CN110183680A - A kind of method that the pre- place of microwave-assisted tetrahydrofurfuryl alcohol takes walnut shell to extract lignin - Google Patents

A kind of method that the pre- place of microwave-assisted tetrahydrofurfuryl alcohol takes walnut shell to extract lignin Download PDF

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Publication number
CN110183680A
CN110183680A CN201910385011.9A CN201910385011A CN110183680A CN 110183680 A CN110183680 A CN 110183680A CN 201910385011 A CN201910385011 A CN 201910385011A CN 110183680 A CN110183680 A CN 110183680A
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China
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tetrahydrofurfuryl alcohol
microwave
walnut shell
lignin
assisted
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CN201910385011.9A
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Chinese (zh)
Inventor
徐建
赵勇
徐霞
王超
汪伟
张楷
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Anhui University of Technology AHUT
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Anhui University of Technology AHUT
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07GCOMPOUNDS OF UNKNOWN CONSTITUTION
    • C07G1/00Lignin; Lignin derivatives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08HDERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00Macromolecular compounds derived from lignin, e.g. tannins, humic acids

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Compounds Of Unknown Constitution (AREA)

Abstract

The present invention provides a kind of method that the pre- place of microwave-assisted tetrahydrofurfuryl alcohol takes walnut shell to extract lignin, it is related to preprocessing substance and Comprehensive Utilization of Agricultural Wastes field, the following steps are included: by walnut shell by crushing, being sieved, washing, dry, controlling its water content is 1-15%, acidified tetrahydrofurfuryl alcohol is added, it is pre-processed under microwave condition, microwave power is 600-1000W, pretreatment time is 30-600s, filtrate is obtained after non-woven fabrics filters, filtrate is through adding water settle, be centrifuged, being lyophilized and to obtain lignin.The present invention handles walnut shell using microwave-assisted tetrahydrofurfuryl alcohol, the processing time is greatly reduced, and keep the removal effect of lignin and hemicellulose in walnut shell more obvious, the effect of acid also can make the hemicellulose split away off degrade simultaneously, to promote lignin purity, the lignin of high-purity is obtained.

Description

A kind of method that the pre- place of microwave-assisted tetrahydrofurfuryl alcohol takes walnut shell to extract lignin
Technical field
The present invention relates to biomass pretreatment and Comprehensive Utilization of Agricultural Wastes fields, and in particular to a kind of microwave is auxiliary The method for helping the pre- place of tetrahydrofurfuryl alcohol that walnut shell is taken to extract lignin.
Background technique
Biomass energy substitutes fossil resources with it as emerging renewable energy, and fossil resources reserves are limited, with Industrial expansion is increasingly depleted, and biomass resource is as the most abundant recyclable, renewable, degradable important on the earth Resource is presented in face of researcher with its unique advantage, causes the extensive interest of people.It will by biorefinery technology It is the research hotspot in a very long time from now on that biomass, which is converted into the energy, chemicals and material, and solves the mankind from now on Environment, resource and the inevitable means of energy problem.
Walnut is one of world-renowned four big dry fruits, has good nutritive value and brain-healthy effect, is known as " long-lived Fruit ".China is a walnut plantation big country, and walnut is widely distributed, and walnut shell is the waste after walnut kernel-taking, due to going out now The deep process of walnut is showed, such as walnut kernel is taken to be processed into beverage, utilize walnut kernel oil expression etc..This necessarily causes largely Walnut shell waste, currently, the utilization rate of these walnut shell wastes is extremely low, it is most of to be all dropped, also there is part to be used as agriculture Industry fuel is incinerated, and causes the significant wastage of resource, also causes great pollution to environment, there are also parts for walnut shell It is also fewer to the utilization of its higher value using being primarily used to filtrate and polishing material.The main component of walnut shell is wood Quality, cellulose and hemicellulose, although wood fiber biomass has always been considered as being that diastatic fermentation production prepares bio-fuel It is but very low in no conversion ratio by the cellulose before processing with the sustainable resource of other chemicals, it is main former Because being exactly the complexity of its structure.
Biomass pretreatment specifically includes that physics pretreatment, chemical pretreatment, Biological Pretreatment, although to a certain degree The upper extraction efficiency for increasing biomass components, but has not been reached yet ideal effect, and maximum problem is exactly that cost is too high, if It is standby to require height.
It finds that tetrahydrofurfuryl alcohol has preferable effect to the pretreatment of lignocellulosic in research before, but is still not up to Perfect condition, processing time are longer.The invention discloses a kind of microwave-assisted pre- places of tetrahydrofurfuryl alcohol, and walnut shell to be taken to extract lignin Method.It mainly is acidified tetrahydrofurfuryl alcohol using sulfuric acid cheap and easy to get, hydrochloric acid, acetic acid etc., is then reacted under microwave condition For a period of time, the effect of vibration caused by hydrone using microwave, to preferably break the friendship of lignocellulosic complexity itself It is coupled structure, destroys the chemical bond between lignin and hemicellulose, so that the lignin and hemicellulose of biomass preferably remove, And with the change of acid concentration, hemicellulose can also degrade, so that the lignin purity of preparation is higher.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of microwave-assisted pre- places of tetrahydrofurfuryl alcohol, and walnut shell to be taken to extract wood The processing time is greatly reduced in the method for quality, this method, and makes the removing effect of the lignin and hemicellulose in walnut shell Fruit is more obvious, while the effect of acid also can make the hemicellulose split away off degrade, so that lignin purity is promoted, Obtain the lignin of high-purity.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of method that the pre- place of microwave-assisted tetrahydrofurfuryl alcohol takes walnut shell to extract lignin, comprising the following steps: by walnut For shell by crushing, being sieved, washing, dry, controlling its water content is 1-15%, acidified tetrahydrofurfuryl alcohol is added, in micro-strip It is pre-processed under part, microwave power 600-1000W, pretreatment time 30-600s, filtrate is obtained after non-woven fabrics filters, Filtrate is through adding water settle, be centrifuged, being lyophilized and to obtain lignin.
Further, walnut powder and the tetrahydrofurfuryl alcohol solid-to-liquid ratio of acidification are 0.15-0.3:1 (g/ml) in step 2), pre- to locate Managing temperature is 100-200 DEG C.
Further, walnut shell powder diameter described in step 1) is -100 mesh of 10 mesh.
Further, in step 2) tetrahydrofurfuryl alcohol by biomass be raw material preparation gained.
Further, additive amount sour in tetrahydrofurfuryl alcohol in step 2) is 40-320mM/L.
Further, acid includes one or more of sulfuric acid, hydrochloric acid, acetic acid in the tetrahydrofurfuryl alcohol of step 2) acidification.
(3) beneficial effect
The present invention provides a kind of methods that microwave-assisted pre- place of tetrahydrofurfuryl alcohol takes walnut shell to extract lignin, have as follows The utility model has the advantages that
1, wood is carried out to content of lignin height, close structure, scleroid walnut shell using microwave-assisted tetrahydrofurfuryl alcohol The high-purity of quality is extracted, and under the action of microwave, the processing time reduces significantly, has saved time cost.
2, processing mode is simple and convenient, and acidizing reagent is cheap and easy to get.
3, treatment temperature is relatively low, energy saving.
4, tetrahydrofurfuryl alcohol can be that raw material is produced by biomass.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other Attached drawing.
Fig. 1 is the process flow chart that walnut shell of the present invention extracts lignin.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention, Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
Walnut shell smashes it through 2mm sieve by drying, and takes 20g as the pretreated raw material of biomass, it is aqueous to control its Amount is 5%, tetrahydrofurfuryl alcohol of the 100ml through sulfuric acid acidification (160mM/L) is added by 20% solid-to-liquid ratio, in the micro- of 800W power 50s is handled under wave, after pretreatment, non-woven fabrics is filtered, and filtrate is slowly added dropwise into 800ml water, settles, is centrifuged, dries, then Component analysis calculating is carried out to the lignin of filter residue and drying.
Through analyzing, the removal efficiency of lignin is 74.32%, and the rate of recovery of lignin is 55.12%, and the purity of lignin is 82.56%.
Embodiment 2:
Walnut shell smashes it through 2mm sieve by drying, and takes 15g as the pretreated raw material of biomass, it is aqueous to control its Amount is 8%, tetrahydrofurfuryl alcohol of the 100ml through sulfuric acid acidification (120mM/L) is added by 15% solid-to-liquid ratio, in the micro- of 1000W power 120s is handled under wave, after pretreatment, non-woven fabrics is filtered, and filtrate is slowly added dropwise into 800ml water, settles, is centrifuged, dries, so Component analysis calculating is carried out to the lignin of filter residue and drying afterwards.
Through analyzing, the removal efficiency of lignin is 75%, and the rate of recovery of lignin is 65.57%, and the purity of lignin is 87.55%.
Embodiment 3:
Walnut shell smashes it through 2mm sieve by drying, and takes 20g as the pretreated raw material of biomass, it is aqueous to control its Amount is 10%, tetrahydrofurfuryl alcohol of the 100ml through sulfuric acid acidification (160mM/L) is added by 20% solid-to-liquid ratio, in the micro- of 800W power 300s is handled under wave, after pretreatment, non-woven fabrics is filtered, and filtrate is slowly added dropwise into 800ml water, settles, is centrifuged, dries, so Component analysis calculating is carried out to the lignin of filter residue and drying afterwards.
Through analyzing, the removal efficiency of lignin is 78.58%, and the rate of recovery of lignin is 56.49%, and the purity of lignin is 83.45%.
Embodiment 4:
Walnut shell is dried by crushing smashes it through 2mm sieve, takes 15g as the pretreated raw material of biomass, controls it Water content is 12%, tetrahydrofurfuryl alcohol of the 100ml through sulfuric acid acidification (200mM/L) is added by 15% solid-to-liquid ratio, in 100W power Microwave under handle 500s, after pretreatment, non-woven fabrics is filtered, and filtrate is slowly added dropwise into 800ml water, settles, is centrifuged, dries It is dry, component analysis calculating then is carried out to the lignin of filter residue and drying.
Through analyzing, the removal efficiency of lignin is 86.58%, and the rate of recovery of lignin is 67.49%, and the purity of lignin is 84.54%.
To sum up, the embodiment of the present invention has the following beneficial effects: that 1-4 of the embodiment of the present invention utilizes microwave-assisted tetrahydrofurfuryl alcohol Walnut shell is handled, the processing time is greatly reduced, and makes the removal effect of lignin and hemicellulose in walnut shell more Obviously, while the effect of acid also can make the hemicellulose split away off degrade, to promote lignin purity, obtain high The lignin of purity.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although with reference to the foregoing embodiments Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation Technical solution documented by example is modified or equivalent replacement of some of the technical features;And these modification or Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.

Claims (6)

1. a kind of method that pre- place of microwave-assisted tetrahydrofurfuryl alcohol takes walnut shell to extract lignin, which is characterized in that including following step Rapid: by walnut shell by crushing, being sieved, washing, dry, controlling its water content is 1-15%, and acidified tetrahydrofurfuryl alcohol is added, It is pre-processed under microwave condition, microwave power 600-1000W, pretreatment time 30-600s, after non-woven fabrics filters Filtrate is obtained, filtrate is through adding water settle, be centrifuged, being lyophilized and to obtain lignin.
2. the method that the microwave-assisted pre- place of tetrahydrofurfuryl alcohol as described in claim 1 takes walnut shell to extract lignin, feature exist In walnut powder and the tetrahydrofurfuryl alcohol solid-to-liquid ratio of acidification are 0.15-0.3:1 (g/ml), pretreatment temperature 100-200 in step 2) ℃。
3. the method that the microwave-assisted pre- place of tetrahydrofurfuryl alcohol as described in claim 1 takes walnut shell to extract lignin, feature exist In walnut shell powder diameter described in step 1) is -100 mesh of 10 mesh.
4. the method that the microwave-assisted pre- place of tetrahydrofurfuryl alcohol as described in claim 1 takes walnut shell to extract lignin, feature exist In tetrahydrofurfuryl alcohol is raw material preparation gained by biomass in step 2).
5. the method that the microwave-assisted pre- place of tetrahydrofurfuryl alcohol as described in claim 1 takes walnut shell to extract lignin, feature exist In additive amount sour in tetrahydrofurfuryl alcohol is 40-320mM/L in step 2).
6. the method that the microwave-assisted pre- place of tetrahydrofurfuryl alcohol as described in claim 1 takes walnut shell to extract lignin, feature exist In acid includes one or more of sulfuric acid, hydrochloric acid, acetic acid in the tetrahydrofurfuryl alcohol of step 2) acidification.
CN201910385011.9A 2019-05-09 2019-05-09 A kind of method that the pre- place of microwave-assisted tetrahydrofurfuryl alcohol takes walnut shell to extract lignin Pending CN110183680A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111410727A (en) * 2020-05-28 2020-07-14 安徽工业大学 Synthetic method of lignin-based phenolic resin adhesive
CN112694867A (en) * 2020-12-22 2021-04-23 安徽工业大学 Method for preparing adhesive by water-settling acidified tetrahydrofurfuryl alcohol-treated biomass

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111410727A (en) * 2020-05-28 2020-07-14 安徽工业大学 Synthetic method of lignin-based phenolic resin adhesive
CN112694867A (en) * 2020-12-22 2021-04-23 安徽工业大学 Method for preparing adhesive by water-settling acidified tetrahydrofurfuryl alcohol-treated biomass

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Application publication date: 20190830