CN115725006A - Method for extracting hemicellulose from coffee shells by virtue of ultrasonic-microwave synergy - Google Patents
Method for extracting hemicellulose from coffee shells by virtue of ultrasonic-microwave synergy Download PDFInfo
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- CN115725006A CN115725006A CN202211502830.5A CN202211502830A CN115725006A CN 115725006 A CN115725006 A CN 115725006A CN 202211502830 A CN202211502830 A CN 202211502830A CN 115725006 A CN115725006 A CN 115725006A
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- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 75
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000605 extraction Methods 0.000 claims abstract description 21
- 230000002195 synergetic effect Effects 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000004898 kneading Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 239000003513 alkali Substances 0.000 abstract description 13
- 230000001007 puffing effect Effects 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 239000002994 raw material Substances 0.000 description 6
- 239000002028 Biomass Substances 0.000 description 5
- 239000006004 Quartz sand Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 239000010903 husk Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 210000000630 fibrocyte Anatomy 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a method for extracting hemicellulose from coffee shells by the aid of ultrasonic and microwave synergism, the coffee shells are added into deionized water and pretreated under the ultrasonic-microwave synergistic effect, the coffee shells are cleaned and dried after pretreatment is finished, the coffee shells are added into a NaOH solution, and the hemicellulose is extracted by microwave heating treatment, so that the hemicellulose extraction rate can reach 65%; the method shortens the extraction time of the hemicellulose, reduces the alkali consumption and reduces the cost.
Description
Technical Field
The invention belongs to the field of biomass refining and extraction, and relates to a method for extracting coffee shell hemicellulose by ultrasonic-microwave synergy.
Background
The planting area of the coffee in Yunnan province accounts for 98% of the national coffee planting area, the coffee shells are used as main byproducts in the coffee industry and are not utilized in a high-value mode, and except a small part of coffee shells are applied to biological adsorbents and fertilizers, most of the coffee shells are discarded as agricultural and forestry wastes, so that resources are wasted and the ecological environment is polluted. Coffee husks are mainly composed of cellulose, hemicellulose, and lignin, but research in the field of biomass refining is rare, and therefore, in order to make high-value use of coffee husks, coffee husks can be developed and used as a biomass resource. And because the structure of the hemicellulose is complex and the separation theory is deficient, the hemicellulose is easy to degrade and difficult to extract, so that the utilization and development of the hemicellulose of the coffee shells are limited, and the implementation of biomass refining is hindered.
The existing extraction method of hemicellulose has the problems of high alkali consumption, low yield and the like, and the problems are improved to a certain extent by means developed in recent years such as novel ionic solvent, supercritical extraction and the like, but the problems of large investment, high production cost and the like exist, and the method is difficult to adapt to the requirement of industrial development. Therefore, the invention is suitable for the extraction process of the hemicellulose in the coffee shells, improves the high-value utilization of the coffee shells, and has important influence on the implementation of the field of biomass refining.
Disclosure of Invention
According to the method, the coffee shells are pretreated by ultrasonic-microwave water, so that the fibrocytes of the coffee shells are swelled, the structure is loose, the pores are enlarged, the hemicellulose is extracted by adopting a microwave-alkali method under the condition of low alkali concentration, alkali liquor is easy to permeate into the coffee shells, the hemicellulose is easy to dissolve out, and the extraction rate of extracting the hemicellulose by adopting the method is high.
The technical scheme of the invention is as follows:
a method for extracting hemicellulose from coffee shells by ultrasonic-microwave synergy comprises the following specific steps:
(1) Pretreating coffee shell raw materials by using ultrasonic-microwave water: completely drying coffee shells, adding the completely dried coffee shells into deionized water with a certain solid-to-liquid ratio, uniformly kneading, standing, pretreating under the ultrasonic-microwave synergistic effect, cleaning the pretreated coffee shells and drying;
(2) Extracting hemicellulose of the coffee shell by a microwave-alkali method: and (2) adding the dried coffee shells in the step (1) into a sodium hydroxide solution, uniformly kneading and standing for 10-20min, and extracting hemicellulose from the coffee shells by using the mixture under a microwave condition.
The mass volume ratio g: mL of the oven-dried coffee shells to the deionized water is 1:4-5; standing for 1-3 hours.
The temperature of pretreatment under the synergistic action of ultrasound and microwave in the step (1) is 60-100 ℃, the microwave power is 600-1000W, and the pretreatment time is 1-3min; the ultrasonic power is 20kHz-24kHz.
In the step (2), the mass concentration of the sodium hydroxide solution is 2-3%; the mass volume ratio g: mL of the dried coffee shells to the sodium hydroxide solution is 1.
In the step (2), the microwave power is 800-1000W when the microwave heating extraction is carried out, the extraction temperature is 90-100 ℃, and the extraction time is 30-40min. The invention has the technical effects that:
(1) According to the invention, the puffing rate of the pretreated coffee shells and the hemicellulose content in the extracting solution after the hemicellulose of the coffee shells is extracted by a microwave-alkali method are measured, so that the effect of the ultrasonic-microwave water pretreatment on the extraction of the hemicellulose is determined.
(2) The method has the characteristics of short extraction time, low alkali consumption and high hemicellulose yield, and the microwave-puffing technology is environment-friendly and energy-saving and has good application prospect.
Drawings
FIG. 1 is an optical image of a coffee shell before pretreatment with ultrasonic-microwave water in example 1;
fig. 2 is an optical diagram of the coffee shells after ultrasonic-microwave water pretreatment in example 1.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the scope of the present invention is not limited thereto.
Example 1
A preparation method for extracting coffee shell hemicellulose by ultrasonic-microwave synergy comprises the following specific steps:
(1) Pretreating coffee shell raw materials by using ultrasonic-microwave water: taking 30g of absolutely dry coffee shells, adding the absolutely dry coffee shells into 120mL of ionized water, uniformly kneading and standing for 1 hour, then carrying out ultrasonic-microwave synergistic action, wherein the ultrasonic treatment power is 20kHz, the temperature is 90 ℃, the microwave power is 900W, the synergistic treatment puffing time is 3min, and cleaning and drying the pretreated coffee shells;
determining the puffing rate of the pretreated coffee shells in the step (1) by a sand setting method: a5 g sample of coffee husk (before and after pretreatment) was placed in a 500mL graduated cylinder, and 60 mesh quartz sand was gently sprinkled into the graduated cylinder until the quartz sand completely covered the sample, and the volume value (V) before and after pretreatment was recorded 1 And V 2 ) The volume of the silica sand sprinkled into the measuring cylinder can be determined by weighing the mass (m) of silica sand sprinkled into the measuring cylinder 1 And m 2 ) To calculate (the density of the quartz sand is 1.2 g/cm) 3 ) The Expansion Ratio (ER) equation is as follows:
in the formula, V 1 、V 2 -the total volume of coffee shells and quartz sand before and after pre-treatment; m is 1 、m 2 -the mass of the quartz sand sprinkled into the measuring cylinder before and after the pretreatment;
(2) Extracting hemicellulose of the coffee shell by a microwave-alkali method: adding the residual coffee shells dried in the step (1) into a sodium hydroxide solution, wherein the mass concentration of the sodium hydroxide solution is 2%, the mass volume ratio g: mL of the dried coffee shells to the sodium hydroxide solution is 1;
(3) And (3) filtering the product treated in the step (2), reserving an extracting solution, taking 2mL of the extracting solution to dilute 250 times, fixing the volume to a 500mL volumetric flask, taking 2mL of the diluent from the volumetric flask, adding 1mL of phenol solution with the mass fraction of 5% and 5mL of concentrated sulfuric acid with the mass fraction of 98%, shaking up, putting into a boiling water bath for 15min, taking out, cooling in an ice water bath for 1min, measuring the polysaccharide content in the extracting solution by using an ultraviolet spectrophotometry method, and obtaining the hemicellulose extraction rate through calculation.
Fig. 1 is an optical diagram of a coffee shell before ultrasonic-microwave water pretreatment in example 1, and fig. 2 is an optical diagram of a coffee shell after ultrasonic-microwave water pretreatment in example 1, and it can be found by comparing fig. 1 and fig. 2 that, during ultrasonic-microwave water pretreatment, water penetrating into the interior of the coffee shell is rapidly changed into water vapor, so that fibers are expanded, the fiber pores of the coffee shell are increased, the structure is loose, and cells are dispersed.
In the embodiment, the puffing rate of the pretreated coffee shells is 32%, and the extraction rate of hemicellulose is 60%.
Example 2
A preparation method for extracting coffee shell hemicellulose by ultrasonic-microwave synergy comprises the following specific steps:
(1) Pretreating coffee shell raw materials by using ultrasonic-microwave water: taking 30g of absolutely dry coffee shells, adding the absolutely dry coffee shells into 150mL of ionized water, uniformly kneading and standing for 1 hour, then carrying out ultrasonic-microwave synergistic action, wherein the ultrasonic treatment power is 22kHz, the temperature is 90 ℃, the microwave power is 900W, the synergistic treatment puffing time is 3min, and cleaning and drying the pretreated coffee shells;
determining the puffing rate of the pretreated coffee shells of step (1) according to the method of example 1;
(2) Extracting hemicellulose of the coffee shell by a microwave-alkali method: adding the residual coffee shells dried in the step (1) into a sodium hydroxide solution, wherein the mass concentration of the sodium hydroxide solution is 2%; and (2) uniformly kneading the dried coffee shells and a sodium hydroxide solution according to a mass-volume ratio g: mL of 1.
In this example, the puffing rate of the pretreated coffee shells was 44%, and the extraction rate of hemicellulose was 65%.
The BET of the coffee shells before and after the ultrasonic-microwave water pretreatment in this example is shown in table 1:
TABLE 1
Example 3
A preparation method for extracting coffee shell hemicellulose by ultrasonic-microwave synergy comprises the following specific steps:
(1) Pretreating coffee shell raw materials by using ultrasonic-microwave water: taking 30g of absolutely dry coffee shells, adding the absolutely dry coffee shells into 130mL of ionized water, uniformly kneading and standing for 1 hour, then carrying out ultrasonic-microwave synergistic action, wherein the ultrasonic treatment power is 24kHz, the temperature is 90 ℃, the microwave power is 900W, the synergistic treatment puffing time is 3min, and cleaning and drying the pretreated coffee shells;
determining the puffing rate of the pretreated coffee shells of step (1) according to the method of example 1;
(2) Extracting hemicellulose of the coffee shell by a microwave-alkali method: adding the residual coffee shells dried in the step (1) into a sodium hydroxide solution, wherein the mass concentration of the sodium hydroxide solution is 2%; the mass volume ratio g: mL of the dried coffee shells to the sodium hydroxide solution is 1.
In this example, the puffing rate of the pretreated coffee shells was 45%, and the extraction rate of hemicellulose was 64%.
Example 4
A preparation method for extracting coffee shell hemicellulose by ultrasonic-microwave synergy comprises the following specific steps:
(1) Pretreating coffee shell raw materials by using ultrasonic-microwave water: taking 30g of absolutely dry coffee shells, adding the absolutely dry coffee shells into 140mL of ionized water, uniformly kneading and standing for 3 hours, then carrying out ultrasonic-microwave synergistic action, wherein the ultrasonic treatment power is 24kHz, the temperature is 60 ℃, the microwave power is 1000W, the synergistic treatment puffing time is 1min, and cleaning and drying the pretreated coffee shells;
determining the puffing rate of the pretreated coffee shells of step (1) according to the method of example 1;
(2) Extracting hemicellulose from coffee shells by a microwave-alkali method: adding the residual coffee shells dried in the step (1) into a sodium hydroxide solution, wherein the mass concentration of the sodium hydroxide solution is 2.5%; the mass volume ratio g: mL of the dried coffee shells to the sodium hydroxide solution is 1.
In this example, the puffing rate of the pretreated coffee shells was 37%, and the yield of hemicellulose was 61%.
Example 5
A preparation method for extracting coffee shell hemicellulose by ultrasonic-microwave synergy comprises the following specific steps:
(1) Pretreating coffee shell raw materials by using ultrasonic-microwave water: taking 30g of absolutely dry coffee shells, adding the absolutely dry coffee shells into 120mL of ionized water, uniformly kneading and standing for 2 hours, then carrying out ultrasonic-microwave synergistic action, wherein the ultrasonic treatment power is 20kHz, the temperature is 100 ℃, the microwave power is 600W, the synergistic treatment puffing time is 2min, and washing and drying the pretreated coffee shells;
determining the puffing rate of the pretreated coffee shells of step (1) according to the method of example 1;
(2) Extracting hemicellulose of the coffee shell by a microwave-alkali method: adding the residual coffee shells dried in the step (1) into a sodium hydroxide solution, wherein the mass concentration of the sodium hydroxide solution is 3%, the mass volume ratio g: mL of the dried coffee shells to the sodium hydroxide solution is 1.
In this example, the puffing rate of the pretreated coffee shells was 28%, and the extraction rate of hemicellulose was 60%.
Comparative example 1
Adding a sodium hydroxide solution into absolutely dry coffee shells, wherein the mass concentration of the sodium hydroxide solution is 3%, the mass volume ratio g: mL of the coffee shells to the sodium hydroxide solution is 1.
The extraction rate of hemicellulose in this example was 40%.
It can be seen that the extraction rate of the hemicellulose in examples 1-5 is much higher than that in comparative example 1, which shows that the extraction rate of the hemicellulose can be improved by the pretreatment method in example 1.
Claims (5)
1. A method for extracting hemicellulose from coffee shells by the aid of ultrasound and microwaves is characterized by comprising the following specific steps:
(1) Adding absolutely dry coffee shells into deionized water, uniformly mixing and standing, pretreating under the synergistic action of ultrasound and microwaves, and cleaning and drying the pretreated coffee shells;
(2) And (2) adding the dried coffee shells in the step (1) into a sodium hydroxide solution, uniformly kneading and standing for 10-20min, and extracting hemicellulose from the coffee shells by microwave heating.
2. The method for extracting hemicellulose from coffee shells by the aid of the ultrasonic waves and the microwaves in a coordinated mode according to claim 1, wherein the mass-to-volume ratio g: mL of the absolutely dry coffee shells to the deionized water in the step (1) is 1:4-5; standing for 1-3 hours.
3. The method for extracting hemicellulose from coffee shells by the aid of the cooperation of ultrasound and microwaves according to claim 1, wherein the pretreatment temperature in the step (1) under the cooperation of the ultrasound and the microwaves is 60-100 ℃, the microwave power is 600-1000W, and the pretreatment time is 1-3min; the ultrasonic power is 20kHz-24kHz.
4. The method for extracting hemicellulose from coffee shells by the aid of the ultrasonic waves and the microwaves in a coordinated mode according to claim 1, wherein the mass concentration of the sodium hydroxide solution in the step (2) is 2-3%; the mass volume ratio g: mL of the dried coffee shells to the sodium hydroxide solution is 1.
5. The method for extracting hemicellulose from coffee shells by using the combination of ultrasonic waves and microwaves as claimed in claim 1, wherein the microwave power in the microwave heating extraction in the step (2) is 800-1000W, the temperature is 90-100 ℃, and the extraction time is 30-40min.
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- 2022-11-28 CN CN202211502830.5A patent/CN115725006A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2012235720A (en) * | 2011-05-11 | 2012-12-06 | Hbi Kk | Method for manufacturing reducing sugar |
| CN108456263A (en) * | 2017-12-29 | 2018-08-28 | 北京林业大学 | A kind of method of quick separating extraction hemicellulose |
| CN108729285A (en) * | 2018-05-08 | 2018-11-02 | 昆明理工大学 | A kind of method of the puffing extraction bagasse hemicellulose of microwave- |
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Non-Patent Citations (1)
| Title |
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| 王宇等: ""咖啡壳纤维素提取工艺的优化及其微观结构"", 《化工进展》, vol. 36, no. 6, pages 2262 - 2269 * |
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