JPS6031570A - Dye refining apparatus - Google Patents

Abstract

PURPOSE:To yield a refined dye soln. well suited for a recording liq. efficiently, by a process wherein heavy metal ions in a dye soln. are captured through an ion-exchange resin column and a concn. of heavy metal ions in the effluent from the column is detected to fractionate the effluent. CONSTITUTION:Dye powder 22 and pure water 26 are fed to a blender 24 and mixed with each other to prepare an aq. dye soln. After insoluble matter in said dye soln. is removed by a filter 29, the filtrate is fed through a supply tank to a refining unit 41. By passing through an ion-exchange resin column 44-1, etc., heavy metal ions contained in the dye soln. are removed by capturing with the ion-exchange resin. Then, a concn. of heavy metal ions in the effluent from the column 44-1, etc. is detected by a sensor of concn. of heavy metal ions 46-1, etc. to fractionate the effluent by control of a control unit 61 in order that when the indication is under a prescribed value, the effluent is fed into a storage tank 49 while when it is above the value, it is returned to the supply tank 31 by a pump 51.

Description

DETAILED DESCRIPTION OF THE INVENTION (Technical Field) The present invention relates to a dye refining device that continuously supplies a purified dye suitable for preparing a recording liquid (generally referred to as ink) suitable for inkjet recording, writing instruments, etc. Regarding 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 caused by a piezo vibrator, has been made by mixing various dyes and FU4 materials with water or other organic materials. It is known that it is dissolved in a liquid medium consisting of a solvent or heated to 78F. 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 whose main components are a water-soluble dye, water as its solvent, and the king of glycols as an anti-drying agent.

Here, water-soluble dyes usually contain inorganic heavy metal ions such as thorium chloride and sodium sulfur.

When recording ink is prepared using dyes containing such inorganic ions, the following disadvantages arise. That is, inorganic ions reduce the stability of dye dissolution in the ink, causing aggregation and precipitation of the dye. In addition, in ink sheet recording heads and writing utensils, ejection orifice
Ink evaporates nearby! Changes in composition now cause precipitation of inorganic salts. All of these causes aging of the discharge orifice, which should be avoided most.

Therefore, in order to eliminate such adverse effects, it is necessary to control the inorganic ion concentration to be within a predetermined range during ink production. This is essential when a general Ichiichizaka dye containing inorganic ions as impurities is used in the preparation of inkjet printing inks, 6tt printing inks, and printing inks.

(Objective) In view of these points, the object of the present invention is to remove heavy metal ions contained in a dye solution and continuously supply a purified dye solution suitable for preparing inkjet recording ink, writing instrument ink, etc. An object of the present invention is to provide a dye refining device that can obtain dyes.

(Example) Hereinafter, the present invention will be described in detail with reference to the drawings.

FIG. 1 shows an embodiment of the apparatus of the present invention.

Here, 21 is a dye supply section that stores dye powder 22, and supplies the dye powder 22 to a mixing tank 24 via a dye valve 23. Further, pure water is supplied to the mixing tank 2/1 via a pure water supply pipe 2G in which a pure water valve 25 is inserted.

In the mixing tank 24, the supplied dye powder 22 and pure water are dissolved by the mixing tank stirrer 27 to prepare an aqueous dye solution. , the amount is detected by the mixing tank liquid level detector 28.Dye powder particles that were not dissolved in the pure water remain in the dye aqueous solution obtained in the mixing tank. For this filter 29, ordinary filter paper or Fluoropore (trade name) can be used.The dye solution that has passed through the filter 28 to remove particles, etc., is passed through the dye solution supply valve 30. It is supplied to the supply tank 31.

A supply tank liquid level sensor 32 is disposed in the supply tank 31, and the dye solution supply valve 30 is controlled to open and close based on the output of this sensor, thereby controlling the liquid level height in the supply tank 31.

Next, 41 is a purification section that removes heavy metal ions from the dye aqueous solution, and includes a plurality of processing units, in this example, three first to third processing units 71, 42-1, 42-2 and Consists of 42-3. Each processing unit 42 (,42-1~
42-3), the aqueous dye solution in the supply tank 31 is supplied to the ion exchange resin columns 44 (44-1 to 44-3) via the supply valves 43 (43-1 to 43-3). The ion exchange resin column 44 separates JR heavy metal ions from the dye aqueous solution by so-called ion exchange separation. That is, due to ion exchange within the column, highly adsorbable heavy metal ions contained in the aqueous dye solution are captured by the ion exchange resin and remain in the column white. here,
Inside the column are valves 45C45-1 to 45 for controlling the liquid level.
-3) to control the amount of dye aqueous solution supplied into the column. Further, the ram 44 is made detachable from the processing unit, and whether or not a column is attached is detected by a filter replacement end switch (not shown).

Next, 1 heavy metal ion concentration sensor 413 (48-1 to 4B
-3) at the lower end of the column 44;
heavy metal in the effluent solution from column 44)
Detect A ion concentration. As the detection power method for the heavy metal ion concentration, for example, a measurement method using a metal ion electrode or a measurement method using atomic absorption spectroscopy is used. Melt tM sensors 47 (47-]] to 47-3 are similarly disposed in the outflow solution passage to detect the presence or absence of the outflow solution in the outflow δ liquid path.

The effluent solution from column 44 is discharged in the first discharge/\lube 4 days (4
8-1 to 48-3) from the edge of the storage tank 49.

Further, the water is refluxed to the supply tank 31 via the second discharge valves 50 (50-1 to 50-3) by the action of the circulation pump 51. Opening/closing control of both valves 48 and 50 is performed based on the detection results of the heavy metal ion concentration sensor 46 as described later.

The aqueous dye solution obtained in the storage tank 48 from which heavy metal ions have been removed is taken out via the supply valve 52.

θl is a control unit that controls the drive of each part, and 62
is an operation section equipped with various display sections, drive switches, etc.

:fS2 Figure shows the control system of the apparatus shown in Figure 1. Here, 101 is a controller, which controls the drive of each part.

A read-only memory (ROM) 102 stores a control program such as the operating procedure shown in FIG. 103
A random access memory (RAM) is used to temporarily store various data. Reference numeral 104 denotes various switches arranged in the operation section B2, which send various command signals to the controller 101 via the human output buffer circuit 105. Reference numeral 108 denotes a display disposed in the operation 7+Be2, which displays the first to third unit/filter exchange display and the fourth processing unit, which displays that the column in each processing unit needs to be replaced, as described later. Turn on the first to third unit operating indicators that indicate that the unit is in the process of purifying the aqueous dye solution. 107 is a drive unit 1-1 from the controller 101;
This is a drive circuit that controls the display of the display 108.

The detection outputs of the mixing tank liquid level detector 28 and the supply tank liquid level sensor 32 are sent to the controller 10 via an input buffer circuit 108.
1. The drive circuits 110 to 114 are connected to a controller 101 supplied via an output buffer circuit 10EI.
(to the drive control signal from), (on, each load (valve 2)
3. On/off control of 25, 52, stirrer 27, and pump 51).

Next, 120 is a control system of the processing unit 42-1.

Since the configuration of each processing unit is the same, the other units 42-2 and 42-3 are omitted in the IA. The detection signal from the heavy metal ion crop increase sensor 48-1 is digitized via the A/D converter 121, and then sent to the controller 10 via the large cover/sofa circuit 122.
1. Further, a digital detection signal is output from the solution sensor 47-1 and is supplied to the controller 101 via the input buffer circuit 122. 123.

124 and 125 are the aforementioned valves 43-1.11.
8-1 and 50-1, respectively, and is a drive circuit for opening and closing the output buffer circuit 12 from the controller 101.
On/off Mi is controlled by drive No. 44 supplied through No. 8.

In this embodiment configured as described above, each of the processing units 44-1 to 44-3 is sequentially replaced to remove heavy metal ions based on the detection output of the heavy metal ion agricultural sensor 46. That is, there is a limit to the ability of the ion exchange resin in the ion exchange resin column 44 to capture heavy metal ions, and if a certain amount of heavy metal ions are adsorbed, ion exchange separation will not be performed. The dye solution containing lA ions is discharged as is, and the concentration of heavy metal ions in the solution t(a) flowing out from the column 44 increases. By detecting this concentration increase, the use of the ion exchange resin column is disabled, and the other two Subsequent purification of the dye solution !tk is carried out using either one of the two columns.In addition, the ion exchange resin column that is no longer usable is replaced with a new column, or the ion exchange resin is regenerated and processed again. Refining is carried out in the unit to produce 4Q.

FIG. 3 shows the operation of each such processing unit.

Here, each flag is used to make the following determinations: Unit filter replacement flag: This is a flag that instructs to replace the filter in each processing unit, that is, the ion exchange resin column. When this flag is turned on, The filter replacement indicator of the corresponding unit will indicate that the filter needs to be replaced.

Unit change request flag: This is a flag that requests a change in the processing cap. When this flag is turned on, the unit
- The processing unit indicated by the selection counter is selected and the dye refining operation is moved to that processing unit.

Unit operation flag: A flag indicating that the corresponding processing unit has been selected.

Unit I/Operating Flag 2 This flag indicates that the corresponding Jllj unit is in operation.

Unit discharge flag: This is a flag that turns on when the concentration of heavy metal ions in the solution flowing out from the column in the corresponding processing unit exceeds a set value, and instructs the pump 51 to start the reflux operation of the solution flowing out to the supply 1fi31.

Next, each step shown in FIG. 3 will be explained.

In FIG. 3(A), each display and data are initialized in step STI. In step ST2, the processing unit change request flag is turned on, and the contents of the unit selection counter are set to "1". In step ST3,
Based on the detection output of the supply tank liquid level sensor 32, it is determined whether a predetermined amount of dye solution is stored in the supply tank 31. When the predetermined amount of water is stored, the dye solution supply valve 30 is closed in step ST4, and then the process proceeds to step ST8. However, if the predetermined amount has not been reached, the supply valve 30 is opened in step ST5 to supply the aqueous dye solution to the supply tank.

Step ST8 is a processing step when there is a filter replacement request in the first processing unit l-42-1, and consists of steps 5T8-1 to STfl-3. First, when it is determined in step 5T8-1 that the first unit filter replacement flag is in the on state, step 5T8-2
Next, it is determined whether or not the second filter replacement end switch is on. If it is on, step 5
Proceeding to 6-3, the first unit filter replacement flag is turned off, and the display indicating that replacement is required, which was displayed on the first unit filter replacement display, is erased. After this, the process advances to step ST7. Note that when the filter replacement flag is off in step 5T8-1 and when the filter replacement end switch is off in step 5T8-2, step ST? Proceed to.

Step ST7 and step ST8 are the second
Processing unit 42-2 and first processing unit 42-3
This is a processing step when there is a filter replacement request in
The contents are the same as step ST8, and the explanation thereof will be omitted.

In step 5TII, it is determined whether or not the unit change request flag is in the on state, and if the determination is positive, the process proceeds to step 5TIO, and if the determination is negative, the process proceeds to step 5TIB in FIG. 3(B). In step 5 TIO, the contents of the unit 1 selection counter are determined and the contents are rl
If it is "J", proceed to step 5T13; if "2", proceed to step 5T14. If r3 J, step 5T1
Steps 5T13 to 5T15 are each processing unit l-42-
These are processing steps when 1 to 42-3 are selected.

Since the contents of each of steps 5T13 to 5T15 are the same as 1, the contents of step 5T13 when the first processing unit l-42-1 is selected will be explained. First, step 5
At T13-i, it is determined whether the first unit filter replacement flag is in the OFF state. When the judgment is negative, t
Proceed to step 5T13-5, and if it is self-propelled, proceed to step 5T13-2.In step 5T13-2, turn on the 1st unit operation indicator and 1%5! l
! Displays that unit 4.2-1 is in operation. In step 5T13-3, the supply valve 43-1 and the second cell IJj 0rev 50-1 are opened. Subsequently, in step 5T13-4, the first unit operation flag is turned on, and the unit I/change request flag is turned off. Next, in step 5T13-5, the content of the unit selection counter is set to "2", and then the process goes to step 5T16.

Here, the content of the unit selection counter is r2 J
, r3 J , rl J , r2J , . . 11 "
It is a ring counter that changes to 1, and by executing step 5T14, its content changes to ``3'', and
By executing step 5T15, the contents are NJ
Changes to

Next, steps 5T1B, 5T17, and 5T18 in FIG. 3(B) are steps for controlling the output of the effluent solution from the ion exchange resin column in each processing unit. Since the contents of each of these steps are the same, step 5T18 indicating control in the first processing unit 42-1
The contents will be explained only for the following.

First, in step 5T18-1, it is determined whether or not the first 22nd operation flag is in the on state.

If the determination is negative, the process jumps to step 5TlG-5, and if the determination is self-sufficient, the process proceeds to step 5Tle-2. Step 5
718-2, heavy metal ions 1i in the column outflow solution detected by the heavy metal 14 ion C sensor 46-1
2 degrees is set (&j or less is determined. If the determination is negative, proceed to step 5T18-5; if the determination is self-sufficient, proceed to step 5T18-3. Step 5TII3-
3, the second discharge valve 50-1 is closed and the first JJI
Open the outlet valve 48-1. As a result, in the ion exchange resin column 44-1, the aqueous dye solution in which heavy metal ions have been removed to a value below the set value is discharged into the storage tank 49 via the q'S 1 discharge pulp 48-1. next,
In step 5TII3-4, the first unit operation flag is turned off, and the first unit operation flag is turned on, and then the process proceeds to step 5T1e-5.

In step 5T18-5, it is determined whether the first unit operating flag is in the on state. If it is in the off state, the process advances to step 5T19-10, and if it is in the on state, the process advances to step 5T113-8. In step 5T18-8, it is determined whether the concentration detected by the heavy metal ion concentration sensor 46-■ exceeds a set value. If the set value is not exceeded, the process proceeds to step 5TII3-10, and if it is exceeded, the process proceeds to step S18-7. After turning off the first unit operation indicator in step 5T18-7, the process proceeds to step 5T18-8, where the supply pulp 4
3-1 and the first discharge valve 48-1 are closed. Furthermore,
While opening the second discharge valve 50-1, the circulation pump 51
f! :, a reflux operation is started in which the solution flowing out from the column 44-1 is refluxed to the supply tank 31 via the second discharge valve 50-1. Next, in step ST9, the first unit I operating flag is turned off, and the first unit discharge flag is turned on, after which the process advances to step 5T181o.

Next, in step 5T18-10, it is determined whether or not the first unit output flag is in the on state. If it is not in the on state, the process advances to step 5T17, and if it is in the on state, step 5T18- Proceed to step 11. Step 5T
At step 18-11, it is determined whether the solution sensor 47-1 disposed in the outflow solution passage of the column 44-1 is off, that is, whether or not the outflow solution remains in the outflow solution passage. When it is not in the OFF state, that is, when a solution is detected, the process proceeds to step 5T17, and when it is in the OFF state, the process proceeds to step 5T18-12. This off state means that all of the aqueous dye solution discharged from the column 44-1 and having a heavy metal ion concentration higher than the set value has been refluxed to the supply tank 31. Step 5 Tlf! -1
In step 2, the first unit filter replacement indicator is turned on to display that the column of the 1st filter unit needs to be replaced. Next, in step 5T1G-13, the second discharge valve 50-1 is closed and the pump 51 is turned off.
and stop the reflux operation. Next, step 5T11
In step 3-14, the first unit υ1 output flag is turned off, the first unit filter replacement flag is turned on, and then the unit change fee request flag is turned on. After this, step 5T
Proceed to step 17.

Next, step ST1? After passing through 5T18, the process returns to step ST3 shown in No. 31811(A).

By performing each step described above, 6 places J! [!
The aqueous dye solution 71.42-1 to 42-3 is purified, and a purified aqueous dye solution in which the concentration of heavy metal ions is lower than the set value is obtained in the storage tank 48.

(Effects) As explained above, according to the present invention, ion exchange separation is performed to capture heavy metal ions in a dye solution, and the dye and solution after the ion exchange separation are separated to separate heavy metal ions. Since the dye solution that was not removed is collected and ion exchange Ni is performed again, it is possible to efficiently produce a dye solution suitable for preparing ink cartridge recording ink and the like.

[Brief explanation of the drawing]

1 IN is a schematic diagram showing the complete configuration of the device according to the present invention; FIG. 2 is a block 1Δ showing the control section of the equipment shown in FIG. 1; FIGS. B) is a flowchart showing the purification operation of the apparatus shown in FIG. 21...Dye supply unit, 22...Dye powder, 23...Dye valve, 24...Blending tank, 25...¥1m water help, 26...Pure water supply? 6., 27... Preparation tank stirrer, 28... Preparation tank liquid level detector, 28... Filtration filter, 30... Dye solution supply valve, 31... Supply tank, 32... Supply tank liquid level sensor, 41... Purification section, 42... Processing unit, 43... Supply valve, 44... Ion exchange tree 11tt column, 45... Di", 46... Heavy metal ion Concentration sensor, 47... Solution sensor, 48... 1st" 1st output valve, 48... Storage tank, 50... 2nd J 1st output/help, 52... Supply valve, 81. ...Control unit, 62...Operation〆;B. 101...11 controller, 102...read only 7, 103...random access memory, +04...switch, 105...input/output buffer circuit, 106...indicator, lθ7 ...Drive circuit, 108...Input 4727 circuit, +1)S...Output buffer circuit. 110-114...Drive circuit, 121...A/D converter, 122...Input 71727 circuit, 123.124,125...Drive circuit, 12G.
...7 output buffer circuits.

Claims (1)

[Claims] A means for producing a dye solution. Perform ion exchange separation to remove heavy metal 177 in the dye solution.
', a dye solution processing means for trapping ions, and a liquid separation control means for separating the A effluent from the processing means. A dye purification apparatus comprising: a circulation system for supplying an electric current to a part of the separated liquid to the processing means. (Margin below)