JPH08215557A - Method and apparatus for initiating and/or promoting chemical or physical process of substance,in more detail, sample substance - Google Patents

Abstract

PURPOSE: To provide a method and an apparatus for preventing or at least suppressing possibilities of breaks of a substance reception apparatus and carrying out rational substance treatment. CONSTITUTION: The method for starting and/or promoting chemical or physical process of a substance, more specifically, a sample substance by heating and pressurizing the substance in a reaction chamber 2 capable of heating the substance by a heating means, more specifically, a microwave heating means includes at first exposing the substance to an initial pressure in the reaction chamber 2 and then heating the substance.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a method and apparatus for initiating and / or accelerating a chemical or physical process of a substance, and more particularly a sample substance.

[0002]

2. Description of the Prior Art Analytical chemistry, especially when preparing a substance (preferably a sample substance) or converting an initial substance into a reaction product, it is necessary to carry out a treatment under heat and pressure (excess pressure). Is a common practice. Because only under these conditions the desired process is realized, modified or forced.

A method and device of the above type is described in the German patent publication DE-A-39 33 992. In this known method, a short-wavelength radiation is generated by irradiating a gas under pressure with a long-wavelength electromagnetic wave, and this radiation is applied to the initial substance, or the initial substance itself is placed under a low pressure and long-wavelength Irradiate electromagnetic waves directly. For this purpose, a device is used which comprises a heating chamber surrounded on all sides by a housing, which seals the initial substance introduced into the openable and closable receptacle so that it can be heated under low pressure. It will be closed in the closed state. The low pressure is
An air pump that is generated by an air pump that is connected to the heating chamber (FIGS. 1 and 4 of the above patent publication) or, in the case of a closable receiver, an air pump that is connected to the receiver via a vacuum line. , FIG. 2 and FIG. 3).

[0004]

However, in this known device it is also possible to heat the initial substance introduced into the closed receptacle under excess pressure. For this reason, an overpressure valve is connected to the closable receiver, which overheats the initial substance when the initial substance or substances contained in the receptor are heated by irradiation. It ensures a certain overpressure that is automatically generated in the receiver by evaporation during the reaction (ibid., Figure 2).

In another known device for decomposing sample material in a closed overpressure sample receiver, an overpressure valve is connected to each sample receiver, which valve is at a certain pressure. When reached, it opens and releases the overpressure in the sample receiver. Even in this known device, heating, and thus evaporation caused by the heating, automatically causes an overpressure in the sample receiver, which causes heating of the air or gas components present in the sample receiver. Has already occurred.

It has been suggested to connect the exhaust line from the heating chamber with an overpressure valve in order to be able to monitor, measure and analyze gas emissions.

It should be emphasized that when treating the substances present with heat, in principle, it is preferable to obtain relatively high pressures in order for the reactions of the substances to take place stronger, faster and economically. Should be.

However, the treatment of substances at high pressure is associated with various difficulties. On the one hand, it is necessary to select a suitable sample material for both the sample receiver and the overpressure valve. That is, the sample material must be able to withstand erosive materials and have the strength to withstand high pressures and to maintain integrity and effectiveness even at the relatively high temperatures that occur.

In addition, the pressure and / or pressure generated in the sample receiver
Or the temperature is difficult to control and therefore repeated ruptures of the receptor are not acceptable as they not only damage the receptor but also contaminate the heating chamber and the surrounding environment.

Another difficulty is the heating of the material, which on the one hand is strong and abrupt and on the other hand also leads to the rupture of the receptor, in particular the rupture of the receptor when it is heated rapidly. is there.

A first object of the present invention is to provide a method and device of the type mentioned at the outset, which makes it possible to prevent or at least reduce the risk of rupture while at the same time allowing a rational substance treatment. It is in.

A second object of the present invention is to construct an apparatus of the type described in the preamble of claim 25 in the scope of the claims so that the reaction chamber can be easily loaded.

[0013]

The first purpose is to heat a substance (31), more specifically a sample substance, in a reaction chamber (2) heated by a heating means (3), more specifically a microwave heating means. In a method of initiating and / or promoting a chemical or physical process of a substance (31) by applying pressure to the substance (31), the substance (31) is first exposed to an initial pressure in the reaction chamber (2) and then Or a reaction chamber (2) surrounded on all sides by a housing (11) and a reaction chamber (2)
More specifically, the heating means (3) has a microwave heating means and a gas outlet (9b) of the housing (11), and the gas outlet (9b) has a reaction chamber ( 2) Outlet valve (V for the purpose of releasing the internal pressure inside)
1, V2) are connected and further comprise an inlet (9a) of the housing (11), said inlet (9a)
Is achieved by means of a device connecting a pressure source and a control device for supplying a pressurized gas before switching on the heating means (3).

According to the method of the present invention, the generation of the initial pressure results in the heating of the substance at a high pressure, and thus a stronger, faster and more economical treatment of the substance can be achieved.
This considerably reduces the risk of rupture of the reaction chamber, since the volume ratio between the reaction chamber and the substance is considerably higher, and thus also avoids burst pressure peaks.
Another advantage of the present invention is that the initial pressure reduces or prevents evaporation of materials that are likely to evaporate in the reaction chamber. As a result, the material can be processed more accurately, and the formation of condensation due to evaporation and the distortion of the measurement result are reduced, so that more accurate analysis can be performed.

The device of the present invention is capable of carrying out the method of the present invention and is characterized by a structure which is simple, economical to manufacture and functionally superior.

Devices of the type considered here have different configurations as far as the reaction chamber is concerned. The reaction chamber is, for example, the above-mentioned German Patent Publication (DE-A-39 33 992 Al).
Can be configured as a cabinet-like chamber as described in U.S.A., and such a reaction chamber is not structured to work at overpressure. Therefore, in order to carry out the substance treatment at overpressure, the substance or sample substance is placed in a closable, particularly pressure-resistant receiver and one or several such sample substance receivers are used for substance treatment. It must be located in the reaction chamber. In addition to such a cabinet-shaped reaction chamber, a pot-shaped reaction chamber which is pressure-resistant closed by a lid is suggested, and such a pot-shaped pressure reaction chamber is disclosed in German Patent Publication (DE 41 14 525 A).
It is disclosed in l). In this device, microwaves are directed directly to a receptacle for sample material formed by the reaction chamber. However, this known device can only form a single sample receiver capable of receiving a single sample due to the small container surrounding the reaction chamber.

The German patent publication (DE 40 38 273 Al) discloses devices of various constructions of the type considered here. In this device, the wall (FIG. 1), lid (FIG. 2) or base (FIG. 3) of the housing is displaced between a closed position and an open position by a displacement device in order to open the housing surrounding the reaction chamber. To be done. Each wall of the housing to be opened is provided with at least one fixture for the sample receiver, such as a locating plate, for displacing each wall to move the sample receiver into and out of the reaction chamber. can do. While this facilitates placement and removal of the at least one sample receiver within the reaction chamber or housing, it requires special fittings for the at least one sample receiver. Also, the sample receiver (s) cannot be easily positioned on the floor of the housing. Furthermore, due to the presence of the mounting device and for other structural reasons, this known device is arranged such that the sample substance can be placed directly in the housing (ie without the use of a special sample receiver). Not not. Another drawback of this known device is that the structure with a liftable lid for the reaction chamber (FIG. 2) has very limited accessibility into the reaction chamber. That is, even if the lid is lifted from the housing,
Since the lid is located above the housing, it is difficult to access the upper housing opening.

Some constructions of devices of the type considered here are described in the international patent application (WO / 93/22650). In this device, a mounting device in the form of a rotor is provided in the reaction chamber for receiving several pot-shaped sample receivers. As a result, the sample receiver is inserted by horizontal movement between the positioning plate that engages with the lower portion of the sample receptor and the lid that engages with the upper portion of the sample receiver at the upper opening, and the closure is performed. The lid is part of the mounting device and remains on the mounting device after removal of the sample receiver. This known device requires manual grasping of the sample receiver during insertion into and removal from the mounting device, which
Especially after treating the material, it is very difficult due to the high temperature.
Also, the sample material must be purposefully inserted into the mounting device. Furthermore, this known device is not suitable for large reaction chambers, since in the case of large reaction chambers the weight is too great to handle by hand. This known construction requires several sample receivers if it is desired to process several sample substances at the same time, each of which is purposefully moved horizontally for insertion into the working position and after processing. I have to pull it out again.

A second object of the invention is to have a reaction chamber (2) surrounded on all sides by a housing (11), the housing (11) being a pot-shaped lower housing part (12) and a lid (13). Consists of the lower part of the housing (1
2) or lid (13) in closed or actuated position (4
4) and a substantially vertical lifting device (42) for raising and lowering between the preparation position (44b) and the device (31), more particularly a device for initiating and / or promoting a chemical or physical process of a sample material. A substantially horizontal guide (46) for relatively displacing at least one of the lid (13) or the lower housing part (12) to a loading position (44) which is laterally displaced with respect to the other. ,
And the lower part (12) or lid (13) of the housing when opened
Is achieved by means of which the lifting device (42) begins to function before the horizontal displacement of the.

In this embodiment of the invention, not only is the lower part of the housing or its lid enclosing the reaction chamber displaced by the lifting device into the open-ready position, but also the lower part of the housing or the lid is in the loading position (and the loading position). It is displaced almost horizontally (from the position). This greatly improves the accessibility of the reaction chamber, so that the sample substance (s) can be placed directly in the reaction chamber in a simple and easy manner or placed in the sample receiver for reaction. It can be located in the chamber. The displacement of the lid or the lower part of the housing can be done manually or by a power drive. In order to displace the lid or the lower part of the housing in a substantially vertical direction, it is necessary to overcome these weights, so that the power drive device is effective. At the same time, such a displacement device also forms a closure device for the housing. For displacing the lid or the lower part of the housing substantially horizontally, a manual displacement in the guide is advantageous for simplicity and control of the device.

The features of the claims are features which contribute to the achievement of the simple structure which is the object of the present invention, which are simple and fast, and thus economical and reliable, the energy consumption. And features enabling economics and enabling efficient and reliable control of the treatment process.

Further, the present invention is not only characterized by a simple, economical and compact structure and convenient operation, but also a special structure which can highly utilize heating energy and can operate economically and reliably. A device having.

Furthermore, the present invention relates to another superior structure in which the pressure regulating element of the device is separate from the reaction chamber and is simply constructed as a special structural part which can be connected to the reaction chamber via a connecting line, and The present invention relates to an excellent structure of a pressure control element such as a valve that can perform a reliable and reliable process step.

[0024]

Operation: The generation of the initial pressure causes the material to be heated at a high pressure. This considerably reduces the risk of rupture of the reaction chamber, since the volume ratio between the reaction chamber and the substance is considerably higher, and thus also avoids burst pressure peaks. The initial pressure reduces or prevents evaporation of substances that are likely to evaporate in the reaction chamber. As a result, the material can be processed more accurately and the formation of condensation due to evaporation and the distortion of the measurement result are reduced.

[0025]

The present invention and other advantages achievable by the present invention will now be described in more detail with reference to the preferred embodiments of the present invention and the accompanying drawings.

The main part of the apparatus of the present invention, generally indicated by reference numeral 1, is a reaction chamber 2, a heating device (more specifically, a microwave heating device) 3 for the reaction chamber 2, and
A pressure supply device 4 for the reaction chamber 2, a pressure control block 5 for controlling the pressure in the reaction chamber 2,
It comprises a control device 6 for performing functional control of the device 1 (more particularly the heating device 3 and the working pressure), each addressable control component to be connected being connected via a control line of the control device 6. ing.

The substance to be treated can be placed directly in the reaction chamber or in reaction chamber 2 in one or several receptacles. One or several receptors 7
If (FIG. 2) is used, for handling reasons, the carrier frame (more specifically, a carrier frame made of plastic or microwave transparent or semi-transparent material) and the receiver 7 are connected. , Which allows the receptacle 7 to be easily placed in and removed from the reaction chamber 2.

For this purpose, the reaction chamber 2 has an upper loading opening for the introduction and withdrawal of the substance to be treated.

In this example, the device 1 is a microwave autoclave which functions at high temperature and pressure for the treatment or preparation of substances (more particularly sample substances intended for analysis).

There are several valves for controlling the pressure in the reaction chamber 2, which are arranged in a separately arranged control block 5. The control block 5 is connected to the reaction chamber 2 via a connection line (rigid or flexible pipeline or hose line, more specifically a plastic line) 9.

The reaction chamber 2 is surrounded by a housing 11. The housing 11 comprises a pot-shaped lower housing part 12 with an edge flange 12a for loading into the reaction chamber 2 and a preferably substantially flat lid 13 which is detachably attachable to the lower housing part 12. It is preferably formed. For the sake of clarity, the fixing device of the lid 13 to the housing lower part 12 is not shown. The fixing device is
The schematically illustrated screw 11a or lock ring half 11 with a U-shaped cross section arranged horizontally opposite one another
b. The lock ring half 11b is between a closed position (shown), which engages by hand or a power driven tool, above the lid 13 and below the edge flange 12a, and an outwardly offset release position (not shown). You can move with.

The housing 11 is a metal housing.
Microwave coupling into housing 11 is at the base of housing 11 (preferably arcuate downwards) 1.
4 from below. A cooling device, generally designated by reference numeral 15, is connected to the housing 11. The cooling device 15 has one or several cooling lines or cooling channels arranged inside or outside along the wall of the housing 11 through which a coolant (in this case water) is pumped 16 Supplied by and cooler 16a
Cooled inside.

The inside of the housing 11 is preferably lined with a lining material having corrosion resistance and heat resistance (preferably also having a heat insulating property). In this exemplary embodiment, a pot-shaped lining portion 17a that fits the inner contour of the lower housing part 12 and a lining lid plate 17b arranged on the lower surface of the lid 13 are provided, and the lining lid plate 17b is located below the lining lid plate 17b. It is preferable that the protruding portion 17c protruding inward is engaged in the lining portion 17a.

Between the base 17d of the lining part 17a and the base 14 of the lower housing part 12 it is preferable to provide an additional plate-shaped lining base 17e of microwave-transparent material and / or plastic. A central opening 18 is preferably provided in the base portion 14 for introducing microwaves (coupling). Inside or below this opening 18 a coupling radiating element such as a magnetron 19 or a waveguide or antenna 19a is arranged.
Provided on the upper edge of the opening 18 is a radiating element 21 having a bowl-shaped or hollow ball-shaped cross-sectional shape made of a microwave transparent material (preferably quartz), and the radiating element 21 corresponds to the base portion 17e. Is disposed in the recess formed by the above. Providing a cylindrical radiating element with a vertical axis,
It is also possible to insert the antenna 19a with a movable play in a hole provided in the radiating element.

The support of the housing 11 is designated by the reference numeral 20, on which the housing is arranged and, if appropriate, fixed.

In the exemplary embodiment shown in FIG. 2, a sealing lip 17f is provided to improve the sealing between the lining lid plate 17b and the upper edge of the lining portion 17a. The sealing lip 17f is preferably
It is formed as one piece on the cover plate 17b and engages with the inside of the lining portion 17a so as to abut against the inner wall of the lining portion 17a in a sealed manner. Also, the lid plate 17b is
From the outside of the lining portion 17a, the lining portion 17
It can engage with the upper edge of a. In this embodiment, a downwardly projecting annular protrusion 17g engages in an outer recess having a corresponding cross-sectional shape formed at the upper edge of the lining portion 17a. Therefore, the upper edge portion 17a is tapered and engages with the corresponding annular groove 17i of the lid plate 17b.

In this embodiment, in particular, the base region of the housing 11 is sufficiently insulated by the base 17d and the additional base 17e. Therefore, the cooling device 15 is merely arranged laterally adjacent to the reaction chamber 2 in or on the sheath of the lower housing part 12.
In this embodiment, the cooling device is in the form of an annular cooling channel 22 in the wall of the lower housing part 12, which channel 22 is preferably circular in horizontal cross section.

The lid plate 17b is seated on the lid 13 so that the centering member 17l on the upper surface of the lid plate 17b enters into the corresponding lower surface recess of the lid 13. The lid 13 has a centering member (centering ring in this embodiment) 13a on the lower surface. The centering member 13a engages in the peripheral wall of the housing lower part 12 to center the lid 13 in its closed position.

In the area of the housing 11, two temperature sensors T1 and T2 are provided. The first temperature sensor T1 is arranged in the base region of the lower housing part 12 and serves to determine the actual value for the regulation of the heating power and thus the actual temperature in the reaction chamber 2.

The second temperature sensor T2 functions to determine the temperature of the housing sheath and to adjust the cooling device 15 in order to prevent the material of the wall of the housing 11 from overheating.

The connecting line 9 is connected to the upper region of the reaction chamber 2 and, in this embodiment, is preferably inserted in the lid 13 at the center of the lid 13. As the connection line 9,
Those with a relatively thin nominal cross section are sufficient. This nominal cross section is preferably about 6 mm. Therefore, the connecting line 9
Is preferably a flexible line made of plastic so that the lid 13 can move when opening and closing.

In the exemplary embodiment of FIG. 2, the connecting line 9 is T
It branches in the shape fitting 26. The T-shaped fitting 26 is fitted or screwed into the housing 11 (the lid 13 in this embodiment) from above. From the T-fitting 26, a branch (inlet) 9a of the connecting line extends to the supply device 4, and the other branch (gas outlet) 9b of the connecting line extends to the control block 5. The air or gas pump 2 is provided at the branch portion 9a of the connection line described first.
3 and a check valve 27 are provided, which opens in the direction of flow towards the reaction chamber 2 and closes in the opposite direction. In this embodiment, the feed-through channel (common passage) 9c forming the common connecting line portion (in this embodiment the lid 13) is a sleeve 28 (preferably an inner flange) made of a heat and corrosion resistant material (preferably plastic). 28a). Fitting 26, connecting screw ring 26
The a, 26b and the connecting line 9 are also made of heat resistant and corrosion resistant material (more specifically, plastic).

The branch portion 9b of the connecting line has a first block valve in the control block 5, namely a regulating valve V. The valve member of the valve V opens the branch portion 9b when the pressure in the reaction chamber 2 rises to a certain pressure or a pressure range or more, and closes the branch portion 9b when the pressure decreases. This valve V
The valve body is operated in its closed position by a spring force, such as a leaf spring 29 or a spiral spring, and is opened by the pressure in the branch 9b. Two or three bypasses are provided in the control block 5 parallel to the valve, and the respective control valves are arranged in these bypasses. An electrically operated valve V1 is connected to the first bypass 9b1 (preferably a small cross section). The valve V1 is electrically driven (opened / closed) or adjusted based on the pressure in the reaction chamber 2 so that a certain pressure does not become excessive, that is, a desired pressure value is maintained. A pressure relief valve V2 is connected to the second bypass 9b2, which is preferably opened when the pressure rises above a predetermined higher pressure in the reaction chamber 2. In this embodiment, the valve V2 bursts and bypasses 9 when the safety pressure value is exceeded.
It is a rupture disc that opens b2. The branch portion 9b preferably has a cross-sectional dimension larger than that of the first bypass 9b1. The size of the second bypass 9b2 is preferably larger than that of the branch portion 9b.

It is preferable to provide a further bypass 9b3 in which a valve V3, which is operated electrically or preferably manually, is arranged. The valve V3 acts as another safety valve for the purpose of lowering the pressure in the reaction chamber after the treatment process, preferably by opening the valve V3 in case the programmed valve V1 fails. 2 becomes accessible, which allows the pressure to be reduced after the treatment process.

The bypasses 9b1, 9b2, 9b3 are arranged in parallel with each other. That is, each bypass functions independently of the other bypasses, which is ensured by the parallel connection.

A pressure sensor P1 for detecting the pressure in the reaction chamber 2 is also arranged in the control block 5, and more specifically, the pressure sensor P1 is arranged in the region of the connecting line 9 facing the housing 11. ing.

In the area remote from the housing 11, the bypass is reconnected to the branch 9b of the common connection line. The branch portion 9b of the connection line is guided into a container or chimney (not shown) in another discharge direction (see arrow 30).

The substance to be treated (more particularly the sample substance) is introduced into the reaction chamber 2 in bulk or, preferably, in one or several receivers 7. In this example, two receptacles 7 are shown that are open at the top. More specifically, these receivers 7 are hollow cylindrical and have a horizontal receiver base 7a.
In addition to the sample substance 31, an additional substance such as a reaction accelerating substance (more specifically, a solid or liquid drug 32) is placed in the receptor 7. The horizontal cross-sectional size (in this case the diameter of the same receiver 7) is only a fraction of the cross-sectional size of the reaction chamber 2 and therefore the outer peripheral wall of each individual receiver 7 and the inner peripheral wall of the reaction chamber 2 There is a free space between, or between the reaction chamber 2 and some of the receptors 7, and between the receptors. This free space is preferably filled with a microwave absorber (more specifically an indirectly acting liquid heating agent, water 33 in this example) up to about the filling level of the receptacle 7.

It is preferable to provide another indirect heating agent which consists of a microwave absorber. In this example, the indirect heating agent is a horizontal heating plate 34, which is
It is preferably placed on the horizontal upper surface 34a of the housing base 17d. Receptor 7 (single or multiple) is
4a is placed in wide physical contact and thus in large area heat transfer contact.

The device 1 functions as follows.

In order to carry out the treatment (more specifically, the preparation of the substance 31), the substance 31 is treated as described above.
It is introduced inside and the housing 11 is closed. The treatment of the substance 31 is then started under overpressure and heating, so that overpressure, heat and regulation are controlled automatically or manually.

In the preparation process, the supply device 4 is first switched on to generate an initial pressure in the reaction chamber 2 (in this case for example an initial pressure of 80-100 bar). This pressure can be maintained for a period of time with the supply device 4 switched on or by means of the pressure sensor P1 or another pressure sensor. This pressure is generated by introducing or pumping air or a gas (for example an inert gas such as nitrogen). Next, the heating device 3
Is turned on. Thus, in this case,
Substance 31 (as long as this substance is a microwave absorbing substance)
2 is directly heated from below by a microwave as indicated by an arrow s in FIGS. 2 and 7, and the heating agent 33 and the heating plate 34 are also directly heated. The evaporation or reaction of the substance causes a large increase in the pressure and temperature in the reaction chamber 2 or the pressure chamber, whereby the substance is processed under these conditions.

In order to be able to carry out the treatment at a certain pressure and / or a certain temperature, a device is provided which can set or adjust a certain temperature and / or pressure value or a temperature and pressure range. At this time, it must be taken into consideration that the above-mentioned means and processing effects have a crossover effect. Because temperature affects pressure as much as pressure affects temperature (taking into account the reaction of substances).

It is convenient to connect a processor to the control device 6 of the device 1 and control the device according to a program so that the processing of the substance is automatic.

The operating process steps which are carried out regularly, ie the operating process steps which are carried out depending on the pressure and temperature generated, will now be described as advantageous exemplary embodiments.

In the first process step, by turning on the pump 23, a supply pressure in the range of 0 to 150 bar is generated in the reaction chamber 2 as a starting condition. Here, an initial gas pressure of, for example, about 80 bar is generated.

When the supply pressure is reached (whether or not the supply pressure is reached is detected by the pressure sensor P1 and the pressure sensor P1 outputs a corresponding signal to the control device 6), the heating device 3 causes the second process. The process is switched on and the material is heated directly or indirectly as described above. This causes an overpressure in the reaction chamber 2 in the range of up to about 150 bar to occur simultaneously with an increase in temperature and a treatment process (ie forced). At an overpressure of, for example, about 120 bar, the pressure sensor P1 provides another pressure signal for the regulation of the electrically controllable valve V1. The valve V1 is actuated in the opening and closing directions so that the desired pressure value of 120 bar is maintained. In this second process step, the heating power is also controlled or adjusted (switched on and off) according to the desired temperature value so that it does not exceed (preferably remains) the desired temperature value.

If the pressure in the reaction chamber 2 exceeds the desired pressure value (120 bar), for example due to a strong process reaction, then another 140th process step, for example 140
The heating power is reduced or switched off at the burl.

A pressure limiting valve V is provided as another fourth process step. The valve V operates at a pressure above the desired pressure value (for example about 150 bar) and limits the pressure to this pressure value. The pressure limiting valve V can be adjusted to operate only if the adjustment or control of valve V1 (ie temperature adjustment or control) fails.

A safety valve V2 is provided as another fifth process step. The valve V2 opens or bursts for the purpose of explosion protection in the event of a sudden large pressure rise.

Once this process is complete, the housing or reaction chamber 2 is relieved of pressure to allow access. Furthermore, according to the sixth process step, this is achieved by opening the controllable valve V1 or valve V3. The valve V3 arranged in the additional bypass 9b3 is preferably a manually operable valve so that the pressure can be reduced even if the valve V1 fails.

The control block 5 (which is preferably one that can be preliminarily mounted as the structural unit B) is
Made of pressure-resistant metal (more specifically steel). To prevent corrosion, the channels (gas outlets) 9b and the bypasses 9b1, 9b2, 9b3 provided in the control block 5 are lined with corrosion-resistant plastic. This can be advantageously done by first boring the channel and then lining it with a plastic material (more specifically a plastic injection). It is also possible to bore the channel after lining it, ie to fill the channel with plastic and then bore the plastic, whereby the lining forms the channel.

Further details and advantages of the device of the invention will now be described.

The reaction chamber 2 is also a pressure chamber and a sample chamber at the same time, and is protected by the insulating lining from direct contact between the substance and the pressure-resistant wall (more specifically, stainless steel) of the housing 11. The lining is made of plastic (more specifically, PTFE) and functions as a heat protection material and a corrosion protection material. The inner lining and the peripheral wall can be cooled by the cooling device 15 in order to prevent damage due to heat. An initial pressure is generated in the reaction chamber before the start of the reaction in order to prevent condensation and loss due to evaporation of the substance (more specifically the solvent). When the substance 31 is heated by the heating device 3, a further pressure increase to an adjustable operating pressure is achieved. The high boiling point achieved in this way prevents the loss of elements and compounds.

In the spontaneously exothermic reaction, the relatively large total chamber volume (preferably about 3-3.5 dm ³ ) provides an additional safety factor because pressure peaks can be avoided. In the embodiment of the present invention, since the reaction chamber 2 is relatively large,
A large amount of substance 31 can be introduced into the reaction chamber 2 for processing purposes. Also, although relatively large heat of combustion is released into the reaction chamber 2 during processing, this heat is absorbed by the endothermic capacity of the heating agent 33 acting indirectly and the relatively large chamber mass, and is thereby generated. Temperature peaks are also avoided. Therefore, according to the device of the present invention, a large amount of substance 31 can be processed without causing a functional problem.

With the device according to the invention, the receptacle 7, which is preferably made of plastic, can be constructed in a simple and economical manner, so that the receptacle 7 has the same pressure inside and outside. Receive. Thus, receptor 7
A different reaction in the receptor 7 is prevented even if the pressure of the is changed. In addition, the pressure and the boiling point of the substances (solvents, addition products, etc.) are significantly increased, so that the losses and the banding from one receiver to the other are reduced to practically negligible values. That is, the treatment can be carried out at elevated temperatures and nevertheless can be carried out in the closure device.

Further, the means and treatment according to the present invention bring about the automatic boiling point increase due to the pressure increase of the liquid medium forming the indirect heating agent 33. An initial or feed pressure of 100 bar, for example, gives a boiling temperature of 311 ° C. of water. That is, only when this temperature is exceeded, the heating agent 3
An automatic internal pressure rise follows the vapor pressure curve of 4.
Thus, for example, a water temperature of 330 ° C. results in a vapor pressure of 129 bar. In application, this means that the use of a low-boiling point heating agent will automatically generate in the reaction chamber 2 a pressure greater than the vapor pressure of the substance (ie component) 31 to be treated in the receiver 7. To do.

For example, when water is used as the indirect heating agent 34 and nitric acid is used as the substance 31 to be treated or the auxiliary substance (ie, the reactant), the boiling point of water is about 10.
The boiling point of nitric acid is 0 ° C., and the boiling point of nitric acid is about 121 ° C. In this example, the vapor pressure of water is high, thus preventing the vaporization of nitric acid into the gas phase. Thus, the condensation of nitric acid (more specifically, the condensation on the inner wall of the reaction chamber 2) is largely prevented. Theoretically, only gaseous reaction products can enter the free reaction chamber space. This is true not only for the above decomposition example, but also for all chemical reactions using various solvents. This effect can be called automatic pressure compensation or automatic pressure adaptation. Microwave irradiation and solid substance and / or liquid substance (heating agent 33, 3
Direct heat conversion with 4) enables sufficiently quick adjustment. That is, the temperature drops relatively quickly when the microwave power is turned off or switched off, and due to the parametric control, the pressure reacts faster than in conventional devices and a very high safety standard is obtained.

Plastic is suitable as the microwave partial absorbing material. In such materials, components such as particles of microwave absorbing material (more specifically graphite) are mixed or combined, which results in Weflon.
Known as [Product Name].

The lining, the sleeve 28, the heating plate 34 and, if necessary, the base portion 17e require a corrosion resistant material capable of withstanding the acid generated during the processing of the sample substance, and a preferable material is polytetrafluoroethylene (PTF).
E / Teflon [trade name]), tetrafluoro mixed polymer (TFM), quartz, ceramic or glass.

In the exemplary embodiment of FIGS. 3-5, the device 1 is capable of the above structures and functions. Details of the device 1 shown in FIGS. 1 and 2 are not shown in FIGS. 3 to 5 for simplicity. These embodiments mainly illustrate a displacement device for the housing 11, indicated generally by the reference numeral 41, by means of which the sample substance, the sample receiver 7 or the auxiliary means 33, 34 can be loaded. Bottom 12
You will be able to access it easily and conveniently.

The main parts of the displacement device 41 are a lift device 42 that operates substantially vertically and a displacement device 4 that operates substantially horizontally.
It is 3. These devices cause relative movement between the housing lower part 12 and the lid 13, first in a generally vertical and then lateral direction. In the loading position 44a shown schematically in FIGS. 3 to 5, the housing lower part 12 is laterally displaced relative to the lid 13 towards the operating side 45, which allows easy access from above. . The lift device 42 engages the lid 13 in the embodiment of FIGS. 3 and 5, and engages the housing lower portion 12 in the embodiment of FIG. These parts of the housing 11 can be separated from each other in a substantially vertical direction, so that the underside projections 17 of the lid 13 are
Even when c and 17f are engaged with the lower housing 12,
A relative lateral displacement of these parts relative to each other is possible. The relative lateral displacement is in each case provided by the displacement device 43. The displacement device 43 engages the lower housing part 12 in the embodiment of FIGS. 3 and 4 and the lid 13 in the embodiment of FIG. A guide 46 is provided to guide the lower housing 12 for relative lateral displacement (FIGS. 3 and 4) or the lid 13 for relative lateral displacement (FIG. 5).
The guide 46 can be configured to cooperate with the lift device 42 and the displacement device 43, for example, as shown in FIG. 5, or as a specific guide element, as shown in FIGS. 3 and 4.

As shown in FIGS. 3 to 5, the housing 11
Further provided are the supporting part 20 and the lift device 42, the displacing device 43 and the cradle 47, 48, 49 for the supporting part 20. Support 20 and cradle 47, 48, 49
Can be configured as a part of the device to which the device 1 is integrally assembled.

3 to 5, each of the lift device 42 and the displacement device 43 is formed by pneumatic or hydraulic piston cylinders 51 and 52, and these piston cylinders 51 and 52 are arranged in both displacement directions. Is activated. In the embodiment of FIG. 3, the piston cylinders 51 forming the lift device 42 are arranged concentrically in a substantially vertical position between the lid 13 and the coupling cradle 47 with the housing 11 closed. The piston cylinder 52 forming the displacement device 43 is arranged on the side opposite to the operating side 45 and extends in a substantially horizontal direction for engaging the lower housing part 12. The piston cylinder 51 is provided with a substantially vertical guide 50 for movement of the lid 13,
It is preferably fixedly connected to the cradle 47 and the lid 13. The substantially horizontal guide 46 for laterally displacing the lower housing part 12 can be formed as a longitudinal recess 59 in the support 20, which is formed as a plate, for example, as shown in FIG. 3, or Piston cylinder 52
Can also be formed. Piston cylinder 51,
A pneumatic or hydraulic control device 6a for controlling 52 is provided, which control device 6a is connected to the double-acting piston cylinders 51, 52 via a fluid line and to the control device 6 via a control line. Has been done. To open the housing 11, first the piston cylinder 51 is actuated appropriately to lift the lid 13 slightly. Next, the piston cylinder 52 is activated to move the lower housing 12
From the operating position 44 indicated by the solid line to the loading position 44a
The guide 46 is displaced substantially horizontally in the guide 46. The closing of the housing 11 takes place in the reverse displacement or control process. That is, first the lower part 12 of the housing is displaced back into its operating position 44 and then the lid 13 is lowered from its preparation position 44b to its closed position.

In the exemplary embodiment shown in FIG. 4, the lid 13 is fixed to a pedestal (for example, the pedestal 47), and the supporting portion 20 is substantially formed by a lift device 42 (the lift device 42 is also formed by a piston cylinder 51). It is different from the other embodiments in that it can be displaced in the vertical direction. In this embodiment, the piston cylinder 5 constituting the displacement device 43
2 between the housing lower part 12 and the connection cradle 48,
A joint 61 having a joint axis perpendicular to the plane of vertical movement,
It is convenient to attach to 62. According to this configuration,
To open the housing 11, the housing lower part 12 is slightly lowered to the preparation position 44b, and then the piston cylinder 52 displaces the housing lower part 12 to the loading position 44a. The closing of the housing 11 is performed by the reverse displacement or control process.

In the exemplary embodiment of FIG. 5 (again, the same or like parts are designated by the same reference numbers), the lifting device 42 and the displacement device 43, ie both piston cylinders 51, 52, are fitted with a lid 13. The piston cylinder 51, which is engaged and forms the lifting device 52, has a joint 63, 64 with a joint axis perpendicular to the plane of vertical movement of the lid 13.
3 is different from the exemplary embodiment of FIG. The displacement control of the piston cylinders 51 and 52 is the same as that of the embodiment of FIG. 3, but first, only the lid 13 is displaced to the preparation position 44b, and then to the open position on the side opposite to the operating side, that is, the loading position 44a. To be done. Since the lid 13 is doubly connected, the integral guide 46 is formed in this case. The piston rod of the piston cylinder 51 may be configured to be pushed out when moved to the open position 58, or may be pulled out by the piston cylinder 52.

The device 1 is integrated, reference numeral 7 in its entirety.
1 has a rectangular housing 72, which in the front region facing the operating side 45 has a working plate 7 with a height h which is approximately equal to the height of the table.
3 The rear region of the housing 72 is raised stepwise to form an assembly 74. The device 1 is arranged or integrated in the device 71 as follows. That is, the housing 11 is in its operating position in the rear region of the device 71 (i.e. below the assembly 74), so that the lower housing part 12 can be displaced towards the operating side 45 in the front region of the device 71. This allows
In the loading position 44a, the housing 11 is the housing 72.
Near the front side surface 75 of the and edge flange 12a thereof
Is in the area of the work plate 73 (preferably the work plate 7
It slightly protrudes upward from 3). For this purpose, the working plate 73 has an elongated hole 76 extending from the rear to the front, the midpoint of which is the operating position 44 of the lower housing part 12.
And in the loading position 44a. 6 and 7 show only the components of the lift device 42 of the lid 13 and the displacement device 43 of the housing lower part 12 of the displacement device 41. That is, the support portion 20 in the shape of the carrier ring 20a
(A stepped taper portion provided on the lower surface of the housing lower portion 12 is arranged in the support portion 20) and a guide 46 (here, two guide rods 46a arranged on both sides of the housing lower portion 12 are used. None) is shown. The traveling sleeve 46b is placed in the operating position 44 and the loading position 4
The carrier ring 20a is mounted on the guide 46 by manual displacement with respect to 4a. In order to allow the displacement of the lower housing part 12 and the lid 13, as in the embodiment of FIGS. 3 to 5, the signal line, supply line or discharge line connected to the device is made flexible. A guide rod 46a is attached to the end region of the housing 72. The piston cylinder 51 of the device 42 is shown in FIG. The cradle 47 connected to the piston cylinder 51 is part of the device 71 or the housing 72 of the device 71 and can be formed, for example, by a tie bar and / or the upper wall of the housing 72.

A suction device 81 (not shown in FIGS. 1 to 5) for sucking the vapor exiting the open housing 11 is associated with the device 1 in all embodiments. The suction device 81 has a suction opening 82 arranged at the rear of the housing 11 at the height of an open slit formed in the opening of the lid 13.
Have. The suction openings 82 preferably have the shape of slits that extend horizontally in the horizontal direction and generate a wide range of suction streams 83 that extend in the substantially horizontal direction. In addition, the suction opening 82
Is preferably strong enough to cover the entire width of the opening of the lower housing part 12 and to suck the vapor discharged from the lower housing part 12 (from the front side to the rear side in this embodiment) at the loading position 44a. The sucked vapor passes through a continuous discharge line 84 led from the housing 72 to the outside,
It is discharged outside the building or into a chimney (not shown).

On the one hand, there is provided a substantially horizontally extending guide plate 85 which improves the suction effect and on the other hand functions as a mechanical safety device. The guide plate 85 is arranged at a small distance a few cm above the opening of the housing lower portion 12 at the loading position 44a, and can be displaced between an operating position that covers the opening and a release position that exposes the opening. It is installed. In this embodiment, the guide plate 85 is arranged so that it can be tilted upward from the opening, for example, laterally (rearward in the embodiment of FIG. 6).
A hinge 86 is provided for this purpose, which in this embodiment is located between the rear end of the guide plate 85 and the adjacent front side of the assembly 74. It is fixed to the section. The guide plate 85 preferably has a side leg 85a when viewed from the front. The guide plate 85 has an inverted U-shaped cross section, so that the outflowing vapor is prevented from spreading laterally and the suction flow 8
The guidance and suction of 3 are improved. The side leg 85a is preferably configured to stand on the work plate 73. The guide plate 85 not only protects the opened housing lower portion 12 from impurities that may fall into the housing lower portion 12 in the covering position, that is, the operating position, but also displaces the housing lower portion 12 to the loading position 44a. Sometimes it also functions as a protective device to prevent the risk of the operator's hands being caught. Therefore, for safety reasons, the lower housing part 12 is only in the loading position 44a when the guide plate 85 is in the operating position.
It is advantageous to design the control device of the device 1 so that it can be displaced. This is achieved by a contact device 87 on the housing which is actuated by the guide plate 85 when it is in its actuated position and is connected via signal lines to the corresponding control device 6, 6a.

The guide plate 85 is preferably made of a transparent material (more specifically, plastic) such as plexiglass so that the inside of the housing lower portion 12 can be visually recognized.

Working plates 7 present on both sides of the guide plate 85
The wide surface portion 85a of 3 can be used as a surface for placing the sample receiver 7, for example.

The closing ring halves 11b (which are also present in the embodiment of FIG. 6) are actuated by a drive motor, each half 11b having a joint 88 with a vertical joint axis at each end. It is pivotally attached. The fitting 88 is preferably located behind the housing 11 and is secured to the housing 72 or a component attached to the housing 72. The drive motor (not shown) may be located in the area of the fitting 88 or integrated with the fitting 88. The closure ring half 11b or other closing means should be released before the housing 11 is opened by the lifting device 42 and closed after the lifting movement.

The electrically conductive housing lower part 12 (more particularly made of a corrosion resistant material such as metal, more particularly stainless steel) is made as an integral piece with its base 14 and the base 14 is made. It is very stable because it is continuously connected to.

[0084]

According to the method of the present invention, the generation of the initial pressure results in the heating of the substance at a high pressure, so that a stronger, faster and more economical treatment of the substance can be achieved. This considerably reduces the risk of rupture of the reaction chamber, since the volume ratio between the reaction chamber and the substance is considerably higher, and thus also avoids burst pressure peaks. Another advantage of the present invention is that the initial pressure reduces or prevents evaporation of materials that are likely to evaporate in the reaction chamber. As a result, the substance can be processed more accurately, and the formation of condensation due to evaporation and the distortion of the measurement result are reduced, so that there is an effect that a more accurate analysis can be performed.

According to the apparatus of claim 10 of the present invention, there is an effect that the method of the present invention can be carried out, and it is simple and economical to manufacture and has a functionally excellent structure.

According to the twenty-fifth aspect of the present invention, not only is the housing lower part or the lid surrounding the reaction chamber displaced into the opening preparation position by the lift device, but also the housing lower part or the lid is loaded. It is displaced in a substantially horizontal position (and from the loading position). This greatly improves the accessibility of the reaction chamber, so that the sample substance (s) can be placed directly in the reaction chamber in a simple and easy manner or placed in the sample receiver for reaction. It can be located in the chamber. The displacement of the lid or the lower part of the housing can be done manually or by a power drive. In order to displace the lid or the lower part of the housing in a substantially vertical direction, it is necessary to overcome these weights, so that the power drive device is effective. At the same time, such a displacement device also forms a closure device for the housing. Displacement of the lid or the lower part of the housing substantially horizontally has advantages such as manual displacement in the guide being advantageous for simplicity and control of the device.

Further, the device of the present invention is not only characterized by a simple, economical and compact structure and convenient operation, but also has a structure which can highly utilize heating energy and can operate economically and reliably. Have.

Furthermore, the device according to the invention has an excellent structure in which the pressure-regulating element of the device is separate from the reaction chamber and is designed as a special structural part which can simply be connected to the reaction chamber via a connecting line, It also has an excellent structure of pressure control elements, such as valves, that can perform fault-free and reliable process steps.

[Brief description of drawings]

1 is a highly simplified side sectional view showing the device of the present invention. FIG.

FIG. 2 is an enlarged vertical sectional view showing an embodiment of a reaction chamber of the apparatus of the present invention.

FIG. 3 is a schematic side view of a modification of the device according to the invention.

FIG. 4 is a schematic side view of another modification of the device of the present invention.

FIG. 5 is a schematic side view of a further modification of the device according to the invention.

6 is a perspective view, partly broken away, of a device of the invention constructed according to the principles of the device of FIG.

FIG. 7 shows a partial longitudinal section of the device in the region of the reaction chamber.

[Explanation of symbols]

 1 Device 2 Reaction Chamber 3 Heating Device 4 Pressure Supply Device 5 Pressure Control Block 6 Controller 7 Receptor 9b Gas Outlet 9b1 Bypass 9b2 Bypass 9b3 Bypass 11 Housing 12 Lower Housing 13 Lid 14 Base 15 Cooling Device 16 Pump 17a Lining Part 17b Lining Cover plate 17c Projection part 17d Base part 17e Lining base part 19 Magnetron 21 Radiating element 22 Cooling channel 26 T type fitting 27 Check valve 28 Sleeve 31 Substance to be treated 33 Microwave absorber (water, heating agent) 34 Horizontal heating plate (heating) Agent) 3 42 Lift device 43 Displacement device 51 Piston cylinder 52 Piston cylinder 63 Joint 64 Joint 71 Device 72 Housing 73 Working plate 85 Guide plate

Claims (33)

[Claims] 1. The substance (31), more specifically, a sample substance,
Heating means (3), more specifically a method for initiating and / or promoting a chemical or physical process of a substance (31) by heating and applying pressure in a reaction chamber (2) heated by microwave heating means. In which the substance (31) is first exposed to an initial pressure and then heated in the reaction chamber (2). 2. The pressure (P in the reaction chamber (2)
Method according to claim 1, characterized in that the heating power is adjusted for the purpose of maintaining a predetermined temperature or a predetermined temperature range based on 1) and / or the temperature (T1). 3. Method according to claim 1 or 2, characterized in that the heating means (3) is switched off when a certain pressure is reached in the reaction chamber (2). 4. The method according to claim 1, wherein the pressure in the reaction chamber (2) is adjusted to a certain value. 5. The process according to claim 1, wherein the walls of the reaction chamber (2) are cooled, in particular in their upper and / or lateral regions. 6. The material according to claims 1 to 5, characterized in that the substance (31) is treated in one or more open receptacles (7).
The method according to any one of claims 1 to 4. 7. The material (31) is heated directly by microwave irradiation and / or indirectly by a heating agent (33, 34) arranged in the reaction chamber (2). The method according to any one of claims 1 to 6. 8. A heating agent (3) in which the microwave irradiation is performed more specifically from below and acts first indirectly.
Method according to any one of claims 1 to 7, characterized in that it is passed through a reaction chamber (3, 34) and then into the reaction chamber (2). 9. As an indirectly acting heating agent (33), a substance having a boiling point lower than that of the substance (31) to be treated or an auxiliary substance or a reacting substance associated with the substance (31) to be treated, The method according to claim 1, characterized in that a liquid is used in particular. 10. A reaction chamber (2) surrounded on all sides by a housing (11), a heating means (3) for the reaction chamber (2), more particularly a microwave heating means, and a housing (11). Gas outlet (9b) of the outlet valve (V1, V1) for the purpose of releasing the internal pressure in the reaction chamber (2) exceeding a predetermined value.
2) is connected, and further comprises an inlet (9a) of the housing (11), the apparatus for performing the method according to any one of the preceding claims 1 to 9, wherein the inlet (9a) comprises: A device, characterized in that a pressure source and a control device are connected for supplying pressurized gas before switching on the heating means (3). 11. The outlet (9b) and inlet (9a)
Is formed by a common passageway (9c) of the housing (11) and a pipeline or hose connected to the passageway (9c), which pipeline branches to the outlet valve on the one hand and pressure on the other hand. 11. Device according to claim 10, characterized in that it branches into a source. 12. The housing according to claim 10 or 11, characterized in that the housing (11), preferably made of metal, more particularly stainless steel, is lined on the inside with a corrosion and heat resistant material, more particularly plastic. Equipment. 13. The housing (11) comprises a pot-shaped lower housing part (12) and a lid (13), preferably the inlet (9a), outlet (9b), passage (9c).
13. Device according to any one of claims 10 to 12, characterized in that at least one of the is arranged on the lid (13). 14. One or more receptors (7) for the substance (31) can be connected to the substance (31) in the reaction chamber (2) and can be placed in the reaction chamber (2). 14. A device as claimed in any one of claims 10 to 13 characterized. 15. The one according to any one of claims 10 to 14, characterized in that the outer cross-sectional size of one or more of said receivers (7) is smaller than the horizontal cross-sectional size of the reaction chamber (2). Equipment. 16. A heating agent (33, 34) consisting of a solid or liquid substance that absorbs at least part of the microwave,
Device according to any one of claims 10 to 15, characterized in that it is in high surface area contact with the substance (31) and / or the receiver (7) in the reaction chamber (2). 17. A base (1) of the reaction chamber (2).
4) More specifically, there is arranged a plate-shaped support element for supporting the substance (31) or the single or multiple receptors (7), which support element is at least one of the microwaves. 17. A device according to claim 16, characterized in that it comprises a plastic which contains a microwave absorbing substance, more particularly a substance which absorbs parts. 18. Device according to claim 10, characterized in that it is provided with a coupling device for guiding microwaves from below into the reaction chamber (2). 19. A regulator is connected which regulates an internal pressure based on the internal pressure and / or temperature in the reaction chamber (2), and preferably the outlet valve or Device according to any one of claims 10 to 18, characterized in that the further outlet valve (V1) is the adjusting element of the adjusting device. 20. An adjusting device for adjusting a predetermined temperature in the reaction chamber (2), more specifically, a constant temperature, is connected, and heating power is used as a control means.
20. Device according to any one of claims 10 to 19, characterized in that it is reduced or reduced or switched off based on a predetermined temperature, preferably at high temperature. 21. The outlet (9b) has a first bypass (9).
21. A valve according to any one of claims 10 to 20, characterized in that it has a b1), more particularly a valve (V1) which is controlled or regulated on the basis of the internal pressure is arranged in the bypass. The described device. 22. A second bypass (9b2) is connected to the outlet (9b), and the second bypass (9b2) is connected.
22. Device according to any one of claims 10 to 21, characterized in that it is provided with a rupture valve, more particularly a safety valve, which opens automatically when the internal pressure rises. 23. Alternative bypass (9b3) for releasing the pressure in the reaction chamber (2) after completion of the process
Valve (V1) or another valve, preferably a manually operable valve (V3), is arranged.
Item 23. The device according to any one of items 22 to 22. 24. The reaction chamber (2) is connected to a manually or electrically adjustable valve (V1, V3) for releasing the initial pressure before opening the reaction chamber (2). Device according to any one of claims 10 to 23, characterized in that 25. The reaction chamber (2) is surrounded on all sides by a housing (11), the housing (11) being a pot-shaped lower housing part (1).
2) and lid (13), which is a substantially vertical lifting device (42) for raising and lowering the housing lower part (12) or lid (13) between a closed or working position (44) and a preparation position (44b). A substance (31), more particularly a device for initiating and / or accelerating a chemical or physical process of a sample substance, or a device comprising at least one of the features according to claims 10 to 24; (13) or at least one of the housing lower part (12) is laterally displaced with respect to the other loading position (44)
Is provided with a substantially horizontal guide (46) for relative displacement, and when opened, the lower part of the housing (1
2) or the lifting device (42) before the horizontal displacement of the lid (13)
A device characterized by the fact that the. 26. The housing lower part (12) or lid (13) is manually displaced or the guide (3)
26. Device according to claim 25, characterized in that it is displaced by the motor drive or displacement device (43) of 6). 27. The lift device (42) has a lid (13).
27. Device according to claim 25 or 26, characterized in that it is connected to the lower part of the housing (12) and the guide (46) is connected to the lower part of the housing (12) or the lid (13). 28. The housing lower part (12) is displaceable relative to the lid (13) towards the operating side (45) or front side of the device (1, 71). 28. The device according to any one of 27. 29. The lid (13) has a protrusion (17) on the lower surface.
c, 17f) engages with the lower part (12) of the housing, and a substantially vertical lifting movement amount causes the protrusion (17) to move.
29. Device according to any one of claims 10 to 28, characterized in that it is somewhat larger than the height of c, 17f). 30. A suction device (81) for sucking vapor emitted from the housing (11) when the housing (11) is opened is connected to the suction device (81).
Is preferably a guide (4) with respect to the housing (11).
30. Device according to any one of claims 10 to 29, characterized in that it is arranged on the opposite side of 6), preferably behind the housing (11). 31. In the laterally displaced loading position (44a) of the housing lower part (12), a substantially horizontal guide plate (85) is connected to the opening of the housing lower part (12), 85) is preferably spaced above the opening and displaceable between an operating position covering the opening and a release position exposing the opening, more particularly in the upward and outward directions 31. The device according to any one of claims 10 to 30, which is capable of tilting. 32. A reaction chamber (2) surrounded on all sides by a housing (11), a heating means (3) for said reaction chamber (2), more particularly a microwave heating means, a housing (11) ) Gas outlet (9b), and an outlet valve (V, V1, V for releasing internal pressure exceeding a predetermined value in the reaction chamber (2) at the outlet (9b)).
Device for carrying out the method according to any one of claims 1 to 9 or claim 10 to 31 above, wherein 2) is connected and further comprises an inlet (9a) of the housing (11). A device with one or more features according to claim 1, wherein a heating agent (33, 34) acting indirectly on the substance (31) is provided between the microwave coupling device and the reaction chamber (2). ) Is arranged. 33. Reaction chamber (2) surrounded on all sides by a housing (11), heating means (3) for said reaction chamber (2), more particularly microwave heating means, housing (11) ) Gas outlet (9b), and an outlet valve (V, V1, V for releasing internal pressure exceeding a predetermined value in the reaction chamber (2) at the outlet (9b)).
Device for carrying out the method according to any one of claims 1 to 9 or claim 10 to 31 above, wherein 2) is connected and further comprises an inlet (9a) of the housing (11). A device with one or more features according to claim 1, wherein in a block (5) spaced from the housing (11) are one or more valves (V, V) arranged parallel to one another.
1, V2, V3) and the block (5) is connected to the housing (11) via a pipe or hose connection (9b).