CN112213352A - Method for measuring liquid evaporation change rate in high vacuum environment - Google Patents
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- 239000007788 liquid Substances 0.000 title claims abstract description 183
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- 238000004519 manufacturing process Methods 0.000 claims abstract description 25
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- 238000012360 testing method Methods 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 description 12
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- 239000002904 solvent Substances 0.000 description 6
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- 238000005259 measurement Methods 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
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Abstract
The invention discloses a method for measuring the liquid evaporation change rate in a high vacuum environment, which is characterized in that the relation between the average liquid change rate and the time is calculated in the process of searching a vacuum heating process for a novel organic material, whether the organic material is stopped being heated is judged according to the average liquid change rate, the whole vacuum heating process is convenient, the vacuum heating process of the mass-produced organic material is optimized, the number of times of testing the liquid end face height when the average liquid change rate is close to a target value can be aimed at, and the production and manufacturing process is more accurate and stable. The invention solves the problem of measuring the height of the sealed high-temperature liquid, does not need to directly contact the measured liquid, calculates the change speed of the measured liquid, ensures that the production and manufacturing process is more accurate and stable, and improves the controllability of the production process.
Description
Technical Field
The invention relates to the technical field of external devices for heating and purifying organic small molecular materials under high vacuum and changing the purification rate of the organic small molecular materials, in particular to a method for measuring the liquid evaporation change rate under a high vacuum environment.
Background
The performance of organic electroluminescent (OLED) diode displays depends greatly on the purity of the organic small molecule starting material. In the prior art, organic solvent recrystallization and heating purification under high vacuum are generally adopted for purifying organic electroluminescent materials.
The organic solvent recrystallization method utilizes the result of physical and chemical actions to dissolve organic materials in the solvent and then recrystallize the organic materials from the solution, thereby refining crystal grains or changing the crystal form of the crystal. In the recrystallization process, the material is dissolved in a solvent, and the crystallization speed and yield are controlled to remove impurities according to the adjustment of different solvent proportions. When the amount of the solvent is small, the operation of filtration while hot is troublesome, and when the amount of the solvent is large, the yield is impaired. The solvent needed for large-scale production is more, and the characteristics of volatility, flammability and the like of the organic solvent also increase the risk of operation. In addition, the industrial solvent generally has impurities (particularly colored impurities), and when part of the original impurities are removed, other newly added impurities are introduced or the material is discolored. Therefore, the process of the method for recrystallizing an organic solvent requires more parameters to be identified, and the introduced risk is higher.
The high vacuum heating and purifying method is one physical method with high repeatability and high material yield, and is one essential production link before making display. During purification, the organic material is placed in a quartz tube of uniform diameter and varying length, one end of the tube being completely sealed and the other end being sealed. After heating to melt the material, the vapor exits through a portion of the sealed end and is collected in another tube adjacent to the quartz tube. The schematic diagram of the apparatus is shown in fig. 1, and after heating, the organic material becomes liquid and evaporates, and the interface of the liquid gradually falls, but the rate of the fall fluctuates. The rate of liquid reduction changes with time, and particularly for materials that are susceptible to thermal decomposition, the likelihood of material decomposition increases with time. The optimal heating time is selected in the production process by monitoring the change of the liquid reduction rate along with the time, which is the key for reducing the production time, improving the production efficiency and ensuring the product quality, and the detection of the change of the rate is a very important production process.
The rate of reduction of liquid material may be reflected in the rate of reduction of liquid weight or liquid level. However, in practice, when the organic material is in a high vacuum, high temperature environment, direct measurement of the weight of the material or measurement of the liquid level is difficult to achieve. Currently, the liquid level is usually observed visually, and the rate of liquid material reduction is estimated empirically and perceptually, resulting in large errors.
Therefore, the invention provides the external method and the device for measuring the liquid change rate, which have small measurement error and convenient reading and recording and operation, and can accurately measure and record the rate change of the vacuum heating process of the organic material, guide the selection of the heating time, ensure the product quality and improve the production efficiency.
Disclosure of Invention
In order to solve the problems, the invention provides a technical scheme of a method for measuring the liquid evaporation change rate in a high vacuum environment, which can be externally arranged on organic material purification equipment to measure the liquid height change in vacuum equipment so as to calculate the liquid change rate, has small measurement error, is convenient for reading and recording, is convenient to operate, and can accurately measure and record the rate change of the organic material in the vacuum heating process, guide the selection of heating time, ensure the product quality and improve the production efficiency.
In order to achieve the above object, according to an aspect of the present invention, there is provided a method for measuring a liquid evaporation change rate in a high vacuum environment, the method is based on an apparatus for measuring a liquid evaporation change rate in a high vacuum environment, the apparatus includes an infrared distance meter and a supporting rotating frame, a material level is visible from an end surface of a measured liquid container, the infrared distance meter is connected to the supporting rotating frame, the infrared distance meter is rotatable up and down, the method includes the following steps:
s100, constructing a volume change model of container liquid with a circular end face;
s200, starting vacuum heating on the organic material, measuring the initial liquid end face height by using an infrared distance meter when the organic material forms a liquid surface after the organic material starts to melt, and measuring the liquid end face height after the time t1 by using the infrared distance meter again after the time t 1;
s300, calculating the liquid volume change amount after the time t1 by using a volume change model;
s400, calculating the average liquid change rate in the time t1 process according to the liquid volume change quantity;
and S500, judging whether to stop heating the organic material according to the average liquid change rate.
Further, in S100, a method of constructing a volume change model of the container liquid having a circular end surface includes:
and (3) setting the horizontal distance between the infrared distance meter and the end surface of the container to be L, the top distance between the infrared distance meter and the end surface of the liquid to be measured to be L1, the bottom distance between the infrared distance meter and the end surface of the liquid to be measured to be L2, the liquid level height from the top to the bottom of the end surface of the liquid to be measured to be H, and calculating to obtain the liquid level height H as follows:
for the organic material vacuum heating process, the end face of the container is round, the radius is R, the organic material is changed into liquid, the liquid level of the liquid is in the lower semicircle, and the relation between the liquid level width Z of the detected liquid and the liquid level height H is calculated as follows:
the relationship between the end surface area S of the measured liquid and the liquid level height H can be calculated as follows:
according to the length Y of the container, canThe relation between the volume V of the measured liquid and the liquid level height H is obtained by calculation, namely the volume change model of the container liquid with the circular end face is as follows:
further, in S300, the method of calculating the liquid volume change amount after the elapse of the time t1 by the volume change model is: after time t1, the liquid volume change Δ V is:
further, in S400, the method for calculating the average rate of liquid change during the time t1 according to the liquid volume change amount is as follows: from the liquid density ρ, the average rate of change of the liquid K1 during the time t1 is given by:
further, in S500, the method for determining whether to stop heating the organic material according to the average rate of liquid change is as follows:
when K1 is less than K, the average rate of liquid change is less than the target threshold value K, heating is stopped, and the reduction of the average rate and the reduction of the production efficiency caused by continuous heating can be avoided;
when K1>When K is reached, the average rate of liquid change is greater than the target threshold K, heating is continuously kept, after the time t2 passes, the height H2 of the liquid end face after the time t2 passes can be obtained through the test of the infrared distance meter again, and the formula is adopted
Obtaining the average rate of change K2 of the liquid, comparing with the target threshold K when K2<When K is reached, the average rate of change of the liquid is smaller than a target threshold value K, and then heating is stopped;
repeating the steps until the height Hn of the liquid end surface after the time tn is tested by the infrared distance meter, and obtaining the liquid end surface height Hn by a formula
Stopping heating when the obtained average rate Kn of liquid change is less than a target threshold K;
and K is an average target threshold of the production rate of the organic material set according to the production process of the organic material, and the value is generally the average melting rate of the organic material. Wherein the times t1, t2 to tn are linearly increasing times.
The invention has the beneficial effects that: the invention provides a method for measuring the liquid evaporation change rate in a high vacuum environment, which needs to increase the times of testing the liquid end surface height in the whole heating stage in the process of searching a vacuum heating process stage of a novel organic material, and is convenient for comprehensively knowing the change conditions of the liquid reduction rate of the organic material in the whole vacuum heating process. The optimization of the vacuum heating process of mass-produced organic materials can ensure that the production and manufacturing process is more accurate and stable aiming at the times of testing the height of the liquid end face when the average liquid change speed approaches the target value. The invention solves the problem of measuring the height of the sealed high-temperature liquid, does not need to directly contact the measured liquid, calculates the change speed of the sealed high-temperature liquid, ensures that the production and manufacturing process is more accurate and stable, improves the controllability of the production process, does not need to directly contact the measured liquid, does not pollute the measured liquid, has no requirements on the environmental pressure, the temperature, whether the measured liquid is corrosive, whether the liquid is sealed and the like, and has the advantages of simple structure, convenient operation and convenient industrial popularization.
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The above and other features of the present invention will become more apparent by describing in detail embodiments thereof with reference to the attached drawings in which like reference numerals designate the same or similar elements, it being apparent that the drawings in the following description are merely exemplary of the present invention and other drawings can be obtained by those skilled in the art without inventive effort, wherein:
FIG. 1 is a schematic diagram of the use of a device for measuring the rate of decrease of a liquid in an apparatus for measuring the rate of change of evaporation of a liquid under a high vacuum environment;
FIG. 2 is an end view of a liquid container under test;
FIG. 3 is a graph of the height of the end face of the liquid being measured at different times;
FIG. 4 is a graph of average rate of change of liquid versus time.
Detailed Description
The conception, the specific structure and the technical effects of the present invention will be clearly and completely described in conjunction with the embodiments and the accompanying drawings to fully understand the objects, the schemes and the effects of the present invention. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The invention provides a method for measuring the evaporation change rate of liquid in a high vacuum environment, as shown in figure 1, the method is based on a device for measuring the evaporation change rate of liquid under a high vacuum environment, comprises an infrared distance meter and a supporting rotating frame, the liquid level of a material can be seen from the end face of a measured liquid container, the infrared distance meter is connected with the supporting rotating frame and can rotate up and down, in fig. 1, 1 of fig. 1 is an infrared distance measuring instrument, 2 of fig. 1 is a supporting rotary frame, 3 of fig. 1 is a liquid container to be measured, l in FIG. 1 is the horizontal distance between the infrared distance meter and the end face of the container, L1 in FIG. 1 is the top distance between the infrared distance meter and the end face of the liquid to be measured, l2 in FIG. 1 is the distance from the infrared distance meter to the bottom of the measured liquid end face, H in FIG. 1 is the height from the top to the bottom of the measured liquid end face, and Y in FIG. 1 is the length of the container;
the method for measuring the evaporation change rate of the liquid in the high vacuum environment comprises the following steps:
s100, constructing a volume change model of container liquid with a circular end face;
s200, starting vacuum heating on the organic material, measuring the initial liquid end face height by using an infrared distance meter when the organic material forms a liquid surface after the organic material starts to melt, and measuring the liquid end face height after the time t1 by using the infrared distance meter again after the time t 1;
s300, calculating the liquid volume change amount after the time t1 by using a volume change model;
s400, calculating the average liquid change rate in the time t1 process according to the liquid volume change quantity;
and S500, judging whether to stop heating the organic material according to the average liquid change rate.
Further, in S100, a method of constructing a volume change model of the container liquid having a circular end surface includes:
and (3) setting the horizontal distance between the infrared distance meter and the end surface of the container to be L, the top distance between the infrared distance meter and the end surface of the liquid to be measured to be L1, the bottom distance between the infrared distance meter and the end surface of the liquid to be measured to be L2, the liquid level height from the top to the bottom of the end surface of the liquid to be measured to be H, and calculating to obtain the liquid level height H as follows:
for the vacuum heating process of the organic material, the end face of the container is round, the radius is R, the organic material is changed into liquid, the liquid level of the liquid is in the lower semicircle, as shown in FIG. 2, Z in FIG. 2 is the liquid level width of the liquid to be measured, and R in FIG. 2 is the radius of the end face of the container; and H in FIG. 2 is the height from the top to the bottom of the end surface of the liquid to be measured, and the relation between the liquid level width Z of the liquid to be measured and the liquid level height H is calculated as follows:
the relationship between the end surface area S of the measured liquid and the liquid level height H can be calculated as follows:
according to the length Y of the container, the relation between the volume V of the measured liquid and the height H of the liquid level can be calculated, namely the volume change model of the container liquid with the circular end face is as follows:
further, in S300, the method of calculating the liquid volume change amount after the elapse of the time t1 by the volume change model is: after time t1, the liquid volume change Δ V is:
further, in S400, the method for calculating the average rate of liquid change during the time t1 according to the liquid volume change amount is as follows: from the liquid density ρ, the average rate of change of the liquid K1 during the time t1 is given by:
further, in S500, the method for determining whether to stop heating the organic material according to the average rate of liquid change is as follows:
when K1 is less than K, the average rate of liquid change is less than the target threshold value K, heating is stopped, and the reduction of the average rate and the reduction of the production efficiency caused by continuous heating can be avoided;
when K1>When K is reached, the average rate of liquid change is greater than the target threshold K, heating is continuously kept, after the time t2 passes, the height H2 of the liquid end face after the time t2 passes can be obtained through the test of the infrared distance meter again, and the formula is adopted
Obtaining the average rate of change K2 of the liquid, comparing with the target threshold K when K2<When K is reached, the average rate of change of the liquid is smaller than a target threshold value K, and then heating is stopped;
as shown in fig. 3, H0 in fig. 3 is the liquid end height at the time of initial liquid level formation, H1 in fig. 3 is the liquid end height after the lapse of time t1, H2 in fig. 3 is the liquid end height after the lapse of time t2, and Hn in fig. 3 is the liquid end height after the lapse of time tn;
repeating the steps until the height Hn of the liquid end surface after the time tn is tested by the infrared distance meter, and obtaining the liquid end surface height Hn by a formula
Stopping heating when the obtained average rate Kn of liquid change is less than a target threshold K; as shown in fig. 4, fig. 4 is a graph of average rate of change of liquid versus time.
And K is an average target threshold of the production rate of the organic material set according to the production process of the organic material, and the value is generally the average melting rate of the organic material.
Although the present invention has been described in considerable detail and with reference to certain illustrated embodiments, it is not intended to be limited to any such details or embodiments or any particular embodiment, so as to effectively encompass the intended scope of the invention. Furthermore, the foregoing describes the invention in terms of embodiments foreseen by the inventor for which an enabling description was available, notwithstanding that insubstantial modifications of the invention, not presently foreseen, may nonetheless represent equivalent modifications thereto.
Claims (5)
1. A method of measuring the rate of change of evaporation of a liquid in a high vacuum environment, the method comprising the steps of:
s100, constructing a volume change model of container liquid with a circular end face;
s200, starting vacuum heating on the organic material, measuring the initial liquid end face height by using an infrared distance meter when the organic material forms a liquid surface after the organic material starts to melt, and measuring the liquid end face height after the time t1 by using the infrared distance meter again after the time t 1;
s300, calculating the liquid volume change amount after the time t1 by using a volume change model;
s400, calculating the average liquid change rate in the time t1 process according to the liquid volume change quantity;
and S500, judging whether to stop heating the organic material according to the average liquid change rate.
2. The method for measuring the evaporation change rate of liquid in the high vacuum environment according to claim 1, wherein in S100, the method for constructing the volume change model of the container liquid with the circular end face comprises the following steps:
and (3) setting the horizontal distance between the infrared distance meter and the end surface of the container to be L, the top distance between the infrared distance meter and the end surface of the liquid to be measured to be L1, the bottom distance between the infrared distance meter and the end surface of the liquid to be measured to be L2, the liquid level height from the top to the bottom of the end surface of the liquid to be measured to be H, and calculating to obtain the liquid level height H as follows:
for the organic material vacuum heating process, the end face of the container is round, the radius is R, the organic material is changed into liquid, the liquid level of the liquid is in the lower semicircle, and the relation between the liquid level width Z of the detected liquid and the liquid level height H is calculated as follows:
the relationship between the end surface area S of the measured liquid and the liquid level height H can be calculated as follows:
according to the length Y of the container, the relation between the volume V of the measured liquid and the height H of the liquid level can be calculated, namely the volume change model of the container liquid with the circular end face is as follows:
3. the method of claim 2, wherein in step S300, the method of calculating the volume change of the liquid after the time t1 according to the volume change model comprises: after time t1, the liquid volume change Δ V is:
4. the method for measuring the evaporation change rate of liquid under the high vacuum environment according to claim 3, wherein in S400, the method for calculating the average liquid change rate during the time t1 according to the liquid volume change amount comprises the following steps: from the liquid density ρ, the average rate of change of the liquid K1 during the time t1 is given by:
5. the method of claim 4, wherein in step S500, the method for determining whether to stop heating the organic material according to the average liquid change rate comprises:
when K1< K, the average rate of change of the liquid is less than a target threshold K, and the heating is stopped;
when K1>When K is reached, the average rate of liquid change is greater than the target threshold K, heating is continuously kept, after the time t2 passes, the height H2 of the liquid end face after the time t2 passes can be obtained through the test of the infrared distance meter again, and the formula is adopted
Obtaining the average rate of change K2 of the liquid, comparing with the target threshold K when K2<When K is reached, the average rate of change of the liquid is smaller than a target threshold value K, and then heating is stopped;
repeating the steps until the height Hn of the liquid end surface after the time tn is tested by the infrared distance meter, and obtaining the liquid end surface height Hn by a formula
Change of the obtained liquidIf the average speed Kn is smaller than a target threshold value K, stopping heating; the target threshold K is an average target threshold of the production rate of the organic material set according to the production process of the organic material, and the value is an average melting rate of the organic material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113466322A (en) * | 2021-06-17 | 2021-10-01 | 新疆众和股份有限公司 | Method for detecting pollution degree of contact material for high-purity aluminum smelting on aluminum liquid |
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