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 PDFInfo
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- 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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- Prior art keywords
- tetrahydrofurfuryl alcohol
- microwave
- walnut shell
- lignin
- assisted
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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
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.
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Cited By (2)
| 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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| SU672260A1 (en) * | 1977-11-09 | 1979-07-05 | Архангельский Ордена Трудового Красного Знамени Лесотехнический Институт Им. В.В.Куйбышева | Ligno-cellulose material delignification method |
| CN102644210A (en) * | 2012-04-25 | 2012-08-22 | 中国科学院过程工程研究所 | Method for pretreating biomass through microwave coupling high boiling alcohol |
| CN108316037A (en) * | 2018-03-05 | 2018-07-24 | 安徽工业大学 | A kind of method of liquid nitrogen coupling microwaves pretreatment extraction lignin from biomass |
| CN109134708A (en) * | 2018-07-25 | 2019-01-04 | 中国科学院广州能源研究所 | A kind of method of lignocellulose-like biomass component separation |
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2019
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| SU672260A1 (en) * | 1977-11-09 | 1979-07-05 | Архангельский Ордена Трудового Красного Знамени Лесотехнический Институт Им. В.В.Куйбышева | Ligno-cellulose material delignification method |
| CN102644210A (en) * | 2012-04-25 | 2012-08-22 | 中国科学院过程工程研究所 | Method for pretreating biomass through microwave coupling high boiling alcohol |
| CN108316037A (en) * | 2018-03-05 | 2018-07-24 | 安徽工业大学 | A kind of method of liquid nitrogen coupling microwaves pretreatment extraction lignin from biomass |
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Cited By (2)
| 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 |