KR20180100886A - Apparatus for pressure-reduced type cellulose nano conversion using ultrasonic wave - Google Patents

Abstract

The present invention relates to a decompression cellulose nano-device using an ultrasonic wave, which is capable of decomposing a washed nanocellulose raw material in a decompression chamber by using ultrasonic waves and forming an optimal vibration and temperature condition to obtain homogeneous nanocellulose at a high yield. will be.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a cellulose nano-

The present invention relates to a cellulose nano-device, and more particularly, it relates to a cellulose nano-device which decomposes a washed nanocellulose raw material in a decompression chamber by using ultrasonic waves to form an optimum vibration and temperature condition so as to obtain homogeneous nanocellulose at a high yield. To a decompression cellulose nano-device using ultrasound.

Nanotechnology (NT: nanotechnology) is a technology that obtains the desired characteristics by using specific characteristics of nano-sized particles. Recently, interest in environmentally friendly polymers has increased with active research of nanotechnology. This is an eco-friendly polymer that is a substitute for solving the environmental problems of conventional fossil fuel-based polymers. Of these natural polymers, cellulose accounts for the largest amount of organic matter on the earth.

Such cellulose is advantageous in that it can be easily supplied from natural materials and can lower the cost, and is capable of reproduction and relatively less load on nature when used.

Isolation methods for obtaining nanocellulose from cellulose can be roughly divided into chemical treatment and physical treatment. Chemical treatment methods include acid hydrolysis method of producing nano-sized cellulose by removing the amorphous region of cellulose by using strong acid. Physical methods include high intensity ultrasonic treatment, high pressure refiner treatment, grinder treatment, high pressure homogenizer treatment, In addition, the nanocellulose can be isolated using an enzyme.

The double ultrasonic treatment method is advantageous in that homogeneous nanocellulose can be obtained by applying ultrasound to horn immersed in a nanocellulose raw material to nano cellulose. However, due to the influence of ultrasonic vibration, And as the erosion part is generated, the vibration frequency changes and the performance degradation and the energy consumption are increased. In addition, as the temperature is increased due to the generation of heat due to the ultrasonic wave oscillation for a long time, the raw material may be deteriorated, and therefore, it is difficult to be limited by the use time.

Patent Registration No. 10-1550442 (Aug. 31, 2015)

SUMMARY OF THE INVENTION The present invention has been made in order to solve the above-mentioned problems, and an object of the present invention is to provide a method of manufacturing a nanocellulose, which can operate for a long time through a horn having an optimal shape for durability and amplification, To provide a decompression cellulose nano-device using ultrasound.

In order to solve the above-mentioned problems, the present invention provides a cellulose nanohardener, comprising: a first supply pipe and a first supply valve connected to a supply tank and a supply pump to supply a raw material to an upper side surface thereof; 1 tubular disassembly tank coupled with a connector; A decompression unit having a decompression unit connected to the decompression pipe and the decompression valve to decompress the inside of the decomposition tank; An amplification unit that is disposed along the inside of the decomposition tank in combination with the oscillator and is protruded so as to perform ultrasonic amplification corresponding to the frequency, And an ultrasonic horn having protrusions protruding in a conical shape corresponding to the lower side and formed with helical grooves; A circulation pipe and a circulation pump for sucking the raw material from the side of the decomposition tank and discharging and circulating the raw material through the first connection pipe into the decomposition tank and a decomposition state of the nanocellulose of the raw material passing through the circulation pipe through the optical sensor A circulation unit provided in the circulation pipe and having a heat exchange unit for cooling the circulating raw material; A storage tank connected to the first connection pipe through a first discharge valve to receive a raw material having undergone the decomposition work; A control unit for controlling the decompressor in accordance with the detection result of the first sensor unit and controlling the oscillation unit, the circulation pump, and the heat exchange unit according to a result of the detection by the second sensor unit; .

A third supply pipe connected to the distilled water tank and a third supply pipe connected to the raw water tank and the raw material pump and supplied with the raw material, And a fourth sensor unit for sensing the level of the raw material. The second sensor unit is connected to the second connection pipe and the third discharge valve, which is narrowed to the lower center and transfers the diluted and washed raw material to the supply tank, Washing tank; A stirrer comprising a rotating shaft formed vertically inside the washing tank, a plurality of stirring vanes formed on the rotating shaft, and a driving unit rotating the rotating shaft; A waste tank connected to the washing tank through a discharge pipe having a second discharge valve and a nanofilter unit; And the control unit is configured to control opening and closing of the second supply valve, the third supply valve, and the third discharge valve according to the measurement results of the third sensor unit and the fourth sensor unit.

According to the present invention, even when the ultrasonic horn is operated for a long time, it is possible to obtain optimal dispersion efficiency without causing breakage such as erosion and to obtain homogeneous nanocellulose without deterioration through cooling of the raw material and monitoring of the degree of nanoization.

1 is a sectional view showing the structure of a decomposition tank according to a preferred embodiment of the present invention,
2 is a partial cross-sectional view showing the structure of a cleaning tank according to a preferred embodiment of the present invention,
3 is a partial perspective view showing the structure of an ultrasonic horn according to a preferred embodiment of the present invention,
4 is a block diagram illustrating an electrical configuration and a connection relationship according to a preferred embodiment of the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the structure of a decompression cellulose nano-device using ultrasound according to the present invention will be described in detail with reference to the accompanying drawings.

FIG. 1 is a cross-sectional view showing a structure of a decomposition tank according to a preferred embodiment of the present invention. FIG. 1 shows a decomposition tank 110 as a treatment tank for ultrasonic dispersion of cellulose into a nanofiber apparatus.

The decomposition tank 110 includes a first supply pipe 111 connected to the supply tank 101 and the supply pump 102 and supplied with liquid nano-cellulose raw material to an upper side of the decomposition tank 110, And a first connecting pipe 113 for discharging nano-sized cellulose or for circulating the raw material are coupled to an end narrowed to the lower center. That is, the raw material of the nanocellulose stored in the supply tank 101 is introduced into the decomposition tank 110 through the supply pump 102 and the first supply pipe 111 while the first supply valve 112 is opened.

In addition, in the present invention, the cellulose raw material is dispersed through the ultrasonic waves, and at the same time, an internal decompression environment is created in order to increase the fluidity of the raw material contained in the decomposition tank 110. For this purpose, a first sensor unit 121, 124 are provided.

The first sensor unit 121 is a pressure sensor for measuring the pressure inside the decomposition tank 110. The decompressor 124 is connected to the decompression tank 110 and the decompression pipe 122, And a decompression tank 110 connected to the decomposition tank 110 through a decompression tank 123 to decompress the decomposition tank 110. The decomposition tank 110 is a vacuum pump capable of forming a vacuum inside the decomposition tank 110.

In addition, a decomposition unit 150 for dispersing and decomposing the cellulose raw material contained in the decomposition tank through ultrasonic waves is provided as a key construction of the present invention.

The decomposition unit 150 includes an oscillator 151 and an oscillator 152 for generating and outputting ultrasonic waves of a predetermined frequency and is disposed along the inner side of the decomposition tank 110 in combination with the oscillator 152, And an ultrasonic horn 154 for applying ultrasonic waves.

At this time, the oscillation unit 151 generates ultrasound having a frequency of about 20 to 28 kHz to decompose the cellulose raw material, and the frequency can be varied within a set range. The ultrasonic waves generated through the oscillating unit 151 are outputted through the vibrator 152 provided on the upper side of the decomposition tank 110. When the temperature of the vibrator rises due to the vibration due to the ultrasonic output for a long time, The cooling fan 153 can be installed at the same time.

 A cylindrical ultrasonic horn 154 spaced apart from the inner wall of the decomposition tank 110 is coupled under the vibrator 152 to uniformly apply ultrasonic waves to the inside of the raw material. At this time, the vibrator 152 and the ultrasonic horn 154 are coupled with each other through the stud bolt to securely secure the ultrasonic wave. In order to maintain the strength of the ultrasonic horn 154 due to the ultrasonic vibration, (154).

3 is a partial perspective view illustrating a structure of an ultrasonic horn according to a preferred embodiment of the present invention.

In addition, the ultrasonic horn 154 has a columnar shape having a predetermined length, and an ultrasonic wave amplification unit 155 (having a protruding shape) for amplifying ultrasonic waves corresponding to frequencies generated and transmitted as the ultrasonic waves are transmitted from the upper side to the lower side Is formed. In the accompanying drawings, one amplifying unit 155 is formed at an intermediate portion to amplify the ultrasonic wave according to the frequency of the ultrasonic wave to smoothly apply the ultrasonic wave. The amplification unit 155 can maximize the ultrasonic wave amplification The ultrasonic wave can be adjusted through the oscillation unit 151.

In the present invention, the lower end of the ultrasonic horn 154 is formed with a conical protrusion 156 corresponding to the lower side of the decomposition tank 110, and a helical groove 157 is formed in the protrusion 156 do.

The end portion of the conventional ultrasonic horn is straight, and in the present invention, the nano-scale is rapidly promoted through the contact surface enlargement through the conical V-shaped cross section, and the protrusion 156 has the same inclination angle as the bottom surface of the decomposition tank 110 The raw material circulated and discharged through the first connection pipe 113 flows along the helical groove 157 by contacting the protruding portion 156 as described below, The longer the residence time in contact with the nanoparticles can be increased. In addition, relatively large non-nanoized inclusion contents are moved downward due to the inclination of the bottom surface of the decomposition tank 110 and the protrusions 156, so that relatively large cellulose particles can be smoothly decomposed.

In addition to the configuration of the decomposing unit 150, the circulating unit 160 is provided for continuously circulating the raw material until sufficient nanotization of the raw material is achieved.

The circulation unit 160 basically sucks the raw material from the side of the decomposition tank 110 and discharges and circulates the raw material through the first connection pipe 113. A circulation pipe 161 and a circulation pump 162 are connected to the circulation pipe 160, Respectively. At this time, a part or the whole of the circulation pipe 161 is made of a transparent material so that the nano-level of the circulated raw material can be monitored, and the decomposition state of the raw material nanocellulose passing through the circulation pipe 161 is checked through an optical sensor A second sensor unit 163 is provided.

Specifically, the second sensor unit 163 includes a light emitting unit that emits light of a wavelength and a color set to the circulation pipe 161 of transparent material, and a light receiving sensor that receives light passing through the circulation pipe 161 It is possible to monitor the degree of nanoization of the cellulose material in the raw material according to the result of receiving light.

In addition, in order to prevent the temperature of the raw material from rising and deteriorating due to the temperature rise of the ultrasonic horn 154 as the raw material receives the ultrasonic wave for a long time in the decomposition tank 110, a raw material circulating in the circulating pipe 161 is set A heat exchanging portion 164 is provided for cooling to maintain the temperature range.

The heat exchanging unit 164 is connected to a temperature sensor unit installed in the decomposition tank 110 and measures the temperature of the raw material contained in the decomposition tank 110. The heat exchanging unit 164 exchanges the raw material passing through the circulation pipe 161 through a cooling means such as a water- The cooling water can be cooled.

The first connection pipe 113 is connected with the circulation pipe 161 through a first discharge valve 114 and connected to a storage tank 106 for receiving a raw material to be decomposed. That is, while the first discharge valve 114 is closed, it is circulated so that the cellulose raw material can sufficiently be nanoized. When it is confirmed that the nanoization is sufficiently performed through the second sensor unit 163, The nanoized raw material is transferred to the storage tank 106.

The process of nano-structuring the cellulose raw material through the above-described structure is as follows.

First, as the first supply valve 112 is opened and the supply pump 102 is driven, the cellulose raw material contained in the supply tank 101 is transported in a predetermined amount to the decomposition tank 110. Thereafter, the decompression valve 123 is opened and the pressure in the decomposition tank 110 is reduced until the pressure is set through the operation of the decompressor 124. The decompression tank 151 is operated to operate the decomposition tank 110 are subjected to ultrasonic decomposition of the raw materials. At this time, the raw material is continuously circulated through the circulation pump 162, the nano-level is monitored through the second sensor unit 163, and the raw material is cooled through the heat exchanging unit 164. The nanoized raw material is transferred to the storage tank 106 by opening the first discharge valve 114 as it is confirmed that the nanoization is sufficiently performed through the second sensor unit 163.

2 is a partial cross-sectional view illustrating the structure of a cleaning tank according to a preferred embodiment of the present invention.

The cleaning tank 170 serves to dilute a high concentration of salt at a low concentration in order to clean the cellulose material contained in the raw material in order to enhance the efficiency of ultrasonic decomposition, and the washed raw material is stored in the supply tank 101 .

The cleaning tank 170 is a cylindrical tank having a narrow bottom portion like the decomposition tank 110. The cleaning tank 170 is connected to the raw material tank 103 and the raw material pump 104, The second supply pipe 171 and the second supply valve 172 are connected.

The third supply pipe 173 and the third supply valve 174, which are connected to the distilled water tank 105 containing the distilled water as a means for cleaning, are supplied with distilled water according to the cleaning sequence. A third sensor unit 191 for sensing the pH of the raw material and a fourth sensor unit 192 for sensing the level of the supplied raw material.

In addition, a second connection pipe 175 and a third discharge valve 179 are connected to an end of the lower center of the washing tank 170 to transfer the diluted and washed raw material to the supply tank 101.

Inside the washing tank 170, an agitating unit 180 is installed for smooth mixing and washing of the distilled water and the raw material. The stirring unit 180 includes a rotating shaft 181 formed vertically from above the washing tank 170 and a plurality of stirring vanes 182 formed on the rotating shaft 181 and a driving unit 183 for rotating the rotating shaft 181 And the number of the stirring blades 182 formed according to the size of the washing tank 170 can be appropriately selected.

A waste liquid tank 107 connected to the lower side wall of the washing tank 170 through a discharge pipe 178 having a second discharge valve 176 and a nanofilter 177 is disposed in the lower side wall of the washing tank 170, So that the cellulosic material can be discharged in a filtered state.

The nano filter unit 177 is a filter for preventing the nanocellulose particles contained in the raw material from being discharged together with the cleaning liquid discharged through the discharge pipe 178, that is, the waste liquid. Basically, .

Various commercial filters can be applied. For example, a nano-sized filter can be manufactured by appropriately setting the diameter according to the growth of carbon nanotubes, thereby preventing leakage of cellulose particles.

The process of washing the cellulose raw material through the above-described constitution is as follows.

First, the second supply valve 172 is opened and the raw material pump 104 is driven, and the cellulose raw material contained in the raw material tank 103 is transported in a predetermined amount to the washing tank 170. Thereafter, the third supply valve 174 is opened to receive the distilled water contained in the distilled water tank 105 and to maintain the predetermined level through the fourth sensor unit 192, and then, through the agitator 180 Mix raw material and distilled water.

After the agitation for a predetermined period of time, the second discharge valve 176 is opened to discharge the waste liquid. Further, the third supply valve 174 is opened to supply distilled water and stir. After lowering the pH to 7, the third discharge valve 179 is opened to transfer the washed raw material to the supply tank 101.

FIG. 4 is a block diagram showing an electrical configuration and a connection relationship according to a preferred embodiment of the present invention, in which the aforementioned valves, namely, the first supply valve 112, the second supply valve 172, The first discharge valve 114, the second discharge valve 176, the third discharge valve 179 and the pressure reducing valve 123 are electronically operated, and at the same time, And control of the electrical configuration including the feed pump 102 and the raw material pump 104 and the circulation pump 162 is also performed together.

Specifically, in the nano-fabrication process, the controller 190 controls the decompressor 124 according to the detection result of the first sensor unit 121, and controls the decompressor 124 based on the detection result of the second sensor unit 163, The circulation pump 162, the heat exchanging unit 164, and the first discharge valve 114 are controlled.

In the cleaning process, the controller 190 controls the second supply valve 172 and the third supply valve 174 in accordance with the measurement results of the third sensor unit 191 and the fourth sensor unit 192, 3 discharge valve 179, and this series of procedures can be sequentially controlled through sequence control.

It is to be understood that the invention is not limited to the disclosed embodiment, but is capable of many modifications and variations within the scope of the appended claims. It is self-evident.

101: Feed tank 102: Feed pump
103: raw material tank 104: raw material pump
105: distilled water tank 106: storage tank
107: waste tank 110: decomposition tank
111: first supply pipe 112: first supply valve
113: first connection pipe 114: first discharge valve
120: Pressure reducing section 121: First sensor section
122: Pressure reducing pipe 123: Pressure reducing valve
124: Pressure reducer 150:
151: oscillator 152: oscillator
153: cooling fan 154: ultrasonic horn
155: amplification unit 156:
157: helical groove 160: circulation part
161: Circulation piping 162: Circulation pump
163: second sensor unit 164: heat exchanger
170: Cleaning tank 171: Second supply pipe
172: second supply valve 173: third supply pipe
174: third supply valve 175: second connection pipe
176: second discharge valve 177: nano filter part
178: discharge pipe 179: third discharge valve
180: Agitator 181:
182: stirring wing 183:
190: control unit 191: third sensor unit
192:

Claims (2)

In the cellulose nano-device,
And a first supply pipe 111 and a first supply valve 112 which are connected to the supply tank 101 and the supply pump 102 and are supplied with the raw material and are narrowed to the lower center and connected to the first connection pipe 113 A decomposition tank 110 having a cylindrical shape;
A decompression unit 124 connected to the decomposition tank 110 through a decompression pipe 122 and a decompression valve 123 for decompressing the decomposition tank 110; a first sensor unit 121 for measuring a pressure inside the decomposition tank 110; A pressure-reducing portion 120 having a pressure-receiving portion 120;
An oscillator 151 and an oscillator 152 for generating and outputting an ultrasonic wave having a predetermined frequency and an oscillator 152 for generating ultrasonic waves corresponding to the frequencies, which are positioned along the inside of the decomposition tank 110 in combination with the oscillator 152, And an ultrasonic horn 154 having a protruding portion 156 protruding in a conical shape corresponding to the lower side of the decomposition tank 110 and having a helical groove 157 formed therein, A decomposition unit 150;
A circulation pipe 161 and a circulation pump 162 for sucking the raw material from the side of the decomposition tank 110 and discharging and circulating the raw material through the first connection pipe 113 into the decomposition tank 110, A second sensor portion 163 for confirming the decomposition state of the raw material nanocellulose passing through the circulation pipe 161 and a heat exchanging portion 164 for cooling the circulating material installed in the circulation pipe 161 A circulation unit 160;
A storage tank (106) connected to the first connection pipe (113) through a first discharge valve (114) to receive a raw material subjected to the decomposition work;
And controls the decompression unit 124 according to the detection result of the first sensor unit 121 and controls the oscillation unit 151 and the circulation pump 162, A control unit 190 for controlling the control unit 164; Wherein the decompression cellulosic nano-
The method according to claim 1,
A second supply pipe 171 and a second supply valve 172 which are connected to the raw material tank 103 and the raw material pump 104 and supplied with the raw material on the upper surface thereof and a third supply pipe 172 connected to the distilled water tank 105, A third sensor part 191 for sensing the pH of the internal raw material and a fourth sensor part 192 for sensing the level of the raw material and is provided with a supply pipe 173 and a third supply valve 174, A cylindrical washing tank 170 having a second connecting pipe 175 and a third discharging valve 179 coupled to feed the diluted and washed raw material to the supply tank 101;
A rotating shaft 181 vertically formed inside the washing tank 170 and a plurality of stirring blades 182 formed on the rotating shaft 181 and a driving unit 183 rotating the rotating shaft 181 180);
A waste tank 107 connected to the washing tank 170 through a discharge pipe 178 having a second discharge valve 176 and a nanofilter portion 177; Further comprising:
The controller 190 controls the second supply valve 172 and the third supply valve 174 and the third discharge valve 179 according to the measurement results of the third sensor unit 191 and the fourth sensor unit 192, And controlling the opening and closing of the decompression cellulosic nanohardening device.

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