JP3069599B2 - Preparation method of multi-component compound solution - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an automatic preparation of a compounding solution when a small amount of both powder and liquid are used as a compounding component and a plurality of components (including a single component) are compounded. And a method for quickly and accurately performing the method. It has a wide range of applications, such as automatic preparation of a dyeing dye bath for color matching tests with dyes, compounding of reagents in analysis, and automatic preparation of compounding solutions of pharmaceuticals.

[0002]

2. Description of the Related Art A method for automatically preparing a multi-component blended solution by mixing a powdery component and a liquid component has been demanded, but the technique has not been established and has not been carried out at all. The dyeing industry has the most advanced technology in this regard, but the preparation of the mother liquors of the respective component dyes is carried out semi-automatically even with the most advanced. The dye mother liquor prepared by the semi-automatic means is mounted on a dye bath automatic preparation apparatus generally called a color kitchen, and collected and blended by a dye mother liquor collection dispenser or siphon. Techniques related to the conventional color kitchen are disclosed in Japanese Patent Publication No. 58-12386 (Kurashiki Spinning), Japanese Patent Publication No. 60-18349, and Japanese Patent Publication No. 6-43663.
(Sumitomo Chemical Co., Ltd.) and Japanese Patent Publication No. 56-159342 (Nippon Xlan Industry Co., Ltd.), etc., and practical application is currently progressing in the dyeing industry. Since these techniques are mainly related to the dyeing industry, they will be described below with reference to examples relating to the dyeing.

[0003] These apparatuses (automatic dye bath preparation apparatus, color kitchen) are equipped with a mother liquor of a certain concentration of a large number of dyes (whether powder or liquid) prepared in advance by hand and controlled by a computer. The weighing and blending is performed by a volume method or a weight method using a dispenser or a siphon. A method for semi-automatically preparing a mother liquor of the dye used here and automatically preparing a dye bath for dyeing using this mother liquor is described in April 20, 1982.
"Microcomputer Application Research Report (JMA SpecialR) by Microcomputer Application Study Group issued by Japan Management Association
report No. Pp. 2753-65) ”in detail in comparison with the conventional manual operation method. This method is based on a "mechanism for roughly separating powdered raw materials", a "mechanism for precisely weighing the separated powder with the required accuracy" and a "mechanism for measuring the required amount of liquid from the weighed powder. And a mechanism for precisely injecting the calculated required amount of liquid with the required accuracy. These methods are semi-automatic methods, in which dyes roughly separated by a spatula or the like are automatically weighed, and then the mother liquor is automatically collected and blended in accordance with the formulation from the preparation of the mother liquor by the automatic dissolution dilution method. A method of preparing a dye bath for a dyeing test using an apparatus capable of performing the above operations under automatic control by a computer is described.

Although a method aiming at complete automation of this operation has been filed as Japanese Patent Application Laid-Open No. Hei 4-23208, it seems that the method mainly uses a semi-automated method using a spatula or the like. It seems that the method by the mechanism for automatically roughly separating the powder raw material has not been realized because it has not been clearly explained. Further, it can be said that an apparatus and a method which can be commonly applied to both powder dyes and liquid dyes usually called liquid are unfinished technologies. Therefore, at the present stage, there has not been developed a practical device for automatically and continuously processing the entire process from the preparation of the mother liquor to the preparation of the dye bath. The fact is that they are performed in separate devices. The semi-automated apparatus for preparing the mother liquor at the preceding stage is sold by some color kitchen manufacturers under the name of "mother liquor preparation apparatus" or the like.

Next, the biggest problem of the current color kitchen will be described. Dye mother liquors have been found to produce a 10-20% reduction in concentration upon storage for 2-3 days, even with dispersions of disperse dyes which are said to be very poorly stable. For this reason the mother liquor has to be re-prepared almost every day,
Since it is very troublesome to re-prepare dozens of dye mother liquors to be stored every day, it is necessary to directly use the dye of the weight corresponding to the formulation as a powder without storing the mother liquor. Development is coming. Examples of this type of method include JP-A-3-37525 (CIBA-GEIGY), JP-A-61-269022, and JP-A-63-27718, 277.
19 (Sumitomo Chemical), JP-A-7-225145, Japanese Patent Application No. 7
-329379 (applicant). However, in the case of the method of directly collecting the dye powder, the minimum collection weight is about 1 mg even under the best condition. In the case of a very light color in a dyeing test, a fineness of 1 mg or less is required, so that it may not be possible to completely cope with it. In addition, in order to precisely weigh and mix a minute amount of dye in the powder state, the number of corrections for adjusting the collection weight in the powder dye collection stage increases, so a combination of at least three components in one formulation If this is performed, three samplings and a finer weight adjustment step are required, so that it takes a long time for the sampling. For example, in the case where one combination group has 16 prescriptions and all the three primary color dyes are used, the total number of ejected samples is 3 × 16 = 48. Assuming that the weight correction operation is performed about five times for each sampling, 5 × 48 = 240, which is 240
It requires multiple sampling operations. In this case, even if the single discharge time is 20 seconds including the weighing time, the time required for collection is 20 × 240 = 4800 seconds, which is a long time of 80 minutes, which is inefficient. In order to improve this, it is necessary to select a method of reducing the number of times of collecting the dye in the powder form. For this reason, as a result of various studies, the inventors have invented that a new system by combining with a mother liquor system used in a conventional color kitchen is advantageous. In other words, for the individual dyes used, powder or liquid dyes are weighed and collected only once, thereby preparing a mother liquor, and then using this mother liquor to prepare a compound dyeing bath. is there. Also, in the method using mother liquor, a slight error in weighing and collecting is allowed, so that the collecting accuracy is 1 m as in the case of directly collecting powder dye.
A fine weight adjustment operation of not more than g is not required. For this reason, the number of weight corrections at the stage of collecting the powder dye can be significantly reduced. In addition, collection of the mother liquor is performed in a volumetric manner by a dispenser, so that collection and blending can be completed in a short time.

In the case of a liquid dye, droplets adhere to the opening of the discharge nozzle due to the effect of surface tension, and the minimum liquid collection amount is about 0.02 ml. Therefore, in the case of the direct measurement and sampling method, the minimum discharge amount is 20 mg. As described above, the method using the mother liquor of the present invention is most suitable because it is not suitable for minute precision sampling.

Further, in a conventional apparatus for storing a mother liquor (color kitchen), there is a method of preparing, storing and using a mother liquor of the same dye in a plurality of concentration steps (for example, 1% and 0.1%) having different solution concentrations. Has been adopted. Therefore, the number of mother liquors stored in the apparatus increases, the storage space of the apparatus increases, and the number of applicable dyes decreases drastically. Since the whole is large, it is extremely disadvantageous in terms of the device price, the installation area, and the like.

[0008]

A method of automatically preparing and storing a mother liquor which is easily degraded in a solution state such as a dye solution in advance and storing the mother liquor in advance has a problem in the stability of the mother liquor at present. It is considered to be an effective method because it has the highest liquid collection accuracy and the fastest preparation speed. However, considering the deterioration due to the aging of the mother liquor, this is quite restless and actually causes a large error. In addition, if a constant solution concentration (for example, 1%) is always fixed, it is impossible to cope with extremely light colors, and if it is forcibly used, the number of dyes that can be mounted will be drastically reduced. As a solution to this, if a method for automatically preparing the necessary concentration and the required amount of fresh mother liquor easily as needed in each dye bath preparation is developed as a solution to this problem, this method can be combined with a conventional apparatus to achieve this kind of solution. The disadvantages are eliminated at once and an ideal preparation method can be established. In addition, the dye to be collected can be used in both powder and liquid forms regardless of whether the dye is in the form of a powder or a liquid. It is also necessary to develop a method that can be freely selected in a wide range such as%.

[0009]

SUMMARY OF THE INVENTION The present invention uses a dye mother liquor used for compounding in order to improve the conventional mother liquor storage method which has been problematic due to the extremely poor stability of the dye mother liquor in a solution state. Immediately before, the required sampling weight is automatically determined according to the number of ingredients used, the amount used, and the required concentration of the dye bath preparation, and the mother liquor corresponding to only the combination group at this time is prepared immediately before the preparation of the dye bath. Establish a method. If the preparation of the mother liquor used for compounding can be performed very easily and quickly as needed, it is sufficient to prepare only the necessary kind of mother liquor when needed, as in the case of the color kitchen method conventionally used. Prevents generation errors due to incorrect use of mother liquor that has degraded and deteriorated due to aging due to long-term storage.For components with very low frequency of use, it is necessary to prepare only when necessary. The inefficiency that wasteful repetition of re-preparation of the mother liquor of a dye that does not occur can be prevented.

As described above, since the system in which fresh mother liquor is always prepared and supplied as needed can be easily implemented, the disadvantages of the conventional color kitchen system can be solved at once. In order to achieve this, it is necessary to establish a technology that accurately separates a certain weight within a practically acceptable error range, rather than simply roughly collecting a fixed weight at the initial dye separation stage as in the conventional method. is there. If it can be collected accurately, the concentration of the prepared mother liquor can be given in a wide range of concentration levels such as 1%, 0.1%, 0.01%, etc., and it is used immediately after preparation. Not only is it not affected by the decomposition of the mother liquor, but also has the effect of significantly improving the collection and blending accuracy of the mother liquor. If this technology is established, it will be possible to efficiently prepare a multi-component mixed solution in combination with the mother liquor collection mechanism of a conventional mother liquor storage type color kitchen.

[0011]

According to the present invention, a mother liquor having an optimum concentration is always prepared for each component corresponding to a formulation by using a powdery or liquid component (dye, etc.), and the influence of a change over time is always obtained. Since it is possible to prepare a compound solution using a fresh mother liquor that has not been subjected to the treatment, the efficiency and accuracy of the preparation operation of the compound solution mainly in a laboratory can be greatly improved.

[0012]

FIG. 1 is a longitudinal sectional view of a container for measuring and discharging a powdery dye used in the present invention. At the center of the container, a multi-stage measuring shaft 1 in which the volume of the recessed space 2 increases stepwise as it advances vertically from the lower end to the upper end is mounted so as to be reciprocally driven in the vertical direction. In this embodiment, the recessed space 2 has five spaces and the space volume is sequentially 0.00 from the lower end.
1 ml, 0.005 ml, 0.025 ml, 0.125
ml, 0.625 ml, the volume ratio in one stage is 5
It is designed to double. The multi-stage measuring shaft 1 is shown in FIG.
The reciprocating drive based on the projecting length corresponding to the discharge capacity and the number of times of driving is provided by the vertical movement driving devices 34 and 35 located above the outside as shown in FIG. When the multi-stage measuring shaft 1 is located at the top dead center in the discharge container, the powder dye dispersed by the agitating brush 3 is supplied to each of the concave spaces 2. The total volume of all recessed spaces is 0.781 ml, and when one reciprocating drive is performed at the maximum stroke, about 0.3 g of a dye having a bulk specific gravity of 0.4 is discharged. When 500 ml of a dye mother solution having a solution concentration of 1% is prepared, it is necessary to discharge 5 g of the dye. Therefore, the entire recessed space of the multi-stage measuring shaft 1 has a drive width that protrudes to the outside. Approximately 5 g of dye is cut out and discharged
become. 0.5 g for preparing 0.1% mother liquor
Since the volume is 1.25 ml, one full width drive of five steps is performed once (0.781 ml) and 4
If the drive of the width up to the stage is performed three times (0.468 ml), the total volume becomes 1.249 ml, and the purpose is achieved. It is recommended that an excess of about 20% be taken in consideration of the loss in the preparation step of the actual compounding solution. Further, these recessed spaces do not need to be provided in five stages, and can be manufactured by appropriately changing the space according to the collection capacity range and the required collection accuracy.

Further, since the bulk specific gravity of the powder changes at that time, the discharge weight actually fluctuates. Therefore, the discharge weight must be confirmed by weighing it with an electronic balance for confirmation.
If the result of weighing is insufficient, correct ejection is performed to replenish the insufficient amount. If the concentration is excessive, the concentration of the mother liquor becomes high. Therefore, a correction factor relating to the concentration of the solution is obtained to adjust the amount of mother liquor to be collected at the time of preparing the blended solution. In this way, it may be considered that a shortage of about 10% is allowable in the case of preparing a mother liquor.

The most problematic problem when handling powder is the solidification phenomenon. When the solidification occurs, the powder cannot be discharged, and the device stops functioning. As a countermeasure, this embodiment employs a method in which the stirring brush 3 in the container is rotated by magnetic force induction from the outside of the container to re-disperse the solidified powder around the concave space 2 of the multi-stage measuring shaft 1. Has adopted. That is, a method in which the outer coupling magnet 4 is rotated and the opposing inner coupling magnet 5 is rotated by magnetic induction, and the stirring brush 3 is provided on the inner surface of the hollow shaft 6 to which the inner magnet 5 is attached. Hair transplanted. Thus, the depressed space of the multi-stage measuring shaft 1 is always cleaned and the dispersed powder is supplied.

FIG. 2 shows the structure of a liquid dye discharge container. The shape and dimensions of the container are the same as those of the powder discharge container, so that they can be used in a common transfer device. 1
Reference numeral 1 denotes a liquid storage container, at the lower part of which a discharge pump by a cylinder 12 is attached. The lid 13 has a vertically moving stirrer 1 which returns to a top dead center by the action of a spring 14.
5 is attached. The drive units 34 and 35 of the multi-stage measuring shaft in the container for measuring and discharging the powder dye also serve as a vertical driving device of the stirrer 15. The liquid dye stored is homogenized by this vertical stirring action.

The discharge pump provided at the bottom has two check valves 1
A reciprocating piston system for sending liquid downward by means of 6, 17 passes through a liquid passage 19 through the center of a piston 18, and the discharged liquid moves downward through it and is discharged. The piston 18 is made of a ferromagnetic material, and discharges the liquid dye corresponding to the sampling volume by driving the external driving cylindrical magnet 20 up and down with a width corresponding to the discharging volume. The lower end of the piston 18 is configured to allow the liquid to flow in the lateral direction, and the tip of the lower end is conical so that it can be in close contact with the discharge port of the cylinder. Shut off, leaking liquid,
Evaporation is prevented, and the tip of the discharge port at the lowermost end of the cylinder portion is tapered, and the conical portion at the bottom of the piston 18 is combined to form a sharp point, so that the liquid runs out well and the The accumulation and adhesion are minimized. In this discharge pump, the driving cylindrical magnet 20 is driven by the control of a pulse motor 36 in a vertical linear motion device 38 shown in FIG. By adjusting the vertical drive width of the linear motion device 38 in accordance with the amount of the collected liquid and driving the linear motion device 38, an arbitrary volume of liquid dye can be discharged. In this embodiment, the structure is simplified by adopting a system in which the linear motion device 38 is shared with the powder discharge container.

FIG. 3 shows the powder dye discharge containers 30, 30 'and the liquid dye discharge containers 31, 31' used in this embodiment.
Shows a mechanism for discharging, collecting, and weighing a dye. A dual-axis drive system in which two turntables are used for the transfer device (A) 32 for mounting each dye discharge container and the transfer device (B) 48 for mounting the collection container 41, and these are independently and individually driven to rotate. 1 shows a basic configuration employing the above. A large number of dye discharge containers 30 and 31 containing dye are attached to the transfer device (A) 32 at predetermined addresses. In this embodiment, a discharge container for powder dye and a discharge container for liquid dye are mixed, and a discharge container 31 for liquid dye is mounted inside a turntable 32 and a discharge container 30 for powder dye is mounted outside. . In FIG. 3, the discharge container 3 for powder is located at the dye collection position.
The state where 0 is located is shown. When the discharge container 31 for liquid is used, the inner discharge container is slid outward by the extrusion device 49 using an air cylinder. By employing such a structure, the number of dyes accommodated in the turntable (A) 32 can be doubled. In this embodiment, each of the inner and outer layers 16
Since the dyes of the items are mounted, 32 items can be mounted.

A drive unit 3 for vertical movement is provided above the sampling position.
4 and 35 are provided, and the multi-step measuring shaft 1 shown in FIG. 1 is driven by a vertical movement width according to the volume of the collected powder to perform the metering and discharging of the powder dye, and the liquid dye shown in FIG. The two functions of driving the stirring device 15 to stir the liquid dye are provided. This vertical drive device is an air cylinder 3
4 and four cam blocks 35 for setting the drive width. By selecting a cam block for setting the stroke width of the air cylinder 34 corresponding to the sampling volume and extruding it in the direction of the drive shaft to serve as a stopper for the air cylinder, dye sampling at an arbitrary volume level is possible. In the case of powder dye, coupling magnets 4, 5 are used to prevent solidification.
The stirring brush 3 is rotated to stir the inside of the container, and the stirring power is transmitted by two pulse motors 36,
This is performed by a lifting / lowering stirring device 38 using 37. First, the ball screw 3 rotated by the pulse motor 36
The rotation device 45 to which the coupling magnet rotating pulse motor 37 is attached is raised by 9 to connect the clutch of the coupling magnet, and then the pulse motor 37 rotates for stirring. As a result, the solidified powder around the concave space 2 of the multi-stage measuring shaft 1 is redispersed and supplied to the concave space 2 of the shaft. In this state, by operating the air cylinder 34, the powder dye corresponding to the stepwise capacity of the recessed space is cut out and discharged into the sampling container 41 below.

The discharged powder dye is transferred to a collection container 41 at a collection position by a turntable (B) as a transfer device.
The sample is collected by a collection container 41 which is being conveyed to a collection position by 40. An electronic balance 43 for measuring the weight of the collected dye including the collection container (corresponding to a tare) 41 below the collection position of the turntable (B) 40.
And is mounted on the lifting device 42. First, when the collection container 41 is conveyed to the collection position and fixed, the electronic balance 43 is lifted by the elevating device 42 and pushes up the collection container 41 from below to perform tare weighing. Then, the weight of the discharged dye is measured. If the weight of the discharged dye does not reach the target value, the correction discharge is repeated until the weight reaches the target value.

In the present embodiment, the liquid discharge container 31 is located inside the discharge container transfer turntable 32. Therefore, the liquid discharge container 31 is pushed out by the pushing device 50 at the collection position of the turntable and replaced with the outer powder discharge container 30. I do. Since the discharge containers 30 and 31 at the same rotation angle position of the turntable are attached to the common slide holder 44, the discharge container 30 for powder is naturally pushed out of the turntable. Next, in a state where the rotation of the coupling magnet rotating device 45 attached to the elevating device 38 which moves up and down by the pulse motor 36 is stopped, the coupling magnet rotating device 45 is raised and the point of contact with the magnet 46 is used as a reference point for the liquid dye to be collected. The liquid dye corresponding to the target weight is ejected by repeating the vertical drive with setting the rise / fall width corresponding to the capacity. Since the piston type pump installed at the lower part of the discharge container 31 for the liquid dye can set the discharge amount by a pulse motor by a continuous value, the reciprocating drive width and the number of times of driving of the piston 18 shown in FIG. Can be done easily.

When the discharge and collection of one dye are completed, the turntable 32 for the discharge container is driven to send the next dye discharge container 30 or 31 to the collection position, and the lower turntable 40 for transferring the collection container at the lower position. To transfer the collection container 41 to the next collection position (usually an adjacent position). The next component is collected at this position. This operation is repeated to complete individual sampling of all components contained in the formulation.

When the discharge and collection of all the dye components used in the compounding group are completed, the process proceeds to a mother liquor preparation step by dissolution and dispersion. Normally, it is desirable to use another device adjacent to this operation.
It is not impossible to share one transfer device (B) 40. Here, a method using a separate transfer device will be described. Turn the collection container 41 from the collection position to the turntable 40
Extrusion device 4 at a position where it has rotated a half turn (180 °)
9 and is slid and conveyed to an adjacent dissolution transfer device (C) 48. On the dissolving transfer device (C) 48, a collection container for all the dyes used in the grouping is mounted according to the collection order.

When the transfer is completed, preparation of a mother liquor is carried out, and then a mother liquor corresponding to the compounding prescription is entered and a mixed solution preparation stage is started. FIG. 5 illustrates this operation. Each collection container containing the discharged and collected dye is a mother liquor transfer device (C) 4
8 each time the full-scale capacity is 100
Using a large-sized dispenser 70 ml, a certain amount of solvent is injected to dissolve and disperse to prepare a mother liquor. In this case, for example, when preparing 500 ml of mother liquor, a method is used in which the dispenser 70 is operated five times to inject the mother liquor. In the case of a water-soluble dye as a solvent, first add 100 ml of hot water to dissolve it, then add 400 ml of cold water.
The concentration of the solution is adjusted by adding ml to a predetermined liquid volume (500 ml). In addition, for a disperse dye which does not dissolve in water and is in a dispersed state, first, cool water with 100 m
l, wet, stir and disperse, then 400m of cold water
1 to make the total volume 500 ml.

In this case, since the solution concentration of the mother liquor may slightly fluctuate due to a sampling error of the dye, the correction factor is set by obtaining the ratio of the actual sampling weight to the target sampling weight.
This correction factor is used to finely adjust the amount of mother liquor to be collected in the next mother liquor collection and blending stage. In the case of liquid dyes, a certain amount of solvent is added and dissolved,
Is performed, the capacity increases due to the effect of the liquid component contained in the liquid dye, so a correction coefficient for this is also required. Since the collection container is sequentially sent from the collection transfer device (B) 40 on the right side of FIG. 3 to the mother liquor transfer device (C) 48, the preparation of the mother liquor is performed sequentially in this order. When the preparation of the mother liquor has been completed for all the containers, the next step of collecting and mixing the mother liquor is started.

The mixed solution preparation container 75 is sequentially conveyed to the mother liquor pouring position by the transfer device (D) 49 for the mixed solution preparation container. Inject into the preparation container. FIG. 4 shows a typical configuration of the auto dispenser used at this time. This is a normal type dispenser 60 having a capacity matching the mother liquor collection scale, an air cylinder 65 for driving the stroke width of the piston of the dispenser in accordance with the amount of collected liquid, a stopper 66 for setting the amplitude of the air cylinder 65, It is composed of a pulse motor 63 for controlling the rotation of a screw 64 for positioning the stopper 66 and the like. As the dispenser 60, it is desirable to use a plurality of dispensers having different full-scale capacities and to be appropriately switched depending on the range of the sampling amount. For example, the operating full-scale capacity of the piston 67 is 5 ml using two kinds of 10 ml and 1 ml. A 10 ml dispenser is used for the above sample volume, and a sample having a full-scale capacity of 1 ml is used for a sample volume of 5 ml or less.

FIG. 5 shows the steps from preparation of a mother liquor to preparation of a compound dyeing bath using the auto dispenser shown in FIG. The method for preparing the compound dyeing bath will now be specifically described. A large dispenser (full scale 100 ml) 70 for preparing mother liquor and a small capacity dispenser (10 ml) 72 for collecting dye liquor mother are provided in the apparatus. A collection container 41 from which dyes of a necessary weight are collected from the dye discharge containers 30 and 31 is turned into a mother liquor turntable (C) 4 from a transfer container turntable (B) 40.
8 sequentially. A dispenser 70 for injecting a diluting solvent for preparing a mother liquor includes a solvent tank (usually water or hot water) 7.
A solvent necessary for dissolution and dispersion is collected from 1 and injected into the collection container 41 via a nozzle 74 by switching a two-way electromagnetic valve 73 for switching between a mother liquor container and a compound solution preparation container 75.
Although not shown here, a stirrer such as a magnetic stirrer is used. In this embodiment, the dispenser 70 for preparing the mother liquor is 100 ml full-scale, so that the dissolution and dispersion are performed by repeated driving of five full scales to prepare 500 ml of the mother liquor. As described above, the injection pipe 74 of the dispenser can be selected from two paths, that is, the mother liquid injection pipe 74 and the injection pipe 76 of the blended solution preparation container 75 by the two-way solenoid valve. At this stage, the correction coefficient for the increase in the liquid amount due to the actual dye collection weight and the liquid dye volume has already been obtained.

When the injection of the solvent into all of the collection containers 41 is completed and the mother liquor is prepared, the stage for preparing the actual dye-containing solution is started. Here, it is assumed that the inside of the dispenser 72 for collecting mother liquor has already been washed. The dye mother liquor is selected and transported to the sampling position according to the control of the computer for the formulation, and the residual water is first removed from the cylinder of the dispenser 72 by co-washing. For this purpose, the mother liquor sampling pipe 77 penetrating through the washing pipe 76 is pushed out and the tip is inserted into the mother liquor 41. This is the mode of sample collection and co-washing in the state of A. The dispenser 72 sucks the mother liquor through the mother liquor sampling pipe 77. In this co-washing mode, the discharge port 83 of the dispenser 72 is connected to the
8 position. By reducing the stroke of the piston of the dispenser 72 and repeatedly operating it several times, the water in the cylinder of the dispenser 72 is removed and replaced with the mother liquor in perfect condition. Upon completion of the co-washing, the piston is set to the position of the sampling volume 0 by the action of the air cylinder 65. Next, the stopper 6 is driven by the pulse motor 63 and the screw 64 described with reference to FIG.
Adjust the position of 6 to set the amount of liquid to be collected and set the air cylinder 6
Activate 5 to perform sampling / injection. In this case, the amount of liquid taken in one stroke is an evenly divided value of the amount of liquid taken according to the prescription of the dye at this time, and a value as close as possible to the full-scale capacity of the dispenser. For example, when collecting a mother liquor of 48 ml using a dispenser having a full-scale capacity of 10 ml, the amount of the mother liquor is set to 8 ml and the operation is performed six times.

It is efficient to inject the mother liquor in a manner that one dye mother liquor is sequentially and continuously injected into a compounding solution preparation container of a formulation requiring the dye. That is, while the mother liquor transfer turntable (C) 48 makes one rotation at the maximum, the compounding solution preparation container rotates by the number of dyes used for the compounding at this time. In this manner, the number of times of cleaning / co-washing of the dispenser can be minimized.

When a common dispenser 72 is used for each dye as in the method of the present invention, when the dye to be collected is changed, the dispenser 72 used for the previous dye is used.
When is repeatedly used for the next other dye (so-called color change), it is necessary to wash the inside and to wash the remaining washing water with the next dye mother liquor. Something is needed to do it. The method of washing and co-washing in switching the mother liquor will be described with reference to FIG.

In FIG. 5, mother liquor 41 is sequentially mounted on a turntable (C) for transferring mother liquor. The mother liquor sampling tube suction 77 for collecting the mother liquor penetrates through the inside of the washing tube 76, and is mounted so as to slide in the washing tube 76 in the direction of this tube. The pipe is attached at an angle so that it can be inserted into the mother liquor 41 from an oblique direction. Also, a sponge-like lid 79 is provided at the lower opening of the washing tube.
In the center, there is a hole through which the pipe can slide, so that even if washing water flows into the washing pipe 76, it does not jet downward. Further, the lid 79 attached to the lower part of the washing pipe 76 has the outlet of the sponge-shaped lid (the outlet of the suction nozzle) outside the opening of the mother liquor container 41 because the washing pipe 76 is obliquely attached. The washing water thus dropped does not mix with the mother liquor. A water supply pipe 80 is attached to a lower part of the washing pipe 76, and a drain pipe 81 is attached to an upper part of the washing pipe 76 to circulate washing water. A rubber pipe 82 is attached to the upper part of the mother liquid sampling pipe suction 77 and is connected to a suction port 83 of a dispenser. When two or more dispensers having different full-scale sampling capacities are used in combination, they are connected to a common inlet of a suction branch pipe.

When the co-washing with the mother liquor, the collection of the mother liquor, and the injection are completed for all of the compounding containers requiring the dye, the inside of the dispenser is washed for the next dye. In the cleaning mode, the discharge port 83 of the dispenser is placed on the drain port 78, and the mother liquid collection pipe 77 is pulled up from the mother liquid to remove the pipe 7.
The suction port at the tip of 7 is drawn into the washing tube 76. This state is B in FIG. Cleaning water is injected from a lower water inlet 80 of the cleaning pipe 76 and drained by overflow from an upper drain 81. In this state, the dispenser 72 is repeatedly operated at full scale to clean the inside, the mother liquor 41 to be collected next is transferred to the collection position, the injection port of the dispenser 72 is switched to the drain port 78, and the washing is returned to the co-washing mode. This operation is sequentially repeated to advance the preparation of the compounding dye bath. As a result, the entire process of collecting the dye, preparing the mother liquor, and preparing the compound dyeing bath is automatically and continuously performed.

The injection of the mother liquor into the compounding solution preparation container 75 is sequentially performed for the compounding solution preparation container 75 that requires one dye, and when the dye is completed, the mother liquor transfer device (C) 48 is operated. The most efficient method is to switch to the next mother liquor 41 and sequentially inject the dye into the necessary compounding solution preparation container 75 for preparation.

After the injection of the mother liquor of the volume corresponding to the prescription into all the compounding solution preparation containers 75 is completed, the solvent (water or the like) for adjusting the whole liquid amount is injected to complete the preparation.
In this case, the flow path of the dispenser 70 for preparing mother liquor is switched to the side of the blending solution preparation container 75 by the electromagnetic valve 73, and injection is first performed in units of 100 ml, and if the amount is less than 100 ml, the mother liquor sampling pipe 77 is pulled up to dispenser 72. Is set to the washing mode, water is circulated through the washing tube 76, and the injection tube of the dispenser is positioned on the side of the blended solution preparation container 75, and water for fine adjustment is added to adjust the necessary liquid amount.

[0034]

As described above, the method for preparing a multi-component compound solution according to the present invention enables the compounding operation on a laboratory scale to be performed rapidly and with high accuracy, regardless of whether the compounded component is a powder or a liquid. It is possible to completely automate. The conventional apparatus method had a major problem that the mother liquor to be stored had to be re-prepared with enormous effort to avoid the influence of aging, but this problem was solved and used for compounding. Since the optimum concentration of the mother liquor can be freely selected according to the level of the sampled amount, it exhibits the characteristic that it can accurately handle extremely small amounts of blending. Also, unlike conventional color kitchens, there is no need to store mother liquor in multiple solution concentration stages, such as high-, medium-, and low-concentration solutions at all times. The cost can be reduced as well. As a result, most of the problems of the conventional device could be solved.

[Brief description of the drawings]

FIG. 1 is a longitudinal sectional view of a container used for the present invention for storing a powder component and discharging a powder of an arbitrary volume;

FIG. 2 is a longitudinal sectional view of a container for storing a liquid component and discharging a liquid of an arbitrary volume used in the present invention.

FIG. 3 is a diagram illustrating a mechanism for adjusting the discharge weight by discharging and weighing the amounts required for preparation of a mother liquor for a powder component and a liquid component into a collection container, It is a front view of the part of the mechanism which performs the process until the collected collection container is transferred to the mother liquor preparation mechanism.

FIG. 4 is a diagram illustrating the configuration of an auto-dispenser as an automatic dispenser used for injection for collecting and mixing a mother liquor and for injecting a solvent for finely adjusting the amount of a mixed solution according to the present invention.

[FIG. 5] In the present invention, steps from preparation of a mother liquor to collection of a mother liquor, injection for blending, washing of a dispenser after collection of the mother liquor, co-washing with the mother liquor, and adjustment of the amount of the blended solution by solvent injection are automatically continued. FIG. 5 is a diagram for explaining an operation sequence performed by the user.

[Description of Signs] 1 ... Multi-stage measuring shaft 2 ... Recessed space of multi-stage measuring shaft 16 ... Suction-side check valve of measuring pump for micro-discharge of liquid discharge container 17 ... Same as above Top Discharge-side check valve 18: Magnetically actuated piston of metering pump for minute discharge of liquid discharge container 30: Powder discharge container 31: Liquid discharge container 32: Transfer device for discharge container ( A) 34 ... Air cylinder of discharge driving device 35 ... Cam block for setting drive width of multi-stage measuring shaft of discharge driving device 40 ... Transfer device of sampling container (B) 41 ... Collection container 43: Electronic balance 46: Measuring pump for discharging a minute amount of liquid 48: Transfer device for mother liquor (C) 49: Transfer device for mixed solution preparation container (D) 70: Injection for preparation of mother liquor Apparatus (100ml dispenser) 72 ・ ・ ・ Data for collecting mother liquor Spencer 75 ... compound solution preparation vessel 76 ... dispenser cleaning washing pipe 77 ... mother liquor solution sampling piece pipe 78 ... water drainage portions 83 ... mother liquid injection pipe

Claims (4)

(57) [Claims] (1) a plurality of individual measuring and discharging containers having a mechanism for storing individual components of powder and liquid used in the compounding preparation and discharging an arbitrary sampling volume by external driving;
A discharge container transfer device (A) which mounts these at a unique position and transports them to a collection position by control, and mounts a number of collection containers corresponding to the number of prescriptions to be prepared at a unique position, and selects any of these A transfer device (B) for selecting a collection container by control and transporting it to a collection position, a driving device for discharging a component having a capacity approximately corresponding to the collection weight from the measurement discharge container at the collection position, and a transfer device (B). Using a weighing device that accurately measures the weight of the components discharged and collected in the collection container using an electronic balance at the collection position, first discharge an approximate amount by the volume collection method, and the collected weight is reduced to the specified weight If this is not the case, each component commonly used in the formulation of one preparation group can be individually and accurately collected individually by means of adjusting the discharge to a predetermined sampling weight by repeating the discharge for correction. The first step to be weighed collected. (A) A means for sequentially transporting the collection containers containing the weighed and collected components to the mother liquor transfer device (C) for preparing a mother liquor, and controlling the solvent collection by controlling these collection containers for the mother liquor preparation. Mother liquor transfer device (C) for transporting to additional position
And a second step of preparing a mother liquor of each component using a solvent injection device for preparing a mother liquor by injecting a predetermined amount of a solvent required for preparing a mother liquor at a solvent injection position. (C) A transfer device (D) that mounts a plurality of compounding solution preparation containers corresponding to the number of compounding prescriptions at a unique position and conveys it to a mother liquor collection and pouring position by control, and a co-washing with the mother liquor at the mother liquor collecting and pouring position First, the inside of the mother liquor sampling dispenser is provided with a mother liquor sampling dispenser, which is provided with the functions of measuring and collecting the mother liquor, injecting it into the blended solution preparation container, and washing the wetted part after collection. After the co-washing is performed, a third step of accurately collecting a mother liquor in a volume required for preparing a blended solution and injecting the mother liquor into a blended solution preparation container. (D) After the collection and injection of one mother liquor is completed, the piping system of the mother liquor dispenser is switched to a washing mode, and the suction and discharge operations of the washing liquor are repeated to wash the mother liquor dispenser. Next, the discharge pipe of the dispenser is switched to the side of the blending solution preparation container to inject the diluting solvent, and the means for adjusting the volume to a predetermined volume prepares a multi-component blending solution that matches the blending recipe. Four stages. A method for preparing a multi-component blend solution comprising the above first to fourth steps. 2. In the first step, when a powder having a volume approximately corresponding to the sampled weight is discharged from a powder discharge container for storing powder components, a plurality of steps are provided in a lower part attached to the inside of the container. Using a multi-stage measuring shaft that reciprocates up and down by driving from the outside on a shaft provided with a concave space having a different space capacity, and by setting the combination of the protruding length of the shaft and the number of reciprocating drivings, 2. The method for preparing a multi-component blend solution according to claim 1, wherein a powder discharge container provided with a structure for cutting out and discharging a volume of powder components to the outside is provided. 3. In the first step, when discharging an arbitrary amount of liquid from a liquid discharge container for storing a liquid component,
At the lower part of the discharge container, a small-discharge metering pump in which a small-diameter piston is reciprocated by an external magnetic force is installed, and a check valve that allows liquid to pass only in the discharge direction is installed inside the piston. 2. The multi-component mixed solution according to claim 1, wherein a reciprocating drive width is set by control, and a liquid discharge container that discharges a required volume of liquid component by setting a combination of the reciprocating drive width and the number of reciprocating driving times is prepared. Method. 4. A dispenser for collecting mother liquor, wherein a suction port of the dispenser is controlled to control a mother liquor side and a solvent side.
Further, the inlet is switched between the side of the blended solution preparation container and the outlet, and the mother liquor sampling pipe connected to the suction port is provided inside the cylindrical washing pipe attached at an oblique angle. (E) mother liquid liquor collection; the fifth step includes the fifth step and the sixth step below the third step; and the fourth step includes the seventh step below. Fifth step in which the liquid tube is pushed out of the washing tube for dispenser washing, inserted into the mother liquor, the portion of the mother liquor injection tube is positioned in the drainage portion, and the dispenser is actuated several times to perform co-washing. (F) Place the mother liquor injection tube at the injection position on the blending solution preparation container, insert the mother liquor sampling tube into the mother liquor, and operate the dispenser to collect the correct volume of mother liquor corresponding to the blending prescription and the blending solution. The sixth step of sequentially injecting into the preparation container and blending. (G) The suction port at the end of the mother liquor sampling tube is retracted to a position where the washing liquid inside the washing tube can be sucked, the mother liquor injection tube is positioned on the drain port side, and the dispenser is supplied while supplying the washing solution into the washing tube. Is operated to repeat the suction and discharge of the washing liquid to completely wash and remove the residual mother liquor remaining in the dispenser at the time of the previous sampling. The fifth to seventh steps are repeatedly executed by the number of times corresponding to the number of components used in the blending, so that the dispenser commonly used for all components can be washed and used each time the blending components are switched. A method for preparing the multi-component solution according to claim 1.