DE102021201543A1 - Chemical substance, process of making the chemical substance, and use of the chemical substance - Google Patents

Abstract

A chemical substance, in particular a basic nitrate or a basic nitrate mixture, is proposed, which is composed of the following components: - proportion(s) of one or more nitrate groups and/or one or more nitrite groups; - metallic element, preferably element of the 2nd Main group, 3rd main group, 3rd subgroup or other rare earth metal which is in particular bivalent or trivalent;- proportion(s) of one or more hydroxyl groups and/or one or more oxo groups;

Description

State of the art

Nitrates and nitrate mixtures have already been proposed.

Disclosure of Invention

• - Anteil(e) einer oder mehrerer Nitratgruppen und/oder einer oder mehrerer Nitritgruppen;
• - Metallisches Element, vorzugsweise Element der 2. Hauptgruppe, 3. Hauptgruppe, 3. Nebengruppe oder anderes Metall der Seltenen Erden, welches insbesondere zweiwertig oder dreiwertig ausgebildet ist;
• - Anteil(e) einer oder mehrerer Hydroxygruppen und/oder einer oder mehrerer Oxogruppen;
• - Kristallwasser.

A chemical substance, in particular a basic nitrate or a basic nitrate mixture, is proposed, which is composed of the following components:

• - Portion(s) of one or more nitrate groups and/or one or more nitrite groups;
• - Metallic element, preferably element of the 2nd main group, 3rd main group, 3rd subgroup or other metal of the rare earths, which is formed in particular divalent or trivalent;
• - portion(s) of one or more hydroxy groups and/or one or more oxo groups;
• - crystal water.

Nitrates, in particular nitrates with the general formula M(NO ₃ ) ₃ xH ₂ O, are particularly useful as starting materials for the production of other materials, such as ceramic materials such as oxygen ion conductor materials such as yttrium and/or scandium-doped zirconium dioxide or the like. relevant. However, nitrates of this type are usually very hygroscopic and can absorb a large amount of water in a short time. This property is a hindrance to the above manufacturing processes and/or adjusting amounts of the reactants. In addition, nitrates, especially trinitrates, often have an acidic reaction in water. This, too, can be disadvantageous for corresponding processes which use the nitrates as starting materials. Due to the configuration of the chemical substance according to the invention, an advantageously reduced hygroscopicity can be achieved compared to the abovementioned nitrates, in particular with a substantially constant solubility in water and alcohols. In this way, an essentially advantageously constant and constant stoichiometry can be set for target materials or target compounds. Compared to the nitrates mentioned above, an advantageously low acidity can be made possible, in particular when dissolving in water or other solvents. In particular, storage and processing of the chemical substance in air can be achieved, in particular without significant changes in weight. The nitrate group(s) preferably has/have a general chemical formula NO ₃ . Naturally, such groups usually also have varying amounts of water of crystallization or otherwise bound water. The chemical substance preferably comprises, in particular as an element of main group 2, main group 3, subgroup 3 or another rare earth metal, Sc, Y or La. The chemical substance, in particular the basic nitrate or the basic nitrate mixture, particularly preferably does not include any further components apart from the nitrate group(s) and/or nitrite group(s) listed above in particular, the element of the 2nd main group, 3rd main group, 3rd Subgroup or other rare earth metal, the hydroxy group(s) and/or oxo group(s) and water of crystallization. In particular, the water of crystallization is in the form of bound water with the chemical formula H ₂ O. In particular, the chemical substance is present, particularly under standard conditions, as a dry, particularly granular, substance. Preferably, the chemical substance does not change its molecular mass significantly within at least 3 days, preferably at least 5 days and preferably at least 7 days of storage under standard conditions, in particular as a result of water absorption or water loss. Preferably, the chemical substance comprises, except for the element, the portions of the hydroxy group(s) and/or the oxo group(s) and except for the water of crystallization, only portions of nitrate groups, only portions of nitrite groups or a combination of portions of nitrate group(s) and nitrite group(s). It is conceivable that the nitrate groups and/or nitrite groups in the chemical substance are present in non-stoichiometric proportions. It is conceivable that the hydroxy groups and/or the oxo groups are present in the chemical substance in non-stoichiometric proportions. It is conceivable that crystal water is present in non-stoichiometric proportions in the chemical substance.

• - $$M{\left(N{O}_3\right)}_a{\left(N{O}_2\right)}_b{O}_c{\left(OH\right)}_{3-a-b-2c}\cdot {\left(H_{2}O\right)}_d,$$
  
  wenn M eine dreiwertige Metallspezies ist, insbesondere eine Spezies eines Elements der 3.Hauptgruppe, der 3. Nebengruppe oder ein anderes Metall der Seltenen Erden mit der Wertigkeit 3, wobei a + b einem Wert von 0,5 bis 2,5, c einem Wert von 0 bis 1,25 und d einem Wert von 0,5 bis 6 entspricht. Vorzugsweise beträgt ein Wert des Terms α + b + 2c maximal 3.
• - $$M{\left(N{O}_3\right)}_a{\left(N{O}_2\right)}_b{O}_c{\left(OH\right)}_{2-a-b-2c}\cdot {\left(H_{2}O\right)}_d$$
  
  wenn M eine zweiwertige Metallspezies ist, insbesondere eine Spezies eines Elements der 2.Hauptgruppe ein anderes Metall der Seltenen Erden mit der Wertigkeit 2, wobei α + b einem Wert von 0,25 bis 1,75, c einem Wert von 0 bis 0,875 und d einem Wert von 0,5 bis 6 entspricht. Vorzugsweise beträgt ein Wert des Terms α + b + 2c maximal 2.

The chemical substance particularly preferably has one of the following general chemical formulas:

• - $$M{\left(N{O}_3\right)}_a{\left(N{O}_2\right)}_b{O}_c{\left(OH\right)}_{3-a-b-2c}\cdot {\left(H_{2}O\right)}_{\mathrm{i.e}},$$
  
  if M is a trivalent metal species, in particular a species of an element of main group 3, subgroup 3 or another rare earth metal with the valency 3, where a+b has a value of 0.5 to 2.5, c one value from 0 to 1.25 and d corresponds to a value from 0.5 to 6. Preferably, a value of the term α + b + 2c is at most 3.
• - $$M{\left(N{O}_3\right)}_a{\left(N{O}_2\right)}_b{O}_c{\left(OH\right)}_{2-a-b-2c}\cdot {\left(H_{2}O\right)}_{\mathrm{i.e}}$$
  
  if M is a divalent metal species, in particular a species of an element of main group 2, another rare earth metal with valency 2, where α + b has a value from 0.25 to 1.75, c has a value from 0 to 0.875 and d corresponds to a value of 0.5 to 6. Preferably, a value of the term α + b + 2c is at most 2.

It is further suggested that the chemical substance has the chemical formula: M(NO ₃ ) _x (OH) _3-x · (H ₂ O) _y where x has a value from 0.5 to 2.5 and y has a value from 0.5 to 6 corresponds. An advantageous configuration of the chemical substance for further production processes can be achieved. In particular, the cation M is formed as an element of the 2nd main group, the 3rd main group, the 3rd subgroup or as another metal of the rare earths. For example, in a preferred embodiment, the chemical substance has the chemical formula: Sc(NO ₃ ) _x (OH) _3-x · (H ₂ O) _y with x≈1.5 and y≈2.5. In particular, the parameters x and y each have a tolerance of at most 10%, preferably at most 8% and preferably at most 5%. Configurations of the chemical substance with oxygen instead of a hydroxy group are also conceivable. In particular, it is conceivable that the / a proportion (s) of the nitrate group (s), in particular in the aforementioned chemical formula, partially or completely by (a) proportion (s) of one or more nitrite group (s) is / are replaced, which in particular each has/have the formula NO ₂ . The parameters a, b, c and d or x and y, which in particular are mentioned above, preferably determine the proportion(s) of the respective substances/groups of substances of the chemical substance, in particular those mentioned above.

• - Lösen eines, insbesondere des vorher genannten, Nitrats, insbesondere eines Trinitrats, welches insbesondere ein Element der 3. Nebengruppe umfasst, in zumindest einem organischen Lösungsmittel, insbesondere Alkohol, mit einem Verhältnis in einem Bereich von 1/100 bis 50/100, vorzugsweise 2/100 bis 45/100 und bevorzugt 4/100 bis 40/100;
• - Eindampfen der Nitrat-Lösung, insbesondere Nitrat-Alkohol-Lösung, bei einer Temperatur zwischen 0°C und 200°C, vorzugsweise zwischen 45°C und 120°C und bevorzugt zwischen 60°C und 100°C;
• - Trocknen der Nitrat-Lösung, insbesondere Nitrat-Alkohol-Lösung, bei einer Temperatur zwischen 0°C und 200°C, vorzugsweise zwischen 45°C und 120°C und bevorzugt zwischen 60°C und 100°C.

In addition, a method for producing a chemical substance according to the invention, in particular the aforementioned chemical substance, in particular the basic nitrate or basic nitrate mixture, is proposed, which comprises the following process steps:

• - Dissolving a nitrate, in particular the aforementioned one, in particular a trinitrate, which in particular comprises an element of subgroup 3, in at least one organic solvent, in particular alcohol, with a ratio in a range from 1/100 to 50/100, preferably 2/100 to 45/100 and preferably 4/100 to 40/100;
• - evaporation of the nitrate solution, in particular nitrate-alcohol solution, at a temperature between 0°C and 200°C, preferably between 45°C and 120°C and preferably between 60°C and 100°C;
• - drying the nitrate solution, in particular nitrate-alcohol solution, at a temperature between 0°C and 200°C, preferably between 45°C and 120°C and preferably between 60°C and 100°C.

Preferably, the nitrate is dissolved in the organic solvent until the nitrate solution is a clear liquid. Preferably, the nitrate is dissolved in the organic solvent while the mixture is agitated, preferably by stirring or shaking. In particular, the nitrate is dissolved in the organic solvent until a clear nitrate solution is obtained. The nitrate is preferably dissolved in the organic solvent at a temperature between 0°C and 100°C, preferably between 45°C and 120°C and preferably between 60°C and 100°C. Drying of the nitrate solution preferably follows directly after evaporation of the nitrate solution. It is conceivable that the nitrate, in particular the trinitrate, is formed as a nitrate of an element of the 2nd main group, the 3rd main group, the 3rd subgroup or another of the rare earths. The nitrate, in particular the trinitrate, is preferably in the form of a nitrate of an element of subgroup 3, for example Sc, Y, La. For example, the nitrate Sc(NO ₃ ) ₃ is dissolved in the organic solvent.

The chemical substance according to the invention can advantageously be produced by the configuration of the method according to the invention. Compared to the nitrates mentioned above, an advantageously reduced hygroscopicity can be achieved, while in particular the solubility in water and alcohols is essentially retained. Compared to the nitrates mentioned above, an advantageously low acidity can be made possible, in particular when dissolving in water or other solvents.

Furthermore, it is proposed that the evaporation and/or drying of the nitrate solution, in particular nitrate-alcohol solution, be carried out at least temporarily at a negative pressure, in particular at an ambient pressure of less than 10 ³ hPa, preferably less than 600 hPa and preferably less than 200 hPa. Volatile components such as water can advantageously be removed quickly and easily. The nitrate solution can be evaporated and dried at an advantageously low temperature. As a result, an advantageously gentle drying process can be made possible. It is conceivable that the nitrate solution, in particular nitrate-alcohol solution, is evaporated at a reduced pressure, preferably at an ambient pressure of less than 10 ³ hPa. Evaporation and drying are preferably carried out directly following each other, with in particular an ambient pressure and/or a temperature of the nitrate solution or the reaction environment being at least substantially maintained during the transition from evaporation to drying. A production of the chemical substance according to the invention is preferably also conceivable without generating negative pressure, in particular without significant differences in the chemical substance produced.

It is also proposed that dissolving the nitrate in the organic solvent, evaporating the nitrate solution, in particular the nitrate-alcohol solution, and/or drying the nitrate solution, in particular the nitrate-alcohol solution, with one movement , preferably with stirring and/or shaking. An advantageously uniform heat distribution can be made possible. Advantageously, uniform evaporation and escape of water can be achieved. Artificial mixing or homogenization of the mixture/solution can be achieved. Evaporation and/or drying of the nitrate solution is preferably carried out with regular circulation. For example, the nitrate solution is circulated at, in particular regular, time intervals. For example, the nitrate solution is circulated every 30 minutes, preferably every 20 minutes and particularly preferably every 10 minutes during evaporation and/or during drying.

It is also proposed that the evaporation and/or drying of the nitrate solution, in particular a nitrate-alcohol solution, be carried out over a period of between 10 minutes and 100 hours, preferably between 20 minutes and 50 hours and preferably between 30 minutes and 10 hours. he follows. Advantageous properties of the chemical substance can be achieved, in particular an advantageously high mass constancy, which can be measured, for example, via thermogravimetry. For example, an advantageously high stability and advantageous binding properties of the chemical substance can be made possible with a relatively short period of time for evaporation and/or drying, in particular within a previously mentioned temperature range. Evaporation and/or drying preferably takes place at least until a granular and/or dry chemical substance remains, in which case the liquid solvent(s) have at least essentially completely escaped. Evaporation and/or drying preferably takes place for a large part of the time of evaporation and/or drying under at least essentially constant conditions, in particular temperature and/or pressure, with the temperature of the nitrate-alcohol solution and/or the Reaction environment over the entire period of evaporation and / or drying by at most 5 ° C, preferably at most 3 ° C and preferably at most 1 ° C, changes and / or wherein the pressure of the nitrate-alcohol solution and / or the The reaction environment changes by at most 10 hPa, preferably at most 5 hPa and preferably at most 1 hPa over the entire period of evaporation and/or drying. It is conceivable that ambient conditions, in particular the pressure and/or the temperature, are changed over different time intervals during evaporation and/or drying, with the temperature and/or the pressure preferably being kept at least essentially constant in the individual time intervals.

Furthermore, it is proposed that the at least one organic solvent be used as butanol, as pentanol, as hexanol or isomers of hexanol, as methyl glycol, as ethyl glycol, as methanol, as ethanol, as 1-propanol, as 2-propanol and/or as 1 -Methoxy-2-propanol is formed. Beneficial properties of the chemical can be achieved.

In addition, it is proposed that the method comprises at least one step in which at least one additional organic solvent, preferably ester, orthoester, an organic carbonate and/or related compounds such as dicarbonate. An advantageously efficient removal of water molecules from the solution can be effected. Favorable interaction can be achieved with an organic solvent formed as an alcohol. It is conceivable that the additional organic solvent is mixed with the organic solvent before adding the nitrate. It is conceivable that a mixture of the aforementioned substances is added to the nitrate solution or the organic solvent as an additional organic solvent.

It is further suggested that the drying occurs until the chemical is in the form of a solid product. An advantageous consistency of the chemical can be achieved while the chemical is storable and processable in air without significant weight loss. If the chemical is dried at temperatures above room temperature, exposure of the chemical to normal ambient conditions is beneficial. A certain amount of water of crystallization can be absorbed in the process. After this outsourcing phase, the described storage and/or processing of the chemical substance can also be carried out in ambient air without significant weight loss.

In addition, the use of a chemical substance according to the invention, in particular the aforementioned one, in particular the basic nitrate mixture, which was preferably produced in a method according to the invention, is proposed for producing an oxygen ion conductor material, for example yttrium and/or scandium-doped zirconium dioxide.

By using the chemical substance according to the invention, an advantageously simple and cost-efficient production method can be made possible, in particular due to the advantageously high stability of the chemical substance under room conditions. An advantageously low acidity can be achieved when the chemical substance is dissolved in water, for example, which can be advantageous for processing. Preferably, an advantageously simple handling of the chemical substance can be achieved in the production of the oxygen ion conductor material, in particular in comparison to production using scandium nitrate.

The chemical substance according to the invention and/or the method according to the invention should/should not be limited to the application and embodiment described above. In particular, the chemical substance according to the invention and/or the method according to the invention can/can have a number of individual elements and method steps that differs from the number of individual elements and method steps mentioned herein in order to fulfill a functionality described herein. In addition, in the value ranges specified in this disclosure, values lying within the specified limits should also be considered disclosed and can be used as desired.

character list

Further advantages result from the following description of the drawings. In the drawing an embodiment of the invention is shown. The drawing, the description and the claims contain numerous features in combination. The person skilled in the art will expediently also consider the features individually and combine them into further meaningful combinations.

• 1 eine schematische Darstellung eines beispielhaften Ablaufs eines erfindungsgemäßen Verfahrens zu einer Herstellung eines erfindungsgemäßen chemischen Stoffs, welcher als ein basisches Nitratgemisch ausgebildet ist.

Show it:

• 1 a schematic representation of an exemplary sequence of a method according to the invention for producing a chemical substance according to the invention, which is designed as a basic nitrate mixture.

Description of the embodiment

In 1 An exemplary sequence of a method 10 for producing a chemical substance in the form of a basic nitrate or basic nitrate mixture is shown schematically, preferably for producing the chemical substance with the chemical formula: M(NO ₃ ) _x (OH) _3-x . (H ₂ O) _y where x is from 0.5 to 2.5 and y is from 0.5 to 6. The chemical substance consists of the following components: proportions of several nitrate groups, metallic element, in particular scandium (Sc), proportions of several hydroxyl groups and water of crystallization. Preferably, the process 10 produces the chemical having the chemical formula: Sc(NO ₃ ) _x (OH) _3-x .(H ₂ O) _y , where x≈1.5 and y≈2.5. However, the method 10 is also analogously conceivable for other configurations of the chemical substance, with the chemical substance comprising a different number of nitrate groups and/or nitrite groups or a different proportion of nitrate groups and/or nitrite groups. Alternatively or additionally, it is conceivable that the chemical substance includes a different number of hydroxy groups and/or alternatively or additionally includes one or more oxo groups and/or includes a different proportion of hydroxy groups and/or oxo groups. Alternatively or additionally, it is conceivable that the chemical substance includes a different amount of water of crystallization or bound water.

In a process step 12 of the process 10, a nitrate, in particular Sc(NO ₃ ), is dissolved in an alcohol, in particular ethanol, with a mass ratio of 40/100. Other configurations of an organic solvent for dissolving the nitrate are also conceivable. When dissolving the nitrate in the alcohol, the mixture is stirred at a temperature between 60°C and 100°C.

It is also conceivable to dissolve the nitrate in the alcohol without stirring the mixture. Alternatively or additionally, it is conceivable that the nitrate is dissolved in the alcohol at room temperature.

In a further process step 14 of the process 10, at least one additional organic solvent, preferably an ester, an orthoester or an organic carbonate, is added to the nitrate-alcohol solution before evaporation and drying. Specifically, the additional organic solvent is mixed such that a mass ratio of alcohol to the additional organic solvent is 1/100 to 1/1. It is conceivable that the additional organic solvent is mixed in before dissolving the nitrate, when dissolving the nitrate in the alcohol or after dissolving the nitrate in the alcohol. Preferably, the additional is mixed in organic solvent before evaporating and drying the nitrate-alcohol solution. In particular, it is conceivable that the admixing of the additional organic solvent takes place while the mixture is being moved, for example while stirring. However, refinements of the method 10 are also conceivable in which no additional organic solvent is used to produce the chemical substance, in which case method step 14 in particular is omitted.

In a further method step 16 of method 10, the nitrate-alcohol solution is evaporated at a temperature between 60° C. and 100° C., although other temperatures are also conceivable. In a further method step 18 of method 10, the nitrate-alcohol solution is dried. The evaporation and the drying of the nitrate-alcohol solution preferably take place directly after one another. It is conceivable that the evaporation and drying of the nitrate-alcohol solution takes place in a single process step 16/18. The drying of the nitrate-alcohol solution is carried out with agitation of the nitrate solution, preferably by stirring, for a period of between 30 minutes and 10 hours. The nitrate-alcohol solution is dried under reduced pressure. Drying occurs until the chemical is a solid product. Alternatively, it is conceivable that the drying and/or evaporation takes place over a shorter or longer period of time, depending on the respective temperature, without moving the nitrate alcohol solution and/or takes place/takes place under standard conditions/room conditions, in particular ambient pressure.

Claims (10)

Chemical substance, in particular basic nitrate or basic nitrate mixture, which is composed of the following components: - Portion(s) of one or more nitrate groups and/or one or more nitrite groups; - Metallic element, preferably element of the 2nd main group, 3rd main group, 3rd subgroup or other metal of the rare earths, which is formed in particular divalent or trivalent; - portion(s) of one or more hydroxy groups and/or one or more oxo groups; - crystal water. chemical substance after claim 1 , characterized by the chemical formula: M(NO ₃ ) _x (OH) _3-x · (H ₂ O) _y where x is from 0.5 to 2.5 and y is from 0.5 to 6 . Method for producing a chemical substance, in particular the basic nitrate or basic nitrate mixture claim 1 or 2 , with the following process steps: - dissolving a nitrate, in particular a trinitrate, which in particular comprises an element of subgroup 3, in at least one organic solvent, in particular alcohol, with a mass ratio in a range from 1/100 to 50/100 ; - evaporation of the nitrate solution at a temperature between 0°C and 200°C; - Drying the nitrate solution at a temperature between 0°C and 200°C. procedure after claim 3 , characterized in that the evaporation and/or drying of the nitrate solution takes place at least at times at a negative pressure. procedure after claim 3 or 4 , characterized in that the nitrate is dissolved in the organic solvent, the nitrate solution is evaporated and/or the nitrate solution is dried with agitation, preferably with stirring and/or shaking. Procedure according to one of claims 3 until 5 , characterized in that the evaporation and/or drying of the nitrate solution takes place over a period of between 10 minutes and 100 hours. Procedure according to one of claims 3 until 6 , characterized in that the at least one organic solvent as butanol, as pentanol, as hexanol or isomers of hexanol, as methyl glycol, as ethyl glycol, as methanol, as ethanol, as 1-propanol, as 2-propanol and/or as 1- Methoxy-2-propanol is formed. Procedure according to one of claims 3 until 7 , characterized by at least one step (14) in which at least one additional organic solvent, preferably ester, orthoester, an organic carbonate and/or related compounds such as dicarbonate, is added to the nitrate solution or the organic solvent before evaporation and before drying . Procedure according to one of claims 3 until 8th , characterized in that the drying is carried out until the chemical substance is present as a solid product. Use of a chemical substance, in particular the basic nitrate mixture, after claim 1 or 2 and / or which in a method according to one of claims 3 until 9 was manufactured, to a manufacture of an oxygen ion Conductor material, such as yttrium and / or scandium-doped zirconia.

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