JP7412199B2 - Method for manufacturing heat storage material - Google Patents

Description

The present invention relates to a method for manufacturing a heat storage material.

BACKGROUND OF THE INVENTION Some products, such as pharmaceuticals and foods, need to be kept cold or warm within a predetermined temperature range during transportation in order to maintain their quality.

Conventionally, as a method of keeping such items cold or warm, a heat storage material that has been melted or solidified in advance is placed inside an insulating transport container, and the latent heat of this heat storage material is used to store the goods in the transport container. There are known methods for keeping objects cool or warm. In order to maintain items to be kept cold or warm within a predetermined temperature range for a long time, a heat storage material that has a melting temperature and/or solidification temperature within a predetermined temperature range and a large amount of latent heat is required. It is preferable to use

Many products such as pharmaceuticals and foods need to be transported under temperature control of 2° C. to 8° C., and the development of heat storage materials that enable such temperature control is currently underway.

Examples of the form of the heat storage material include a form in which a main agent is filled in a container. At this time, if the base agent is a flammable substance (for example, tetradecane, which is classified as a dangerous substance, class 4, petroleum, under the Fire Service Act), it is necessary to gel the base agent and make it non-hazardous. be. Therefore, gelling agents (for example, Patent Documents 1 and 2) for gelling liquid oils and fats, which are main ingredients, and heat storage materials in which liquid main ingredients are fixed (solidified) are currently being developed ( For example, see Patent Documents 3 and 4).

Japanese Patent Application Publication No. 9-316436 Japanese Patent Application Publication No. 2000-109787 Japanese Patent Application Publication No. 2009-120734 Japanese Patent Application Publication No. 2014-122320

As described above, heat storage materials in which a liquid main ingredient is solidified have been developed, but there is still room for further improvement in the manufacturing process of such heat storage materials.

One aspect of the present invention aims to realize a new technique for efficiently manufacturing a gelled heat storage material composition.

As a result of intensive studies to solve the above problems, the present inventors found that a heat storage material composition containing a specific base ingredient, a specific gelling agent, and a specific gelling auxiliary agent has a temperature equal to or higher than the solidification start temperature of the base ingredient. We discovered that acceleration of gelation can be suppressed in an environment of 15.0°C or lower, and when producing a gelled heat storage material composition, we put the heat storage material composition in a container while suppressing the acceleration of gelation of the liquid main ingredient. The present invention has been completed in which a heat storage material is produced by filling the container into a container and gelling the heat storage material composition within the container after filling.

That is, one embodiment of the present invention includes the following configuration.

[1] It has a preparation step of preparing a heat storage material composition containing a base agent, a gelling agent, and a gelling auxiliary agent, and a filling step of filling a container with the heat storage material composition obtained in the preparation step. , the main agent is at least one selected from the group consisting of tetradecane, pentadecane, and methyl laurate, the gelling agent is aluminum 2-ethylhexanoate, and the gelling aid is a fatty acid compound. , and higher alcohol, and in the preparation step and the filling step, the heat storage material composition is maintained at a temperature not lower than the solidification start temperature of the main ingredient and not higher than 15.0° C. Method for manufacturing heat storage material.

[2] The method for producing a heat storage material according to [1], wherein the viscosity of the heat storage material composition in the filling step is less than 100 mPa·s.

[3] The method for producing a heat storage material according to [1] or [2], wherein the filling step is performed 2.0 hours or more after the preparation step.

According to one aspect of the present invention, it is possible to efficiently produce a gelled heat storage material composition.

1 is a graph showing the measurement results of the viscosity of a heat storage material composition in an example of the present invention.

An embodiment of the present invention will be described below, but the present invention is not limited thereto. The present invention is not limited to each configuration described below, and various changes can be made within the scope of the claims. Further, embodiments or examples obtained by appropriately combining technical means disclosed in different embodiments or examples are also included in the technical scope of the present invention. Furthermore, new technical features can be formed by combining the technical means disclosed in each embodiment. Note that all academic literature and patent literature described in this specification are incorporated as references in this specification. In addition, unless otherwise specified in this specification, the numerical range "A to B" is intended to be "above A (including A and greater than A) and less than or equal to B (including B and less than B)."

[1. Technical idea of one embodiment of the present invention]
The present inventor tried two methods in developing a heat storage material according to an embodiment of the present invention. First, the present inventor mixed a base agent, a gelling agent, and a gelling aid to gel the base agent, and then performed a method of filling a container with the base agent. However, in this method, (i) the gelled base agent contains a lot of air when it is filled into the container, making it difficult to fill the container with the base agent, and (ii) the base agent remains in the filling device. It has been found that a problem arises in that it takes time to wash the gelled base agent.

Therefore, the present inventor attempted a method of gelling the base agent within the container by separately filling the container with the base agent, gelling agent, and gelling aid. However, it has been found that this method has a problem in that (iii) the concentrations of the three components within the container are not uniform, resulting in incomplete gelation of the base ingredient.

Therefore, in order to solve the above-mentioned problems (i) to (iii), the inventors of the present invention have conducted further studies and found that a specific base agent, a specific gelling agent, and a specific gelling auxiliary agent are used. It has been found that the heat storage material composition containing the above-mentioned heat storage material can extend the time required for gelation in an environment where the temperature is higher than the solidification start temperature of the main ingredient and lower than 15.0°C. Based on this new knowledge, after preparing a heat storage material composition containing a base agent, a gelling agent, and a gelling aid, the liquid heat storage material composition is poured into a container while delaying gelation of the heat storage material composition. The present invention has been completed, which makes it possible to efficiently produce a solidified heat storage material by filling the container and gelling the heat storage material composition within the container. Hereinafter, one embodiment of the present invention will be explained in detail.

[2. Method for manufacturing heat storage material]
A method for manufacturing a heat storage material according to an embodiment of the present invention includes a preparation step of preparing a heat storage material composition containing a base agent, a gelling agent, and a gelling auxiliary agent, and a heat storage material composition obtained in the preparation step. The main agent is at least one selected from the group consisting of tetradecane, pentadecane, and methyl laurate, and the gelling agent is aluminum 2-ethylhexanoate. The gelling aid is at least one selected from the group consisting of fatty acid compounds and higher alcohols, and in the preparation step and the filling step, the heat storage material composition is heated to 15.0° C. above the coagulation start temperature of the main ingredient. Keep below.

The heat storage material composition described above contains specific materials, and each material can be uniformly mixed in the preparation process. With this configuration, (i) the heat storage material composition can be uniformly gelled within the container.

The heat storage material composition described above can extend the time required for gelation in an environment where the temperature is higher than the solidification start temperature of the main ingredient and lower than 15.0°C. For example, the heat storage material composition may remain in a liquid state for 2.0 hours or more. With this configuration, (ii) the container can be filled with the heat storage material composition while ensuring a long working time. If a long working time can be secured, for example, it is possible to perform a desired separate process between the preparation process and the filling process, and/or to fill a large amount of the heat storage material composition into a large container over time. .

The heat storage material composition described above may be filled into a container in a liquid state. With this configuration, (iii) it is possible to easily fill the container with the heat storage material composition, and (iv) it is possible to prevent the gelled heat storage material composition from remaining in the filling device.

Each step will be explained below.

[2-1. Preparation process]
The preparation step is a step of preparing a heat storage material composition containing a base agent, a gelling agent, and a gelling auxiliary agent.

In the preparation step, (1) the heat storage material composition may be prepared by stirring the base agent, the gelling agent, and the gelling auxiliary agent at the time of mixing, or (2) after preparing the heat storage material composition, the heat storage material composition may be mixed. The heat storage material composition may be stirred, or (3) both of the above-mentioned stirring (1) and (2) may be performed. Note that the method of stirring is not limited, and for example, stirring may be performed using a known stirrer. According to this configuration, it is possible to obtain a heat storage material composition in which the base agent, gelling agent, and gelling auxiliary agent are mixed more uniformly. Moreover, according to the configuration, the time required for gelation of the heat storage material composition can be extended by stirring.

In each of the above-mentioned stirrings (1) to (3), stirring may be performed for a desired time by repeating a cycle consisting of (i) stirring treatment and non-stirring treatment a desired number of times, or (ii) Stirring may be performed for a desired time by performing only the stirring process.

In the preparation step, the heat storage material composition is maintained at a temperature higher than the solidification start temperature of the main ingredient and lower than 15.0°C. The upper limit of the temperature is preferably 13°C or lower, more preferably 10°C or lower, and most preferably 8°C or lower. The lower limit of the temperature is preferably the coagulation start temperature of the main ingredient + 1°C or more, more preferably the coagulation start temperature of the main ingredient + 2°C or more, and most preferably the coagulation start temperature of the main ingredient + 3°C or more. With this configuration, the time required for gelling the heat storage material composition can be extended for a longer time without solidifying the base agent. The main agent is at least one selected from the group consisting of tetradecane, pentadecane, and methyl laurate. The coagulation onset temperature of tetradecane is 2.0°C, the coagulation onset temperature of pentadecane is 9.0°C, and the coagulation onset temperature of methyl laurate is 1.4°C.

The method for maintaining the heat storage material composition at the above-mentioned temperature is not particularly limited. For example, the preparation step may be performed in a tank set to the above-mentioned temperature range by a cooling device.

Below, each component constituting the heat storage material composition, the physical properties of the heat storage material composition, etc. will be explained.

[A. Main ingredient]
As used herein, the term "base agent" refers to a substance that accounts for 50% by weight or more in 100% by weight of the heat storage material composition. The main agent is at least one selected from the group consisting of tetradecane, pentadecane, and methyl laurate. From the viewpoint of transporting the article under temperature control of 2° C. to 8° C., the main ingredient preferably contains at least tetradecane or methyl laurate.

The content of the main agent in the heat storage material composition is preferably 50% by weight or more, more preferably 65% by weight or more, even more preferably 80% by weight or more, and 90% by weight or more based on 100% by weight of the heat storage material composition. is particularly preferred.

[B. Gelling agent]
The gelling agent is aluminum 2-ethylhexanoate.

The content of the gelling agent in the heat storage material composition is preferably 0.5% to 20% by weight, more preferably 1% to 15% by weight, and more preferably 1% to 10% by weight based on 100% by weight of the heat storage material composition. % by weight is more preferred, and 2% to 6% by weight is particularly preferred.

[C. Gelling aid]
The gelling aid is at least one selected from the group consisting of fatty acid compounds and higher alcohols. Fatty acid compounds include fatty acids, metal salts of fatty acids, and fatty acid esters.

Note that the main agent and the gelling aid are different substances. For example, methyl laurate can serve as a main ingredient, but since it is a fatty acid ester, it can also function as a gelling aid. Therefore, when methyl laurate is used as the main ingredient, it is preferable to use a fatty acid compound other than methyl laurate as the gelling aid.

The content of the gelling aid in the heat storage material composition is preferably 0.1% to 30.0% by weight based on 100% by weight of the heat storage material composition. When the gelling aid is a fatty acid compound, the content of the gelling aid in the heat storage material composition is preferably 0.2% to 5.0% by weight, and preferably 0.3% to 4.0% by weight. is more preferred, and 0.4% by weight to 3.0% by weight is particularly preferred. When the gelling aid is a higher alcohol, the content of the gelling aid in the heat storage material composition is preferably 1.0% to 30.0% by weight, and 3.0% to 30.0% by weight. is more preferable, and 5.0% by weight to 25.0% by weight is particularly preferable.

When the gelling aid is a fatty acid compound, the amount of the gelling aid is preferably 1/2 to 1/3 times the amount of the gelling agent. When the gelling aid is a higher alcohol, the amount is preferably 1 to 6 times the amount of the gelling agent. With this configuration, not only can gelation of the heat storage material composition be delayed for a long time, but also the heat storage material composition can be sufficiently gelled within the container.

The fatty acid compound is not particularly limited, and may be, for example, a fatty acid compound that is solid at room temperature (for example, 25° C.), but is preferably a fatty acid compound that is liquid at room temperature.

The fatty acid in the fatty acid compound may be a saturated fatty acid or an unsaturated fatty acid. The lower limit of the number of carbon atoms constituting the fatty acid compound is not limited, and may be, for example, 4, 5, 6, 7, or 8. The upper limit of the number of carbon atoms constituting the fatty acid compound is not limited, and may be, for example, 30, 28, 26, 24, or 22.

Specific examples of the above-mentioned fatty acids include, for example, caprylic acid, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, and behenic acid, and mixtures of these fatty acids.

Specific examples of the metal salts of the fatty acids mentioned above include sodium caprylate, sodium laurate, sodium myristate, sodium palmitate, sodium stearate, sodium oleate, and sodium behenate, and mixtures of these metal salts. can be mentioned.

As a specific example of the above-mentioned fatty acid ester, for example, sorbitan fatty acid ester can be mentioned.

Specific examples of the above-mentioned sorbitan fatty acid esters include sorbitan monocaprylate, sorbitan monolaurate, sorbitan monomyristate, sorbitan monopalmitate, sorbitan monostearate, sorbitan monooleate, and sorbitan monobase. henate, sorbitane dicaprylate, sorbitane dilaurate, sorbitane dimyristate, sorbitane dipalmitate, sorbitan distearate, sorbitan dioleate, sorbitan dibehenate, sorbitan tricaprylate, sorbitan trilaurate, sorbitan trimistate , sorbitan tripalmitate, sorbitan tristearate, sorbitan trioleate, sorbitan tribehenate, sorbitan sesquicaprylate, sorbitan sesquilaurate, sorbitan sesquimyristate, sorbitan sesquipalmitate, sorbitan sesquistearate, sorbitan sesquioleate , sorbitan sesquibehenate, and the like.

Among these, sorbitan monofatty acid ester in which one fatty acid is ester bonded to sorbitan, or sorbitan sesquifatty acid ester in which three molecules of fatty acid are bonded to two molecules of sorbitan are more preferable. Further, it is more preferably at least one selected from the group consisting of sorbitan monooleate, sorbitan monolaurate, sorbitan sesquioleate and sorbitan monostearate, and more preferably at least one selected from the group consisting of sorbitan monooleate and sorbitan sesquioleate. It is particularly preferable to use at least one selected from the following.

In addition, as long as it has an ester bond consisting of sorbitan and fatty acid, sorbitan fatty acid ester has other structures, such as the structure of polyoxyethylene (also referred to as POE) (structural formula: - [OCH ₂ CH ₂ ] _n - (n is any number)). Sorbitan fatty acid ester having a polyoxyethylene structure is sometimes referred to as POE sorbitan fatty acid ester or POE(X) sorbitan fatty acid ester. The above X represents the number of repeating units of oxyethylene, and represents the value of n in the above structural formula.

Specific examples of POE sorbitan fatty acid esters include POE (20) sorbitan monolaurate, POE (6) sorbitan monolaurate, POE (20) sorbitan monopalmitate, POE (20) sorbitan monostearate, POE ( 6) Sorbitan monostearate, POE (20) sorbitan tristearate, POE (20) sorbitan monooleate, POE (6) sorbitan monooleate, POE (20) sorbitan trioleate, POE (160) sorbitan triisostere POE (20) sorbitan monolaurate.

The sorbitan fatty acid ester is preferably a sorbitan monofatty acid ester or a sorbitan sesquifatty acid ester. More preferably, the sorbitan fatty acid ester is at least one selected from the group consisting of sorbitan monooleate, sorbitan monolaurate, sorbitan sesquioleate, and sorbitan monostearate. According to this configuration, the solidification start temperature of the obtained heat storage material composition can be 1°C to 10°C. As a result, there is an advantage that the temperature of the temperature-controlled article can be maintained more stably and with higher accuracy within the range of 1° C. to 10° C. and at a desired controlled temperature.

As mentioned above, the gelling aid may be a higher alcohol. The higher alcohol is not limited, and examples thereof include higher alcohols having 10 or more carbon atoms, 12 or more carbon atoms, or 14 or more carbon atoms. At this time, the upper limit of the number of carbon atoms is not limited, and may be, for example, 30, 28, 26, 24, or 22. Specific examples of the higher alcohol include decanol, lauryl alcohol, and myristyl alcohol.

[D. Other ingredients]
The heat storage material composition may contain other components in addition to the base agent, gelling agent, and gelling aid.

The content of other components in the heat storage material composition is preferably 50 parts by weight or less, when the total amount of the main agent, gelling agent, and gelling auxiliary agent contained in the heat storage material composition is 100 parts by weight. More preferably 40 parts by weight or less, more preferably 30 parts by weight or less, more preferably 20 parts by weight or less, more preferably 10 parts by weight or less, most preferably 5 parts by weight or less.

Specific examples of the other components include, for example, metals such as light metals and heavy metals, metal ions such as light metal ions and heavy metal ions, crystal nucleating agents, phase separation inhibitors, fragrances, colorants, antibacterial agents, high molecular weight polymers, Other organic compounds or other inorganic compounds can be mentioned.

Specific examples of the light metal include aluminum, magnesium, beryllium, and titanium. Heavy metals include iron, lead, gold, platinum, silver, copper, chromium, cadmium, mercury, zinc, arsenic, manganese, cobalt, nickel, molybdenum, tungsten, tin, bismuth, uranium, and plutonium.

[E. Physical properties of heat storage material composition]
The heat storage material composition may have a melting temperature within the range of 1°C to 10°C. As used herein, the "melting temperature" of a heat storage material composition is intended to mean "the temperature that a solid heat storage material composition exhibits while it melts and gels." For example, if the heat storage material composition in a solidified state is placed in a thermostatic oven and then the temperature of the thermostatic oven is raised from a low temperature (for example, -50°C) at a constant temperature increase rate, the temperature of the heat storage material composition changes in the following order (1) to (3): (1) rises at a constant rate; (2) hardly changes at temperature T ₁ due to the latent heat of _the heat storage material composition; A constant temperature is maintained until T ₂ ; (3) After the temperature reaches T ₂ , the increase is resumed. In this specification, temperature T ₁ is referred to as "melting start temperature" and temperature T ₂ is referred to as "melting end temperature". The temperature T ₃ at the midpoint between the temperatures T ₁ and T ₂ is defined herein as the “melting temperature”.

The melting temperature of the heat storage material composition may be 1°C to 10°C, preferably 1°C to 9°C, more preferably 2°C to 8°C, even more preferably 2°C to 7°C, and even more preferably 3°C to 5°C. is particularly preferred. According to this configuration, there is an advantage that the temperature-controlled article can be kept warm at a desired controlled temperature with higher accuracy.

The melting start temperature of the heat storage material composition is not particularly limited, but is preferably 1°C to 10°C, more preferably 1°C to 8°C, even more preferably 1°C to 6°C, particularly preferably 2°C to 4°C. . This configuration has the advantage that the temperature-controlled article can be maintained at a desired controlled temperature with higher accuracy.

The melting end temperature of the heat storage material composition is not particularly limited, but is preferably 1°C to 10°C, more preferably 2°C to 9°C, even more preferably 2°C to 7°C, and particularly preferably 3°C to 6°C. . This configuration has the advantage that the temperature-controlled article can be maintained at a desired controlled temperature with higher accuracy.

The absolute value of the difference between the melting start temperature and the melting end temperature (temperature T ₁ - temperature T ₂ ) of the heat storage material composition is not particularly limited, but is preferably from 0 to 10, more preferably from 0 to 8, and from 0 to 8. 5 is more preferred, 0 to 4 is more preferred, 0 to 3 is even more preferred, and 0 to 2 is particularly preferred. This configuration has the advantage that the temperature-controlled article can be maintained at a desired controlled temperature with higher accuracy.

The heat storage material composition preferably has a solidification start temperature within the range of -2°C to 10°C. In this specification, the "solidification start temperature" of a heat storage material composition refers to "the temperature that the gel-like heat storage material composition exhibits when it begins to solidify, in other words, when it begins to solidify." intend to. For example, when a molten heat storage material composition according to an embodiment of the present invention is placed in a thermostatic oven, and then the temperature of the thermostatic oven is lowered from a high temperature (for example, 50°C) at a constant temperature decreasing rate. , the temperature of the heat storage material composition changes in the following order (1) to (3): (1) the temperature decreases at a constant rate until the temperature T ₄ ; (2) the temperature decreases slightly from the temperature T ₄ to the temperature T ₅ (3) After temperature _T5 , the temperature hardly changes due to the latent heat of the heat storage material composition, and the temperature is maintained constant from temperature _T5 to temperature _T6 ; (3) After temperature _T6 , the temperature starts to decrease again. In this specification, temperature T ₄ is referred to as "solidification start temperature" and temperature T ₆ is referred to as "solidification end temperature". Further, in this specification, the temperature _T5 is referred to as "maximum temperature during solidification."

The solidification start temperature of the heat storage material composition is more preferably -2°C to 10°C, more preferably -1°C to 10°C, more preferably 0°C to 10°C, more preferably 1°C to 10°C, and more preferably 1°C to 10°C. C. to 7.degree. C. is more preferable, and 2.degree. C. to 5.degree. C. is particularly preferable. This configuration has the advantage that the temperature-controlled article can be maintained at a desired controlled temperature with higher accuracy.

The temperature at which the solidification of the heat storage material composition ends is not particularly limited, but is preferably -5°C to 10°C, more preferably -3°C to 8°C, more preferably -2°C to 7°C, and -1°C to 7°C. The temperature is more preferably 0°C to 7°C, even more preferably 1°C to 7°C, and particularly preferably 2°C to 5°C. This configuration has the advantage that the temperature-controlled article can be maintained at a desired controlled temperature with higher accuracy.

The absolute value of the difference between the solidification start temperature and the solidification end temperature (temperature T ₄ - temperature T ₆ ) of the heat storage material composition is not particularly limited, but is preferably from 0 to 10, more preferably from 0 to 8, and from 0 to 8. 5 is more preferred, 0 to 4 is more preferred, 0 to 3 is even more preferred, and 0 to 2 is particularly preferred. This configuration has the advantage that the temperature-controlled article can be maintained at a desired controlled temperature with higher accuracy.

In the heat storage material composition, the absolute value of the difference between the maximum temperature during solidification and the temperature at which solidification ends (temperature T ₅ - temperature T ₆ ) is not particularly limited, but is preferably from 0 to 10, more preferably from 0 to 8. 0 to 5 are more preferred, 0 to 4 are more preferred, 0 to 3 are even more preferred, and 0 to 2 are particularly preferred. This configuration has the advantage that the temperature-controlled article can be maintained at a desired controlled temperature with higher accuracy.

The absolute value of the difference between the melting start temperature and the solidification start temperature (temperature T ₁ - temperature T ₄ ) of the heat storage material composition is not particularly limited, but is preferably 0 to 10, more preferably 0 to 8, and 0 to 5 is more preferred, 0 to 4 is more preferred, 0 to 3 is even more preferred, and 0 to 2 is particularly preferred. This configuration has the advantage that the temperature-controlled article can be maintained at a desired controlled temperature with higher accuracy.

[2-2. Filling process]
The filling step is a step of filling a container with the heat storage material composition obtained in the preparation step.

In the filling step, the heat storage material composition is maintained at a temperature higher than the solidification start temperature of the main ingredient and lower than 15.0°C. The upper limit of the temperature is preferably 13°C or lower, more preferably 10°C or lower, and most preferably 8°C or lower. The lower limit of the temperature is preferably the coagulation start temperature of the main ingredient + 1°C or more, more preferably the coagulation start temperature of the main ingredient + 2°C or more, and most preferably the coagulation start temperature of the main ingredient + 3°C or more. With this configuration, the time required for gelling the heat storage material composition can be extended for a longer time without solidifying the base agent.

In addition, in the filling process, it is sufficient that the temperature of the heat storage material composition can be maintained at least within the above-mentioned temperature range until it is filled into the container, and the temperature of the heat storage material composition after being filled into the container is within the above-mentioned temperature range. The temperature may or may not be maintained within the above-mentioned temperature ranges.

The method for maintaining the heat storage material composition at the above-mentioned temperature is not particularly limited. For example, after performing the above-mentioned preparation process in a tank set to the above-mentioned temperature range by a cooling device, the prepared heat storage material composition is filled into a container using a pump (e.g., Mono pump) and a filling machine. do it. In this case, the pump and/or the filling machine may or may not be set within the above-mentioned temperature range, but it is preferable that the pump and/or the filling machine be set within the above-mentioned temperature range.

The heat storage material composition used in the present invention can extend the time required for gelation at temperatures below 15.0°C. Therefore, the viscosity of the heat storage material composition in the filling process (for example, the viscosity of the heat storage material composition immediately before filling the container (for example, 30 minutes, 10 minutes, or 1 minute before filling the container) ) is preferably less than 100 mPa·s, more preferably 90 mPa·s or less, more preferably 80 mPa·s or less, more preferably 70 mPa·s or less, more preferably 60 mPa·s or less, more preferably 50 mPa·s or less, It may be more preferably 40 mPa·s or less, more preferably 30 mPa·s or less, more preferably 20 mPa·s or less, and most preferably 10 mPa·s or less. The lower limit of the viscosity of the heat storage material composition in the filling step is not limited, and may be, for example, 1 mPa·s, 3 mPa·s, or 5 mPa·s.

The method of filling the container with the heat storage material composition is not limited, and for example, the heat storage material composition is supplied to a known filling machine using a known pump (for example, Mono pump), and the heat storage material composition is poured into the container from the filling machine. What is necessary is just to fill it with a composition.

The container is not limited, and any known container can be used.

The container is preferably made mainly of resin (for example, synthetic resin) from the viewpoint of preventing liquid leakage due to rust and corrosion caused by the heat storage material composition. Examples of the resin include polyvinyl chloride, polyethylene terephthalate, nylon, and polyester.

These materials may be used alone, or in order to improve heat resistance and barrier properties, two or more of these materials may be used in combination. From the viewpoint of handling and cost, it is preferable to use a container made of nylon or polyvinyl chloride.

The shape of the container is not limited, but from the viewpoint of efficiently exchanging heat between the heat storage material composition and the temperature-controlled article or the surrounding space through the container, it is thin and has a small surface area. A shape that allows for a large space is preferred. A heat storage material can be formed by filling these containers with a heat storage material composition.

As a more specific example of the above-mentioned container, there can be mentioned a container disclosed in JP-A No. 2015-78307. This document is incorporated herein by reference.

The timing of performing the filling process is not limited. Of course, the filling step can be performed after 0.5 hours, 1 hour, or 1.5 hours have elapsed after the preparation step, but the heat storage material composition has a temperature of 15.0° C. or lower, which is the time required for gelation. Even after 2.0 hours or more, 2.5 hours or more, 3.0 hours or more, 3.5 hours or more, or 4.0 hours or more after the preparation process, , a filling process can be performed. From the viewpoint of more reliably filling the container with the liquid filler composition, it is preferable to carry out the filling process within 24 hours after the preparation process, more preferably within 15 hours, and it is preferable to carry out the filling process within 15 hours. It is more preferable to carry out the filling process within 5 hours, and most preferably to carry out the filling process within 5 hours.

EXAMPLES Hereinafter, the present invention will be explained in more detail with reference to Examples, but the present invention is not limited to these Examples.

<Raw materials>
The raw materials used in the examples and comparative examples are as follows.

(base agent)
・Tetradecane (manufactured by JXTG Energy, TS paraffin TS4)
・Methyl laurate (manufactured by NOF Corporation, methyl laurate 95)
(gelling agent)
・Aluminum 2-ethylhexanoate (manufactured by Hope Pharmaceutical Co., Ltd., Octope Aluminum A)
(gelling aid)
・Oleic acid (manufactured by NOF Corporation, NAA-34)
・Lauryl alcohol (Kao Corporation, Calcol 2098)
<Production of heat storage material composition-1>
947.5 g of tetradecane was heated to a predetermined temperature (specifically, 7.0 to 8.5°C, 13.5 to 15.0°C, 18.5 to 20.0°C, 23.5-25.0°C or 30.0-31.5°C).

35.0 g of aluminum 2-ethylhexanoate was added to the tetradecane and stirred.

After confirming that the temperature of the mixture of tetradecane and aluminum 2-ethylhexanoate was at the predetermined temperature described above, an additional 17.5 g of oleic acid was added to the mixture.

After a predetermined period of time has elapsed since the addition of oleic acid, a portion of the mixture is taken as a sample, and after confirming that the temperature of the sample is at the predetermined temperature described above, the viscosity of the sample is was measured. After measuring the viscosity, the heat storage material composition was filled into a container.

<Production of heat storage material composition-2>
947.5 g of methyl laurate was adjusted to a predetermined temperature (specifically, 13.5 to 15.0° C.) using a water bath and ice.

35.0 g of aluminum 2-ethylhexanoate was added to the methyl laurate and stirred.

After confirming that the temperature of the mixture of tetradecane and aluminum 2-ethylhexanoate was at the predetermined temperature described above, an additional 17.5 g of oleic acid was added to the mixture.

After a predetermined period of time has elapsed since the addition of oleic acid, a portion of the mixture is taken as a sample, and after confirming that the temperature of the sample is at the predetermined temperature described above, the viscosity of the sample is was measured. After measuring the viscosity, the heat storage material composition was filled into a container.

<Production of heat storage material composition-3>
800.0 g of tetradecane was adjusted to a predetermined temperature (specifically, 13.5 to 15.0° C.) using a water bath and ice.

50.0 g of aluminum 2-ethylhexanoate was added to the tetradecane and stirred.

After confirming that the temperature of the mixture of tetradecane and aluminum 2-ethylhexanoate was the above-mentioned predetermined temperature, an additional 120.0 g of lauryl alcohol was added to the mixture.

After a predetermined period of time has elapsed since the addition of lauryl alcohol, a portion of the mixture is taken as a sample, and after confirming that the temperature of the sample is at the predetermined temperature described above, the viscosity of the sample is determined. was measured. After measuring the viscosity, the heat storage material composition was filled into a container.

<Measurement of viscosity>
The viscosity of the heat storage material composition was measured using a tuning fork type viscosity meter (Tuning fork vibration rheometer RV-10000A, manufactured by A&D Co., Ltd.). Note that the specific measurement method was in accordance with the protocol attached to the tuning fork type viscosity meter. Note that if the viscosity of the heat storage material composition is less than 100 mPa·s, the heat storage material composition is in a liquid state and can be easily filled into a container.

<Test results-1>
The test results when the temperature was changed (test results of the heat storage material composition prepared in <Production of heat storage material composition-1> described above) are shown in FIG. As shown in Figure 1, when the temperature is 7.0 to 8.5°C or 13.5 to 15.0°C, 2.0 hours have passed after adding the gelling aid. In both cases, the heat storage material composition remained in a liquid state and did not gel. This indicates that with the heat storage material composition, it is possible to fill a container with the liquid heat storage material composition after securing sufficient working time (at least 2.0 hours of working time). ing. Moreover, the heat storage material composition could be easily filled into a container.

On the other hand, as shown in FIG. After 2.0 hours, the heat storage material composition gelled. This indicates that in the case of the heat storage material composition concerned, it is difficult to secure sufficient working time for filling the container with the liquid heat storage material composition. Further, the heat storage material composition could not be easily filled into a container or could not be filled into a container.

In addition, from the above test results, the temperature of the heat storage material composition was maintained at 7.0 to 8.5°C or 13.5 to 15.0°C, and the liquid heat storage material composition was filled into the container. After that, if the temperature of the obtained heat storage material is raised to, for example, 18.5 to 20.0°C, 23.5 to 25.0°C, or 30.0 to 31.5°C, It can be understood that the heat storage material composition can be gelled.

<Test results-2>
(i) The heat storage material composition prepared under the conditions of 13.5 to 15.0°C in <Production of heat storage material composition-1> described above, (ii) The heat storage material composition prepared as described above For each of the heat storage material composition prepared in <Production-2> and (iii) the heat storage material composition prepared in <Production-3 of heat storage material composition> described above, a gelling auxiliary agent is added. The viscosity was measured 2.0 hours after adding the gelling aid, and those with a viscosity of less than 100 mPa・s at the time of 2 hours after adding the gelling aid were evaluated as "○", and the gelling aid was evaluated as "○". Those with a viscosity of 100 mPa·s or more 2 hours after the addition of the agent were evaluated as "x". The test results are shown in Table 1 below.

As shown in Table 1, all of the heat storage material compositions remained liquid and did not gel even after 2.0 hours had passed after adding the gelling aid, and the evaluation was "○". Met. This indicates that with the heat storage material composition, it is possible to fill a container with the liquid heat storage material composition after securing sufficient working time (at least 2.0 hours of working time). ing. Moreover, the heat storage material composition could be easily filled into a container. Furthermore, it has been shown that any of the heat storage material compositions can be gelled in the container if the temperature of the heat storage material is raised to 15.0°C or higher after 2.0 hours have passed since the addition of the gelling aid. confirmed.

INDUSTRIAL APPLICABILITY The present invention can be widely used in the field of manufacturing heat storage materials (e.g., heat storage materials suitable for storing and transporting various articles such as pharmaceuticals, medical devices, cells, specimens, organs, chemicals, and foods).

Claims (3)

A preparation step of preparing a heat storage material composition containing a base agent, a gelling agent, and a gelling auxiliary agent, and a filling step of filling a container with the heat storage material composition obtained in the preparation step,
The main agent is at least one selected from the group consisting of tetradecane and methyl laurate,
The gelling agent is aluminum 2-ethylhexanoate,
The gelling aid is at least one selected from the group consisting of stearic acid, oleic acid, decanol, lauryl alcohol, and myristyl alcohol ,
The content of the gelling agent in the heat storage material composition is 0.5% to 20% by weight based on 100% by weight of the heat storage material composition,
The amount of the gelling aid in the heat storage material composition is 1/2 to 1/3 times the amount of the gelling agent when the gelling aid is stearic acid or oleic acid; When the gelling aid is decanol, lauryl alcohol or myristyl alcohol, the amount is 1 to 6 times the amount of the gelling agent,
In the preparation step and the filling step, the heat storage material composition is maintained at a temperature higher than the solidification start temperature of the main ingredient and lower than 15.0°C. The method for producing a heat storage material according to claim 1, wherein the viscosity of the heat storage material composition in the filling step immediately before being filled into the container is less than 100 mPa·s. The method for manufacturing a heat storage material according to claim 1 or 2, wherein the filling step is performed 2.0 hours or more after the preparing step.

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