CN112250775A - Extraction equipment and extraction method for extracting hemicellulose from straws - Google Patents

Extraction equipment and extraction method for extracting hemicellulose from straws Download PDF

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CN112250775A
CN112250775A CN202011175019.1A CN202011175019A CN112250775A CN 112250775 A CN112250775 A CN 112250775A CN 202011175019 A CN202011175019 A CN 202011175019A CN 112250775 A CN112250775 A CN 112250775A
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straws
hemicellulose
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extracting
mixing reactor
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雷映霞
周青平
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Southwest Minzu University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/006Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/90Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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Abstract

The invention discloses an extraction device for extracting hemicellulose from straws, which comprises a pulverizer, a pretreatment device, a mixing reactor, an ultrasonic reaction kettle, a condensation filter, a centrifugal device and a liquid storage tank, wherein the pretreatment device is arranged on the pulverizer; the pulverizer is connected with the pretreatment device through a conveyor belt, the pretreatment device, the mixing reactor, the ultrasonic reaction kettle, the condensation filter and the centrifugal device are sequentially connected through pipelines, and the liquid storage tank and the mixing reactor are connected with the bottom end of the centrifugal device through a pipeline and connected with the mixing reactor through a pipeline; the pretreatment device is sequentially provided with a material mixing device and a plate-and-frame filter press, and the liquid storage tank stores mixed solution. The technical scheme disclosed by the invention adopts the straws as the raw materials, fully and reasonably utilizes the advantages of rich straw resources in China, provides cheap and rich raw materials for extracting hemicellulose, provides a feasible scheme for recycling waste straw resources, is an important technical support for ecological construction and development, and has excellent industrialization prospect.

Description

Extraction equipment and extraction method for extracting hemicellulose from straws
Technical Field
The invention relates to the technical field of crop waste treatment, in particular to an extraction device and an extraction method for extracting hemicellulose from straws.
Background
With the increasing severity of the problems of environmental pollution and energy shortage, the utilization of crop straws is widely concerned by researchers, crop straws are generally used as fuel at present, however, the combustion of straws not only greatly wastes the effective resources, but also pollutes the environment.
The crop straw contains rich hemicellulose, and the straw contains 36.5-38.6% of cellulose, 38.0-38.8% of hemicellulose and 12.3-17.6% of lignin.
Hemicellulose is a heteromultimer composed of several different types of monosaccharides, these sugars being five-and six-carbon sugars, including xylose, arabinose, galactose, and the like. Hemicellulose xylan, which accounts for 50% of the total amount in the woody tissue, is bound to the surface of cellulose microfibrils and is interconnected, these fibers constituting a rigid interconnected network of cells; hemicellulose has hydrophilic properties, which cause swelling of the cell wall and may impart elasticity to the fiber. The hemicellulose has wide application, is not only a main raw material in the paper making industry, but also can be used as an animal feed and a raw material for preparing membrane materials, and can also be used for producing hydrogel, ethanol, butanol, xylitol, levulinic acid and the like. Therefore, the hemicellulose has important utilization value in various fields such as industry, food additives, chemical production, medicine and health and the like.
Most of the existing methods for extracting hemicellulose from crop straws have low extraction efficiency, low hemicellulose purity and serious resource waste.
Therefore, it is an urgent technical problem to be solved by those skilled in the art to provide an extraction apparatus and an extraction method capable of extracting hemicellulose from crop straws with high efficiency and energy saving.
Disclosure of Invention
In view of the above, the present invention provides an extraction apparatus for extracting hemicellulose from straws;
in order to achieve the purpose, the invention adopts the following technical scheme:
an extraction device for extracting hemicellulose from straws comprises a pulverizer, a pretreatment device, a mixing reactor, an ultrasonic reaction kettle, a condensation filter, a centrifugal device and a liquid storage tank;
the pulverizer is connected with the pretreatment device through a conveying belt, the pretreatment device, the mixing reactor, the ultrasonic reaction kettle, the condensation filter and the centrifugal device are sequentially connected through pipelines, and the liquid storage tank is connected with the mixing reactor through a pipeline; the bottom end of the centrifugal device is connected with the mixing reactor through a pipeline;
the pretreatment device is sequentially provided with a material mixing device and a plate-and-frame filter press, and the liquid storage tank stores mixed solution.
Preferably, the ultrasonic reaction kettle is provided with a temperature sensor for controlling the reaction temperature.
The preferable beneficial effects are as follows: the temperature sensor is arranged on the ultrasonic reaction kettle, so that the temperature during ultrasonic reaction can be effectively controlled, and intermolecular motion is accelerated through the ultrasonic effect, so that the extraction rate and the purity of hemicellulose are improved.
Preferably, a stirring paddle is arranged in the mixing device; the top end of the mixing device is provided with a feeding hole, and the bottom end of the mixing device is provided with a discharging hole; the side wall of the mixing device is provided with a plurality of lenses.
More preferably, the pretreatment apparatus further comprises a degreasing tank; and a degreasing solution is contained in the degreasing tank, and the degreasing solution is n-hexane.
The preferable beneficial effects are as follows: the mixing device defined by the invention can further mix the crushed straws, so that the dissolution of hemicellulose in the straws is accelerated; the straw can be degreased in advance by additionally arranging the degreasing tank, so that the extraction purity of the hemicellulose is improved.
Preferably, the mixed solution is a mixed solution of a sodium hydroxide solution and butanol.
The preferable beneficial effects are as follows: the mixed solution can fully dissolve the hemicellulose in the plate-frame filtrate into the mixed solution, thereby effectively improving the extraction rate and the extraction purity of the hemicellulose.
The invention also provides an extraction method for extracting hemicellulose from straws, which adopts the extraction equipment for extraction and comprises the following steps:
(1) putting the straws into a crusher for crushing, and conveying the crushed straws into a pretreatment device through a conveyor belt for pretreatment to obtain straw filtrate;
(2) conveying the straw filtrate to a mixing reactor, and simultaneously adding the mixed solution into the mixing reactor for reaction to obtain a reaction solution;
(3) carrying out ultrasonic treatment on the reaction solution of the reaction solution to obtain an ultrasonic treatment solution;
(4) condensing and filtering the ultrasonic treatment liquid, centrifuging, taking supernate, adding absolute ethyl alcohol to carry out alcohol precipitation to obtain hemicellulose, returning the centrifuged residual liquid, conveying the returned liquid to the mixing reactor, and continuing to react.
Further, the straw is one or a mixture of more of wheat straw, corn straw, rice straw, sugarcane straw and cotton straw;
the pretreatment in the step (1) comprises degreasing, stirring and plate-frame filtering the crushed straws in sequence;
adopt above-mentioned further beneficial effect to lie in: according to the method disclosed by the invention, the straw is sequentially degreased, stirred and filtered by the plate frame, so that the dissolving-out degree of the hemicellulose in the crushed straw can be increased, and the extraction rate of the hemicellulose is further improved.
Further, the mixing reaction temperature in the step (2) is 40-50 ℃, and the reaction time is 10-18 h;
the mixed solution is obtained by mixing sodium hydroxide solution and butanol according to the mass ratio of 1: 0.8-1.2; the concentration of the sodium hydroxide solution is 1-2 mol/L.
Further, the ultrasonic power in the step (3) is 600-.
Further, the centrifugation rotating speed in the step (4) is 5000-.
Adopt above-mentioned further beneficial effect to lie in: according to the invention, the hemicellulose obtained after ultrasonic extraction is subjected to high-speed centrifugation, so that the cellulose and the solution can be effectively separated, and the purity of the hemicellulose obtained by subsequent alcohol precipitation is higher.
The invention has the beneficial effects that: the technical scheme disclosed by the invention adopts the straws as the raw materials, fully and reasonably utilizes the advantages of rich straw resources in China, provides cheap and rich raw materials for extracting hemicellulose, provides a feasible scheme for recycling waste straw resources, and has excellent industrialization prospect.
Drawings
FIG. 1 is a schematic view of the structure of a hemicellulose extraction apparatus according to the present invention;
FIG. 2 is a schematic structural diagram of a mixing device according to the present invention.
In the drawings, the structures represented by the reference numerals are listed below: 1-a pulverizer, 2-a pretreatment device, 3-a mixing reactor, 4-an ultrasonic reaction kettle, 5-a condensation filter, 6-a centrifugal device and 7-a liquid storage tank;
21-a degreasing tank, 22-a mixing device, 23-a plate and frame filter press and 41-a temperature sensor;
221-stirring paddle, 222-feeding hole, 223-discharging hole and 224-lens.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
Examples
An extraction device for extracting hemicellulose from straws comprises a pulverizer 1, a pretreatment device 2, a mixing reactor 3, an ultrasonic reaction kettle 4, a condensation filter 5, a centrifugal device 6 and a liquid storage tank 7;
the pulverizer 1 is connected with the pretreatment device 2 through a conveyor belt, the pretreatment device 2, the mixing reactor 3, the ultrasonic reaction kettle 4, the condensation filter 5 and the centrifugal device 6 are sequentially connected through pipelines, and the liquid storage tank 7 is connected with the mixing reactor 3 through a pipeline; the bottom end of the centrifugal device 6 is connected with the mixing reactor 3 through a pipeline;
the pretreatment device 2 is sequentially provided with a material mixing device 22 and a plate-and-frame filter press 23, and a liquid storage tank 7 stores mixed solution.
In one embodiment, the ultrasonic reaction vessel 4 is provided with a temperature sensor 41 for controlling the reaction temperature.
In one embodiment, the mixing device 22 is internally provided with a stirring paddle 221; the top end of the mixing device is provided with a feed inlet 222, and the bottom end is provided with a discharge outlet 223; the side wall of the mixing device is provided with a plurality of lenses 224.
In another embodiment, the pretreatment device 2 further comprises a degreasing tank 21; the degreasing tank 21 contains degreasing fluid which is n-hexane.
In one embodiment, the mixed solution is a mixed solution of sodium hydroxide solution and butanol.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by those skilled in the art.
Example 1
The extraction method for extracting the hemicellulose from the straws by adopting extraction equipment comprises the following steps:
(1) putting 50kg of rice straws and 50kg of sugarcane straws into a crusher for crushing, conveying the crushed straws into a pretreatment device through a conveyor belt, degreasing the crushed straws by using normal hexane, and then stirring and filtering the crushed straws by using a plate frame to obtain straw filtrate;
(2) conveying the straw filtrate to a mixing reactor for reacting for 15 hours at 48 ℃, and simultaneously adding the mixed solution into the mixing reactor for reacting to obtain a reaction solution; the mixed solution is obtained by mixing 2mol/L sodium hydroxide solution and butanol according to the mass ratio of 1: 1.1;
(3) carrying out ultrasonic treatment on the reaction solution of the reaction solution at 650W and 950 ℃ for 15min to obtain an ultrasonic treatment solution;
(4) condensing and filtering the ultrasonic treatment liquid, centrifuging for 10min at 5500r/min, taking supernate, adding absolute ethyl alcohol into the supernate to carry out alcohol precipitation to obtain hemicellulose, returning the centrifuged residual liquid to the mixing reactor, and continuously reacting.
Example 2
The extraction method for extracting the hemicellulose from the straws by adopting extraction equipment comprises the following steps:
(1) putting 100kg of wheat straws into a pulverizer for pulverizing, conveying the pulverized straws into a pretreatment device through a conveyor belt, degreasing the straws by using normal hexane, and then stirring and filtering the straws by using a plate frame to obtain a straw filtrate;
(2) conveying the straw filtrate to a mixing reactor for reacting for 18 hours at 40 ℃, and simultaneously adding the mixed solution into the mixing reactor for reacting to obtain reaction liquid; the mixed solution is obtained by mixing 2mol/L sodium hydroxide solution and butanol according to the mass ratio of 1: 0.8;
(3) carrying out ultrasonic treatment on the reaction solution of the reaction solution at 800W and 100 ℃ for 10min to obtain an ultrasonic treatment solution;
(4) condensing and filtering the ultrasonic treatment liquid, centrifuging at 7000r/min for 5min, taking supernate, adding absolute ethyl alcohol to carry out alcohol precipitation to obtain hemicellulose, returning the centrifuged residual liquid to the mixing reactor, and continuously reacting.
Example 3
The extraction method for extracting the hemicellulose from the straws by adopting extraction equipment comprises the following steps:
(1) putting 100kg of cotton straws into a crusher for crushing, conveying the crushed straws into a pretreatment device through a conveyor belt, degreasing the crushed straws by using normal hexane, and then stirring and filtering the straws by using a plate frame to obtain straw filtrate;
(2) conveying the straw filtrate to a mixing reactor for reaction for 10 hours at 50 ℃, and simultaneously adding the mixed solution into the mixing reactor for reaction to obtain reaction liquid; the mixed solution is obtained by mixing 1mol/L sodium hydroxide solution and butanol according to the mass ratio of 1: 1.2;
(3) carrying out ultrasonic treatment on the reaction solution of the reaction solution at 600W and 80 ℃ for 20min to obtain an ultrasonic treatment solution;
(4) condensing and filtering the ultrasonic treatment liquid, centrifuging for 10min at the speed of 5000r/min, taking supernate, adding absolute ethyl alcohol into the supernate to carry out alcohol precipitation to obtain hemicellulose, returning the centrifuged residual liquid to the mixing reactor, and continuously reacting.
Example 4
The extraction method for extracting the hemicellulose from the straws by adopting extraction equipment comprises the following steps:
(1) putting 100kg of rice straws into a pulverizer for pulverizing, conveying the pulverized straws into a pretreatment device through a conveyor belt, degreasing the straws by using normal hexane, and then stirring and filtering the straws by using a plate frame to obtain straw filtrate;
(2) conveying the straw filtrate to a mixing reactor for reaction for 12 hours at the temperature of 45 ℃, and simultaneously adding the mixed solution into the mixing reactor for reaction to obtain reaction liquid; the mixed solution is obtained by mixing 1.5mol/L sodium hydroxide solution and butanol according to the mass ratio of 1: 1;
(3) performing ultrasonic treatment on the reaction solution of the reaction solution at 700W and 9500 ℃ for 15min to obtain an ultrasonic treatment solution;
(4) condensing and filtering the ultrasonic treatment liquid, centrifuging at 6000r/min for 8min, taking supernate, adding absolute ethyl alcohol into the supernate to carry out alcohol precipitation to obtain hemicellulose, returning the centrifuged residual liquid to the mixing reactor, and continuously reacting.
Example 5
The extraction method for extracting the hemicellulose from the straws by adopting extraction equipment comprises the following steps:
(1) putting 100kg of corn straws into a crusher for crushing, conveying the crushed straws into a pretreatment device through a conveyor belt, degreasing the crushed straws by using normal hexane, and then stirring and filtering the straws by using a plate frame to obtain straw filtrate;
(2) conveying the straw filtrate to a mixing reactor for reacting for 16h at 42 ℃, and simultaneously adding the mixed solution into the mixing reactor for reacting to obtain a reaction solution; the mixed solution is obtained by mixing 1.8mol/L sodium hydroxide solution and butanol according to the mass ratio of 1: 0.9;
(3) carrying out ultrasonic treatment on the reaction solution of the reaction solution at 750W and 90 ℃ for 18min to obtain an ultrasonic treatment solution;
(4) condensing and filtering the ultrasonic treatment liquid, centrifuging for 10min at 6500r/min, taking supernate, adding absolute ethyl alcohol for alcohol precipitation to obtain hemicellulose, returning the centrifuged residual liquid to the mixing reactor, and continuously reacting.
Test examples
The hemicellulose yields of examples 1-5 were calculated while the purity of the hemicellulose obtained in examples 1-5 was checked, and the results are shown in table 1.
TABLE 1
Figure BDA0002748461230000091
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (10)

1. An extraction device for extracting hemicellulose from straws is characterized by comprising a pulverizer, a pretreatment device, a mixing reactor, an ultrasonic reaction kettle, a condensation filter, a centrifugal device and a liquid storage tank;
the pulverizer is connected with the pretreatment device through a conveying belt, the pretreatment device, the mixing reactor, the ultrasonic reaction kettle, the condensation filter and the centrifugal device are sequentially connected through pipelines, and the liquid storage tank is connected with the mixing reactor through a pipeline; the bottom end of the centrifugal device is connected with the mixing reactor through a pipeline;
the pretreatment device is sequentially provided with a material mixing device and a plate-and-frame filter press, and the liquid storage tank stores mixed solution.
2. The extraction equipment for extracting the hemicellulose from the straws as claimed in claim 1, wherein a temperature sensor for controlling the reaction temperature is arranged on the ultrasonic reaction kettle.
3. The extraction equipment for extracting the hemicellulose from the straws as claimed in claim 1, wherein a stirring paddle is arranged inside the mixing device; the top end of the mixing device is provided with a feeding hole, and the bottom end of the mixing device is provided with a discharging hole; the side wall of the mixing device is provided with a plurality of lenses.
4. The extraction equipment for extracting the hemicellulose from the straws as claimed in claim 1 or 3, wherein the pretreatment device further comprises a degreasing tank; and a degreasing solution is contained in the degreasing tank, and the degreasing solution is n-hexane.
5. The extraction equipment for extracting the hemicellulose from the straws as claimed in claim 1, wherein the mixed solution is a mixed solution of sodium hydroxide solution and butanol.
6. An extraction method for extracting hemicellulose from straws is characterized in that the extraction equipment of any one of claims 1-5 is adopted for extraction, and the steps are as follows:
(1) putting the straws into a crusher for crushing, and conveying the crushed straws into a pretreatment device through a conveyor belt for pretreatment to obtain straw filtrate;
(2) conveying the straw filtrate to a mixing reactor, and simultaneously adding the mixed solution into the mixing reactor for reaction to obtain a reaction solution;
(3) carrying out ultrasonic treatment on the reaction solution of the reaction solution to obtain an ultrasonic treatment solution;
(4) condensing and filtering the ultrasonic treatment liquid, centrifuging, taking supernate, adding absolute ethyl alcohol to carry out alcohol precipitation to obtain hemicellulose, returning the centrifuged residual liquid, conveying the returned liquid to the mixing reactor, and continuing to react.
7. The method for extracting hemicellulose from straws as claimed in claim 6, wherein the straws are one or more of wheat straws, corn straws, rice straws, sugar cane straws and cotton straws;
the pretreatment in the step (1) comprises degreasing, stirring and plate-frame filtering the crushed straws in sequence.
8. The method for extracting hemicellulose from straws as claimed in claim 6, wherein the mixing reaction temperature in step (2) is 40-50 ℃ and the reaction time is 10-18 h;
the mixed solution is obtained by mixing sodium hydroxide solution and butanol according to the mass ratio of 1: 0.8-1.2;
the concentration of the sodium hydroxide solution is 1-2 mol/L.
9. The method for extracting hemicellulose from straws as claimed in claim 6, wherein the ultrasonic power in step (3) is 600-800W, the ultrasonic time is 10-20min, and the ultrasonic temperature is 80-100 ℃.
10. The method as claimed in claim 6, wherein the centrifugation speed in step (4) is 5000-7000r/min, and the centrifugation time is 5-10 min.
CN202011175019.1A 2020-10-28 2020-10-28 Extraction equipment and extraction method for extracting hemicellulose from straws Pending CN112250775A (en)

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Publication number Priority date Publication date Assignee Title
CN115446069A (en) * 2022-09-20 2022-12-09 军安绿色新材料科技(广州)有限公司 Integrated preparation system for multi-component efficient separation of biomass
CN115446069B (en) * 2022-09-20 2023-06-27 军安绿色新材料科技(广州)有限公司 Integrated preparation system for efficient separation of multiple components of biomass

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Application publication date: 20210122