Working medium for creating pressure and method of using working medium for creating pressure

Abstract

FIELD: working media for creating pressure.SUBSTANCE: use of at least one organic compound (A) comprising an element of group 14 as a pressure generating medium is proposed, wherein the compound (A) is selected from the group consisting of a compound (A1) represented by the general formula (a1) and a compound (A2) represented by the general formula (a2), where each of the substituents Ra11, Ra12, Ra13 and Ra14 represents the same unbranched alkyl group having 4 carbon atoms, each of the substituents Ra21, Ra22, Ra23 and Ra24 represents the same unbranched alkyl group having from 3 to 4 carbon atoms, and Za1 and Za2 denote a silicon atom. A method of using the working medium to create pressure is also proposed.EFFECT: pressure generating medium has a freezing pressure at room temperature greater than 2.7 GPa and a flash point significantly above room temperature.8 cl, 1 tbl, 3 ex

Description

Field of technology

[0001] The present invention relates to a working medium for creating pressure and to a method for using a working medium for creating pressure.Background of the invention

[0002] In recent years, research related to the synthesis of substances, studies involving changes in the physical properties of substances, and other such studies have been widely conducted at ultrahigh pressures above 1.0 GPa. This research requires applying ultrahigh pressure to a substance hydrostatically. When applying ultrahigh pressure to a substance, a working medium is typically used to generate the pressure.

[0003] Examples of properties required for ultra-high-pressure pressurizing fluids include maintaining the fluid in a liquid state without solidifying over a wide pressure range. This is because when the pressurizing fluid solidifies midway through the pressure application, uniaxial compression occurs at higher pressures, making uniform compression impossible.

[0004] In recent years, various studies have been conducted on pressure-generating fluids that satisfy this required property. As an example, Patent Document PD 1 describes that a pressure-generating fluid oil containing a 1-olefin oligomer achieves a solidification pressure of 2.7 GPa at room temperature. Citation ListPatent Literature

[0005] PD 1: WO 2007 / 058064Summary of the inventionTechnical problem

[0006] Although the pressure-generating medium described in PD 1 has a high solidification pressure at room temperature, in recent years, there has been a requirement to develop a pressure-generating medium that has an even higher solidification pressure. In addition, from a safety perspective, the pressure-generating medium is required to have a flash point significantly higher than room temperature (such as 60°C or more).

[0007] The object of the present invention is to provide a working medium for creating pressure, which has a solidification pressure at room temperature of more than 2.7 GPa and a flash point significantly higher than room temperature, as well as a method of using the working medium for creating pressure. In the present description, “room temperature” means 25°C. Solution to the problem

[0008]

[0001] and [2].

[0001] A working medium for creating pressure, including at least one organic compound (A) containing an element of group 14 selected from the group consisting of a compound (A1) represented by the general formula (a1) and a compound (A2) represented by the general formula (a2): where each of the substituents R a11 , R a12 , R a13 and R a14 independently represents an alkyl group having from 3 to 6 carbon atoms, and Z a1 means a carbon atom or a silicon atom; where each of the substituents R a21 , R a22 , R a23 and R a24 independently represents an alkyl group having from 3 to 6 carbon atoms, and Z a2 means a silicon atom, a germanium atom, a tin atom, or a lead atom.

[0002] A method of using a working medium to create pressure, which comprises applying pressure to a substance through a working medium to create pressure in accordance with the above item [1].Advantageous effects of the invention

[0009] According to the present invention, a working pressure medium that has a solidification pressure at room temperature of greater than 2.7 GPa and a flash point significantly higher than room temperature, as well as a method for using a working pressure medium can be provided. Description of embodiments

[0010] The upper limit values ​​and lower limit values ​​of the numerical ranges given in this specification may not necessarily be combined. For example, when "A-B" and "C-D" are described as numerical ranges, the numerical ranges "A-D" and "C-B" are also included in the scope of the present invention. In addition, the numerical range "from the lower limit value to the upper limit value" described in this specification means the lower limit value or greater and the upper limit value or less, unless otherwise specified. In addition, in the present specification, the numerical values ​​in the examples are numerical values ​​that can be used as the upper limit value or the lower limit value.

[0011] Working medium for creating pressureThe working medium for creating pressure according to the present embodiment contains at least one organic compound (A) containing a Group 14 element selected from the group consisting of a compound (A1) represented by the general formula (a1) and a compound (A2) represented by the general formula (a2): where each of the substituents R a11 , R a12 , R a13 and R a14 independently represents an alkyl group having from 3 to 6 carbon atoms, and Z a1 means a carbon atom or a silicon atom; where each of the substituents R a21 , R a22 , R a23 and R a24 independently represents an alkyl group having from 3 to 6 carbon atoms, and Z a2 means a silicon atom, a germanium atom, a tin atom, or a lead atom.

[0012] A thorough study has been conducted to solve the above problems. As a result, it has been found that the above problems can be solved by using at least one organic compound (A) containing a Group 14 element (hereinafter may also be referred to as "component (A)") selected from the group consisting of a compound (A1) represented by the general formula (a1) and a compound (A2) represented by the general formula (a2). Although the reason why the solidification pressure of the compound (A1) and the compound (A2) is high is unclear, part of the reason is presumably due to the appropriate balance of overlap between the electron orbital of the central atom that forms these compounds and the electron orbital of the alkyl group or alkoxy group surrounding the central atom.

[0013] The working pressure medium of the present embodiment is preferably composed of only the component (A), but may contain components other than the component (A), as long as the effects of the present invention are not significantly deteriorated. In the working pressure medium of the present embodiment, the content of the component (A) is preferably from 70 to 100% by mass, more preferably from 80 to 100% by mass, even more preferably from 90 to 100% by mass, even more preferably from 95 to 100% by mass, and even more preferably from 98 to 100% by mass, based on the total amount of the working pressure medium.

[0014] Below, each component contained in the pressure generating working medium of the present embodiment is described in detail.

[0015] Compound (A)The pressurizing medium of the present embodiment contains a component (A).The component (A) is at least one component selected from the group consisting of a compound (A1) represented by the general formula (a1) and a compound (A2) represented by the general formula (a2).As the compound (A1) represented by the general formula (a1), one type may be used alone, or two or more types may be used in combination.As the compound (A2) represented by the general formula (a2), one type may be used alone, or two or more types may be used in combination.From the viewpoint of further easily increasing the solidification pressure at room temperature, the component (A) preferably contains the compound (A2) represented by the general formula (a2), and is more preferably composed of the compound (A2).When the component (A) contains the compound (A2) represented by the general formula (a2), the content of the compound (A2) is preferably 50 to 100% by mass, more preferably 60 to 100% by mass, even more preferably 70 to 100% by mass, even more preferably 80 to 100% by mass, and even more preferably 90 to 100% by mass, based on the total amount of the component (A).

[0016] Below are the details of connection (A1) and connection (A2).

[0017] Compound (A1)Compound (A1) means a compound represented by the general formula (a1):

[0018] In the general formula (al), each of the substituents R a11 , R a12 , R a13 and R a14independently represents an alkyl group having 3 to 6 carbon atoms. When the alkyl group has 2 or fewer carbon atoms, it is difficult to achieve a flash point significantly higher than room temperature. When the alkyl group has 7 or more carbon atoms, the solidification pressure becomes low. When conducting electrical conductivity measurements, etc., under ultra-high pressure, a conductive paste can be used for the electrode. When the alkyl group contains 7 or more carbon atoms, the conductive paste can dissolve. Although R a11 , R a12 , R al3 and R al4 may represent the same alkyl group or different alkyl groups, R a11 , R al2 , R al3 and R al4are preferably the same alkyl group from the viewpoint of more easily achieving the effects of the present invention. In the present description, “the same alkyl group” means an alkyl group having the same number of carbon atoms and the same structure.

[0019] From the viewpoint of more easily achieving the manifestation of the effects of the present invention (in particular, from the viewpoint of further easily increasing the solidification pressure), an alkyl group that can be selected as R a11 , R al2 , R al3 and R al4 , preferably has 3 to 5 carbon atoms and more preferably has 4 carbon atoms.

[0020] Alkyl group that can be selected as R a11 , R a12 , R a13 and R a14 , may be linear or branched, but is preferably linear from the point of view of more easily achieving the manifestation of the effects of the present invention.

[0021] In the general formula (a1) Z a1 means a carbon atom or a silicon atom. From the point of view of more easily achieving the manifestation of the effects of the invention Z a1 preferably represents a silicon atom.

[0022] Compound (A2)Compound (A2) means a compound represented by the general formula (a2):

[0023] In the general formula (a2), each of the substituents R a21 , R a22 , R a23 and R a24independently represents an alkyl group having 3 to 6 carbon atoms. When the alkyl group has 2 or fewer carbon atoms, it is difficult to achieve a flash point significantly higher than room temperature. When the alkyl group has 7 or more carbon atoms, the solidification pressure becomes low. When conducting electrical conductivity measurements, etc., under ultra-high pressure, a conductive paste can be used for the electrode. When the alkyl group contains 7 or more carbon atoms, the conductive paste can dissolve. Although R a21 , R a22 , R a23 and R a24 may represent the same alkyl group or different alkyl groups, R a21 , R a22 , R a23 and R a24 are preferably the same alkyl group from the viewpoint of more easily achieving the manifestation of the effects of the present invention.

[0024] From the viewpoint of more easily achieving the manifestation of the effects of the present invention (in particular, from the viewpoint of further easily increasing the solidification pressure), an alkyl group that can be selected as R a21 , R a22 , R a23 and R a24 preferably has from 3 to 5 carbon atoms, more preferably has from 3 to 4 carbon atoms, and even more preferably has 3 carbon atoms.

[0025] Alkyl group that can be selected as R a21 , R a22 , R a23 and R a24 , may be linear or branched, but is preferably linear from the point of view of more easily achieving the manifestation of the effects of the present invention.

[0026] In the general formula (a2) Z a2means a silicon atom, a germanium atom, a tin atom or a lead atom. From the viewpoint of more easily achieving the manifestation of the effects of the present invention (in particular, from the viewpoint of further easily increasing the solidification pressure), Z a2 preferably represents a silicon atom.

[0027] Components Other than Compound (A)The pressure generating medium of the present embodiment may contain other components other than the component (A), provided that the effects of the present invention are not significantly deteriorated, and does not need to contain other components other than the component (A). Examples of such other components include at least one additive selected from antioxidants, corrosion inhibitors, extreme pressure agents, friction modifiers, rust inhibitors, antifoam agents, and viscosity index improvers. The total content of such additives is preferably 0.01 to 30 mass%, more preferably 0.01 to 20 mass%, even more preferably 0.05 to 15 mass%, and even more preferably 0.1 to 10 mass%, based on the total amount of the pressure generating medium.

[0028] The pressurizing working medium of the present embodiment may contain a raw material compound or a by-product obtained in the synthesis process of component (A), provided that the effects of the present invention are not significantly deteriorated. However, the content of the raw material compound and the by-product is preferably small. More specifically, the content of the raw material compound and the by-product each independently is preferably 5% by mass or less, more preferably 1% by mass or less, and even more preferably 0.1% by mass or less.

[0029] Various physical properties of the pressurizing working medium. Solidification pressure. The pressurizing working medium of the present embodiment has a solidification pressure of greater than 2.7 GPa at room temperature. The solidification pressure is preferably greater than 3.0 GPa, more preferably greater than 3.5 GPa, even more preferably greater than 4.1 GPa, even more preferably 4.5 GPa or more, even more preferably 5.0 GPa or more, and even more preferably 5.2 GPa or more. Therefore, the pressurizing working medium of the present embodiment can maintain a liquid state and can sufficiently function as a pressurizing working medium even under ultra-high pressure conditions.The value of the upper limit of the solidification pressure at room temperature of the working medium for creating pressure according to the present embodiment is not particularly limited, and the larger the value of the upper limit, the better, and the value of the upper limit is usually less than 6.0 GPa. In the present description, the solidification pressure at room temperature means the value measured by the method described in the examples below.

[0030] The kinematic viscosity at 40°C of the pressure generating working medium of the present embodiment, the kinematic viscosity at 40°C is preferably greater than 1.0 mm 2 / sec, more preferably 1.5 mm 2 / sec or more and even more preferably 2.0 mm 2 / sec or more in terms of leakage suppression from the working fluid pressure sensor to create pressure during pressure application. Typically, it is 10 mm 2 / sec or less. In this specification, the kinematic viscosity at 40°C means the value measured in accordance with JIS K2283:2000.

[0031] Melting pointIn the pressurizing working medium of the present embodiment, the melting point is preferably -50°C or less, more preferably -60°C or less, and even more preferably -70°C or less, from the viewpoint of obtaining a pressurizing working medium that does not solidify even at a low temperature and that can be used even in low-temperature experiments.The lower limit of the melting point of the pressurizing working medium of the present embodiment is not particularly limited and is usually -100°C or more.In the present description, the melting point means a value measured by a differential scanning calorimetry method (hereinafter, may also be referred to as the "DSC method").

[0032] Flash pointIn the pressurizing working medium of the present embodiment, the flash point is preferably 60°C or more, more preferably 65°C or more, and even more preferably 70°C or more from the viewpoint of ensuring safety at a temperature significantly higher than room temperature.The upper limit value of the flash point of the pressurizing working medium of the present embodiment is not particularly limited and is generally 100°C or less.In the present description, the flash point means a value measured in a closed cup by the Pensky-Martens method (PM method) in accordance with the JIS K2265-3:2007 standard.

[0033] Use of a pressure generating mediumThe pressure generating medium of the present embodiment has a solidification pressure at room temperature of more than 2.7 GPa and a flash point significantly higher than room temperature. Therefore, the pressure generating medium of the present embodiment is suitable as a pressure generating medium used in a pressure application system that applies pressure to a substance. Therefore, according to the pressure generating medium of the present embodiment, methods (1) and (2) are provided below.(1) A method of using a pressure generating medium, which includes applying pressure to a substance through the pressure generating medium of the present embodiment.(2) A method of using a pressure generating medium according to the above item (1), in which the pressure is more than 2.7 GPa.The method of using the working medium for creating pressure according to the above item (2) is carried out under conditions of room temperature or in a temperature range near it. However, after applying a predetermined pressure to the substance through the working medium for creating pressure, the working medium for creating pressure can be cooled and solidified at the maintained pressure, and the pressure can be continuously applied to the substance.

[0034] As described above, in the working environment for creating pressure according to the present embodiment, the solidification pressure at room temperature is preferably greater than 3.0 GPa, more preferably greater than 3.5 GPa, even more preferably greater than 4.1 GPa, even more preferably 4.5 GPa or more, even more preferably 5.0 GPa or more, and even more preferably 5.2 GPa or more. Therefore, the pressure range according to the above aspect (2) may be any of these ranges.

[0035] One proposed embodiment of the invention

[0001] -

[12] .

[0001] A working medium for creating pressure, including at least one organic compound (A) containing an element of group 14 selected from the group consisting of a compound (A1) represented by the general formula (a1) and a compound (A2) represented by the general formula (a2): where each of the substituents R a11 , R a12 , R a13 and R a14 independently represents an alkyl group having from 3 to 6 carbon atoms, and Z a1 means a carbon atom or a silicon atom; where each of the substituents R a21 , R a22 , R a23 and R a24 independently represents an alkyl group having from 3 to 6 carbon atoms, and Z a2 means a silicon atom, a germanium atom, a tin atom, or a lead atom.

[0002] The working medium for creating pressure according to the above item [1], in which in the general formula (a1) R a11 , R a12 , R a13 and R a14 represent the same alkyl group.

[0003] The working medium for creating pressure according to the above item [1] or [2], in which in the general formula (a2) R a21 , R a22 , R a23 and R a24 represent the same alkyl group.

[0004] A working medium for creating pressure according to any of the above items [1]-[3], in which in the general formula (a1) Z a1 means silicon atom.

[0005] Working environment for creating pressure according to any of the above items [1]-[4], in which in the general formula (a2) Z a2 means silicon atom.

[0006] A pressure-generating working medium according to any one of the above items [1] to [5], which has a solidification pressure at 25°C greater than 4.1 GPa.

[0007] A pressure-generating working medium according to any one of the above items [1] to [6], which has a kinematic viscosity at 40°C greater than 1.0 cm 2 / sec.

[0008] A pressure-generating working medium according to any one of the above items [1] to [7], which has a melting point of -50°C or less.

[0009] A pressurizing working medium according to any one of the above items [1] to [8], which has a flash point of 70°C or more.

[0010] Working medium for creating pressure according to any of the above items [1] _

[0009] , in which the content of the organic compound (A) containing the element of group 14 is from 70 to 100% by mass, based on the total amount of the working medium for creating pressure.

[0011] A method of using a working medium to create pressure, which comprises applying pressure to a substance through the working medium to create pressure according to any one of the above [1] to

[10] .

[0012] The method of using the working medium to create pressure according to the above item

[11] , in which the pressure is greater than 4.1 GPa. Examples

[0036] The present invention is specifically described by means of the following examples, but the invention is not limited to the examples given.

[0037] Examples 1-3 and Comparative Examples 1-3Various properties from (1)-(4) below are measured or estimated on a pressure-generating medium consisting of any of the following compounds.

[0038] Example 1 Tetra-n-propoxysilane In the general formula (a2), each of the substituents R a21 , R a22 , R a23 and R a24 represents an n-propyl group, Z a2 means silicon atom, and this compound corresponds to compound (A2).

[0039] Example 2Tetra-n-butoxysilaneIn the general formula (a2), each of the substituents R a21 , R a22 , R a23 and R a24 represents an n-butyl group, Z a2 means silicon atom, and this compound corresponds to compound (A2).

[0040] Example 3 Tetra-n-butylsilane In the general formula (a1), each of the substituents R a11 , R a12 , R a13 and R a14 represents an n-butyl group, Z a1 means silicon atom and this compound corresponds to compound (A1).

[0041] Comparative Example 1HexaethyldisiloxaneThis compound is represented by the following structural formula:

[0042] Comparative Example 2Tetrakis(trimethylsiloxy)silaneThis compound is represented by the following structural formula:

[0043] Comparative Example 3TetraethoxysilaneThis compound is a compound in which in the general formula (a2), each of the substituents R a21 , R a22 , R a23 and R a24 means ethyl group.

[0044] Measurement Method or Evaluation Method of Various Physical Properties(1) Kinematic viscosity at 40°CMeasurement is carried out according to JIS-K2283:2000.(2) Melting pointMeasurement is carried out by the differential scanning calorimetry (DSC) method.(3) Flash PointMeasurement is carried out in a closed crucible by the Pensky-Martens method (PM method) in accordance with JIS K2265-3:2007.(4) Freezing PressureIn an environment of 25°C, a strain gauge is placed in a cubic pressure vessel, and the pressure vessel is filled with a working medium to generate pressure. To apply ultra-high pressure, increased pressure is generated in 6 directions in the pressure vessel, and the resistance value of the strain gauge is measured at this time. The relationship between pressure and resistance value is plotted as a graph, and the point at which the curve of resistance value versus pressure suddenly bends is defined as the solidification pressure point.The strain gauge is a tabular measuring device, and the resistance value decreases with increasing compression. When the pressure-generating medium remains liquid, the entire device compresses and contracts uniformly, and the device's compression can be detected. However, when pressure is increased through a solidified pressure-generating medium, the compression of the solidified pressure-generating medium is detected, and therefore, the strain gauge's compression ratio increases, causing the resistance value to rapidly decrease at the boundary of the solidification pressure point. Consequently, a point appears on the pressure-resistance graph where the resistance-pressure curve curve exhibits an inflection point, and this point is identified as the "solidification pressure point."In the case where temperature control at 25°C is difficult, the sample can be analyzed at two temperatures close to 25°C (at a temperature below 25°C and a temperature above 25°C), and the solidification pressure at 25°C can be calculated as a linear interpolation value.

[0045] The results are presented in Table 1.

[0046]

[0047] The data in Table 1 show the following. Each of the pressure-generating working media of Examples 1-3 has a high solidification pressure and a flash point significantly higher than room temperature. On the other hand, each of the pressure-generating working media of Comparative Examples 1 and 2 has a low solidification pressure. The pressure-generating working medium of Comparative Example 3 has a low flash point. It was tested whether the conductive paste would dissolve in each of the pressure-generating working media of Examples 1-3 and Comparative Examples 1-3, and it was confirmed that the conductive paste did not dissolve in any of the pressure-generating working media of Examples 1-3 and Comparative Examples 1-3.

Claims

1. The use of at least one organic compound (A) containing an element of group 14 as a pressure generating medium, wherein the compound (A) is selected from the group consisting of a compound (A1) represented by the general formula (a1) and a compound (A2) represented by the general formula (a2): where each of the substituents R a11 , R a12 , R a13 and R a14 represents the same unbranched alkyl group having 4 carbon atoms, and Z a1 means silicon atom; where each of the substituents R a21 , R a22 , R a23 and R a24 represents the same unbranched alkyl group having from 3 to 4 carbon atoms, and Z a2 means silicon atom.

2. The use according to paragraph 1, according to which the pressure-generating medium has a solidification pressure at 25°C greater than 4.1 GPa.

3. The use according to paragraph 1 or 2, according to which the pressure generating medium has a kinematic viscosity at 40°C greater than 1.0 mm 2 / sec.

4. The use according to any one of paragraphs 1-3, according to which the pressure-generating medium has a melting point of -50°C or less.

5. The use according to any one of paragraphs 1-4, according to which the pressure generating medium has a flash point of 70°C or more.

6. The use according to any one of paragraphs 1-5, according to which the content of the organic compound (A) containing an element of group 14 is from 70 to 100% by weight based on the total amount of the pressure-generating medium.

7. A method of using a pressure-generating medium, which comprises applying pressure to a substance by means of a pressure-generating medium containing at least one organic compound (A) containing an element of group 14, wherein the compound (A) is selected from the group consisting of a compound (A1) represented by the general formula (a1) and a compound (A2) represented by the general formula (a2): where each of the substituents R a11 , R a12 , R a13 and R a14 represents the same unbranched alkyl group having 4 carbon atoms, and Z a1 means silicon atom; where each of the substituents R a21 , R a22 , R a23 and R a24 represents the same unbranched alkyl group having from 3 to 4 carbon atoms, and Z a2 means silicon atom.

8. The method according to claim 7, wherein the pressure is greater than 4.1 GPa.

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