JPS6072740A - Dye refining apparatus - Google Patents

Abstract

PURPOSE:To form a dye refining apparatus which can make a dye solution ideal for the preparation of an ink to be used in inkjet recording and writing tools by removing inorganic salts contained in a dye liquid by executing chromatography and membrane separation. CONSTITUTION:A producing section 1 makes a dye aqueous solution. The refining section 100 provided to remove inorganic salts in the dye aqueous solution has a first refining section 100A for executing chromatography and a second refining section 100B for executing membrane separation. The chromatography and membrane separation are executed in combination to eliminate inorganic salts contained in the dye solution. This enables the formation of a dye solution ideal for the preparation of an ink to be used in inkjet recording and writing tools.

Description

DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to a dye purification device, and particularly to a device for continuously supplying purified dye suitable for preparing a recording liquid (generally referred to as ink) suitable for inkjet recording, 10 marking tools, etc. This invention relates to dye purification equipment.

[Prior Art] Conventionally, ink used in the inkjet recording method, in which recording is performed by ejecting ink in a recording head from an ejection orifice using vibrations such as a Pietz oscillator, has been made by mixing various dyes and pigments with water or other organic solvents. It is known to be dissolved or dispersed in a liquid medium consisting of: It is also known that similar inks are used in writing instruments such as felt pens and fountain pens.

An example of a general basic composition of such an ink is one in which the main components are a water-soluble dye, water as its solvent, and glycols as a drying prevention agent.

Here, water-soluble dyes usually contain inorganic salts such as I.lium chloride and sodium iirate.

When recording ink is prepared using dyes containing such inorganic salts, the following disadvantages occur. That is,
A large amount of inorganic salts reduces the stability of dye dissolution in the ink, leading to aggregation and precipitation of the dye. Furthermore, in inkjet recording heads and writing implements, when the ink evaporates near the ejection orifice and the liquid composition changes, the inorganic salts themselves precipitate. All of these causes the discharge orifice to become clogged, which is the most objectionable cause.

Therefore, in order to eliminate such adverse effects, it is necessary to control the concentration of inorganic salts in the ink to fall within a predetermined range during ink production. This is essential when a commercially available dye containing a large amount of inorganic salts as an impurity is used for preparing an inkjet recording ink or a writing instrument ink.

[Purpose] The purpose of the present invention is to remove inorganic salts contained in a dye solution by carrying out the chromatography method and the Kinbunbatake [1 method], and to remove the inorganic salts contained in the dye solution, thereby making it possible to use it for inkjet recording and writing instruments. An object of the present invention is to provide a dye purification apparatus for producing a dye solution suitable for preparing ink to be used.

[Example] The present invention will be described in detail below with reference to the drawings.

11A shows the overall configuration of an embodiment of the device of the present invention.

Here, l is a production department that produces an aqueous dye solution. 10
0 is a purification section that removes inorganic salts contained in the dye aqueous solution, and a first purification section 10 that executes a chromatography method.
0A and the second purification section 100B that performs the membrane separation method are destroyed. Reference numeral 300 denotes a control section, which controls the nine operations of each section described above.

FIG. 2 shows the structure of the dye solution manufacturing section 1 shown in FIG.

Here, 3 is a dye supply section that stores dye powder 5,
The dye powder 5 is supplied to a mixing tank 9 via a dye valve 7. Further, pure water is supplied to the mixing tank 9 through a pure ice supply pipe 13 into which a pure water 7/herb 11 is inserted.

In this mixing tank 8, the supplied dye powder 5 and pure water are mixed and dissolved by a mixing tank agitator 15 to prepare an aqueous dye solution. The amount of liquid in the aqueous dye solution stored in the mixing tank θ is detected by mixing tank liquid section detection: A]7. The aqueous dye solution obtained in the mixing tank contains particles of dye powder that were not dissolved in the pure water, and these are removed by the filter 19. For this filter 18, ordinary filter paper, Fluorobor (trade name), or the like can be used. The aqueous dye solution from which particles and the like have been removed by passing through the filter 19 is supplied to the supply tank 21 .

The aqueous dye solution supplied to the supply tank 21 is supplied to the purification section 100, which will be described next, via the supply pipe 23. Here, this supply tank 21 is provided with a valve 25 for controlling the liquid level,
To suppress the amount of dye aqueous solution stored in the supply tank to a certain amount or less.

FIG. 3 shows a first purification section 100A in which inorganic salts are removed from the aqueous dye solution in the purification section 100 of FIG. 1 by chromatography. As shown in the figure, the purification section 100A includes a plurality of salt reduction processing units) IIN (101-1 to It
)IN). In the salt reduction processing unit 101, +03 (103-1 to +03-N) is a supply valve opening/closing part, +05 (105-1 to 105-N) is a salt reduction filter part and 107 (107-1 to +07-N).
) is the discharge valve opening/closing part.

The supply valve opening/closing section 103 includes a dye aqueous solution supply pipe 109.
(109-1 to 10!3-N), pure water supply pipe 111 (
+11-1 to 111-N) and secondary solution supply pipe +13
(113-1 to 1 l3-N) are communicated with each other.

The aqueous dye solution is supplied from the supply tank 21 to the opening/closing section 103 through the supply pipe 23 and In in sequence, and the pure water is supplied to the opening/closing section 103 through the supply pipe 1
3 and 111 in sequence. Further, a secondary solution, which will be described later, is supplied from the secondary solution storage tank 115 to the supply valve opening/closing section 103 via the supply pipe 117 and +13 in sequence.

The supply valve opening/closing section 103 controls whether or not the supplied aqueous dye solution, pure water, and secondary solution are supplied to the salt reduction filter section +05.

The salt-reducing filter section 105 uses chromatography to remove inorganic tJi from the aqueous dye solution and secondary solution supplied from the supply valve opening/closing section 103.

By controlling the discharge valve opening/closing unit 107, the aqueous dye solution whose inorganic salt concentration has become less than a predetermined value (for example, 5% by weight relative to the dye) due to such purification is discharged at a point θ(1
19-1 to +l9-N) to the storage tank 12+. In addition, the aqueous solution discharged from the filter section 105 is
Depending on the component concentration, the discharge pipe +23 (+23-1 to 1
23-N) to the inorganic salt solution discharge section 125 or the discharge pipes 127 (127-1 to 127-N).

One end of this discharge pipe 127 is connected to the purchasing port of the circulation pump 129, and the aqueous dye solution discharged to the discharge pipe 127 is transferred to a secondary source by this pump 129 via the discharge pipe 131 connected to the discharge port. The solution is pumped to the solution storage tank 115. In this way, the aqueous dye solution applied with electric current from the discharge side of the purification section 100A is used as a secondary solution, and then the purification section 100A is re-introduced.
00A for purification (salt reduction).

133 and 135 are release valves disposed in the storage tank 121 and the discharge tank 125, respectively;
The aqueous dye solution is supplied to the purification section 100B through the valve 135, and the inorganic salt concentration is discharged through the valve 135.

FIG. 4 shows the structure of the salt reduction treatment unit 101 shown in FIG.

In the figure, the opening and closing of the first supply valve 137 in the supply valve opening/closing section 103 is controlled to control the flow of pure water supplied to the salt reduction filter section 105 via the supply pipe III. Similarly, the second supply valve 138 and the third supply valve 1
41 is opened and closed to control the supply of the secondary solution and dye aqueous solution to the salt-reducing filter section 105, respectively.

Next, the salt-reducing filter section 105 separates inorganic salts from the dye aqueous solution by chromatography. That is, an aqueous dye solution is supplied from the supply valve opening/closing part 1 (13) to the upper end of the chromatography column 143. While the supplied aqueous dye solution descends within the column 143, each component in the aqueous solution is separated. By operation (chromatography),
The components with the weakest adsorption properties flow out first. Therefore,
By detecting the component concentration of the effluent solution, it is possible to extract only the aqueous dye solution in which the concentration of inorganic salts is below a predetermined concentration from the effluent solution based on the detection result.

Inorganic salt concentration detector 145 and dye concentration detector 147
is for detecting the concentration of ammunition salts and dye in the solution flowing out from the column 143, and is disposed in the flowing liquid passage 148 at the lower end of the chromatography column 143. As a method of detecting each component, there are a method of measuring conductivity, a method of using ionic current, a method of measuring spectrophotointensity, etc., and any of them may be used.

The dye aqueous solution is supplied to the chromatography column 143 in fixed amounts for purification (salt reduction), and for this purpose, a liquid level position detector 151 is provided at the upper end of the column.
Based on the detection result, the amount of aqueous solution supplied from the supply valve opening/closing section 103 is controlled.

Here, the stationary phase filled in the column 143 generally includes ion exchange resins, chelate resins, etc.
In this example, an ion retardation resin, such as Retartion IIA, is used.
-8 (trade name: manufactured by Dow Chemical Company) is used. Ion retardation resins do not require regeneration agents, can be regenerated with pure water, and are nearly neutral, so they are advantageous for desalting substances that are unstable to acids and alkalis.

FIG. 5 shows an outflow curve in which the concentration of each component of the outflow solution from the chromatography column 143 is plotted against the time axis, that is, the fractionation characteristics.As shown in the figure, dye concentration (curve I)
reaches its peak between times Tl and T2, and the inorganic salt concentration (curve ■) reaches its peak between times 13 and 14. In this example,
Based on such classification characteristics, the inorganic salt concentration detector 14
5 and dye concentration detector 14? Based on the detected value, the effluent solution from the chromatography column 143 is fractionated and extracted as follows.

That is, the dye concentration of the effluent solution is less than the predetermined value 02 (effective dye concentration), and the inorganic salt concentration is the predetermined value 4+NC3 (
(between times 11 and 72), the effluent solution is directed to storage tank 121. However, the concentration of inorganic salts is 11! jC3, and the dye concentration is the value C
2, drain the effluent solution into inorganic salt solution discharge tank 1.
Leads to 25. Also, during the period from when the inorganic salt concentration reaches the value 03 or more until the dye concentration becomes the value C2 or lower (time 12
13), the effluent melt is returned to the secondary solution storage tank 115.

Again in FIG. 4, the discharge valve opening/closing part 107 is 1=
As mentioned above, the outflow solution is separated, and the outflow passage 148 is branched into three prongs, and each branch pipe and the discharge pipe 123,
127 and 119, respectively. They are communicated via second and third exhaust valves 153, 155 and 157. With this configuration, the effluent solution can be discharged to the inorganic salt solution discharge tank 125 by listening to the first discharge valve 153, and in the same way, the second and third discharge valves 15 can be discharged.
5 and 15? By opening, the brewing solution can be led to the secondary solution storage tank +15 and the storage tank 121, respectively.

In this way, the aqueous dye solution whose concentration of inorganic tBs has become below a predetermined value is supplied from the storage tank 121 to the second purification section 100B via the valve 133.

FIG. 8 shows a second purification section 10 in which inorganic m species are removed from the dye aqueous solution in the purification section 100 of FIG. 1 by the Il diseparation method.
Indicates 0B. In the figure, 161 is a salt reduction tank, 163 is several filters, and 165 is a salt removal tank. Salt reduction tank 16
1 is supplied with an aqueous dye solution via a supply valve 133. This supplied aqueous dye solution is transferred to the salt-reducing tank stirrer 16.
9 to homogenize the aqueous solution, and an inorganic salt concentration detector 171 detects the inorganic salt concentration in the aqueous solution. This concentration detection is performed, for example, by ion chromatography. Further, the dye concentration in the aqueous solution is detected by the dye concentration detector 173. This concentration detection is performed, for example, by spectrophotometry. As described later, when it is detected that the inorganic salt concentration is equal to or higher than a predetermined value (for example, 5% by weight based on the dye), the circulation pump 17
5 is activated to circulate the dye aqueous solution in the salt reduction tank through the salt reduction filter l[i3. As this salt reduction filter, for example, an ultrafiltration filter or a reverse osmosis filter is used. By passing through the salt-reducing filter 63, inorganic salts such as sodium chloride and sodium sulfate contained in the dye aqueous solution are filtered out of the dye aqueous solution as an aqueous solution and discharged into the salt drainage tank 165. In this way, a portion of the water containing the dissolved 6M dye is discharged into the salt discharge tank 185 along with the inorganic salts. Therefore, in addition to replenishing the dye aqueous solution with this discharged water, pure water is supplied to the salt reduction tank 181 via the pure water valve 177 so that a dye aqueous solution with a desired concentration is obtained in the salt reduction tank 181. do.

In this way, an aqueous dye solution having an inorganic salt concentration and a dye concentration within a predetermined range is obtained in the salt reduction tank 181.

Note that the gutter of the aqueous dye solution in the salt reduction tank 181 is detected by the salt reduction tank liquid level detector 178. As mentioned above (low salt)
The purified aqueous dye solution is stored in a storage tank 182 via a storage valve 181.

The purified dye aqueous solution in the storage tank 182 is transferred to the valve 183.
The ink is taken out through the ink and used for ink preparation.

FIG. 7 shows a portion related to the purification section 100A in the control section 3θO of the apparatus shown in FIG.

Here, 301 is a controller, which controls the drive of each part. A read-only memory (ROM) 302 stores control programs such as operating procedures shown in FIGS. 9 and 10. 303 is a random access memory (RAM)
), and performs temporary storage of various data. Reference numeral 304 denotes various switches, which send various command signals to the controller 301 via a single output buffer circuit 305. 306 is a display, and 307 is a drive circuit that controls the display of the display 306 based on a drive signal from the controller 301.

Further, 3oe-i to 308-3 are drive circuits,
Based on the drive signal provided from the controller 301 via the output 4727 circuit 308, the valves 133 and 13
5 and Imp 129.

In this example, in the processing unit 101, analog signals are output from the inorganic salt concentration detector 145 and the dye concentration detector 147, and are converted into digital signals via A/D converters 311 and 312, respectively. It is supplied to the controller 301 via the input buffer circuit 313.

On the other hand, a digital signal is output from the liquid level position detector 151 and is supplied to the controller 301 via the input buffer circuit 313.

314 to 318 are the aforementioned waste valves 137, 139, 1
41.

This is a drive circuit that opens and closes 153, 155, and 157, respectively, and is controlled to be turned on or off by a drive signal supplied from the controller 301 via the output buffer circuit 321.

Note that since the salt reduction processing units IQI-1 to 1q1-H have the same configuration, only the unit 101-1 is shown in the figure, and the other units +01-2 to 10IN are omitted.

FIG. 8 shows a portion related to the purification section 100B in the control section 300 of the apparatus shown in FIG.

In this example, analog signals are output from the inorganic salt concentration detector 171 and the dye concentration detector +73, and the A/D
After being converted into a digital signal via converters 351 and 352, it is sent to the controller 30 via an input buffer circuit 353.
1. On the other hand, a digital signal is output from the depletion tank liquid early detector 179 and is supplied to the controller 301 via the input buffer circuit 30B.

355 to 358 are drive circuits for respectively driving the aforementioned valves 177, 181 and 183, the stirrer 169, and the circulation pump 175;
On/off control is performed by a signal supplied from 01 through the output buffer circuit 360.

FIG. 9 shows the refining section 10 of this embodiment configured as described above.
The operation of each processing unit at 0Ai is shown.

In the figure, when a start command is issued at step STI, the program switch is set to OFF at step ST2. next. In step ST3, the second and third supply valves 139 and 141 are opened, and the supply tank 2
1 and the secondary solution in the secondary solution storage tank 115 are started to be supplied into the chromatography column 143. This supply operation continues until the liquid level in the column 143 reaches the highest position H (see FIG. 4) according to the output of the liquid level position detector 151 in step ST4. When the liquid level reaches the highest level, that is, when the aqueous solution of the predetermined layer has been supplied to the column, the process proceeds to step ST5, and the Jlz valves 139 and 141 are closed on both sides. Next, in step ST8, the first discharge valve 153 is opened and the effluent solution from the chromatography column 143 begins to be discharged to the non-Japanese salt solution discharge tank 125.

In step ST7, it is determined whether the liquid level in the column is at the lowest position (see Figure 4). Immediately after supplying the dye aqueous solution and secondary solution, the liquid level is above the lowest position, so "NO" is selected.
It is determined that this is the case, and the process proceeds to step ST8. In step ST8, the first supply valve 137 is closed, and the process proceeds to step 5TIO. Here, as described above, immediately after the dye aqueous solution and the secondary solution are supplied and the developing operation is started in the column 143, the concentration of each component of the effluent solution is between time 0 and TI in FIG. It is in the state shown.

Therefore, in step ST9, the dye concentration detector 14
The determination as to whether or not the density value detected in step 7 is equal to or greater than the effective dye density value 02 is "NO", and step! 3T1
Go to 1. Furthermore, in step 5TII, the determination as to whether the concentration value detected by the inorganic salt concentration detector 145 is equal to or greater than the cleaning inorganic salt concentration value 01 is determined as "NO", and the process proceeds to step 5T12. In step 5TI2, it is determined whether the program switch is in the on state. In the first loop, since it is in the off state, the determination is "NO" and the process returns to step ST7. Steps like this ST7→ST8→5TIO Pass 5T
The loop of II-5T12 is repeated until rYES J is determined in step 5TIO.

Note that when it is determined that rYES J in step ST7, the process proceeds to step ST9, the first supply pulp 137 is opened, and pure water is supplied to the column 143.

Therefore, in such a case, step ST7→5T111
→5TIO→5T11→'3T12 loop is executed.

In step 5TIO, when the dye concentration value of the solution flowing out from the column 143 becomes equal to or greater than the effective dye concentration value 02 (time T1 in FIG. 5), the process proceeds to step 5TI3. Step 5
At T13, the inorganic salt concentration value detected by the inorganic salt concentration detector 145 is equal to the allowable inorganic salt concentration (++'jC
It is determined whether the number is 3 or more.

Here, due to the development operation of the chromatography column 443, the dye aqueous solution in which the inorganic salts have been classified flows out first (5th column).
(See time T1 to T2 in the figure), and in step 5T13, "N
It is determined as "O" and the process proceeds to step 5T14. In step 5TI4, the first exhaust valve 153 is closed, and in step 5T15, the third exhaust valve 15
7 is performed, and the effluent solution from the chromatography column 143 is discharged to the storage tank 121 through the discharge pipe 119. Next, in step 5TI6, the program switch is turned on, and the process returns to step ST7. Such steps ST7→ST8→5TIO→5T13→5T14→
5T15→5Tlf (or step ST7→ST9→
The loop of 5T10 → 5T13 → 5T14 → 5T15 → 5TI6 is repeated, and an aqueous dye solution purified to an inorganic salt concentration of 03v or less is obtained in the storage tank 121.

Such a loop returns rYES in step 5T13.
This continues until it is determined to be J.

As shown in Figure 5, the outflow of a-free salts begins, and the inorganic salt concentration of the 1st solution increases, and when the value 9 is equal to or higher than the allowable inorganic salt concentration value C3 (Figure 5 At time T2), the process proceeds from step 5TI3 to step 5T17, where the third exhaust valve 157 is closed, and at step 5T18, the second exhaust valve 155 is opened. As a result, the outflow solution is stopped from being discharged to the storage tank 12+ and is discharged to the discharge pipe 127. Here, in this example, the circulation pump! 29 is 7
Assuming that it is driven in synchronization with the opening operation of the helving 155, the outflow solution is discharged to the secondary solution storage tank +15 via the discharge pipes 129 and 131. This operation of refluxing the effluent solution is continued until a "NO" determination is made in step 5TIO. The thus recovered secondary solution is subjected to salt reduction and purification again. Next, when the dye concentration of the effluent solution decreases and its value becomes lower than the effective dye concentration value C2 (time T3 in FIG. 5), "NO" is selected in step 5TIO.
” and the process proceeds to step 5Tll. Now, since the inorganic salts are continuing to flow out, the determination is rYES J in step 5T11, and the process proceeds to step 5T19, where the second discharge valve 155 is closed, and furthermore, in step 5T20, the first discharge valve 153 is opened. Not 0. As a result, the flow of the outflow solution to the secondary solution storage tank 115 is stopped, and the outflow solution starts to be discharged to the inorganic salt solution storage tank 125 via the discharge pipe 127. This draining operation is continued until the inorganic salt concentration of the effluent solution falls below the cleaning inorganic salt concentration value C1.

When the inorganic salt concentration falls below the value CI (Time T4 in Figure 5)
, a determination of "NO" is made in step 5TII, and the process proceeds to step 5T12. Here, since the program switch is set to ON at step 5T113 as described above, rYESJ is set at step 5T12.
It is determined that the process proceeds to step 5T21, the first discharge valve 153 is closed, and the discharge of the outflow solution to the discharge tank 125 is completed.

Next, in step 5T22, the supply valve 13? is closed, and the supply of pure water to the chromato column 143 is stopped. That is, in this example, the first supply valve 13? is controlled to open and close, and pure water is supplied (steps ST8, 5T9). This pure water washes (regenerates) the stationary phase within the chromato column. - As mentioned above, when the inorganic salt concentration of the effluent solution falls below the cleaning inorganic salt concentration CI, it is determined that cleaning (regeneration) has been performed and the supply of pure water is stopped.

After executing step 5T22, step STI is executed again.
Return to and wait for the start command.

One (11N reduction) purification operation is completed as described above. In addition, in this embodiment, each processing unit) 10
Although the operations from 11 to +01-N are executed synchronously, they are not limited to this, and of course may be executed sequentially, for example.

Further, in this embodiment, the collected secondary solution is purified in each processing unit 101, but a separate processing unit exclusively for the secondary solution may be provided to perform the purification.

FIG. 1O shows the purification section 10 of this embodiment configured as described above.
The operating procedure of 0B is shown.

In the figure, in step 5T105, the dye concentration value of the dye aqueous solution in the salt reduction tank 181 detected by the dye concentration detector 173 is displayed on the display 364. In step 5T106, the inorganic salt concentration value similarly detected by the inorganic salt concentration detector 171 is displayed on the display 365.

In step 5T107, it is determined whether the dye concentration detected by the detector 173 is within the dye concentration range set by the switch 361. If it is determined that it is within the setting range, proceed to step 5T108,
If not, step ST]09 i: Proceed.

7.7 Tube 5TI08-c determines whether the concentration of inorganic salts detected by detector 171 is within the range of values set by switch 362. If it is determined that the value is within the set range, the process proceeds to step 5TIIO; otherwise, the process proceeds to step 5T109.

In step 5T109, it is determined whether the liquid level in the salt reduction tank 161 detected by the detector 178 is -1= higher than the high position that defines the setting range. If it is below that high position, proceed to step 5TI11, otherwise proceed to step 5TI12. Step 3 In STILL, supply valve 133 and pure water valve 1
77 is controlled to open and close, and a dye aqueous solution and pure water are supplied into the three tanks 161. As a result, the salt reduction tank +61
The dye JIa degree in the aqueous dye solution in the container is adjusted to be within the range set by the switch 361 as described in I-1. After this, the process advances to step 5T113. on the other hand,
In step 5T112, the supply valve 133 and the pure water 7-helm 177 are closed.

Step ST] At 13, activate the circulation pump +77 and use Makoto 4f! Water-soluble dye in +131! The dye solution is circulated through a salt-reducing filter 163 to remove excretory salts from the dye aqueous solution.

As mentioned above, if the dye concentration and inorganic salt concentration are outside the set range, step 5TIII and step 5T
113 or step 5T112 and step ST
1) Repeat the routine through 3 until the dye concentration and inorganic salt concentration are within the set range (+r4).

After the image density is within the set range, proceed to step 5TII.
Proceed to O.

In step 5TIIO, it is determined whether the liquid level in the salt reduction tank 1131 detected by the detector 179 is above a low position that defines the setting range. If it is above the low position, the process proceeds to step 5T114; otherwise, the process proceeds to step 5T115. In step 5T114, the operation of the circulation pump 175 is stopped, and the valve 181 is stopped.
performs the opening operation. As a result, a predetermined amount of the purified dye aqueous solution obtained in the salt reduction tank 181 is supplied into the storage tank 182.

In step 5T115, the valve 181 is closed and the supply valve 133. Perform the opening operation of the pure water valve 177,
At the same time as ending the supply to the storage tank 182, the salt reduction tank 16
Increase the amount of dye aqueous solution in 1 so that the liquid level is within the set range.

After this, a series of steps 5TIIO and 5T11
By repeating the routine through Steps 3 and 5T112 and 5T113, a predetermined amount of aqueous dye solution whose dye concentration and inorganic salt concentration are within the set range is obtained in the salt reduction tank 181. After this, the process proceeds to two consecutive steps 5T114.

As mentioned above, in this embodiment, the purification section 100
In this method, the aqueous dye solution is purified in constant quantities, and an aqueous dye solution from which inorganic salts have been removed to a predetermined concentration r can be continuously produced.

[Effects] As explained above, according to the present invention, inorganic salts contained in the dye solution are removed by cyclically performing the chromatography method and the membrane separation method. Dye droplets suitable for preparing ink for use in marking instruments can be produced.

Furthermore, according to the present invention, such a purified dye solution can be produced continuously and automatically.

In addition, in the above-mentioned example, after performing the chromatography method, the membrane separation method was performed to remove the inorganic t-groups, but the order of these steps may be reversed.

However, inorganic 1n species can be removed more efficiently when the membrane separation method is performed after the chromatography method as in this example.

[Brief explanation of the drawing]

FIG. 1 is an overall configuration diagram showing an embodiment of the apparatus according to the present invention, FIG. 2 is a configuration diagram showing the dye solution production section in FIG. 1, and FIG. Fig. 4 is a block diagram showing the salt reduction processing unit in Fig. 3; Fig. 5 is a characteristic curve diagram showing the separation characteristics of the gromatoto ram; Fig. 6 is a diagram showing the purification unit in Fig. 1. FIG. 7 and FIG. 8 are block diagrams showing a part of the control section in FIG. 1, respectively. FIG. 8 and FIG. It is a flowchart which shows the refining operation of a refining part. Dye solution manufacturing department 1 7 3...Dye supply unit, 5...Dye powder, 7...Dyeing oil 1 valve, :]...Mixing tank, 11...Pure water valve, 13... Pure water supply pipe, 15... Mixing tank agitator, 17... Mixing tank liquid level detector, 19... Filtration filter, 21... Supply tank, 23... Supply pipe. Purification Department 100 (100A, 1OOB) +00A・
...First purification section 101... Salt reduction processing unit, 103... Supply valve opening/closing section, 105... Salt reduction filter section, 107... Discharge valve opening/closing section, 109... Dye aqueous solution supply pipe , 8 III...Pure water supply pipe, 113...Secondary solution supply pipe, 115...Secondary solution storage tank, 117...A joint pipe, 119...Discharge pipe, 121. ...Storage tank, 123...Discharge pipe, +25...Inorganic salt solution discharge tank, 127...Discharge pipe, 128...Circulation pump, 131...Discharge pipe, 133.135...Discharge /Help, 137, 13! ], 141... Supply valve, 1
43...Chroma I column, +45...Inorganic class M concentration detector, 147...Dye concentration detector, 148...Outflow passage, 151...Liquid level position detector, 153.155, 157...Ejection/Help. 1008...Second purification section 161...Salt reduction tank, 163...'g salt filter, 165...Salt removal tank, 168...Salt reduction tank agitator, 171...Inorganic salt concentration Detector, 173...Dye concentration detector, 175...Circulation pump, 177...Pure water valve, 181...Storage/help, 182...Storage tank, 183...Valve. Control unit 300 301... Controller, 302... Read only memory, 303... Random access memory, 304... Switch, 305... Human output/Hetufa circuit. 3013... Display device, 307.308-1, 308-2, 308-3... Drive circuit, 309... Output eight circuit, 311.312... A/D converter, 313 ... Input buffer circuit, 314-319 ... Drive circuit, 321 ... Output 4777 circuit, 351.352 ... A/D converter, 353 ... Human power 4777 circuit. 355-358... Drive circuit, 360... Output buffer circuit, 3f (1... Dye concentration range setting switch, 3132...
...Inorganic salts concentration range setting switch, 363...7 human output buffer circuits, 364...Dye concentration display, 365...Inorganic salts concentration display. 306 307 305

Claims (1)

[Scope of Claims] A means for producing a dye solution, a first solution processing means for performing chromatography using the dye solution, and a second solution processing means for removing S organic salts from the dye solution by membrane separation.
A dye purification device characterized by comprising: a solution treatment means. (Margin below)