JPS6031574A - Dye refining apparatus - Google Patents

Abstract

PURPOSE:To yield a refined dye soln. surely, by a method 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 by a sensor to cause the column to stop the operation when the indication is above a prescribed value. 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 removing insoluble matter in the dye soln, by a filter 29, the filtrate is fed through a supply tank 31 to a refining unit 41, in which the filtrate is passed through an ion-exchange resin column 44-1, etc. and heavy metal ions contained in the dye soln. are removed by capturing with the ion-exchange resin. Furthermore, a concn. of heavy metal ions in the effluent from the column is detected by a sensor of concn. of heavy metal ions 46-1, etc., and when the indication is above a prescribed value, the control of a control unit 61 causes the effluent to return to the supply tank 31 and the column to stop the operation.

Description

Detailed Description of the Invention (Technical Field) The present invention relates to a dye purification device that continuously supplies a purified dye suitable for preparing a recording liquid (generally referred to as ink) particularly suitable for inkjet recording, writing instruments, etc. This invention relates to dye purification equipment.

(U2RAJ1 (; IHOi) Conventionally, various dyes and pigments have been used as inks used in inkjet recording methods, in which ink in a recording head is ejected from an ejection orifice using vibrations caused by a piezoelectric vibrator. It is known that inks are prepared by dissolving or separating I in a liquid medium consisting of water or other organic solvents.Similar inks are also known to be used in writing instruments such as felt pens and fountain pens. ing.

General No. 1 of such ink (as an example of this configuration,
The main ingredients include water-soluble dyes, water as their solvent, and the king of glycols as anti-drying agents.

Here, the water-soluble dye usually contains an inorganic salt such as planarizing thorium or sodium sulfate, and a heavy metal ion.

When a recording ink is prepared using a dye containing such fi42 ions, the following disadvantageous conditions occur. That is, inorganic ions reduce the stability of dye dissolution in the ink, causing aggregation and precipitation of the dye. Furthermore, in inkjet recording heads and writing instruments, when ink evaporates near the ejection orifice and the liquid composition changes, inorganic salts are precipitated. All of these causes clogging of the discharge orifice, which is most avoided.

Therefore, in order to eliminate such adverse effects, it is necessary to control the inorganic ion production so that it falls within a predetermined range during ink production. This is essential when a general commercially available dye containing an inorganic ion as an impurity is used to prepare an ink for recording ink or an ink for a writing instrument.

(Objective) In view of these points, the object of the present invention is to remove heavy metal ions contained in a dye solution and to create 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 which is capable of supplying and refining 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. In addition, a pure water valve 2 is provided in the mixing tank 24.
Pure water is supplied through a pure water supply pipe 26 with a pipe 5 inserted therein.

In the mixing tank 24, the supplied dye powder 22 and pure water are mixed and dissolved by a mixing tank agitator 27 to create an aqueous dye solution. The amount of the aqueous dye solution stored in the mixing tank 24 is detected by a mixing tank liquid amount detector 28 . 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 29. For this filter 28, ordinary filter paper, Fluoropore (trade name), or the like can be used. The dye solution from which particles and the like have been removed by passing through the filter 28 is supplied to the supply tank 31 via the dye solution supply valve 30.

A supply tank liquid level sensor 32 is disposed in the supply tank 31, and the output of this sensor is determined by l, 1. :Zuki dye solution supply valve 30
The liquid level height in the supply tank 31 is controlled by controlling opening and closing.

Next, 41 is a purification section that removes heavy metal pions from the aqueous dye solution, and includes a plurality of processing units, in this example three first to third processing units, 42-1; 42-2 and 42-1;
Consists of 2-3. Each processing unit, 4'2 (42-1 ~
42-3), the aqueous dye solution in the supply tank 31 is supplied to the ion exchange resin column 44 (44-1 to 44-3) via the supply valve 43' (43-1 to 43-3).

The ion exchange resin column 44 separates heavy metal ions from the dye water '18 M& by so-called ion exchange separation. That is, due to the ion exchange within the column, the adsorbent crystalline gold 111 ions contained in the aqueous dye solution are extracted by the ion exchange tree 11\i j and remain within the column. Here, there is a liquid level jj'l in the column.
A control phase valve 45 (45-1 to 45-3) is provided,
Control the amount of aqueous dye solution fed into the column. In addition, this column 44 is made removable from the processing unit,
It is detected whether a column is attached or not by a filter exchange path r switch indicated by IΔ.

Next, heavy metal ion concentration sensor 46 (46-1 to 4e-
3) is placed in the outflow solution passageway at the lower end of the column 44 to detect the concentration of heavy metals and high ions in the outflow solution from the column 44. As a method for detecting the heavy metal ion concentration, for example, a measuring force method using a metal ion electrode or a constant force method using pretension optical spectroscopy is used. A solution sensor 47 (47-1 to 47-3) is disposed in the outflow solution passage and detects the presence or absence of an outflow solution in the outflow solution passage.

The effluent solution from the column 44 is passed through the first discharge valve 48<48
-1 to 48-3) to 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. 15Fl closing control of both valves 48 and 50,
This 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.

61 is an ib control unit that controls the drive of each part;
Reference numeral 62 denotes an operation section including various display sections and drive switches.

FIG. 2 shows the control system of the apparatus shown in FIG. here 10
Reference numeral 1 denotes a controller, which controls the drive of each part. 10
Reference numeral 2 denotes a read-only memory (ROM), which stores the control program 01 of the operator 11114'5- shown in FIG. 103 is a random access memory (in RA), which temporarily stores various data; 104 is various switches disposed in the operation unit 82, which sends various commands to the controller 101 via an input/output buffer circuit 105; Send a signal. Reference numeral 1013 denotes a display disposed on the operation unit 62, which includes a first unit filter replacement display and a third unit filter replacement display for displaying that columns in each processing unit need to be replaced, as described later. 1st to 3rd units displaying that the processing unit or dye aqueous solution purification operation is in progress.
j Use the in-progress display. A drive circuit 107 controls the display of the display 108 based on a drive signal from the controller 101.

The detection outputs of the mixing tank liquid star detector 28 and the supply tank liquid level sensor 32 are supplied to the 1 (J controller 101) via the manual buffer circuit 108. The drive circuit +10-114
is based on the drive control signal from the controller lot supplied via the output buffer circuit 109.
3, 25, 52, stirrer 27, and pump 51).

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

Since the structure of the valley processing unit is the same, other units 42-2 and 42-3 are omitted in IA. The detection signal from the heavy metal ion concentration sensor 46-1 is digitized via the A/D converter 121, and then sent to the FI controller 1 via the input buffer circuit 122.
01. In addition, a digital detection signal is output from the solution sensor 47-1 and sent to the input circuit 122.
The signal is supplied to the controller 101 via. Reference numerals 123, 124 and 125 are drive circuits for opening and closing the aforementioned valves 43-1, 48-1 and 50-1, respectively. ! 1st road 12B
The on/off control is performed by the drive number 1d supplied through.

On the Kinomi side configured as described above, the RIs (each processing unit) 44-1 to 44-3 are sequentially replaced with the detection output of the heavy metal ion concentration sensor 46 to perform heavy metal ion removal processing. That is, ion exchange resin column 4
There is a limit to the ability of the ion exchange 4b1 fat in 4 to capture heavy metal ions, and once a certain number of heavy metal ions have been adsorbed, ion exchange separation is no longer performed. As a result, Togane 171. The dye solution containing ions is directly discharged v1, and the concentration of heavy metal ions in the effluent from the column 44 increases. When A is detected above this concentration, the use of the ion exchange resin column is disabled, and the subsequent purification of the dye solution is performed using either of the other two columns. In addition, an ion exchange resin column that is no longer usable is replaced with an XJi L column, or the ion exchange resin is regenerated so that it can be purified again in the processing unit.

FIG. 3 shows the operation of each processing unit.

Here, each flag is used to make the following determinations.

Unit filter replacement flag: 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 corresponding unit filter replacement indicator will display that filter replacement is necessary. .

Unit change request flag: A flag that requests a change in the processing unit I. When this flag is turned on, the processing unit 71 indicated by the unit selection counter is selected and the dye refining operation is transferred to that processing unit.

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

Near 1/operating flag: This is a flag that indicates that the corresponding processing unit is in operation.

Unit discharge flag: A flag that is turned 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 refluxing the solution to the supply tank 31.

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

In FIG. 3(A), in step 3-1, each display and data are initialized. In step ST2, the processing unit/
At the same time, the unit selection counter contents rlJ is set. In step ST3, it is determined from the detection output of the supply tank liquid level sensor 32 whether or not a predetermined amount of dye solution is stored in the supply tank 31. When the predetermined amount is stored, the dye solution supply pulp 30 is closed in step ST4, and then the process proceeds to step ST6. 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 ST6 is a processing step when there is a filter replacement request in the il processing unit 42-1, and consists of steps 5Tfi-1 to 5T8-3. First, when it is determined in step 5T13-1 that the first unit filter replacement flag is in the on state, step 5T8-2
Then, it is determined whether or not the first unit filter replacement end switch is on. If it is on, step 5
Step 6-3 turns off the first unit filter replacement flag and erases the display indicating that replacement is required on the first unit filter replacement display. After this, the process advances to step ST7. Note that when the filter replacement flag is off in step 5Te-i and when the filter replacement end switch is off in step 5T8-2, the process goes to step ST? according to the flow of "NO". Proceed to.

Step ST7 and step ST8 are the second
processing unit) 42-2 and third processing unit 42-
Step ST3 is a processing step when there is a filter replacement request, and its contents are the same as step ST8, so the explanation thereof will be omitted.

In step ST'9, it is determined whether or not the uni) h change request flag is in the ON state. If the determination is positive, the process proceeds to step 3-10; if the determination is negative, the process proceeds to step ST'10, as shown in FIG.
) Proceed to step ST18. In step 5TIO, the content of the unit selection counter is determined. If the content is "1", the process goes to step 5T13, if it is "2", the process goes to step 5T14, and if it is "3", goes to step 5T1.
Proceed to step 5 respectively.

Steps 5T13 to 5T15 are each processing unit, )42-
These are processing steps when 1 to 42-3 are selected.

Since the contents of each step 5T13 to 5T15 are the same, the contents of step 5T13 when the first processing unit 42-1 is selected will be explained. First, step 5
At T13-1, it is determined whether the first unit filter replacement flag is in the off state fq+. If the judgment is negative, proceed to step 5T13-5, and if the judgment is 11, proceed to step 5T13-5.
Proceed to step 5T13-2. In step 5T13-2,
The first unit operating indicator is turned on to indicate that the first unit processing unit 42-1 is operating. In the step 5T13-3, the supply valve 43-1 and the second discharge valve 50-1 are opened. Continuing, step 5T13-
In step 4, the first unit operation flag is turned on and the unit change request flag is turned off. Next, step 5T
In 13-5, the content of the unit s selection counter is set to ``2''.
”, the process advances to step 5T16. Here, the content of the unit selection counter is "2".

r3'', rl'', r2'', etc. By executing step 5T14, the content changes to ``3'', and by executing step 5T15, the content changes to ``3''. It changes to "l".

Next, steps 5TIEt, 5T17 and 5TI8 in FIG. 3 CB) are JJ+ output control Nutemps for the effluent solution from the ion exchange resin column in each processing unit, respectively. Since the contents of each of these steps are the same, only the contents of step 5T18 indicating ill 1311 in the first processing unit l-42-1 will be explained.

First, in step 5T18-1, it is determined whether or not the second actuation flag is in the on state.

If the judgment is negative, jump to step 5T19-5,
If it is determined that ij is positive, the process advances to step 5T16-2. In step 5T11 (-2, the heavy metal ion concentration sensor 46
It is determined whether the heavy metal ion concentration in the column outflow solution detected by -1 is below a set value. If the determination is negative, proceed to step 5TI8-5; if the determination is negative, proceed to step 5TII (-3.Step 5T16-
3 closes Q'52 Ejection/Help 50-1 and returns to the 14th
Open Jl outlet valve 48-1. As a result, in the ion exchange resin column 44-1, the aqueous dye from which heavy metal ions or ions have been removed to a value below the set value is slid into the storage tank 48 via the first publication tube 48-1. . next,
In step 5TIB-4, the first unit operation flag is turned off, the first unit operation flag is turned on, and then the step
Proceed to MB5TI6-5.

In step 5T1B-5, it is determined whether the first unit operating flag is in the on state yg. If it is in the off state, proceed to step 5TIB-1 (l; if it is in the on state, proceed to step 5TL13-f (.step 5TI8-
In step 41, it is determined whether the concentration detected by the heavy metal ion concentration sensor 413-H exceeds a set value. 1-Step 5Ti if the set value is not exceeded
Proceed to 6i-IQ, and if it exceeds step 5T16-
Proceed to step 7. After turning off the first unit operating indicator in Stella 7''5T113-7, step 5TI6-8
Proceed to supply valve 43-1 and first discharge valve 48
-Close 1. Furthermore, while listening to the second discharge valve 50-1, the circulation pump 51 is driven to send the effluent solution from the column 44-1 to the supply tank 3 through the second discharge valve 50-1.
1 starts. Next, Ste.

At step 7'ST9, the first unit operating flag is turned off (5), and the first unit discharge flag is turned on (step 5T1B-10).

Next, in step 5T18-10, the first unit υ1
It is determined whether the output flag is in the on state or not, and if it is not in the on state, step STI? If it is in the on state, the process advances to step 5TIB-11. Step 5T18
-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 not in the off state, that is, when a solution is detected, step STI? The process proceeds to step 5T1B-12 when the control is in the off state. This off state means that all of the aqueous dye solution discharged from the column 44-1 whose concentration value of heavy metal ions is higher than the set value has been refluxed to the supply tank 31. In step 5T1B-12, the first unit filter replacement indicator is turned on to indicate that the column of the first processing unit needs to be replaced.

Next, in step 5T18-13, the second discharge valve 5
0-1 and stop the drive of the pump 51,
Stop reflux operation. Next, step 5TII3-1
In step 4, the first unit discharge flag is turned off, the first unit filter exchange flag is turned on, and the unit change request flag is turned on. After this, the process advances to step 5T17.

Next, after passing through steps ST+7 and 5T18, the process returns to step ST3 shown in FIG. 3(A).

By executing each of the above-mentioned steps, the dye aqueous solution jlk is purified in each processing unit) 42-1 to 42-3, and the heavy metal ions a melon are depleted (purified dye aqueous solution that has become below +rt!fk) is obtained in the storage tank 48.

(Effect) As explained above, according to the present invention, the present invention has a processing means for capturing heavy metal ions in a dye solution by performing ion exchange separation, and such an ion exchange method has been achieved. Since the operation of the processing means is controlled based on the concentration of metal ions in the dye solution, heavy metal ions can be reliably removed from the dye solution, resulting in inkjet recording ink, etc. Purified dye solution suitable for the preparation of
fk's! iA construction can be carried out 11] smoothly.

[Brief explanation of drawings]

FIG. 1 is a schematic block diagram of an embodiment of the device+vf according to the present invention, FIG. 2 is a block diagram showing the control section of the device shown in FIG. 1, and FIGS. 3(A) and (B) are 1 is a flowchart showing the purification operation of the apparatus shown in FIG. 1. 21... Dye supply unit, 22... Dye powder, 23... Dye/help, 24... Mixing tank, 25... Pure water valve. 26... Pure water supply pipe, 27... Preparation tank stirrer, 28... Preparation tank liquid level detector, 29... Filtration filter, 30... Dye solution supply/help, 31... Supply tank, 32... Supply tank liquid level sensor, 41... Purification unit, 42... Processing unit, 43... Co-coating valve, 44... Ion exchange resin column. 45 ...31゛, 48...Heavy metal ion 1 agricultural melon sensor. 47...Solution LFK sensor, 48...11) 1 output valve, 49...Storage tank, 51...Circulation pump, 52... Supply valve. 61...Control unit, 82...Operation unit. 101... Controller, 102... Read only memory, 103... Random access memory, 104... Switch, 105... Input/output 4727 circuit. 108...Display unit, 107...Drive circuit, +08...7 large cappuff circuits, 108...8 output 7 circuits. 110-114...Drive circuit. +21... A/D converter, 122... Input 4227 circuit, +23. +24,125...Drive circuit, 12B.
...Output puff circuit.

Claims (1)

[Scope of Claims] Means for producing a dye solution; means for treating a dye solution for trapping heavy metal ions during passage of the solution; and detecting the concentration of the heavy metal ions in a liquid effluent from the treatment means. , and operation control means for stopping the operation of the processing means based on the detected value. (Margin below)