JPH0716593B2 - Preparation method - Google Patents

Description

TECHNICAL FIELD The present invention relates to a liquid preparation method for preparing liquid dyes, auxiliaries, and various other types of chemical liquids to a measurement set value.

[Conventional technology]

Conventionally, a method shown in FIG. 6 has been proposed as a method for accurately adjusting a chemical solution in a short time while performing feedback control. This method is a method in which a large quantity continuous supply Q1 by a large quantity supply solenoid valve, a small quantity continuous supply Q2 by a small quantity supply solenoid valve, and a small quantity intermittent supply Q3 are supplied up to a measurement set value Q in three stages.

This method aims to shorten the time by continuous supply at the beginning of chemical liquid supply, and switches to intermittent supply when the measured set value is approached,
The purpose is to improve the supply accuracy.

[Problems to be Solved by the Invention]

However, in this conventional method, since the supply interval time of the minute amount intermittent supply can be performed only at a predetermined constant time interval, if the opening time of the minute amount supply solenoid valve is shortened, it becomes drip supply, If the open time of the small amount supply solenoid valve becomes longer on the contrary, the supply time becomes longer, but the supply time becomes shorter, but the problem that the quantity exceeds the set value during the supply of the chemical solution and the quantity becomes excessive, causing There was a limit to increase the supply accuracy to the.

Furthermore, since the viscosity of the chemical liquid varies depending on the type and concentration, and also changes depending on the temperature, the amount of chemical liquid actually supplied is not the same in intermittent supply even if the opening time of the small amount supply solenoid valve is constant. The actual condition is that the supply accuracy is worse than it is on the desk, because it depends on the type, concentration, and temperature.

An object of the present invention is to provide a liquid preparation method capable of significantly shortening the supply time and improving the supply accuracy as compared with the conventional method.

[Means for Solving the Problems]

The liquid preparation method of the present invention, each section supply time in the intermittent supply of the chemical solution so as to be able to respond to the change in the viscosity of the chemical solution, as the measured weight value of the supplied chemical solution approaches the measurement set value,
By constantly performing feedback control so that the solution becomes gradually shorter, the time for supplying the chemical solution and the improvement of the supply accuracy are realized.

According to the liquid preparation method of claim (2), the measured weight value is continuously supplied until it reaches a predetermined switching value, and after reaching the switching value, intermittent supply is switched.

The liquid preparation method according to claim (3) is the method according to claim (2), in which two large and small supply paths are provided, and both supply paths are opened until the measured weight value reaches the switching value, and the switching value is changed. When it reaches, the large supply route is closed and the small supply route is used for intermittent supply.

According to the liquid preparation method of claim (4), in the method of claim (2), the weight of the supplied chemical liquid is sampled at regular intervals, and a sampling amount Δ which is a difference between sampling values before and after.
The product ΔW · α of W and the coefficient α is calculated. This product ΔW · α
The switch value correction value W _SVP ′ of W _SVP ′ = W _SV −ΔW · α obtained by subtracting from the measurement set value W _{SV is} set as the switch value from continuous supply to intermittent supply.

In the liquid preparation method of claim (5), in the method of claim (4), sampling is started after a certain start delay time has elapsed after the start of supply.

According to the solution preparation method of claim (6), in the method of claim (5), the switching value W _SVP is a value of (W _SV −Z) obtained by subtracting a fixed value Z from the measured set value W _SV . Further, when the measured weight value reaches the switching value W _SVP before the start delay time for starting the sampling, the switching value correction value W _SVP ′ due to sampling is not calculated and switching is made to intermittent supply.

In the liquid preparation method according to claim (7), when the switching value W _SVP is zero or a negative value in the method according to claim (6), intermittent supply is performed only from the small supply path from the start of the supply.

[Work]

According to the method of the present invention, the segmental supply time of the intermittent supply is long at first, and becomes shorter as it approaches the measurement set value.
Initially, the supply amount per unit time is large, and the supply amount per unit time decreases as the measured set value is approached. Therefore, it is possible to shorten the entire chemical liquid supply time and improve the supply accuracy.

According to the liquid preparation method of claim (2), the supply speed is increased by continuous supply until the switching value is reached to shorten the supply time, and the accuracy is improved by intermittent supply after the switching value is reached.

In the liquid preparation method of claim (3), the time is further shortened by continuous supply through two large and small supply paths, and intermittent supply is performed by the small supply path to improve accuracy.

According to the liquid preparation method of claim (4), one sampling amount ΔW
In other words, the switching value from continuous to intermittent is corrected in accordance with the above, that is, in accordance with the viscosity of the chemical solution to be supplied.

In the liquid preparation method of claim (5), sampling is started after a period of unstable measured weight value immediately after the start of supply.

The liquid preparation method according to claim (6) is such that when the measured set value is small and the measured weight value reaches a predetermined switch value before the start delay time for starting sampling, the switch value correction value by sampling. Switch to intermittent supply without calculating.

According to the liquid preparation method of claim (7), when the metering set value is smaller and the switching value obtained by subtracting the fixed value Z from the metering set value is zero or a negative value, the small supply path is started from the start of the supply. Make intermittent supply only.

〔Example〕

An embodiment of the present invention will be described with reference to FIGS. FIG. 5 shows a liquid preparation device for carrying out this liquid preparation method. A circulation path 3 having a pump 2 is piped in the chemical solution tank 1, and a large supply path 6 and a small supply path 7 for supplying the chemical solution to a container 5 on the electronic balance 4 are provided branching from the circulation path 3. The chemical liquid tank 1 has a float switch 1a.
A large metering valve SV1 and a small metering valve SV2, which are electromagnetic valves, are provided on the large supply path 6 and the small supply path 7, respectively.
A valve control device 8 for controlling opening / closing of SV1 and SV2 is provided. The measurement control device 9 is composed of a computer, performs a predetermined calculation from the measured value of the electronic balance 4, and outputs a control signal to the valve control device 8.

This liquid preparation method takes three patterns, that is, a regular measurement pattern shown in FIG. 1, a small measurement pattern shown in FIG. 2 and a minute measurement pattern shown in FIG. For example, when the regular weighing pattern is 70 g or more (up to 2000 g), the small amount weighing pattern is 60 to 70 g, and the minute weighing pattern is 60 g or less.

1 to 3, (A) shows the relationship between the supply amount and time, the shaded portion of (B) shows the open period of the large metering valve SV1 (Fig. 5), and the shaded portion of (C) shows small. The open period of the metering valve SV2 is shown.

An outline of the regular weighing pattern of FIG. 1 will be described. Predetermined switching value correction value W for switching from continuous supply to intermittent supply
Both large measuring valve SV1 and small measuring valve SV2 are opened until _SVP '(switching point P') is reached. When the switching value correction value W _SVP ′ is reached, the large metering valve SV1 is closed and the small metering valve SV2 is repeatedly opened and closed to perform intermittent supply. In this case, each segment supply time T ₀ is gradually shortened. The switching value correction value W _SVP ′ is a value corrected according to the viscosity of the chemical liquid with respect to the switching value W _SVP fixedly set as described later. In order to calculate the switching value correction value W _SVP ′, the weight of the supplied chemical liquid is sampled in a constant sampling period T ₁₁ . Sampling starts from the sampling start point S when a predetermined start delay time T ₁₀ has elapsed after the start of supply.

The small amount measurement pattern in FIG. 2 is a case where the supply amount reaches the switching value W _SVP by the time when the sampling start delay time T ₁₀ elapses due to the small measurement setting value W _SV , and intermittent supply is performed without sampling. Switch.

The micro-measurement pattern of FIG. 3 is a case where the measurement set value W _SV is even smaller and the switching value W _SVP becomes zero or a negative value, and intermittent supply is performed only by the small metering valve SV2 from the start of supply. .

FIG. 4 is an overall flowchart of this liquid preparation method.
Hereinafter, this liquid preparation method will be described with reference to FIG. In addition,
A and B separated by a chain line indicate a continuous supply process and an intermittent supply process, respectively.

First, enter the measured set value W _SV of the chemical to be prepared (S
1). When the weighing set value W _SV is input, the weighing controller 9
The switching value W _SVP from continuous to intermittent is calculated by the following formula previously input in (FIG. 5) (S2). The formula for calculating the switching value is W _SVP = W _SV -Z. Z is a predetermined fixed value.

After that, W _SVP is compared with the measured weight value W _{SV of} the chemical solution supplied to the container 5 (S3). The weight measurement is performed every fixed time (for example, every 1 second). At the time of comparison before the start of weighing, since the chemical solution supply has not yet started, the measured weight value W _PV = 0
Is. When the switching value W _SVP > 0, the process proceeds to the continuous supply process A, and when the switching value W _SVP ≦ 0, the process directly proceeds to the intermittent supply process B.

(A) When the switching value (W _SVP )> 0 (regular weighing pattern, small amount weighing pattern) will be described.

In this case, the following operations (a) to (g) are performed.

(A) Open both large measuring valve SV1 and small measuring valve 2 (S4),
Start continuous supply of chemicals. At the same time, the sampling start timer T10 is turned on (S5). Since the measured weight value W _{PV of the} sampling start timer T10 is considered to be unstable immediately after the start of supplying the chemical liquid, the start delay time T _{10 is} constant.
The measurement is started after the lapse of (FIG. 1).

(B) The measured weight value W _PV is compared with the switching value W _SVP until the sampling start timer T10 times out (S6, S1
2), the measured weight value W _PV is the switching value W _SVP by the time up
If the value reaches, the process proceeds to the intermittent supply process B. This is the case when the weighing set value W _SV is small (small amount weighing pattern).

(C) If the switching value W _SVP is not reached by the time-up of the sampling start timer T10, step S7
As shown by S11 to S11, the chemical solution is continuously supplied while sampling the measured weight value W _PV at every constant sampling period T ₁₁ (regular measurement pattern).

(D) In this case, first, in step S7, the value of the switching value correction value W _SVP ′ is initialized to the value of the switching value W _SVP , and the weight value W _n−1 before sampling is measured weight value W _PV.
Initialize to. Thereafter, the sampling timer T11 is turned on (S8), and each time the time is up, the sampling amount ΔW is calculated to calculate the switching value correction value W _SVP ′ (S9, S1).
0). Where W _n is the weight value after sampling,
It is the measured weight value W _PV at the time of sampling. Wn _-1 is a weight value before sampling. The sampling amount ΔW for one time is a value of ΔW _n −W _n−1 . The correction formula of the switching value is W _SVP ′ = W _SV −ΔW · α. α is a coefficient that is obtained by experiments and appropriately determined.

After calculating the switching value correction value W _SVP ', it assigns the weight value W _n after sampling the weight value W _n-1 of the previous sampling (S11), and repeats the sampling.

While waiting for time-up of the sampling timer T11, i.e. at each sampling period T _11, the measured weight value W
_{The PV} is compared with the switching value correction value W _SVP ′ (S13), and when the measured weight value W _PV reaches the switching value correction value W _SVP ′, the intermittent supply process B is started.

(E) The intermittent supply is performed by closing the large metering valve SV1 (S16) and opening and closing the small metering valve SV2 (S16, S19). Supply time for each segment of intermittent supply, that is, opening time T of small metering valve SV2
₀ (FIG. 1) sets the interval time open timer TO (S17, S18), the closing time T _S is set by the intermittent time closing timer TS (S20, S21).

The opening time T ₀ is shortened as it approaches the metering set value W _SV based on the following equation (S15). In other words, T ₀ = β and (W _SV -W _PV). β is a coefficient appropriately determined by experiments or the like. The closing time T _S is a fixed time.

(F) During intermittent supply, the measured weight value W _PV is compared with the weighing set value W _SV (S14) after the timer TS for intermittently closing the small metering valve SV2 has timed up (S21), and the weighing set value W
_{When SV} is reached, the weighing is completed.

(G) The measured weight value W _PV is constantly compared with the measured set value W _SV even during the chemical solution supply by the small measuring valve SV2 (S22),
If the metering set value W _SV is reached during the open period T ₀ , that is, before the time is up, the small metering valve SV2 is immediately closed (S2
3), complete weighing.

Before starting intermittent supply, the measured weight value W _PV
When the measured value reaches the measured set value W _SV , the small measuring valve SV2 is closed (S14, S23) and the measuring is completed.

(B) A case in _which the value of the switching value W _SVP is ≦ 0 (micromeasurement pattern) will be described.

(A) When the measured weight value W _PV reaches the value of the switching value W _SVp when the measured weight value W _PV is first compared with the switching value W _SVP (S3), the intermittent feeding process B is started from the beginning. Then, intermittent supply is performed by the small metering valve SV2. In the intermittent supply, similarly to the regular measurement pattern and the small amount measurement pattern, the supply is performed until the measurement set value W _SV is reached (S14, S23). Also in this case, as the measured weight value W _PV approaches the measured set value W _SV , the opening time T ₀ of the small measuring valve SV2 is gradually shortened as described above.

According to this liquid preparation method, the open period T _{0 of the} intermittent supply becomes shorter as the metering set value W _SV is approached as described above, and therefore there is no excessive supply when the metering set value W _SV is reached, and the accuracy of the supply amount is improved. Is further improved. Even when the open period T ₀ is reached, the supply is stopped when the measured set value W _SV is reached, so that the liquid can be prepared with higher accuracy. Also, the weighing set value W _SV
Until the switching value correction value W _SVP ′ is continuously supplied until the open period T ₀ of the intermittent supply is lengthened until the value approaches the value of 1. Therefore, it is possible to accurately adjust the solution to the set value in a short time. Moreover, two large and small metering valves SV
Since continuous supply is performed by 1, SV2, and intermittent supply is performed by the small metering valve SV2, the difference between continuous supply and intermittent supply can be increased, and time can be further shortened and accuracy can be improved.

When switching from continuous to intermittent, the switching value correction value W _SVP ′ is calculated according to the sampling amount, and therefore switching from continuous to intermittent can be performed according to the viscosity of the chemical solution to be supplied, and the viscosity of the chemical solution can be changed. The accuracy can be improved and the time can be shortened even if the values are different.

Moreover, since the small-quantity measuring pattern and the minute-quantity measuring pattern are adopted, liquid preparation can be performed regardless of the measured set value W _SV .

〔The invention's effect〕

According to the method of the present invention, the segmental supply time of the intermittent supply becomes shorter as the value approaches the metering set value, so that the excessive supply when the metering set value is reached is eliminated and the accuracy of the supply amount is further improved. Further, since the segmental supply time for intermittent supply is lengthened until the measured set value is approached, rapid supply can be performed. Therefore, there is an effect that the liquid can be accurately adjusted to the measured set value in a short time.

According to the liquid preparation method of claim (2), since continuous supply is performed until the switching value is reached, the time can be further shortened.

In the liquid preparation method according to claim (3), the large and small supply paths are continuously supplied, and the intermittent supply is performed by the small supply path. Therefore, the difference between the continuous supply and the intermittent supply is increased, and the time is further shortened. Even if it tries, the accuracy can be secured.

In the liquid preparation method according to claim (4), since the switching value is corrected according to the sampling amount, the switching value from continuous to intermittent can be corrected according to the viscosity of the chemical solution to be supplied, even if the viscosity of the chemical solution is different. It is possible to improve accuracy and reduce time.

According to the liquid preparation method of claim (5), the sampling is started after the unstable period of the measured value immediately after the start of the supply, so that the switching value according to the viscosity of the chemical liquid can be corrected well.

In the liquid preparation method according to claim (6), when the measured weight value reaches a predetermined switching value before the start delay time for starting sampling, intermittent supply is performed without calculating the switching value correction value by sampling. Since it is switched to, the measurement can be performed even if the set value is small.

In the liquid preparation method according to claim (7), when the switching value obtained by subtracting a fixed value from the measurement set value is zero or a negative value, intermittent supply is performed only from the small supply path from the start of the supply. Even if the set value is smaller, it is possible to perform accurate liquid preparation for a short time.

[Brief description of drawings]

FIG. 1 is an explanatory view of a regular weighing pattern in one embodiment of the present invention, FIG. 2 is an explanatory diagram of the small amount weighing pattern thereof, FIG. 3 is an explanatory diagram of the minute weighing pattern thereof, and FIG. FIG. 5 is a flow chart of the whole liquid preparation method, FIG. 5 is an explanatory view of the constitution of a liquid preparation apparatus for carrying out this liquid preparation method, and FIG. 1 ... Chemical tank, 2 ... Pump, 3 ... Circulation path, 4 ...
… Electronic balance, 5 …… Container, 6 …… Large supply path, 7 …… Small supply path, 9 …… Measurement control device, SV1 …… Large metering valve, SV2
…… Small metering valve, W _SV …… Measurement set value, W _SVP …… Switching value, W _SVP ′ ... Switching value correction value, W _PV …… Measuring weight value,
ΔW ...... sampling amount, To ...... division opening time is the supply time, between Ts ...... closed, T ₁₀ ...... sampling of the start delay time

 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Masao Takigawa 5-7-1-4 Kasuga-cho, Toyonaka-shi, Osaka Prefecture (72) Inventor Takamitsu Ide 3-6-32 Kiyokojin, Takarazuka-shi, Hyogo

Claims (7)

[Claims] 1. The chemical solution is intermittently supplied up to a metering set value while measuring the weight of the supplied chemical solution, and each segment supply time in this intermittent supply is gradually shortened as the measured weight value approaches the meter set value. Preparation method. 2. The liquid preparation method according to claim 1, wherein the chemical solution is continuously supplied until the measured weight value of the supplied chemical solution reaches a predetermined switching value, and then intermittent supply is performed after reaching the switching value. 3. Large and small supply paths are provided, both supply paths are opened and continuously supplied until the measured weight value reaches the switch value, and when the measured value reaches the switch value, the large supply path is closed and small supply is performed. The liquid preparation method according to claim (2), wherein intermittent supply is performed through a route. 4. The weight of the chemical solution supplied is sampled at regular intervals, and the product ΔW · α of the sampling amount ΔW and the coefficient α, which is the difference between the sampling values before and after, is subtracted from the measurement set value W _SV W _SVP ′ The liquid preparation method according to claim 2, wherein the switch value correction value W _SVP ′ of = W _SV −ΔW · α is set as a switch value from continuous supply to intermittent supply. 5. The liquid preparation method according to claim 4, wherein sampling is started after a certain start delay time has elapsed after the start of the supply. 6. The switching value W _SVP is a value obtained by subtracting a fixed value Z from the weighing set value W _SV (W _SV −Z), and the measured weight value is switched before the start delay time for starting sampling elapses. _6. The liquid preparation method according to claim 5, wherein when the value of the value W _SVP is reached, switching to intermittent supply is performed without calculating the switching value correction value W _SVP ′ by sampling. 7. The liquid preparation method according to claim 6, wherein when the switching value W _SVP is zero or a negative value, the intermittent supply is performed only by the small supply path from the start of the supply.