KR101690475B1 - Nanocellulose making and extracting equipment - Google Patents

Nanocellulose making and extracting equipment Download PDF

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Publication number
KR101690475B1
KR101690475B1 KR1020150116038A KR20150116038A KR101690475B1 KR 101690475 B1 KR101690475 B1 KR 101690475B1 KR 1020150116038 A KR1020150116038 A KR 1020150116038A KR 20150116038 A KR20150116038 A KR 20150116038A KR 101690475 B1 KR101690475 B1 KR 101690475B1
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South Korea
Prior art keywords
suspension
nanocellulose
unit
acid solution
filter
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KR1020150116038A
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Korean (ko)
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전준표
강필현
이진영
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한국원자력연구원
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/08—Fractionation of cellulose, e.g. separation of cellulose crystallites
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/005—Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials

Abstract

The present invention relates to a nanocellulose production and extraction apparatus, and more particularly, to a suspension preparation method for providing a suspension containing nanocellulose; A recovering unit for recovering nanocellulose using a semipermeable membrane by receiving a suspension from the suspension providing unit; And an acid solution separating part for separating the acid solution (acid solution) from the remaining water after recovering the nanocellulose by treating the suspension in the recovery part. Thus, the nanocellulose can be efficiently produced and extracted.

Figure R1020150116038

Description

[0001] NANOCELLULOSE MAKING AND EXTRACTING EQUIPMENT [0002]

The present invention relates to a nanocellulose production and extraction apparatus for producing nanocellulose from a substance containing cellulose by using an acid solution and extracting the nanocellulose by using a semipermeable membrane.

Recently, nanocellulose has attracted much attention because of its excellent mechanical strength and thermal properties and biodegradable polymer. In particular, cellulose nano-crystals (CNC), which is one of nanocelluloses, have excellent strength and linear thermal expansion coefficient of 5 times of iron and 1/10 of glass fiber due to strong hydrogen bonding. It is a natural polymer that can be used in a wide range of applications such as paper manufacturing and cosmetics.

The method of producing nanocellulose is divided into two methods: mechanical milling including homogenizer, micro-fluidizer and grinder, and chemical milling using acid and enzyme hydrolysis. As a method for producing nanocellulose, a method of hydrolyzing using concentrated sulfuric acid can be considered. Cellulose is divided into a crystalline region and an amorphous region. When the cellulose is hydrolyzed by a strong acid, the amorphous region can be selectively removed because the hydrolysis rate of the amorphous region is faster than that of the crystalline region.

However, when preparing nanocellulose by acid hydrolysis, dialysis and centrifugation can be considered for acid removal, which takes a lot of time and cost in the process, and the fine nanocellulose dispersed in the suspension is centrifuged There is a problem in that the obtained yield is remarkably reduced due to no sedimentation.

(Patent Document 1) JP2012-057077 A

Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to provide a nanocellulose manufacturing and extraction apparatus for producing nanocellulose from a substance containing cellulose by using an acid solution and extracting nanocellulose by using a semipermeable membrane It has its purpose.

According to an aspect of the present invention, there is provided a nanocellulose manufacturing and extracting apparatus including: a suspension providing a suspension containing nanocellulose; A recovering unit for recovering nanocellulose using a semipermeable membrane by receiving a suspension from the suspension providing unit; And an acid solution separator for separating the acid solution (acid solution) from the remaining water after recovering the nanocellulose by treating the suspension in the recovery part.

The apparatus for manufacturing and extracting nanocellulose according to an embodiment of the present invention has the effect of improving the yield of obtaining nanocellulose through the above-described structure.

1 is a schematic view of a nanocellulose manufacturing and extracting apparatus according to an embodiment of the present invention.
2 is a view showing a state in which a suspension is continuously filtered in a plurality of suspension filter parts according to an embodiment of the present invention.
3 is a cross-sectional view of an ion exchange unit according to an embodiment of the present invention.
4 is a view showing a connection relationship between the suspension supply part and the recovery part according to an embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings. However, the embodiments of the present invention can be modified into various other forms, and the scope of the present invention is not limited to the embodiments described below. Further, the embodiments of the present invention are provided to more fully explain the present invention to those skilled in the art. The shape and size of elements in the drawings may be exaggerated for clarity.

FIG. 1 is a schematic view of a nanocellulose manufacturing and extracting apparatus according to an embodiment of the present invention. FIG. 2 is a view showing a state in which a suspension is continuously filtered in a plurality of suspension filter units according to an embodiment of the present invention. FIG. 3 is a cross-sectional view of an ion exchange unit according to an embodiment of the present invention, and FIG. 4 is a diagram illustrating a connection relationship between a suspension providing unit and a collecting unit according to an embodiment of the present invention.

An embodiment of the present invention will be described with reference to Fig. The apparatus for preparing and extracting nanocellulose according to an embodiment of the present invention may include a suspension providing unit 100, a collecting unit 200, and an acid solution separating unit 300. The suspension providing unit 100 can produce nanocellulose by adding an acid solution (acid solution) to a substance containing cellulose. The cellulose can be divided into a crystal region and an amorphous region. Since the amorphous region is easily hydrolyzed to an acid solution as compared with a crystal region, when the acid solution is added to the cellulose, the amorphous region of the cellulose is hydrolyzed, . The nanocellulose may be distributed in an acid solution, and the acid solution in which the nanocellulose is distributed is referred to as a suspension.

The suspension supplying unit 100 may include a suspension producing unit 110 and a suspension concentration adjusting unit 120. The suspension producing unit 110 may be manufactured by adding an acid solution to a cellulosic material to manufacture a nanocellulose And the suspension concentration regulator 120 can adjust the acid concentration of the suspension by receiving the suspension from the suspension generator 110. [ The suspension generator 110 may be connected to the acid solution separator 300 and the control valve 40 to receive the acid solution. As shown in FIG. 1, the suspension generator 110 may be configured to load cellulosic material therein and to supply the acid solution from the acid solution separator 300 to produce nano-cellulose. The suspension generator 110 and the suspension concentration controller 120 may include a stirrer 20 to homogenize the suspension.

The recovery unit 200 can extract (recover) the nanocellulose using the semipermeable membrane by receiving the suspension from the suspension supplier 100. The recovery unit 200 includes a recovery unit frame 210, a suspension inflow unit 220, a suspension filter unit 230, a reverse detail unit 240, a process water discharge unit 250 and a process quantity sensor 260 can do. The suspension inlet 220 may be mounted on the recovery unit frame 210 and connected to the suspension supplier 100 by a control valve 40 to receive the suspension. The suspension filter unit 230 may be mounted on the recovery unit frame 210 to allow the suspension introduced from the suspension inlet unit 220 to pass through the semipermeable membrane to recover (extract) the nanocellulose. The remaining acid solution from which the nanocellulose has been extracted is hereinafter referred to as " treated water ".

In the suspension filter unit 230, the suspension may be permeated through the semipermeable membrane to extract the nanocellulose. The suspension filter unit 230 may be supplied with pressure from the gas compressor 10 to increase the extraction efficiency of the nanocellulose. As shown in FIG. 1, the suspension filter unit 230 may include a plurality of suspension filters 230, and gas pressure may be applied to each of the suspension filter units 230. In this case, each of the suspension filter units 230 may be connected to the gas compressor 10 through the pressure gauge 30, the regulating valve 40, and the pressure reducing valve 50 to receive the compressed gas.

When the extracted nanocellulose blocks the pores of the semipermeable membrane, the suspension can not permeate and it is necessary to scatter the nanocellulose accumulated in the semipermeable membrane. The backside detail 240 is connected to the recovery subframe 210 to form a flow of gas in a direction opposite to the direction in which the suspension is permeated through the semipermeable membrane to allow the gas to permeate the semipermeable membrane. When a gas flow occurs in a direction opposite to the direction in which the suspension is permeated into the semipermeable membrane, the nanocellulose accumulated in the semipermeable membrane may be scattered to allow the suspension to permeate the semipermeable membrane. 1, a compressed gas generated in the gas compressor 10 may be supplied to the reverse detail 240 through a regulating valve 40, a pressure reducing valve 50, and the like.

Since the suspension passing through the suspension filter unit 230 is in a state in which the nanocellulose is extracted, it is referred to as a treatment water. 1, the treated water discharging unit 250 is connected to the recovering unit frame 210 to discharge the treated water to the outside. The treatment quantity sensor 260 may be connected to the treatment water discharge unit 250 and may measure the flow rate of the treatment water passing through the treatment water discharge unit 250.

The flow rate information of the process water obtained from the process quantity sensor 260 may be used for operation of the reverse detail 240. When the nanocellulose extracted from the suspension filter unit 230 blocks the pores of the semipermeable membrane, the flow rate of the treated water may decrease, and the flow rate of the treated water is sensed by the treated water sensor 260, Lt; / RTI > Although not shown in FIG. 1, the nanocellulose manufacturing and extracting apparatus may include a controller. The controller receives flow rate information of the process water from the process quantity sensor 260, And may operate the reverse detail 240 accordingly. In order to operate the reverse detail 240, an adjustment valve 40 may be used which is connected to the reverse detail 240 as shown in FIG.

The treated water having passed through the treated water amount sensor 260 can be supplied to the acid solution separating part 300. The treated water may include an acid solution as well as a sugar and a foreign substance generated when the cellulose reacts with an acid. The acid solution separator 300 can separate the acid solution from the supplied treated water and reuse it. The acid solution separator 300 may include a treated water reservoir 310, an ion exchanger 320, and an acid solution concentrator 330.

As shown in FIG. 1, the process water reservoir 310 is connected to the process quantity sensor 260 to receive and store the process water. The ion exchanger 320 may be connected to the treated water storage tank 310 to remove sugars and foreign substances from the treated water supplied from the treated water storage tank and provide the acid solution concentrated water to the acid solution concentration unit 330 . The acid solution concentration unit 330 may be connected to the ion exchange unit 320 to increase the acid concentration of the acid solution supplied from the ion exchange unit 320. The acid solution concentrator 330 may be connected to the suspension generator 110 to supply the acid solution.

The acid solution separator 300 may include a water tank 340. The water tank 340 is connected to the acid solution concentrator 330 so that the concentration of the acid solution The water generated during the process of increasing the concentration of water can be stored. The water tank 340 may be connected to the suspension concentration controller 120 to provide water as shown in FIG.

An embodiment of the present invention will be described with reference to Fig. 2 is a view showing a state in which a suspension is continuously filtered in a plurality of the suspension filter parts 230 according to an embodiment of the present invention. The suspension filter unit 230 may include a support 231, a semipermeable membrane 232, and a filter pressure providing unit 233.

The support 231 may be attached to the recovery unit frame 210 and the semipermeable membrane 232 may be supported by the support 231 to allow the acid solution to permeate through the suspension and to filter out the nano-cellulose. For this purpose, pores may be formed in the semipermeable membrane 232.

The filter pressure providing part 233 may be connected to the recovery part frame 210 to provide pressure to the suspension treated in the semipermeable membrane 232. As shown in FIG. 1, the filter pressure providing unit 233 may be connected to the gas compressor 10 to receive gas. The filter pressure providing part 233 can supply pressure to the suspension treated in the semipermeable membrane 232 by supplying gas to the inside of the recovery part frame 210 as shown in FIG. When the filter pressure providing unit 233 is not provided, the suspension passing through the semipermeable membrane 232 is transmitted through the gravity from top to bottom. On the other hand, when the filter pressure providing unit 233 is provided, the suspension passing through the semipermeable membrane 232 can receive not only gravity but also gas pressure, thereby improving the efficiency of the process.

As shown in FIG. 2, the suspension filter unit 230 may include a plurality of suspension filter units 230 so that the pressure provided by the filter pressure providing unit 233 provided in each of the suspension filter units 230 may be formed differently. can do. 2, the suspension filter unit 230 may be continuously arranged from the suspension inlet 220 side to the treated water outlet 250, and the suspension filter unit 230 The size of the pores of the semipermeable membrane 232 provided in the suspension inlet 220 can be continuously reduced from the suspension inlet 220 to the treated water outlet 250.

The size of the pores of the semipermeable membrane 232 becomes smaller as the distance from the suspension inlet 220 is decreased so that the size of the nanocellulose filtered at the semipermeable membrane 232 becomes farther from the suspension inlet 220 Can be reduced. By arranging the suspension filter part 230 in this manner, the nanocellulose can be classified and extracted according to its size, and the efficiency of the entire process can be improved. As shown in FIG. 2, the suspension filter unit 230 located at the suspension inlet 220 has a size larger than the size of the nanocellulose that is filtered by the suspension filter unit 230, The size of the nanocellulose that is filtered at the portion 230 may be small.

The pressure provided by the filter pressure providing unit 233 provided in the suspension filter unit 230 may be different from the pressure provided by the filter pressure providing unit 233 and may be reduced as the distance from the suspension inlet 220 increases. By distributing the pressure as described above, the upper side pressure of the semipermeable membrane 232 can be made higher than the lower side pressure. When the pressure on the upper side of the semipermeable membrane 232 is higher than the pressure on the lower side, the suspension located above the semipermeable membrane 232 uses the pressure difference between the upper side and the lower side of the semipermeable membrane as well as gravity, Can be extracted.

The suspension permeated through all of the plurality of suspension filter parts 230 can be treated and then introduced into the treated water discharge part 250. The treated water passing through the treated water discharging part 250 may be provided to the treated water amount sensor 260. The flow rate of the process water sensed by the process quantity sensor 260 may be used to operate the retrograde detail 250.

Meanwhile, the functions of the reverse particulars 250 may be replaced by adjusting the filter pressure providing units 233 provided in the plurality of suspension filter units 230. When the pressure provided by the filter pressure providing unit 233 is reduced toward the suspension inlet 220 according to the flow rate information of the treated water sensed by the treatment quantity sensor 260, In this case, the nanocellulose deposited on the upper part of the semipermeable membrane 232 may be scattered by the gas flowing from the lower part of the semipermeable membrane 232 have.

An embodiment of the present invention will be described with reference to FIG. 3 is a cross-sectional view of an ion exchange unit 320 according to an embodiment of the present invention. The ion exchange unit 320 can remove sugars and foreign substances from the treated water supplied from the treated water storage tank 310. The ion exchange section includes an ion exchange section frame 321, a cation exchange resin 322 mounted on the ion exchange section frame 321, and an anion exchange resin 323 mounted on the ion exchange section frame 321 can do.

When cellulose reacts with an acid, glucose or the like is generated. Since glucose has a functional group having a negative charge and other foreign substances also have charge in the treatment water, the cation exchange resin 322 and the anion exchange resin 323) can be used to remove sugars and foreign matter. The hydrogen ions and the like included in the treated water are less influenced by the cation exchange resin 322 and the anion exchange resin 323 because the acid concentration (acid concentration) is low.

An embodiment of the present invention will be described with reference to Fig. 4 is a view showing a connection relationship between the suspension supplying unit 100 and the collecting unit 200 according to an embodiment of the present invention. The embodiment of the present invention shown in Fig. 4 is different from the embodiment of the present invention shown in Fig. 1, the pressure provided to the recovery unit 200 is supplied from the gas compressor 10 through the pressure gauge 30, the control valve 40, and the pressure reducing valve 50 .

On the other hand, in an embodiment of the present invention shown in FIG. 4, the pressure supplied to the recovery unit 200 is supplied from the suspension supply unit 100. The pressure supplied to the suspension supply unit 100 is supplied from the gas compressor 10 via the pressure gauge 30, the regulating valve 40, and the pressure reducing valve 50. When the pressure supplied to the collecting part 200 is supplied through the suspension supplying part 100 as described above, in the embodiment of the present invention shown in FIG. 1, each of the suspension filter parts of the collecting part 200 230 are not separately pressurized, the structure is simplified.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, It will be obvious to those of ordinary skill in the art.

10: gas compressor 20: stirrer
30: pressure gauge 40: regulating valve
50: Reducing valve 100: Suspension supply
110: suspension producing part 120: suspension concentration adjusting part
200: recovery unit 210: recovery unit frame
220: Suspension inlet part 230: Suspension filter part
231: Support body 232: Semi-
233: Filter pressure supply unit 240: Station detail
250: process water discharge part 260: process quantity sensor
300: acid solution separator 310: treated water storage tank
320: Ion exchange part 321: Ion exchange part frame
322: cation exchange resin 323: anion exchange resin
330: acid solution concentrating unit 340: water tank

Claims (11)

A suspension preparation providing a suspension containing nanocellulose;
A recovering unit for recovering the nanocellulose by using a semipermeable membrane provided with a suspension from the suspension providing unit; And
And an acid solution separator for separating the acid solution (acid solution) from the remaining water after recovering the nanocellulose by treating the suspension in the recovery part,
Wherein,
Recovery frame;
A suspension inflow part installed in the recovery part frame for introducing the suspension provided from the suspension supply part;
A suspension filter unit for passing the suspension introduced from the suspension inlet through the semipermeable membrane to recover the nanocellulose;
A treated water discharging portion for discharging the treated water to which the nanocellulose is removed from the suspension; And
And a flow regulator connected to the recovery subframe to form a flow of gas in a direction opposite to the direction in which the suspension is permeated to the semipermeable membrane in the suspension filter section to provide gas to the suspension filter section ; And a device for manufacturing and extracting nanocellulose.
The method according to claim 1,
The suspension providing unit includes:
And a suspension producing part for producing and providing a suspension containing nanocellulose formed from cellulose by dissolving a substance containing cellulose in an acid solution (acid solution).
3. The method of claim 2,
The suspension providing unit includes:
And a suspension concentration regulator for regulating and providing the acid concentration (acid concentration) of the suspension provided by the suspension generator.
delete The method according to claim 1,
The suspension filter unit includes:
A support mounted on the recovery part frame;
A semi-permeable membrane supported by the support and permeable to the acid solution from the suspension to filter out the nano-cellulose; And
And a filter pressure providing unit connected to the recovery unit frame for providing pressure to the suspension treated in the semipermeable membrane.
6. The method of claim 5,
A plurality of the suspension filter portions are provided,
Wherein the pressure provided by the filter pressure providing unit provided in each of the suspension filter units is differently formed.
The method according to claim 6,
Wherein the pressure provided by the filter pressure providing unit provided in each of the suspension filter units is sequentially formed in accordance with the arrangement of the respective suspension filter units.
8. The method of claim 7,
Wherein the suspension filter portion is disposed from the suspension inlet portion to the treated water outlet portion and the pore size of the semipermeable membrane provided in the suspension filter portion is smaller than that of the suspension inlet portion to the treated water outlet portion, Device.
delete The method according to claim 1,
Wherein,
And a process quantity sensor connected to the process water discharge unit and measuring a flow rate of the process water passing through the process water discharge unit.
The method according to claim 1,
Wherein the acid solution separator comprises:
A process water reservoir connected to the recovery unit to receive and store the process water;
An ion exchange unit connected to the treated water storage tank for removing sugars and foreign substances from the treated water supplied from the treated water storage tank; And
And an acid solution concentration unit connected to the ion exchange unit to increase an acid concentration of an acid solution (acid solution) that is treated and supplied in the ion exchange unit.
KR1020150116038A 2015-08-18 2015-08-18 Nanocellulose making and extracting equipment KR101690475B1 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012077697A1 (en) * 2010-12-09 2012-06-14 東レ株式会社 Method for producing concentrated aqueous sugar solution
JP2013501825A (en) * 2009-08-11 2013-01-17 エフピーイノベイションズ Fractionation of effluent streams from nanocrystalline cellulose production

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013501825A (en) * 2009-08-11 2013-01-17 エフピーイノベイションズ Fractionation of effluent streams from nanocrystalline cellulose production
WO2012077697A1 (en) * 2010-12-09 2012-06-14 東レ株式会社 Method for producing concentrated aqueous sugar solution

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