JP2002345940A - Slow-releasing material and method of making for the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a slow-releasing material which performs effectively disposition of the component on porous materials by a simple operation with a few processes without using solvents such as organic solvents, polluting the environment and has persistence of absorber aromatic or deodorant components, medicinal components, mothproof or insecticidal components and other components on the porous materials such as wooden materials, organic polymeric materials such as plastics, inorganic materials such as ceramics and glasses, and to provide a method of making such a slow-releasing material. SOLUTION: The slow-releasing material is obtained by observing the slow- release components into the pores of the porous materials using supertrictical or subcritical fluid as a medium. The method of making the slow-releasing material as achieved by bringing the supertrictical or subcritical fluid into contact with the porous materials and slow-release component-containing raw materials.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a porous material such as a wood material, an organic polymer material such as plastic, an inorganic material such as ceramics and glass, a fragrance component for aroma or deodorization, a medicinal component, and an insect repellent. Alternatively, the present invention relates to a sustained-release material carrying an insecticidal component, a fertilizer component, and other components used to exhibit sustained-release properties, and a method for producing the sustained-release material.

[0002]

2. Description of the Related Art Conventionally, as a technique for supporting a scent component or the like on a porous material such as an organic polymer material such as a wood material or a plastic, or an inorganic material such as ceramic or glass, extraction from a raw material containing a scent component is known. A solution impregnation method of applying or impregnating a material with the extracted extract or artificially synthesized scent component is mainly employed. In addition, scent components are also attached by a vacuum impregnation method.

[0003]

However, in the solution impregnation method, a pre-process of dissolving a scent component in an organic solvent for application or impregnation and a process of attaching the scent component to a material are separate processes. In addition to the complicated process, a separate process for treating a large amount of waste liquid generated in the process is required.

Further, even the vacuum impregnation method has a disadvantage that the process is complicated.

Further, according to the conventional method of loading a scent component on a woody material, the scent component cannot penetrate deep into the pores of the woody material, and the scent component can be uniformly applied to a product having a complicated shape. It was difficult to support.

Further, there is a disadvantage that the adhesion between the scent component and the product base material is weak, and the scent is not maintained.

SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned conventional problems, and is simple, without using a solvent such as an organic solvent which increases the load on the environment as a porous material. It is an object of the present invention to provide a sustained-release material which can carry a sustained-release component efficiently and in a small number of steps by an operation, and has a sustained sustainability.

[0008]

SUMMARY OF THE INVENTION The present invention has been made as a sustained-release material and a method for producing the same in order to solve the above-mentioned problems. The feature of the sustained-release material is a supercritical fluid or That is, a sustained release component is supported in a porous material using a subcritical fluid as a medium.

A feature of the method for producing a sustained-release material is that a supercritical fluid or a subcritical fluid is brought into contact with a porous material and a raw material containing a sustained-release component, so that the porous material has a porous material. The purpose is to produce a sustained release material in which a sustained release component is carried.

Another characteristic of the method for producing a sustained-release material is that impurities such as oil and water adhering to the porous material of the porous material are removed, and the supercritical fluid is added to the material containing the sustained-release component. Or, by contacting a subcritical fluid to extract a sustained release component from the sustained release component-containing raw material, by supporting the extracted sustained release component in the porous material of the porous material, to produce a sustained release material is there.

As the porous material, a woody material, an organic polymer material such as plastic, an inorganic material such as ceramic or glass, or a composite material thereof is used.

Further, the porous material includes not only a material in a narrow sense before being commercialized but also a product itself. Therefore,
It is a wooden product, a plastic product, etc., and includes various products after molding.

Therefore, a supercritical fluid or a subcritical fluid is infiltrated into a finely carved product (for example, a Buddha statue) in detail, a gap between fibers or a woven fabric made of the fiber, together with a sustained-release component. Is included.

Further, as the supercritical fluid or subcritical fluid, for example, carbon dioxide, nitrous oxide, trifluoromethane, or a mixture of two or more thereof is used.

Further, as the raw material containing a sustained release component, for example, a raw material containing a scent component for aroma or deodorant,
A raw material containing a medicinal ingredient, a raw material containing a component for controlling insects or insects, a raw material containing a fertilizer component, and the like are used.

[0016] Here, the sustained release component means various components such as the above-mentioned scent component, and means a component used to exhibit a sustained release property.

[0017]

Embodiments of the present invention will be described below with reference to the drawings.

(Embodiment 1) FIG. 1 is a schematic block diagram of an apparatus used for producing a scent component-bearing wood material as one embodiment.

As shown in FIG. 1, the apparatus used in the method for producing a scent component-carrying wood material of this embodiment contains a scent component-containing material 9 and a wood material 8 to which the scent component-containing material is attached. A high-pressure vessel 1 is provided.

The high-pressure vessel 1 is made of stainless steel,
As shown in the figure, the container body 2 and the lid 3 are configured.

The apparatus for manufacturing a scent component-carrying wood material of this embodiment further includes a cylinder 4, a high-pressure pump 5, a pressure gauge 6, and a back pressure valve 7.

The cylinder 4 is a cylinder for storing a fluid forming a supercritical fluid or a subcritical fluid. In the present embodiment, carbon dioxide is used as the fluid.

The high-pressure pump 5 is a pump for supplying the fluid in the cylinder 4 to the high-pressure container 1, and the pressure of the high-pressure pump 5 is measured by the pressure gauge 6.

The back pressure valve 7 can be opened and closed at a predetermined pressure, and is for maintaining the operating pressure at a predetermined value.

Further, by completely opening the back pressure valve 7 to reduce the pressure, the supercritical fluid is separated from the high-pressure vessel 1 under reduced pressure.

In addition, the apparatus for producing a scent component-carrying wood material of the present embodiment is provided with a pipe section (shown in a diagram) and the like.

Next, an embodiment of a method for producing a scent component-carrying wood material using such an apparatus will be described.

First, a wooden material 8 to which a scent component is to be attached and a Chinese herbal medicine as a scent component raw material 9 are sealed in the high-pressure container 1.

Next, a constant temperature bath (not shown) in which the high-pressure vessel 1 is charged is set to a target temperature, and a back pressure valve 7 is set.
Is set to a target pressure, and then carbon dioxide is supplied from the cylinder 4 to the high-pressure vessel 1 using the high-pressure pump 5.

Carbon dioxide becomes a supercritical fluid under the conditions of a temperature of 31.1 ° C. (critical temperature) and a pressure of 73 atm (critical pressure) or more, and the temperature setting of the constant temperature bath and the back pressure valve 7 as described above. The supercritical state can be maintained by setting the pressure in.

After the temperature and pressure in the high-pressure vessel 1 reach predetermined values, the container is left for a predetermined time. As a result, the scent component is carried on the wooden material 8.

This will be described in more detail. First, a scent component is extracted from a scent component raw material by supercritical carbon dioxide, and then a mixed fluid of the supercritical carbon dioxide and the scent component is mixed with the pores of the woody material 8. Penetrate deep into the surface.

In this case, the porous material of the wood material 8 contains
Although impurities such as oil and moisture remain such as resin and sap, a certain amount of impurities are removed from the inside of the porous material by contact of the supercritical carbon dioxide with the woody material 8, and then the porous material is removed. The scent component penetrates inside.

After allowing the fragrance component to permeate deep into the porous portion of the woody material 8 by leaving it to stand for a predetermined time, the back pressure valve 7 is released.

As a result, the pressure in the flow path is reduced, and the supercritical carbon dioxide returns to a gaseous state due to the pressure decrease.
Supercritical carbon dioxide is naturally diffused and removed from woody materials.

On the other hand, the scent component is adsorbed and captured inside the porous material and remains in the woody material.

In this way, a scent component-carrying wood material carrying the scent component is produced. As described above, carbon dioxide is heated at a temperature of 31.1 ° C. (critical temperature) and a pressure of 73 atm (critical temperature). Since the fluid becomes a supercritical fluid under the conditions of the temperature and the pressure equal to or higher than the pressure, the temperature can be set to a relatively low temperature, so that the degradation of the wood material 8 and the scent component material 9 due to heat can be prevented.

(Embodiment 2) FIG. 2 is a schematic block diagram of an apparatus used for producing a scent component-attached wood material as another embodiment.

The apparatus used in the manufacturing method of this embodiment has two high-pressure vessels.

One high-pressure vessel 1a contains a scent component raw material 9, and the other high-pressure vessel 1b contains a wood material 8.

Flow path from the fluid storage cylinder 4 to the back pressure valve 7
In addition to 10, a circulation path 11 for circulating a supercritical fluid is provided.

The circulation path 11 is provided with a pump 12.

As in the first embodiment, a cylinder 4, a high-pressure pump 5, a pressure gauge 6, and a back pressure valve 7 are provided.

A valve 13 is provided between the high-pressure pump 5 and the pressure gauge 6 in the flow path 10.

Further, the forward path 14 and the return path to one high pressure vessel 1a
15 is provided with valves 16 and 17, respectively.

Further, valves 20 and 21 are provided on the outward route 18 and the return route 19 to the other high-pressure vessel 1b, respectively.

Further, a valve 22 is provided in the flow path 10 between the outward path 14 and the return path 15 to one high pressure vessel 1a, and a valve 22 is provided in the flow path 10 between the outward path 18 and the return path 19 to the other high pressure vessel 1b. 23 are provided.

Further, in the circulation path 11, two valves 24,
25 are provided.

Next, a method for producing a scent component-carrying wood material of this embodiment using the above-described apparatus will be described.

First, impurities remaining in the porous material of the wooden material 8 are removed.

In this drying step, the valves 13, 22, 20, 21
Open, and valves 16, 17, 23, 2
4 and 25 are closed. The back pressure valve 7 is set to open at a predetermined pressure.

As a result, the forward path 14 and the return path 15 to the high-pressure vessel 1a in which the scent component raw material 9 is stored are closed and the circulation flow path 11 is closed, whereby carbon dioxide is stored in the woody material 8. It is supplied to the high pressure vessel 1b.

After carbon dioxide is injected into the high-pressure vessel 1b,
By adjusting to a predetermined temperature and pressure and converting to supercritical carbon dioxide, impurities such as resin components and moisture contained in the porous material of the woody material 8 are removed, and impurities are removed from the woody material 8. Become.

Next, an operation of removing the injected supercritical carbon dioxide from the high-pressure vessel 1b is performed.

In this suction removal step, the open / close state of each valve in the drying step is almost the same.
The difference is that 13 is closed. Also, back pressure valve 7
Shall be fully open.

As a result, the supply of carbon dioxide from the cylinder 4 is stopped, and the supercritical carbon dioxide in the high-pressure vessel 1b is discharged from the return path 19 to the outside of the high-pressure vessel 1b, and further discharged from the back pressure valve 7 to the outside of the system. Is done.

As a result, the supercritical carbon dioxide in the high-pressure vessel 1b has been removed.

Next, while supplying carbon dioxide to the high-pressure vessel 1a containing the scent component raw material 9, the scent component is supplied to the high-pressure vessel 1b together with supercritical carbon dioxide.

In this extraction and supply step, the valves 13, 16, 1
With 7, 20, 21 in the `` open '' state, and valves 22, 2,
3, 24, 25 are closed. The back pressure valve 7 is set to open at a predetermined pressure.

As a result, carbon dioxide is supplied from the cylinder 4 to the high-pressure vessel 1a, and a scent component is extracted from the scent component raw material 9, and the scent component is mixed with supercritical carbon dioxide.
The wood material 8 is supplied to the high-pressure container 1b in which the wood material 8 is stored.

Next, the scent component is carried on the wooden material 8.

In this loading step, the valves 16, 17, 20, 2
With 1, 24 and 25 in the `` open '' state, valves 13, 2
2, 23 are closed. The setting of the back pressure valve 7 is the same as in the previous step.

Thus, the scent component circulates together with the supercritical carbon dioxide in the circulation channel 11, the high-pressure vessel 1a, and the high-pressure vessel 1b without the carbon dioxide being newly supplied from the cylinder 4.

As a result, the extracted scent component is carried on the wooden material 8. More specifically, since the particles of the scent component as described above are carried in the porous material of the woody material 8 from which impurities such as resin components and moisture have been removed as shown in FIG. 3 in the drying step. is there.

Thereafter, the wooden material 8 carrying the scent component
From the high-pressure vessel 1b.

As described above, the manufacture of the scent component-carrying wood material on which the scent component is carried is completed.

Also in this embodiment, similarly to the first embodiment, the temperature can be set to a relatively low temperature by using supercritical carbon dioxide, and deterioration of the wood material 8 and the scent component material 9 due to heat can be prevented. Can be prevented.

In the present embodiment, two high-pressure vessels, a high-pressure vessel 1a for accommodating the scent component-containing raw material 9 and a high-pressure vessel 1b for accommodating the woody material 8, are provided. The operation of removing impurities such as resin components and moisture in the porous material 8 and the operation of extracting the scent component from the scent component-containing raw material 9 can be performed in separate containers. After reliably removing impurities such as resin components and water, supercritically extracted carbon dioxide can be injected into the porous material, so that the scent component can be reliably carried by the wood material. is there.

(Other Embodiments) In each of the above embodiments, supercritical carbon dioxide was used to extract the scent component from the scent component material. However, the operation temperature was lower than the critical temperature or the operation pressure was lower than the critical pressure. It is also possible to use so-called subcritical carbon dioxide, which is similar to the following.

Further, in the above embodiment, supercritical carbon dioxide is used, but a supercritical fluid or a subcritical fluid other than carbon dioxide can be used. Furthermore, methanol, ethanol,
Lower alcohols such as propanol, or acetone,
Several percent of organic solvent such as chloroform to supercritical fluid
It is also possible to add a trace amount.

Further, in the above embodiment, a wood material is used. However, the present invention is not limited to this. A ceramic material may be used, and an organic polymer material may be used. In addition, as the form of the material, spherical, plate-like, and other shapes of solid, fiber, woven fabric, and paper can be used.

Further, the type of the scent component is not limited to the above embodiment, and the type is not limited. Also,
Sustained release components other than scent components, such as drug components, insect repellents,
It is also possible to use components such as insecticides and fertilizers. In short, it is only necessary that a component that is gradually released from the target porous material be used.

[0073]

Embodiments of the present invention will be described below.

(Example 1) As a wood material, 10.30 g of a wooden rosary was prepared, and as a scent component raw material, 5.2 g of a 10-piece incense made by Tamasatsudo was prepared. A stainless steel high-pressure cell having an inner volume of 50 ml was prepared. Enclosed.

The ten kinds of incense are composed of sandalwood, cloves, cinnamon bark, yamana, kasuka, kanmatsu, great fenka, dragon brain, and sediment.

Next, the temperature was set to 50 ° C., the pressure was set to 20 MPa, carbon dioxide was supplied to the high-pressure cell, and the state was changed to supercritical carbon dioxide. Was carried.

After carrying the scent component, the supercritical carbon dioxide was returned to a gaseous state by releasing the back pressure valve and reducing the pressure, and the supercritical carbon dioxide was diffused and removed from the woody material.

As a result of the experiment, a wooden rosary carrying a scent component could be obtained.

(Example 2) As a woody material, 36.34
g of a wooden Buddha statue was prepared, and 18.19 g of a 10-piece incense manufactured by Tamasatsudo was prepared as a scent component material, and sealed in a 300 ml stainless steel high-pressure cell.

The operating conditions of this embodiment are the same as those of the first embodiment.
Therefore, the description is omitted.

As a result of the experiment, the scent component could be attached to the details of the finely carved wooden Buddha image.

(Test Example) In this test example, temperature, pressure, and drying time were tested as variable factors.

First, about 12 g of beads were weighed and sealed in a 50 ml high-pressure cell. Next, carbon dioxide was allowed to flow at a predetermined liquid sending speed, and the temperature of the thermostat was set.

Thereafter, carbon dioxide was continuously circulated to start removing impurities remaining in the rosary. After a lapse of a predetermined time, the beads were taken out under reduced pressure.

The obtained sample was manufactured by Shimadzu Corporation, AEG-
The weight was measured using a 45SM type electronic balance, and the weight before and after drying was compared. The weight loss rate can be expressed by the following equation.

Weight loss rate [%] = ｛(raw material [g] −after drying)
[g]) ÷ Raw material [g]｝ × 100

As a result of the test, as shown in the graph of FIG.
It was found that the rate of weight loss tended to increase as the time increased, but did not increase so much when the drying time was 2 hours or more. In the condition range of this experiment,
The results showed that the amount of weight loss was the largest when the temperature was 40 ° C.

Further, in order to examine the temperature dependency of the weight loss rate, the pressure was 20 MPa, the carbon dioxide was 3 ml / min, and the drying time was 1 hour.
The rate of weight loss under constant conditions was plotted against temperature.

As shown in the graph of FIG. 5, it was found that the peak (maximum) was around 40 ° C., and the weight reduction rate tended to decrease in the temperature range on both sides. This is considered to be due to the fact that, in the supercritical state, under the same pressure condition, the lower the temperature, the higher the density of carbon dioxide and the higher the effect of dissolving the organic matter. It is considered that under the condition of 25 ° C. below the critical temperature, carbon dioxide is not in a supercritical state, so that even if the density of the fluid is high, the effect of dissolving organic substances and the effect of permeating wood are reduced.

[0090]

As described above, in the present invention, the supercritical fluid or the subcritical fluid is brought into contact with the porous material and the scent component raw material, whereby the scent component material is superposed by the supercritical fluid or subcritical fluid. The scent component is extracted from the mixture, and the supercritical fluid or the mixed fluid of the subcritical fluid and the scent component can be permeated deep inside the pores of the porous material.

Further, due to the excellent permeation effect of the supercritical fluid or the like, the scent component can be carried not only on the smooth surface but also on the entire surface having a complicated shape.

Further, since the scent component is deeply penetrated into the porous material, the scent effect can be maintained for a long period of time.

Further, in the present invention, since a large amount of liquid solvent such as water or an organic solvent is not used, it is not necessary to carry out a drying step of the product after the scent component supporting step.

Further, since no waste liquid is generated during the process,
The waste liquid treatment step and the like become unnecessary.

Further, a scent can be applied to a product already completed as a scent application step as a secondary process without breaking its shape.

The supercritical fluid or the subcritical fluid is brought into contact with the porous material to remove impurities such as oil and water remaining in the porous material of the porous material. Or by contacting a subcritical fluid to extract a sustained release component from the sustained release component-containing raw material,
When the extracted sustained-release component is supported on a porous material to produce a sustained-release material, an operation of removing impurities such as oil and moisture in the porous material of the porous material with supercritical carbon dioxide, The operation of extracting the scent component from the scent component-containing raw material can be performed in separate steps, and therefore, after reliably removing impurities such as oil and moisture in the porous material of the porous material, Since the supercritically extracted component can be permeated, there is an effect that the scent component can be surely carried by the wood material.

[Brief description of the drawings]

FIG. 1 is a schematic block diagram of an apparatus for producing an aromatic component-adhered porous material as one embodiment.

FIG. 2 is a schematic block diagram of an apparatus for producing an aromatic component-adhered porous material according to another embodiment.

FIG. 3 is an explanatory view showing an action of attaching a scent component to a porous material.

FIG. 4 is a graph showing a correlation between a weight loss rate and a drying time.

FIG. 5 is a graph showing a correlation between a weight loss rate and a drying temperature.

[Explanation of symbols]

 1 ... high pressure vessel 4 ... cylinder 7 ... back pressure valve

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) A61L 9/01 A61L 9/01 Q 4H061 B01D 11/00 B01D 11/00 C05G 3/00 C05G 3/00 Z 103 103 5/00 5/00 Z (72) Inventor Shunsaku Kato 2217-43 Hayashi-cho, Takamatsu-shi, Kagawa Prefecture High-Temperature-High-Pressure Fluid Research Laboratory (72) Takako Kumagai 2217-43 Hayashi-cho, Takamatsu-shi, Kagawa Pref. Within the Technical Research Institute (72) Inventor Osamu Tada 965 Matsuzaki, Takuma-cho, Mitoyo-gun, Kagawa Prefecture F-term (reference) 3B114 AA11 AA14 AA16 AA23 BA09 4C002 AA03 DD13 HH06 4C080 AA04 BB02 BB03 CC01 HH05 JJ01 KK02 LL56 AB01 AB11 AB15 AB17 AC24 BA16 CA17 4H011 AC01 BA01 BA06 BB22 BC22 DA01 DC10 4H061 AA01 AA02 DD04 EE36 EE42 EE64 HH03

Claims (8)

[Claims] 1. A sustained-release material characterized in that a sustained-release component is supported in a porous material by using a supercritical fluid or a subcritical fluid as a medium. 2. The sustained-release material according to claim 1, wherein the porous material is a wood material, an organic polymer material such as plastic, an inorganic material such as ceramic or glass, or a composite material thereof. 3. A porous material and a raw material containing a sustained release component,
By contacting a supercritical fluid or a subcritical fluid,
A method for producing a sustained-release material, comprising producing a sustained-release material in which a sustained-release component is carried in a porous material. 4. A material containing a sustained release component by removing impurities such as oil and moisture adhering to the porous material of the porous material and contacting the material containing the sustained release component with a supercritical fluid or a subcritical fluid. A sustained release material is extracted from the porous material, and the extracted sustained release component is supported in the porous material of the porous material to produce a sustained release material. 5. The method according to claim 1, wherein the removal of impurities such as oil and moisture adhering in the porous material of the porous material is performed by contacting a supercritical fluid or a subcritical fluid, or by vacuum drying or freeze drying. 5. The method for producing a sustained-release material according to item 4. 6. The sustained-release material according to claim 3, wherein the porous material is a wood material, an organic polymer material such as plastic, an inorganic material such as ceramic or glass, or a composite material thereof. Material manufacturing method. 7. The sustained-release fluid according to claim 3, wherein the supercritical fluid or the subcritical fluid is carbon dioxide, nitrous oxide, trifluoromethane, or a mixture of two or more thereof. Material manufacturing method. 8. The raw material containing a sustained release component contains a raw material containing a scent component for aroma or deodorization, a raw material containing a medicinal component, a raw material containing an insect repellent or insecticidal component, or a fertilizer component. The method for producing a sustained-release material according to any one of claims 3 to 7, which is a raw material.