JP2017106150A - Nanofiber containing plant material manufacturing method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a manufacturing method of a material containing nanofiber (nanofiber-containing plant material) from plant residue.SOLUTION: A manufacturing method of nanofiber containing plant material comprises: an impregnation process S12 to impregnate a ground product of plant residue with a treatment solution containing a fibrillation agent; and a dry process S13 to dry the ground product after the impregnation process. In the impregnation process, concentration of the fibrillation agent in the treatment solution is 33 mass% or higher; temperature of the treatment solution is 25°C or higher; ratio of the treatment solution to the ground product (mass ratio) is 2.5 or higher; and the fibrillation agent is ammonium phosphate. In the dry process, dry temperature of the ground product is 25°C or higher and the plant residue is derived from Solanaceae plant.SELECTED DRAWING: Figure 2

Description

  The present invention relates to a method for producing a nanofiber-containing plant material.

  In plant cultivation of vegetables and the like, handling of plant residues such as stems and leaves remaining after harvesting is a problem. Some plant residues may be reused as compost, livestock feed, etc., but most of them are disposed of as industrial waste. Therefore, it is desired to effectively use plant residues as resources. Under such circumstances, attempts have been made to extract fibers from plant residues as part of effective utilization.

  For example, Patent Document 1 discloses a method of manufacturing fibers from a banana stem (provisional stem) after harvesting by physical defibration. Patent Document 2 discloses a method for producing fibers from beet pulp left as sugar beet (sugar radish) pomace by chemical defibration.

JP 2004-52176 A Japanese National Patent Publication No. 11-501684

  Incidentally, in recent years, it has been desired to produce nano-sized fibers from plant residues. However, the conventional defibration method has been problematic because nano-sized fibers cannot be easily obtained from plant residues.

  For example, when the plant residue is defibrated into nano-sized fibers by physical defibration, the number of steps for making the plant residue finer to the nano level becomes very large. For example, when a plant residue is defibrated using a disc mill, it has been necessary to change it many times in order to gradually narrow the interval between the grinding wheels of the disc mill.

  In addition, when plant residues are defibrated to nano-sized fibers by chemical defibration, an alkaline solution such as caustic soda solution is used as the treatment solution, but the waste solution treatment (neutralization treatment, etc.) of the alkali solution is a problem. It was.

  The objective of this invention is providing the method of manufacturing the material (nanofiber containing plant material) containing a nanofiber from a plant residue.

  As a result of intensive studies to achieve the above object, the present inventors impregnated a pulverized product of a plant residue with a treatment solution containing a fibrillating agent (for example, ammonium phosphate), It was found that when dried, fibrillation and nanofibers appeared on the surface of the pulverized product, and the present invention was completed.

Means for solving the above problems are as follows. That is,
<1> An impregnation step of impregnating a pulverized plant residue with a treatment solution containing a fibrillating agent;
The manufacturing method of the nanofiber containing plant material which has a drying process which dries the said ground material after an impregnation process.

  <2> The method for producing a nanofiber-containing plant material according to <1>, wherein in the impregnation step, the concentration of the fibrillating agent in the treatment solution is 33% by mass or more.

  <3> The method for producing a nanofiber-containing plant material according to <1> or <2>, wherein the temperature of the treatment solution is 25 ° C. or higher in the impregnation step.

  <4> The nanofiber-containing plant material according to any one of <1> to <3>, wherein in the impregnation step, a ratio (mass ratio) of the treatment solution to the pulverized product is 2.5 or more. Manufacturing method.

  <5> The method for producing a nanofiber-containing plant material according to any one of <1> to <4>, wherein the fibrillating agent is ammonium phosphate in the impregnation step.

  <6> The method for producing a nanofiber-containing plant material according to any one of <1> to <5>, wherein the pulverized product has a drying temperature of 25 ° C. or higher in the drying step.

  <7> The method for producing a nanofiber-containing plant material according to any one of <1> to <6>, wherein the plant residue is derived from a solanaceous plant.

  According to this invention, the method of manufacturing the material (nanofiber containing plant material) containing nanofiber from a plant residue can be provided.

Flow chart showing an example of manufacturing process of pulverized product Flow diagram showing an example of a method for producing nanofiber-containing plant material Explanatory drawing schematically showing the configuration of the drip device The figure which shows the SEM image of the nanofiber containing plant material of Example 1. The figure which shows the SEM image of the plant material of the comparative example 1 The figure which shows the SEM image of the plant material of the comparative example 2 The figure which shows the SEM image of the plant material (unprocessed ground material) of the comparative example 3 The figure which shows the SEM image of the nanofiber containing plant material of Example 2. The figure which shows the SEM image of the nanofiber containing plant material of Example 3. The figure which shows the SEM image of the nanofiber containing plant material of Example 4. The figure which shows the SEM image of the nanofiber containing plant material of Example 5. The figure which shows the SEM image of the plant material of the comparative example 4 The figure which shows the SEM image of the nanofiber containing plant material of Example 6. The figure which shows the SEM image of the nanofiber containing plant material of Example 7. The figure which shows the SEM image of the nanofiber containing plant material of Example 8. The figure which shows the SEM image of the nanofiber containing plant material of Example 9. The figure which shows the SEM image of the nanofiber containing plant material of Example 10. The figure which shows the SEM image of the nanofiber containing plant material of Example 11.

[Nanofiber-containing plant material]
The nanofiber-containing plant material is a plant material derived from a plant residue having nano-sized fibers at least on the surface.

  The plant residue used for the nanofiber-containing plant material is not particularly limited as long as the object of the present invention is not impaired, but, for example, a solanaceous plant residue is preferable.

  The solanaceous plant is a state in which useful parts such as fruits are left after being harvested, and mainly consists of stems, leaves, roots and the like. From such a solanaceous plant, stems and leaves are used as plant materials. The part of the solanaceous plant used for the nanofiber-containing plant material may be a stem alone, a leaf alone, or both a stem and a leaf. However, as the part of the solanaceous plant used for the nanofiber-containing plant material, a stem is particularly preferable.

  As a plant raw material such as a stem derived from a solanaceous plant (hereinafter sometimes simply referred to as “plant raw material”), a material from which water-soluble components contained in the plant have been removed is preferable. Plants contain various water-soluble components such as saccharides (monosaccharides, disaccharides, polysaccharides, etc.), plant enzymes, organic components such as amino acids, and inorganic components such as potassium. Since such a water-soluble component may cause discoloration of the material to which the nanofiber-containing plant material is added, it is preferably removed from the plant raw material.

  As a method for removing water-soluble components from plant materials, for example, a method of extracting and removing water-soluble components from plant materials by immersing the plant materials in an aqueous solvent such as water or alcohol or washing the plant materials with the aqueous solvent. And freeze-drying method. In addition, the plant raw material after removing the water-soluble component is appropriately dried.

  As will be described later, the water-soluble component may be extracted and removed simultaneously with the pulverization by pulverizing (pulverizing) the plant raw material in a state of being immersed in an aqueous solvent.

  The solanaceous plant is not particularly limited as long as the object of the present invention is not impaired. For example, a plant belonging to the genus Solanum is preferable, eggplant and tomato are more preferable, and tomato is particularly preferable.

  A nanofiber containing plant material is manufactured by the manufacturing method of the nanofiber containing plant material of this invention shown below.

[Method for producing nanofiber-containing plant material]
The method for producing a nanofiber-containing plant material includes at least an impregnation step and a drying step described below.

(Impregnation process)
The impregnation step is a step of impregnating a pulverized plant residue with a treatment solution containing a fibrillating agent.

  The pulverized product of the plant residue is obtained by pulverizing the above-described plant raw materials (plant residue) such as the solanaceous plant into a powder form. Examples of the method for pulverizing plant raw materials include a method of pulverizing plant raw materials by applying a compressive force, shearing force, frictional force, impact force, etc. by a mechanical method (mechanical pulverization method), explosion, and the like. .

  In the mechanical pulverization method, for example, a high-speed rotary mill, various ball mills (rolling ball mill, vibration ball mill, planetary ball mill), a medium stirring mill, an airflow pulverizer, or the like is used.

  Moreover, you may grind | pulverize (pulverize) a plant raw material in the state immersed in water-based solvents, such as water, using an underwater crushing apparatus (for example, homogenizer).

  You may grind | pulverize plant raw materials in several steps so that a particle size may become small gradually. For example, plant raw materials such as stems may be roughly pulverized to a size of about several centimeters, and the coarsely pulverized product may be further pulverized (pulverized) to about several hundred microns.

  In addition, the pulverized product obtained by pulverizing the plant raw material may be appropriately classified using a sieve or the like.

  The shape, particle size and the like of the pulverized product used in the impregnation step are not particularly limited as long as the object of the present invention is not impaired. For example, the particle size (maximum diameter) of the pulverized product is preferably 1000 μm or less, and 600 μm or less. Is more preferable.

  In addition, you may perform the sterilization process using electromagnetic waves, temperature, a pressure, and a chemical | medical agent with respect to a plant raw material and its ground material.

  Here, an example of the manufacturing method of a ground material is demonstrated, referring FIG. FIG. 1 is a flowchart showing an example of a process for producing a pulverized product.

  As shown in S1 of FIG. 1, the stalk (plant raw material) is roughly pulverized. Thereafter, as shown in S2 of FIG. 1, the obtained coarsely pulverized product is crushed in water. The crushed material obtained after crushing in water is filtered using a filtration device as shown in S3 of FIG. 1, and the residue is recovered. The collected residue is dried as shown in S4 of FIG. In addition, you may repeat the process of S2-S4 of FIG. 1 several times. The dried filtration residue is further finely pulverized (fine pulverized) as shown in S5 of FIG. Thereafter, the obtained pulverized product is sieved (classified) as shown in S6 of FIG. 1 to obtain a pulverized product having a target particle size range (see S7 of FIG. 1).

  The fibrillating agent is impregnated into a pulverized plant residue (plant raw material) in a solution (treatment solution) state to form (expose) nano-sized fibers on the surface of the plant residue.

  As the fibrillating agent, for example, a phosphate such as ammonium phosphate is preferable. As long as the object of the present invention is not impaired, substances other than ammonium phosphate may be used as the fibrillating agent.

  Examples of the solvent used in the treatment solution containing the fibrillating agent include water-based solvents such as water and alcohol, organic solvents, and the like, and aqueous solvents are particularly preferable from the viewpoint of handleability. When the solvent is an aqueous solvent, the fibrillating agent is preferably a phosphate such as ammonium phosphate. One type of fibrillating agent may be used alone, or two or more types may be used. Further, the fibrillating agent may be soluble or insoluble in a solvent as long as the object of the present invention is not impaired. When the fibrillating agent is insoluble, it is preferable that it is uniformly dispersed in the solvent.

  The concentration of the fibrillating agent in the treatment solution is, for example, preferably 33% by mass or more, more preferably 35% by mass or more, and still more preferably 40% by mass. The upper limit of the concentration of the fibrillating agent is not particularly limited. For example, when the fibrillating agent is soluble, the fibrillating agent is added to the solvent until the treatment solution becomes saturated or supersaturated. Also good.

  Various additives other than the fibrillating agent may be added to the treatment solution as long as the object of the present invention is not impaired. Examples of such additives include surfactants, antioxidants, ultraviolet absorbers, colorants, flame retardants, preservatives, carbon nanomaterials (for example, carbon nanotubes, carbon nanofibers, etc.), ceramics, metal powders Etc. These additives may be used alone or in combination of two or more. When the additive is insoluble, it may be dispersed in a solvent. In addition, when dispersing an additive, you may add a suitable additive suitably in a solution, and may adjust the specific gravity and viscosity of a solvent.

  The method of impregnating the pulverized plant residue with the treatment solution is not particularly limited as long as the object of the present invention is not impaired. For example, a method of immersing the pulverized product in the treatment solution or a drip device described later is used. It may be impregnated by the method used.

  In the impregnation step, the temperature of the treatment solution is preferably 25 ° C. or higher, and more preferably 30 ° C. or higher. The upper limit of the temperature of the treatment solution is not particularly limited as long as the object of the present invention is not impaired, but is preferably 60 ° C. or lower, for example.

  In the impregnation step, the ratio (mass ratio) of the treatment solution to the pulverized plant residue is preferably 2.5 or more, more preferably 4.0 or more, and still more preferably 5.0 or more. In addition, as an upper limit of the ratio (mass ratio) of the process solution with respect to the ground material of a plant residue, 8.5 or less are preferable, 8.0 or less are more preferable, 7.5 or less are still more preferable.

(Drying process)
A drying process is a process of drying the ground material after an impregnation process. The pulverized product impregnated with the treatment solution is dried using a known drying facility such as a heater or a drying chamber. In addition, as long as the objective of this invention is not impaired, you may dry by natural drying.

  In the drying step, the drying temperature of the pulverized product is preferably 25 ° C. or higher. The upper limit of the drying temperature of the pulverized product is not particularly limited as long as the object of the present invention is not impaired. For example, it is preferably 65 ° C. or lower, and more preferably 60 ° C. or lower.

  In the drying process, the drying temperature of the pulverized product is preferably set to be equal to the temperature of the treatment solution used in the impregnation process.

  Here, an example of the manufacturing method of a nanofiber containing plant material is demonstrated, referring FIG. FIG. 2 is a flowchart showing an example of a method for producing a nanofiber-containing plant material.

  As shown in S11 of FIG. 2, a fibrillating agent (ammonium phosphate) is dissolved in a solvent to prepare a treatment solution. Next, as shown in S12 of FIG. 2, a separately prepared plant residue pulverized product (for example, see FIG. 1) is impregnated in the treatment solution (an example of an impregnation step). The pulverized product after impregnation is dried (an example of a drying step) and the solvent is removed as shown in S13 of FIG. After drying, a nanofiber-containing plant material is obtained (see S14 in FIG. 2).

  As long as the object of the present invention is not impaired, in the method for producing other nanofiber-containing plant material, an impregnation step and a drying step using a treatment solution are performed in a coarsely pulverized state, and thereafter, as necessary. The nanofiber-containing plant material may be obtained by performing a pulverization treatment.

  Nano-sized fibers are formed on the surface of the nanofiber-containing plant material obtained by the production method of the present invention as described above. This is presumed that the nano-sized fibers protruded from the surface of the plant raw material (pulverized plant residue) during the production process of the nanofiber-containing plant material.

  In addition, the nanofiber-containing plant material finally obtained is usually in a powder form and is composed of a powder of the order of submicron. Therefore, it can be said that the nanofiber-containing plant material has less agglomeration after drying and excellent handleability than, for example, a completely nanonized plant material. In addition, unless the objective of this invention is impaired, the form of a nanofiber containing plant material, a magnitude | size, etc. do not have a restriction | limiting in particular.

  Nanofiber-containing plant materials are added to other materials such as plastics and ceramics, and are used for imparting various functions (for example, improving mechanical strength). Since the nanofiber-containing plant material has a large number of nanofibers formed on the surface, the nanofibers act as an anchor when mixed with other materials (for example, resin), and the miscibility with other materials, etc. Can be improved.

  Hereinafter, the present invention will be described in more detail based on examples. In addition, this invention is not limited at all by these Examples.

Example 1
<Preparation of pulverized product>
The stem of tomato (an example of solanaceous plant) that has finished harvesting is cut into a size of about 1 cm under conditions of 1500 rpm and 15 minutes using a coarse crusher (super mixer, manufactured by Ryobi Co., Ltd.). And pulverized to obtain a coarsely pulverized stalk. Next, the obtained coarsely pulverized product (500 g) was placed in water (2 liters), crushed in water for 2 minutes using a homogenizer, and then filtered. In the same way, the water disintegration treatment was repeated twice again on the filtered product (filtration residue), and the water disintegration was performed three times in total.

  Thereafter, the residue finally obtained was subjected to a drying treatment. The drying process was performed in two stages. First, the drying process at the first stage was performed for the purpose of sterilization by setting the temperature to 130 ° C. and the time to 8 hours. The second drying process was performed by setting the temperature to 105 ° C. and the time to 12 hours.

  The filtered residue after the drying treatment was pulverized to about 500 μm using a pulverizer (homogenizer, manufactured by Osaka Chemical Co., Ltd.) to obtain a pulverized product. Thereafter, the pulverized product was sieved with a sieving device to obtain a pulverized product of 500 μm or less.

<Preparation of ammonium phosphate solution (treatment solution)>
Water was added to ammonium phosphate to prepare an aqueous ammonium phosphate solution (ammonium phosphate concentration: 40% by mass).

<Fibrillation of pulverized product (production of plant material containing nanofibers)>
Using the drip device 10 shown in FIG. 3, the pulverized tomato residue was impregnated with an aqueous ammonium phosphate solution (40% by mass). First, the drip device 10 will be described.

  The drip device 10 is commercially available as a so-called coffee dripper, and mainly includes a holder portion 11, a drip portion 12, a filter 13, and a filtrate collection container 14. The holder portion 11 is a portion where the filter 13 is installed, and has a shape like a funnel opened upward such that the cone is inverted. The filter 13 is made of a filter paper that opens upward such that the cone is inverted. The drip part 12 is provided in the lower part of the holder part 11, and is provided with a through hole (not shown) for dropping the liquid in the holder part 11 downward. The filtrate collection container 14 is a container that collects the liquid dripped from the drip portion 12 in a form of receiving from below. The holder unit 11 is fixed to the upper part of the filtrate collection container 14 using a fixing member (not shown).

  Next, a method for impregnating a pulverized product with an aqueous ammonium phosphate solution using the drip device 10 will be described. First, the filter 13 was installed in the holder part 11, and the pulverized product 3 (1.02 g) was placed in the filter 13. Next, an aqueous ammonium phosphate solution (40 mass%) 15 (5.01 g) was poured into the filter 13, and the pulverized product 3 was immersed in the aqueous ammonium phosphate solution 15. Thereafter, the solution was left for about 3 minutes until the dropping of the aqueous ammonium phosphate solution 15 was completed.

  After the dropping was completed, the pulverized product 3 in the filter 13 was collected, and the pulverized product 3 was dried under the condition of a drying temperature of 30 ° C. In this way, the nanofiber-containing plant material of Example 1 was obtained by impregnating the pulverized product 3 with an aqueous ammonium phosphate solution.

(Comparative Example 1)
Instead of the aqueous ammonium phosphate solution (ammonium phosphate concentration: 40% by mass), using impure water, except that the impregnation treatment conditions were changed to those shown in Table 1, as in Example 1, The plant material of Comparative Example 1 was obtained by fibrillating the pulverized product of tomato residue (impregnating the pulverized product with pure water, etc.).

(Comparative Example 2)
In place of the ammonium phosphate aqueous solution (ammonium phosphate concentration: 40% by mass), while using the disodium phosphate aqueous solution (disodium phosphate concentration: 40% by mass), the impregnation step is replaced by the drip step, and the dipping step ( The plant material of Comparative Example 2 was obtained by fibrillation of the pulverized tomato residue in the same manner as in Example 1 except that it was changed to (immersion for 5 minutes).

(Confirmation of nanofiber formation (confirmation of fibrillation))
The surface of each plant material obtained in Example 1 and Comparative Examples 1 and 2 was observed using a scanning electron microscope (SEM), and according to the evaluation criteria (six-step evaluation by visual observation) shown below, Plant material fibrillation (nanofiber formation) was evaluated. The SEM image of Example 1 is shown in FIG. 4, the SEM image of Comparative Example 1 is shown in FIG. 5, and the SEM image of Comparative Example 2 is shown in FIG. The evaluation results are shown in Table 1. Note that the magnification of each SEM image is 50,000 times (the same applies to the SEM images of the following examples and comparative examples).

<Evaluation criteria>
“◎”: When the fibrillation of the material surface is 70% or more “○”: When the fibrillation of the material surface is 60% or more and less than 70% “△”: The fibrillation of the material surface is 40% or more and less than 60% Case “×”: When the fibrillation of the material surface is 0-30%

(Comparative Example 3)
For the pulverized product that has not been subjected to fibrillation treatment, the surface was observed with an SEM in the same manner as in Example 1 to evaluate fibrillation. The SEM image of Comparative Example 3 is shown in FIG. 7, and the evaluation results are shown in Table 1.

  As shown in the SEM image of FIG. 1, it was confirmed that nano-sized fibers were present on the surface of the nanofiber-containing plant material of Example 1. On the other hand, in the pulverized tomato residue (Comparative Example 3) that has not been subjected to any treatment or the plant material that has been treated with pure water only (Comparative Example 1), most of the nano-sized fibers are present on the material surface. I could not confirm. Moreover, also when the disodium phosphate solution was used as the treatment solution (Comparative Example 2), almost no nano-sized fibers could be confirmed on the surface of the plant material.

(Examples 2 to 5 and Comparative Example 4)
In the same manner as in Example 1, except that the room temperature of the impregnation step in the fibrillation treatment, the solution temperature, the temperature of the drying step after the impregnation step, etc. were changed to those shown in Table 2, Fibrilization was performed to obtain plant materials of Examples 2 to 5 and Comparative Example 4.

  The surface of each plant-derived material of Examples 2 to 5 and Comparative Example 4 was observed with SEM in the same manner as in Example 1 to evaluate the fibrillation (formation of nanofibers) of each plant material. The SEM image of Example 2 is shown in FIG. 8, the SEM image of Example 3 is shown in FIG. 9, the SEM image of Example 4 is shown in FIG. 10, and the SEM image of Example 5 is shown in FIG. The SEM image of Comparative Example 4 is shown in FIG. The evaluation results are shown in Table 2. Table 2 also shows the contents and results of Example 1.

  As shown in FIGS. 8 to 12 and Table 2, when the solution temperature in the impregnation step is 30 ° C., 40 ° C., 49.2 ° C., and 59.2 ° C., the surface of the pulverized tomato residue is nano-sized. It was confirmed that fibers were formed. In addition, when the solution temperature in the impregnation process is 25.3 ° C., it is confirmed that nano-sized fibers are formed on the surface of the pulverized tomato residue, although it is less than the case of 30 to 59.2 ° C. It was. On the other hand, when the solution temperature in the impregnation step was 20.9 ° C., it was confirmed that nano-sized fibers were not formed on the surface of the plant material.

(Examples 6 and 7 and Comparative Example 5)
Except that the amount of ammonium phosphate aqueous solution used in the fibrillation treatment was changed to that shown in Table 3, the pulverized tomato residue was fibrillated in the same manner as in Example 6. 7 and Comparative Example 5 were obtained.

  The surface of each plant material of Examples 6 and 7 and Comparative Example 5 was observed with SEM in the same manner as in Example 1 to evaluate the fibrillation (formation of nanofibers) of each plant material. The evaluation results are shown in Table 3. The SEM image of Example 6 is shown in FIG. 13, and the SEM image of Example 7 is shown in FIG. Table 3 also shows the contents and results of Example 1.

As shown in Table 3, when the amount of the treatment solution used in the impregnation step is 2.50 g (the ratio (mass ratio) of the treatment solution to the pulverized product is about 2.5), the evaluation result is “Δ” (visually However, when the fibrillation of the material surface was 40% or more and less than 60%), it was confirmed that more than half of the surface of the plant material was fibrillated (see FIG. 13). In addition, when the amount of the treatment solution used in the impregnation step is 7.50 g (the ratio (mass ratio) of the treatment solution to the pulverized product is 7.5) (Example 7), 70% or more of the surface of the plant material is more than 70%. It is fibrillated (see FIG. 14).
When the amount of the treatment solution used in the impregnation step is 10.0 g (the ratio (mass ratio) of the treatment solution to the pulverized product is about 10) (Comparative Example 5), the surface of the plant material is almost nano-sized. As a result, no fibers appeared.

(Example 8 and Comparative Examples 6 and 7)
The fibril of the pulverized tomato residue in the same manner as in Example 1 except that the concentration of the aqueous ammonium phosphate and the amount of the aqueous ammonium phosphate used in the fibrillation treatment were changed to those shown in Table 4. The plant material of Example 8 and Comparative Examples 5 and 6 was obtained.

  The surface of each plant material of Example 8 and Comparative Examples 6 and 7 was observed with SEM in the same manner as in Example 1 to evaluate the fibrillation (formation of nanofibers) of each plant-derived material. The SEM image of Example 8 is shown in FIG. The evaluation results are shown in Table 4. Table 4 also shows the contents and results of Example 1.

  As shown in Table 4, when the concentration of the treatment liquid is 35.0% by mass (Example 8), 70% or more of the surface of the plant material is fibrillated (see FIG. 15). On the other hand, when the concentration of the treatment liquid was 20.0% by mass and 30.0% by mass (Comparative Examples 6 and 7), almost no nano-level fibers could be confirmed on the surface of the plant material.

(Examples 9 to 11)
Except having changed the solvent etc. which are used for ammonium phosphate aqueous solution into what is shown in Table 5, it carried out similarly to Example 1, and performed the fibrillation of the ground material of a tomato residue, and Example 9-11 Plant material was obtained.

  The surface of each plant material of Examples 9 to 11 was observed with SEM in the same manner as in Example 1 to evaluate the fibrillation (formation of nanofibers) of each plant material. The SEM image of Example 9 is shown in FIG. 16, the SEM image of Example 10 is shown in FIG. 17, and the SEM image of Example 11 is shown in FIG. The evaluation results are shown in Table 5. In addition, "Tap water 1" in Table 5 (Example 9) is water collected from the water supply installed in Kitagawa Industry Co., Ltd. (1423 Tonmei, Aichi-cho, Kasugai-shi, Aichi Prefecture 101) “Tap water 2” (Example 10) is water collected from the water system installed in the Faculty of Engineering, Shinshu University (4-1, Wakasato, 4-1-1, Nagano City, Nagano Prefecture).

  As shown in Table 5, the amount of nanofibers formed on the surface of the plant material can be increased by using any of tap water 1, 2 and pure water as a solvent for the treatment solution (ammonium phosphate aqueous solution). It was confirmed that there was no difference (see FIGS. 16 to 18).

  DESCRIPTION OF SYMBOLS 3 ... Plant material, 10 ... Drip apparatus, 11 ... Holder part, 12 ... Drip part, 13 ... Filter, 14 ... Filtrate collection container, 15 ... Ammonium phosphate aqueous solution (treatment solution)

Claims (7)

An impregnation step of impregnating a pulverized plant residue with a treatment solution containing a fibrillating agent;
The manufacturing method of the nanofiber containing plant material which has a drying process which dries the said ground material after an impregnation process.   The method for producing a nanofiber-containing plant material according to claim 1, wherein in the impregnation step, the concentration of the fibrillating agent in the treatment solution is 33% by mass or more.   The method for producing a nanofiber-containing plant material according to claim 1 or 2, wherein in the impregnation step, the temperature of the treatment solution is 25 ° C or higher.   In the said impregnation process, the ratio (mass ratio) of the said process solution with respect to the said ground material is 2.5 or more, The manufacturing method of the nanofiber containing plant material as described in any one of Claims 1-3.   In the said impregnation process, the said fibrillation agent is ammonium phosphate, The manufacturing method of the nanofiber containing plant material as described in any one of Claims 1-4.   In the said drying process, the drying temperature of the said ground material is 25 degreeC or more, The manufacturing method of the nanofiber containing plant material as described in any one of Claims 1-5.   The method for producing a nanofiber-containing plant material according to any one of claims 1 to 6, wherein the plant residue is derived from a solanaceous plant.

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