JPS62198730A - Impurity separating device - Google Patents

Abstract

PURPOSE:To separate impurities such as a residual solvent with which a solid sample is impregnated securely on a dry basis by heating an impurity separating device directly or by a reaction treatment. CONSTITUTION:This device consists of a main separating device body 2 whose one end part is closed and a sample chamber 3 at one end part side in it, and a heating device 4 is arranged at the outer peripheral part of one end of the main body 2 while covering the sample chamber 3. Consequently, the solid sample is put in the sample chamber 3, which is heated up to necessary internal temperature while the inside of the sample chamber is held below constant pressure when impurities are separated below 200 deg.C without any heat destruction or in a pressure reduction state by a pressure reducing device 22 when not. The heating is stopped when the specific temperature 18 is obtained in the sample chamber 3 and the time required for the impurities sticking on the solid sample to separate is elapsed sufficiently. A flow rate control valve 10 is controlled and opened and carrier gas 7 is supplied through a gas supply pipe 13. Consequently, the low-density impurities of specific level which stick on the solid sample are separated and a high-purity solid sample is obtained.

Description

[Detailed Description of the Invention] The present invention is directed to the production of 1L solid raw material intermediates and products in the production of pharmaceuticals, electronic and optical parts, etc., and to prevent impurities such as solvents and adsorbed gases remaining on the products. The present invention relates to an impurity separation device that can be suitably used when separating and removing impurities and analyzing these impurities with high sensitivity.

・Future techniques and techniques u''-v Conventionally, in the manufacture of pharmaceuticals, many purification operations such as solvent extraction have been carried out in order to obtain highly pure medicinal ingredients. During the process, impurities may be added to the medicinal ingredients and may remain.

Additionally, in the production of ceramic electronic components and optical components, if dust or adsorbed gas adheres to the surface of solid raw materials such as substrates or product intermediates, the product may not meet the desired electrical or optical properties. Therefore, during the manufacturing process of these products, surface cleaning with solvents is performed to remove contaminants such as dust and adsorbed gases. Even after cleaning, the solvent used for cleaning may not be sufficiently removed and may remain.

Therefore, in the manufacturing field of pharmaceuticals, electronic/optical components, etc., impurities such as solid raw materials, product intermediates, residual solvents impregnated in products, and adsorbed gases adsorbed on the surface can be reliably removed industrially using a dry method. It is also important to quantitatively measure the impurities mentioned above by inspecting raw materials and products.

Conventionally, it has been difficult to dry remove impurities attached to solid samples. For example, with extraction equipment that extracts impurities with low vapor pressure by distillation, the residual solvent with a boiling point of 200°C or higher is removed using normal methods. If you try to remove it with an oven type dryer or distillation device, depending on the type of solid sample, the solid sample may become soft.

It melts and causes deformation such as deterioration and deformation, and the boiling point is 30.
If an attempt is made to remove the residual solvent at a temperature of 0° C. or higher, the solid sample may decompose, so there is a problem in that removal is difficult. In addition, when attempting to remove residual solvents and adsorbed gases with a boiling point of 200°C or lower using an oven dryer or distillation equipment, or removing residual solvents with a boiling point of 200°C or higher using a vacuum oven dryer or vacuum distillation equipment, However, it is virtually impossible to separate impurities that exceed the equilibrium amount in the oven chamber, distillation column, and solid surface, and therefore has the disadvantage that low concentration impurities on the order of ppm are hardly removed. .

For this reason, even when analyzing these impurities, it is difficult to perform dry separation to separate low concentration impurities on the order of ppm from the solid surface, making accurate analysis impossible. When attempting to separate and analyze the adsorbed gas adsorbed on the solid surface by
Reliable separation is not possible with a solvent with a low extraction rate, and it is difficult to perform low concentration separation on the ppm order.
There has been a problem in that it is substantially difficult to analyze impurities such as adsorbed gases adsorbed on the solid surface or residual solvent impregnated in the solid at a low concentration of about m order.

The present invention was made in view of the above circumstances, and can be used online in the manufacturing of pharmaceuticals and electronic/optical components.
Using solid raw materials, product intermediates, and products as samples, it is possible to reliably separate impurities such as residual solvent impregnated into these solid samples and adsorbed gas adsorbed on the surface using a dry method. It is an object of the present invention to provide an impurity separation device that can be suitably used for high-sensitivity qualitative and quantitative analysis devices.

In order to achieve the above-mentioned object, the present invention provides a solid sample to which impurities are attached (impregnated, adsorbed, etc.) that can be separated as a gas by heating the impurity separation device directly or through reaction treatment. The separator main body has a sample chamber that can accommodate the sample chamber airtightly and allow gas flow by switching, and a heating device that can heat the sample chamber in a temperature controllable manner.

The impurity separator of the present invention can airtightly accommodate a solid sample in its sample chamber, preventing the heated and separated impurities from diffusing outside the room, and can also allow gas to flow through switching. By circulating an inert gas such as Ar, N, etc. as a carrier gas and discharging impurities separated from the solid to the outside.

Impurities can be separated at a rate of 100%, and H, 0
By passing a reactive gas such as No. 2, impurities on the surface of the solid can be reacted and converted into a product that can be heated and vaporized almost 100% of the time.

A pressure reduction device can be connected, and by reducing the pressure, the temperature at which impurities are separated can be lowered, thereby preventing thermal damage such as deterioration or deformation of the solid sample due to high temperatures.

Furthermore, since the equipped heating device can heat the sample chamber in a temperature-controllable manner, the temperature can be adjusted to such an extent that the solid sample does not suffer from the above-mentioned thermal destruction, and to achieve an impurity separation rate that matches the speed of the line. It is possible to separate impurities without destroying the solid sample.

Hereinafter, one embodiment of the present invention will be described with reference to FIGS. 1 and 2.

Inuba■ Figures 1 and 2 show an impurity separation device 1 according to an embodiment of the present invention.
This impurity separation device 1 includes a separation device main body 2 having a substantially horizontal cylindrical shape with one end closed. One end of the main body 2 has an elliptical sample chamber 3 into which a solid sample is inserted, and the outer periphery of the one end of the main body 2 is heated by a mantle-type heater and a heat insulating material so as to cover the sample chamber 3. Device 4
is installed. The other end of the main body 2 is configured as a cooling flange 5, and a lid 6 is attached to the opening at the other end of the main body 2 in an openable and closable manner to close the opening. The inside of the main body 2, and therefore the sample chamber 3, is kept airtight through gaskets such as the above.

The main body 2 includes a carrier gas cylinder 7, one end of which is filled with a carrier gas, and an oxidation-reactive gas cylinder 8, which is filled with oxygen gas. The other ends of the gas supply pipes 13, 14, and 15 are connected to a reducing reactive gas cylinder 9 filled with hydrogen gas, and each has a flow control valve 10, 11, and 12 each consisting of a stop valve and a check valve. The temperature sensor 16 is disposed so as to pass through the cooling flange part 5 airtightly and be located at the other end of the sample chamber 3, and the other end of the temperature sensor 16 passes through the cooling flange part 5 airtightly and is located at the other end of the sample chamber 3. It is arranged so that it exists within. One end of this temperature sensor 16 is connected to the heating device 4 and is connected to a temperature controller 17 for controlling the temperature.
is connected to.

The temperature inside the sample chamber 3 detected by the temperature sensor 16 is displayed on a temperature display 18 connected to a temperature controller 17.

A gas outlet hole 29 is bored in the center of one end surface of the main body 2, and one end of a gas outlet pipe 2o having a pressure gauge 19 interposed therein is airtightly connected to this hole 29. The other end of this outflow pipe 2o is connected via a three-way switching valve 21 to the other end of a conduit 23 connected to a pressure reducing device 22, and one end is connected to an impurity concentrator 25 and a gas conduit via a three-way switching valve 24. Gas sampling pipe 2 connected to sampler 26
It is connected to the other end of 7.

Next, I will explain how to use this device.

First, the sample chamber 6 is opened, a solid sample is inserted into the sample chamber 3, and then the sample chamber 3 is closed. Next, if the impurities attached to the solid sample can be separated by heating below 200°C without thermally destroying the solid sample, the three-way switching valve 21 is switched so that the outflow pipe 20 is closed, and the inside of the sample chamber 3 is removed. Leave it under normal pressure, if not, turn the three-way switching valve 21 into the outlet pipe 2o.
After switching so that the and conduit 23 are in communication with each other, the pressure reducing device 22
After starting the sample chamber 3 and measuring the pressure with the pressure gauge 19 to bring the inside of the sample chamber 3 into a desired depressurized state, the three-way switching valve 20 is again switched so that the outflow pipe 20 is closed, and at the same time, the decompression device 22 is stopped. While keeping the inside of the sample chamber 3 in a reduced pressure state, start the temperature control device 17, temperature display 18, and heating device 4, respectively, and adjust the temperature control device 17 so that the inside of the sample chamber 3 reaches the required temperature. After setting, heating is performed, and the temperature inside the sample chamber 3 detected by the temperature sensor 16 is measured by the temperature display 18. When the inside of the sample chamber 3 reaches a predetermined temperature and a sufficient amount of time has elapsed for the impurities adhering to the solid sample to be separated, the heating device 4 and the temperature control device 17. The temperature indicator 18 is stopped and the flow rate control valve 1 is turned off.
0 is opened by adjusting the flow rate, and the carrier gas is allowed to flow in from the carrier gas cylinder 7 through the gas supply pipe 13. Next, the three-way switching valve 21 is connected to the outflow pipe 20 and the gas sampling pipe 27.
The carrier gas containing impurities in the sample chamber 3 is caused to flow out of the sample chamber 3. As a result, impurities with a low concentration of ppm order or PPb, or even ppt level, attached to the solid sample are separated, and a highly pure solid sample is obtained. In addition, when used online in the manufacture of pharmaceuticals or electronic/optical components, etc., the heating device 4, temperature control device 17, and temperature display 18 are
It is also possible to leave it running without stopping it.

When the carrier gas containing impurities in the sample chamber 3 flows out to the outside in the method of using the device described above, the three-way switching valve 2
1 so that the outflow pipe 20 and the gas sampling pipe 27 communicate with each other, and by switching the three-way switching valve 24 so that the gas sampling pipe 27 and the impurity concentrator 25 communicate with each other,
The impurities separated from the solid sample are concentrated and recovered by the impurity concentrator 25. On the other hand, by switching the gas sampling tube 27 and the gas sampler 26 so that they communicate with each other, a fixed amount of the above-mentioned impurities can be sampled. can be introduced into various sensors to perform qualitative and fixed-view analysis tests.

In addition, the method of use described above cannot separate impurities attached to a solid sample, but if the impurities change and can easily be heated and vaporized by performing a reaction treatment such as an oxidation reaction or a reduction reaction, the above method can be used. In the usage method described above, the temperature control device 17, the temperature display 18, and the heating device i! 4 and until the inside of the sample chamber 3 reaches a predetermined temperature, the flow rate control valve 11 or 12 is adjusted and opened, and oxygen gas or hydrogen is supplied from the oxidation reactive gas cylinder 8 or the reduction reactive gas cylinder 9. Impurity separation is performed by introducing a gas and performing a reaction treatment, and after the reaction treatment has been sufficiently performed, an operation of closing the flow rate control valve 11 or 12 is performed.

Here, N2゜Ha, Ne, Ar is used as a carrier gas for flowing out the impurities separated in the sample chamber 3 to the outside.
If the solid sample is inert to oxidation reactions or the like, air gas can also be used.

In the above-mentioned embodiment, the cooling flange portion 5 is provided for rapid continuous loading and unloading of solid samples. 6 may be installed, and depending on the solid sample and attached impurities, an oxidation-reactive gas inflow system consisting of a pressure reducing device 22, an oxidation-reactive gas cylinder 8, a flow rate control valve 11, and a gas supply pipe 14 may be installed. The reducing reactive gas inflow system composed of the reducing reactive gas cylinder 9, the flow rate control valve 12, and the gas supply pipe 15 can also be omitted. In addition, the gas outlet pipe, the impurity concentrator 25 and the gas sampler 26 are connected via the three-way switching valve 21, and the conduit 1723 is connected to the outlet of the impurity concentrator 25 via the on-off valve 28 to connect the pressure reducing device 22. There is no problem in changing the arrangement by connecting them, or changing the shape of the separation device main body 2 and the heating device 4 so that the space inside the sample chamber 3 becomes a cube or a rectangular parallelepiped, depending on the purpose and application of the device. Other configurations may also be modified in accordance with the requirements without departing from the gist of the present invention.

As explained above, according to the present invention, solids impregnated or adsorbed with impurities that can be separated as a gas by heating the impurity separator directly or after reaction treatment are removed. By having a main body of the separator having a sample chamber that can accommodate the sample airtightly and allowing gas to flow through it by switching, the above impurities can be dry-separated without thermally destroying the solid sample. In addition to making it possible to obtain extremely high purity solid samples after impurity separation, it is also suitable for online use, such as in the production of pharmaceuticals and electronic/optical components.

It can be suitably used for the removal of impurities for the purpose of high purity of solid raw materials, I1 product intermediates, and products, and for highly sensitive analysis of trace impurities.

[Brief explanation of drawings]

Fig. 1 is a schematic mechanical diagram showing one embodiment of the present invention, and Fig. 2 is a schematic cross-sectional view showing how a carrier gas supply pipe, a reactive gas supply pipe, and a temperature sensor are attached to the separation device main body. . 1... Impurity separation device 2... Separation device main body 3... Sample chamber 4... Heating device

Claims (1)

[Scope of Claims] 1. A separation device main body having a sample chamber capable of accommodating a solid sample containing impurities that can be separated as a gas either directly or by reaction treatment and heating, in an airtight manner and in a gas-flowable manner by switching. An impurity separation device comprising: a heating device capable of heating the sample chamber in a temperature controllable manner. 2. One end of the carrier gas supply pipe was connected to the carrier gas container, and the other end was placed in the sample chamber, and a gas outlet was provided in the main body, so that the carrier gas from the carrier gas container flowed into the sample chamber. 2. The impurity separation device according to claim 1, wherein the impurity separator is configured to discharge the impurity from the gas discharge port. 3. One end of the reactive gas supply pipe is connected to the reactive gas container, and the other end is arranged in the sample chamber, and a gas outlet is provided in the main body, so that the reactive gas from the reactive gas container is connected to the sample chamber. The impurity separation device according to claim 1 or 2, wherein the impurity separator is configured to flow in a room and then be discharged from a gas outlet. 4. The impurity separation device according to any one of claims 1 to 3, wherein a decompression device is connected to the main body so that the inside of the sample chamber can be degassed.