperature is 45 ° of C, and enzymolysis time is 3 days.Reaction terminates rear taking-up Pericarppium arachidis hypogaeae nano cellulose crystal mixed solution, and filtering separation removing cellulase, lyophilize obtains Pericarppium arachidis hypogaeae nano cellulose crystal, is sugar soln in remaining liq.
Embodiment 3
Take the Powdered Pericarppium arachidis hypogaeae pressed powder of 96g, add the H of 4% by solid-to-liquid ratio 1:15 2o 2the NaOH solution 60ml(V of solution 300ml and 8% h2O2: V naOHfor 5:1), heated and stirred process 2.0h in 40 ° of C water-baths, cooling.Cold go after suspension liquid in the centrifugal 20min of 3000r/min, abandoning supernatant, dries in the loft drier after washing of precipitate to neutrality at 105 DEG C, pulverize, cross 100 mesh sieves, sealing preserve.The 32g Pericarppium arachidis hypogaeae cellulose powder that extracts is dissolved, ultrasonic frequency be 40 kHz, power be 250 W under in 45 ° of C ultrasonication 3h.After by this Pericarppium arachidis hypogaeae cellulose solution and the mixing of 30ml acetic acid-sodium acetate buffer solution, and mix with the ratio of 1:6 with cellulase solution, be placed in constant temperature oscillation case enzymolysis, hydrolysis temperature is 45 ° of C, and enzymolysis time is 3 days.Reaction terminates rear taking-up Pericarppium arachidis hypogaeae nano cellulose crystal mixed solution, and filtering separation removing cellulase, lyophilize obtains Pericarppium arachidis hypogaeae nano cellulose crystal, is sugar soln in remaining liq.

Claims (1)

1. apply the method for Pericarppium arachidis hypogaeae interlock system for nano cellulose crystal and sugar, it is characterized in that, described method comprises the steps: that (1) is by the process of Pericarppium arachidis hypogaeae raw material pulverizing, obtains Powdered Pericarppium arachidis hypogaeae solid particulate; (2) adopt irenine oxidation style, pass through H 2o 2solution and NaOH solution combination treatment, extract Mierocrystalline cellulose from agricultural byproducts powder, and Powdered Pericarppium arachidis hypogaeae solid particulate and treatment solution ratio are 1:15, H 2o 2strength of solution is 4%, and NaOH solution concentration is 8%, V h2O2: V naOHfor 5:1; Water bath heating temperature is 40 DEG C, and the stir process time is 2.0h; Centrifugal rotational speed is 3000r/min, and centrifugation time is 20min, and washing of precipitate is 105 DEG C to neutral rear drying temperature, crosses 100 mesh sieves after pulverizing; (3) adopt ultrasonic pretreatment, ultrasonic frequency is 40kHz, and power is 250W, and treatment temp is 45 DEG C, and the treatment time is 3h, makes Pericarppium arachidis hypogaeae Mierocrystalline cellulose disperse under ul-trasonic irradiation; After Pericarppium arachidis hypogaeae cellulose solution mixed with damping fluid and cellulase solution put in incubator and cultivates obtained nano cellulose crystal, more after filtration and lyophilize obtain Powdered nano cellulose crystal and liquid glucose; Pericarppium arachidis hypogaeae cellulose solution and the mixing of 30ml acetic acid-sodium acetate buffer solution, and mix with the ratio of 1:6 with cellulase solution; Mixed solution is placed in constant temperature oscillation case enzymolysis, hydrolysis temperature is 45 DEG C, and enzymolysis time is 3 days; Reaction terminates rear taking-up Pericarppium arachidis hypogaeae nano cellulose crystal mixed solution, and filtering separation removing cellulase, lyophilize obtains Pericarppium arachidis hypogaeae nano cellulose crystal, is liquid glucose in remaining liq.
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CN103387689A (en) * 2013-08-19 2013-11-13 南京林业大学 Method for preparing nanocellulose fiber optical transparent membrane material from peanut hulls
CN104073533A (en) * 2014-06-19 2014-10-01 中国科学院广州能源研究所 Method for preprocessing biomass through thermal hydrolysis with low energy consumption and device thereof
GB2534338B (en) * 2014-10-08 2021-10-20 Univ Brunel Method of producing nanocellulose
CN104711305A (en) * 2015-03-25 2015-06-17 洪思仪 Method for preparing cellulose nanocrystals through enzyme hydrolysis of bacterial celluloses
CN105603020B (en) * 2016-01-21 2019-05-10 青岛农业大学 A kind of preparation method of nano cellulose crystal
CN106351050B (en) * 2016-08-31 2018-08-24 扬州大学 A kind of method that alkaline process combines ultrasound extraction Cellulose nanocrystal body from grass fiber
CN108410923B (en) * 2018-02-07 2021-07-23 兰州理工大学 Method for preparing microcrystalline cellulose from sorghum straws
CN108589372B (en) * 2018-04-17 2020-12-22 华南理工大学 Spherical nano-cellulose and preparation method thereof
CN108755215B (en) * 2018-05-05 2021-05-18 黎明职业大学 Method for preparing nano cellulose whiskers by using peanut shells
CN109338781A (en) * 2018-10-12 2019-02-15 山东金胜粮油集团有限公司 A kind of steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose
CN109024031A (en) * 2018-10-12 2018-12-18 山东金胜粮油集团有限公司 The method that steam blasting combination ultrasonic treatment prepares peanut shell nano-cellulose
CN111499768B (en) * 2020-03-02 2022-03-01 中科如米(北京)生态农业科技发展有限公司 Preparation method of zwitterionic xylose residue cellulose nanocrystalline
CN112358658A (en) * 2020-11-20 2021-02-12 山东兴泉油脂有限公司 Biodegradable master batch based on peanut shell fibers and preparation method and application thereof
CN113388651B (en) * 2021-06-24 2023-02-03 湖南省天宏药业有限公司 Preparation method of polygonatum odoratum fiber nanocrystal

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CN102061322B (en) * 2010-11-12 2013-10-09 盐城工学院 Method for preparing polysaccharide, flavone and dietary fiber of peanut hulls in united manner

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