CN101532167B - Complex crystal synthesis device that can retard the growth of easily weathered crystal form - Google Patents

Abstract

The invention relates to a complex crystal synthesis device having retardance function for easy-weathered crystal growth, and belongs to monocrystalline growth field. In exploration working of synthesizing small complex crystal by a solvent volatility process at normal temperature and normal pressure, some crystal products with a great amount of crystallization water are generated, is not easily to resolve and is fast weathered and disintegrated, and the purpose of the invention is to inhibit the formation of the crystal. The device comprises a water tank and a cover plate with a plurality of holes, and is characterized in that the device also comprises a annular elastomer which is adhered to edge of each hole and is used for embedding a beaker or a test tube, an ultrasonic wave energy transducer arranged at bottom or side wall of the water tank, and water inlet/outlet with a valve arranged at bottom or side wall of the water tank. The device inhibit the growth of the crystal containing too much crystallization water and with relative loose structure by continuous ultrasonic wave with low power.

Description

Complex crystal synthesis device that can retard the growth of easily weathered crystal form

technical field

The invention relates to a complex crystal synthesis device capable of retarding the growth of easily weathered crystal forms, belonging to the field of C30B single crystal growth.

Background technique

The research work on the synthesis, exploration, structural analysis and application evaluation of small complex crystals has dual meanings. On the one hand, it helps to further explore the relevant scientific laws. On the other hand, some new functional crystals with potential application prospects Materials are also expected to be revealed in the process.

The first thing to do in this type of research is to probe the synthesis conditions of new crystals, of which solvent evaporation at or near room temperature is usually prioritized because of its mildness.

Because there are many conditional factors that may affect the growth rate and crystal quality of small crystals of complexes, screening synthesis experiments are usually necessary. This type of screening experiments is generally carried out using many small beakers or test tubes at the same time. For parallel synthetic probes, the preference for small beakers or test tubes is dictated by the dose for this type of experiment and the solvent-evaporative synthetic means appropriate to that dose.

The above experiments generally only involve a small reaction volume of several milliliters to tens of milliliters of the filtered reaction solution. The general synthesis steps are as follows: first place the filtered reaction solutions prepared according to the design in different beakers or test tubes, and cover the mouth of each small beaker or test tube with a polyethylene film with some tiny holes, and then, Put each small beaker or test tube in a ventilated place in the room, the solvent in each small beaker or test tube volatilizes slowly through the tiny holes on each polyethylene coating, gradually reacts, concentrates, and then forms small crystals of related complexes. After that, the The obtained small crystals of the complex were used for further physical and chemical analysis and evaluation.

The synthesis and exploration of small crystals of new complexes is also an aspect of scientific research in the field of chemistry. During this process, there are also opportunities to discover new crystal materials with practical value. This type of research is worthy of scientific exploration with certain scientific significance.

During the above-mentioned small crystal growth process of the complex, it is usually required to place the reactor, that is, the small beaker, in a relatively quiet environment. The quiet growth environment is generally considered to be an ideal growth environment for growing high-quality small crystals of the complex. The so-called small crystals of high-quality complexes refer to crystals with good crystal morphology, moderate particle size, few or no impurities, not prone to rapid weathering, and, crucially, crystals that are relatively easy to analyze the crystal structure.

In the case of transition metal ions as the central ion of the complex, some transition metal ions with multi-coordination tendency, such as rare earth ions and rare element ions, often attract too many water molecules when forming complex crystals, and there are too many A lot of water molecules exist in the crystal lattice in the form of crystal water. This kind of crystal often has a good crystal shape in the solution. However, because too much crystal water is trapped in the crystal, it brings two problems. The first problem is that this kind of crystal with too much crystal water is prone to rapid weathering when it leaves the solution in which it was grown, and the crystal will collapse and disintegrate quickly in the air. The related crystals are often single crystals that are not long The X-ray diffraction analysis experiment has been partially or completely weathered, which brings a lot of trouble to the single crystal X-ray diffraction analysis experiment. The second is that even if the relevant crystal has withstood several hours of single crystal The X-ray diffraction analysis experiment has generated related diffraction data, and the subsequent data analysis will be very difficult, because there are too many water molecules that are difficult to calibrate in the crystal. In this case, even if Reluctantly analyze the crystal diffraction data, the scientificity and reliability of the analytical results naturally have some unsatisfactory factors.

The small crystals of complexes containing too much crystal water have a loose structure, and the internal bonding force of the crystals is relatively small. In short, such crystals are not compact enough. Weathering defeats all expectations for practical use.

In the research on the synthesis of small crystals of complexes, it is usually more desirable to obtain stable crystals with less crystal water or no crystal water at all. Stable crystal quality is an important prerequisite for its application.

Contents of the invention

The technical problem to be solved by the present invention is to develop a new synthetic experimental device for the above-mentioned work under the premise of maintaining normal temperature and normal pressure synthesis conditions and still using the solvent evaporation method to find and synthesize small crystals of new complexes , the device should be able to help prevent the generated small crystals of the complex from entraining too much water of crystallization, in other words, the device should be able to help inhibit the growth of those containing too many crystal forms, and its application should help In order to lead the synthesis search results to stable crystals containing little or no crystal water.

The present invention solves the technical problem through the following solution, which provides a complex crystal synthesis device that retards the growth of the easily weathered crystal form, the device includes a water tank, the water tank is a tank-shaped object, and has A cover plate with many holes, the cover plate is a movable cover plate, the main point of this case is that the structure of the device also includes an annular elastic member, which is attached to the edge of the hole, and each of the The hole is correspondingly equipped with one of the annular elastic members, and an ultrasonic transducer, the installation position of the ultrasonic transducer is at the bottom of the water tank or the side wall of the water tank, and the water inlet interface and the water outlet interface, Both the water inlet interface and the water outlet interface are connected with the inside of the water tank, and the installation position of the water inlet interface and the water outlet interface is at the side wall position or the bottom position of the water tank, and the water inlet interface is installed with a water inlet valve. a water inlet interface, and the water outlet interface is a water outlet interface equipped with a water outlet valve.

The material of the annular elastic member is an elastic material, and the technical meaning of the word elastic material is well known, and the elastic material is, for example, various rubber materials and plastic materials with certain elasticity.

The ultrasonic transducer is a device that converts high-frequency oscillating electrical signals into high-frequency mechanical oscillations. The technical meaning of the word ultrasonic transducer itself is well known in the field of ultrasonic technology.

The number of the ultrasonic transducers is not limited, for example, the number of the ultrasonic transducers may be one, two, three, four, five, or six.

In the device of this case, the inner diameter size of the annular elastic member can be any size selected according to actual needs, but, in view of this type of experiment, a 100-milliliter beaker is selected as the reaction vessel in most cases, the preferred diameter of the annular elastic member The inner diameter size is between 4.5 cm and 5.0 cm. The inner diameter of the preferred annular elastic member is a size suitable for the outer diameter of a 100-milliliter beaker, which is suitable for holding a 100-milliliter beaker of a common size in it with a moderate grip, and moderate grip means The purpose is that a common size 100ml beaker can be inserted into the ring of the annular elastic member under moderate force for positioning, and also a common size 100 ml beaker that has been placed in the ring can also be positioned under moderate force. The ml beaker is pulled out of its fixed position. The corresponding upper limit value, the corresponding lower limit value, and the corresponding intermediate value of the inner diameter size range of the annular elastic member are all suitable dimensional values.

In order to make the ultrasonic energy sent by the ultrasonic transducer fully act on the reaction system, the water tank should preferably be overhead. Corresponding to this consideration, the preferred structural solution is to install support feet at the bottom of the water tank. The number of said support feet Not limited, for example, the number of the supporting legs may be two, three, four, five, or six.

The term "many" in this case means a larger number, such as ten, twenty, thirty, forty, fifty, sixty, eighty, etc.

The shape of the side wall of the water tank can be any shape, and the cover plate in the structure can be partially sunk in the water tank, or the cover plate can completely cover the edge of the water tank. The preferred solution is that the side of the water tank The cross-sectional shape of the wall is a crank shape, and the edge of the water tank wraps around the edge of the cover plate.

The device of this case can certainly also include some accessories, such as: a high-frequency oscillating electrical signal generator, which can be connected to the ultrasonic transducer, and, a power supply and a switch, the high-frequency oscillating electrical signal generator The oscillating electrical signal generator can be connected to the power supply via a switch; the technical meaning of the term itself of the high-frequency oscillating electrical signal generator is well known in the field of ultrasonic technology; The water outlet interface and the water inlet interface of the tank can be communicated with the water inlet interface and the water outlet interface of the water tank respectively, and the technical meaning of the term super constant temperature tank itself is well known.

In the actual operation of applying the device of this case, the applicable ultrasonic waves are of course low-power ultrasonic waves.

The advantage of the present invention is that an ultrasonic transducer is installed in the structure of the device, and an annular elastic member for constraining a small beaker or a test tube so that it can be suspended in an ultrasonic bath is installed. During the whole process of the growth of small crystals, ultrasonic intervention is continuously applied to the reaction system. In this way, the growth of crystals with relatively loose structures that contain too much crystal water is attacked, suppressed, and destroyed. The application of this device is helpful. In order to lead the synthesis search results to stable crystals containing little or no crystal water.

When the water tank is connected and used in combination with the super constant temperature tank, the super constant temperature tank is started at the same time, and the complex crystal synthesis work with finely controlled temperature can be carried out at any specified water bath temperature.

Description of drawings

Figure 1 is a schematic diagram of the embodiment of this case, which schematically describes the vertical section structure of its main working area, and additionally adds several beakers schematically suspended in the ultrasonic bath, in order to clearly understand its structural details, In the figure, a part of the structure is enlarged and displayed.

In the figure, 1 is the cover plate, 2 is the side wall of the water tank, 3 and 6 are two supporting feet with different installation positions, 4 and 7 are two ultrasonic transducers with different installation positions, and 5 is the water tank , 8 is an annular elastic member, 9 is a beaker schematically inserted therebetween, 11 and 12 are water inlet and water outlet interfaces respectively, and 10 and 13 are water inlet valves and water outlet valves respectively.

Detailed ways

In the embodiment of this case shown in Fig. 1, the structure of the device includes a water tank 5, and a cover plate 1 with many holes, the cover plate 1 is a movable cover plate, and the structure of the device also includes an annular elastic member 8, The annular elastic member 8 is attached to the edge of the hole, and each hole is correspondingly equipped with an annular elastic member 8. There are many holes on the cover plate 1, and correspondingly, there are many annular elastic members. Correspondingly installed together, and, ultrasonic transducer, in this illustration, ultrasonic transducer is ultrasonic transducer 4 and ultrasonic transducer 7, and ultrasonic transducer 4 and ultrasonic transducer 7 are in this example It is installed at the bottom position of the water tank 5, and the ultrasonic transducer 4 and the ultrasonic transducer 7 can certainly also be installed at the side wall position of the water tank 5, and the water inlet interface 11 and the water outlet interface 12, the water inlet interface 11 and the water outlet interface 12 are all communicated with the inside of the water tank 5, and the installation position of the water inlet interface 11 and the water outlet interface 12 is at the bottom of the water tank 5 in this illustration, and the installation position of the water inlet interface 11 and the water outlet interface 12 The setting position can also be the side wall position of the water tank 5 of course, the water inlet interface 11 is the water inlet interface equipped with the water inlet valve 10, and the water outlet interface 12 is the water outlet interface equipped with the water outlet valve 13. Of course, the water interface 11 and the water inlet valve 10 installed thereon can be used interchangeably with the water outlet interface 12 and the water outlet valve 13 installed thereon. In this illustration, the number of supporting feet appears is two, in fact, the number of supporting feet installed can be any number. In this illustration, the number of ultrasonic transducers that appear is two, but in fact, any number of ultrasonic transducers can be installed. In this illustration, the cross-sectional shape of the side wall of the water tank is a crank shape. In fact, the cross-sectional shape of the side wall of the water tank can be any shape. What is shown in the figure of this example is a relatively shallow water tank. In fact, the depth of the water tank is not limited, and the depth of the water tank can be arbitrarily selected according to needs.

Claims (1)

1. A complex crystal synthesis device that retards the growth of easily weathered crystal forms, comprising a water tank, which is in the shape of a tank, and a cover plate with many holes, which is a movable cover plate. The feature is that the structure of the device also includes a ring-shaped elastic member, which is attached to the edge of the hole, and each of the holes is correspondingly equipped with a ring-shaped elastic member, and the ultrasonic transducer energy device, the installation position of the ultrasonic transducer is at the bottom position of the water tank or the side wall position of the water tank, and the water inlet interface and the water outlet interface, the water inlet interface and the water outlet interface are all communicated with the inside of the water tank, and the The installation position of the water inlet interface and the water outlet interface is at the side wall position or the bottom position of the water tank. The water inlet interface is the water inlet interface equipped with the water inlet valve, and the water outlet interface is the water outlet interface equipped with the water outlet valve. The interface, the inner diameter of the annular elastic member is between 4.5 cm and 5.0 cm, the bottom of the water tank is equipped with supporting feet, the cross-sectional shape of the side wall of the water tank is a crank shape, and the edge of the water tank is wrapped around the edge of the cover plate outside.

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