KR101124288B1 - Method for manufacturing cattail fiber bundle, and biocomposites using thereof - Google Patents

Abstract

PURPOSE: A method for fabricating cattail fiber bundle is provided to obtain the fiber bundle without smell and to purify contaminated material. CONSTITUTION: A method for fabricating cattail fiber bundle comprises: a step of softening cattail stems and leaves by alkali treatment; a step of bleaching oxidizer and reducing agent; and a step of mechanically controlling length and width of fiber bundle.

Description

Method for manufacturing cattail fiber bundle, and biocomposites using according to the present invention

The present invention relates to a bundle of bundle fibers, and more particularly, to a method for producing a bundle of bleached fiber bundles for reinforcing biocomposites and a biocomposite material using the same.

Plastic, one of the 20th century's greatest inventions, has a variety of outstanding functions such as durability, processability, and chemical resistance, in addition to being light and relatively inexpensive, which has contributed greatly to the industrial development and convenience of daily life in other fields. In recent years, however, the domestic and foreign plastics market has created a new order, with increasing interest in environmental protection such as high oil prices, exhaustion of petroleum resources, and most importantly, the entry into force of climate change conventions and the strengthening of environmental regulations. On the other hand, as a way to develop new energy materials and protect the environment, R & D of new energy materials with large energy saving and environmental friendliness is rapidly being activated. This is because natural materials are not based on petroleum. It is to apply the product developed based on the application to the application field. Fiber-reinforced composite (FRP) is a functional composite material using synthetic fibers such as glass fiber, carbon fiber and aramid fiber as reinforcement in the polymer matrix, all of which are almost permanently decomposed in the natural environment. The effect on the respiratory system is great. Therefore, natural fiber reinforcement bio-composites have emerged as alternatives to these fiber-reinforced composites, which are currently being used as automotive parts, electronic parts, and building interior materials, or research and development to improve performance and expand into new research fields. This is actively going on.

On the other hand, Genus Typha L. is a perennial herb belonging to the Typhaceae family of 9 to 18 species distributed throughout the world. It is known that three kinds of native oysters, Typha orientalis, Typha angustata, and Typha latifolia, grow wild in Korea. Large parts and zombies are easily distinguished by the width of the leaves, but these two types have stamens and pistils, but the baby parts are characterized by a narrow leaf and the upper part of the pistil and the stamens separated by 4 to 6 cm. In Korea, the most common findings across the country are baby babies. In America, broad-leaved cattail (Typha latifolia L.) or common cattail is called broad-leaved cattail (Typha angustatifolia L.). In the latter case, the surgical and pistil parts are separated like those of native babies in Korea, but their morphological characteristics are somewhat different. The wealthy people dry in winter and hibernate with underground scenes and have a habit of staying young. The pollen of the buds is called phoenix and is used as a herbal medicine, and young shoots, stems, roots, etc. are also used for food. In addition, it is known that it plays a big role in the purification of pollutants in wetlands, the value of its use is increasing gradually, and many people are trying to use aquatic plants for wastewater treatment or water purification in Korea. It is a very meaningful attempt to use wealth as an environmental clean-up plant and further grow it as an edible or resource plant. Departments are attracting attention as future bioenergy crops because of the high level of development of the ground and roots, which produce large amounts of biomass. Whereas straw and reed produce dry weight biomass of 8.5-11.2 tons / ha and 6.4-12.5 tons / ha, respectively, the Department produces 10.6-14.7 tons / ha biomass and 14.5-22.7 tons when fertilizer is used. It has been reported that it produces / hectares of biomass (European, et al., ARPC Report, 2007, p95). Accordingly, the present inventors have attempted to develop a fiber bundle using the parts and a biocomposite including the same.

The inventors of the present invention have studied natural fiber reinforced biocomposite materials having high energy saving and environmental friendliness, and have found that biocomposites can be manufactured using parts as reinforcing materials.

Accordingly, an object of the present invention is to provide a bio-composite material having improved mechanical properties by preparing a bundle of bleached fiber fibers in the form of expressing properties as a reinforcement material of the composite material using the parts and using it as a reinforcement material of the biocomposite material. .

However, the technical problem to be achieved by the present invention is not limited to the above-mentioned problem, another task that is not mentioned will be clearly understood by those skilled in the art from the following description.

One aspect of the present invention comprises the steps of (1) softening the stem and leaves of the parts by alkali treatment and removing the extract; And (2) bleaching the softened parts using an oxidizing agent and a reducing agent. According to one embodiment of the present invention, the bleaching treated fiber bundle may further include adjusting the size of the fiber bundle by performing a mechanical treatment. According to another embodiment of the present invention, the parts may be one or more selected from the group consisting of perennial herb belonging to the family Budaceae and mixtures thereof. Preferably it may be one or more selected from the group consisting of zombies, baby parts, or large parts.

In addition, according to another embodiment of the present invention, in the softening process of step (1), the dried stems and leaves in the range of 5 to 30% activated alkali in the liquid ratio of 1: 4 to 1:10, The temperature may be treated at 50 to 100 ° C. for 0.5 to 5 hours, and sodium sulfide or anthraquinone may be used together with the alkali.

In the bleaching process of step (2), one or more selected from the group consisting of hydrogen peroxide, peracetic acid, sodium percarbonate, ozone, sodium chlorite, chlorine dioxide, and sodium hypochlorite may be used as the oxidizing agent, As the reducing agent, one or more selected from the group consisting of sodium hydrogen sulfite, hydrosulfide, sulfurous acid gas, acidic sodium sulfite, sodium thiosulfate, sodium sulfite and FAS (Formamidine sulfinic acid) can be used. Preferably, the oxidizing agent and the reducing agent may be reacted one or more times at a temperature of 100 ° C. or less for 5 hours or less.

In addition, according to another embodiment of the present invention, it is possible to adjust the length and width of the fiber bundle using a high concentration pulp, calbiter, refiner, defibrillator or cutter system.

Another aspect of the present invention provides a bleached fiber bundles produced by the bleached fiber bundles manufacturing method.

Another aspect of the invention provides a biocomposite material comprising a polymer matrix and using the bleached fiber bundle as a reinforcing material. According to one embodiment of the present invention, the polymer matrix, a biodegradable polymer, starch, polybutylene succinate, polyhydrobutylate, polyhydrobutylate, polylactic acid, polycaprolactone, polyglycolic acid , Polylactic acid, polyorthoester, phosphazine, polypeptides and mixtures thereof. According to another embodiment, the polymer matrix is a non-biodegradable polymer, thermoplastic polymer resin or It may be a thermosetting polymer resin. Preferably, the thermoplastic polymer resin is polyethylene, polypropylene, polyamide resin, polyvinyl chloride resin, vinyl acetate resin, polystyrene, ABS resin, acrylic resin, polybutylene terephthalate, celluloid resin, or polyphenylene sulfide The thermosetting polymer resin may include urea resin, melamine resin, alkyd resin, silicone resin, epoxy resin, urethane resin, or polyester resin. According to another embodiment of the present invention, the biocomposite may include mixing 10 to 70% by weight of the bleached fiber bundle and 30 to 90% by weight of the polymer matrix. According to another embodiment of the present invention, the biocomposite material may be used as an interior or exterior material of an automobile.

Another aspect of the invention is the step of (1) softening the stem and leaves of the parts by an alkali treatment process and removing the extract; (2) bleaching the softened parts with an oxidizing agent and a reducing agent; (3) dehydrating, drying and adjusting the length and width of the fiber bundles; (4) mixing the dried bleached fiber bundles with a polymer resin; And (5) provides a method for producing a bio-composite material comprising the step of producing a bio-composite material by high-temperature compression molding the bundle of bleached fiber fibers mixed with the polymer resin.

In the manufacturing process of the bleached fiber bundle according to the present invention, by using no chlorine bleach in the bleaching process, it is possible to produce a clean and odorless bleached fiber bundle in an environmentally friendly manner. In addition, both the leaves and the stem of the parts can be fiberized, which can have the morphological characteristics as a reinforcing material that can satisfy the mechanical improvement required by the composite material. In addition, the extract generated during the fiber bundle process can be used in the ethanol manufacturing process using carbohydrates, leaves and stems are provided as a reinforcement of the composite material as a fiber bundle. In addition, the departments play a major role in the purification of pollutants in wetlands, so when mass production of departments as a reinforcement material of biocomposites, the reinforcement materials can be produced with high quality at a lower cost than other non-wood fibers. You can also expect the effect.

1 is a view showing a comparison of the form of the bundle raw material, pulp, and bleached fiber bundles.
2 is a view showing a state of measuring the chromaticity of the bleached fiber bundles.
3 is a diagram illustrating a manufacturing process of the bleached fiber bundle according to an embodiment of the present invention.

The present inventors have completed the present invention as a result of studying the natural fiber reinforced biocomposite material according to the research and development of new energy materials with large energy saving and environmentally friendly characteristics.

The parts can fiberize both the leaves and the stems, which can have morphological properties as a reinforcing material that can meet the mechanical improvements required by the composite. In addition, the extract generated during the fiber bundle process can be used in the ethanol manufacturing process using carbohydrates, leaves and stems can be provided as a reinforcement of the composite material as a fiber bundle. In addition, wealth plays a major role in the purification of pollutants in wetlands, so when mass production of parts as a reinforcement material of biocomposites can produce reinforcement with better quality at a lower cost than other non-wood fibers, and it is a secondary effect such as water purification effect. You can also expect the effect. Therefore, the present inventors provide a natural fiber reinforced biocomposite material using the parts. In addition, by using no chlorine bleach at all in the bleaching process of the bundle of bundle fibers to provide a clean and odorless bleached bundle of fibers in an environmentally friendly way.

The method for producing a bundle of bleached fiber bundles is to soften the stems and leaves of the parts by an alkali treatment process (step (1)), and to bleach the softened parts using an oxidizing agent and a reducing agent (step (2)). It may include. In addition, the bleaching fiber bundle may further comprise the step of adjusting the size if necessary (mechanical treatment) (3).

The wealth may be one or more selected from the group consisting of perennial herb belonging to the wealth family and mixtures thereof, and the wealth may be zombies, babies, or large parts.

Step (1) is a step of softening the stems and leaves of the parts, using alkali, and can be reacted at a temperature of 50 ° C. or more for 0.5 hours or more. Preferably, the stem and leaves of the dried parts in the range of 5% to 30% activated alkali in the liquid ratio of 1: 4 to 1:10, the temperature may be made by processing 0.5 to 5 hours at 50 to 100 ℃, more Preferably, the treatment may be performed at 70 to 90 ° C. for 2 to 3 hours. The stems and leaves of the treated parts may not be separated into individual pieces of fiber, but a plurality of pieces of fiber may be combined to form a thin fiber bundle. At this time, the various extracts contained in the parts also come out to form the impurities are removed. Such reaction temperature and time can be controlled through improvements in processes and apparatus (heat supply method, capacity and mechanical agitation). By varying the reaction temperature and the concentration of the alkaline liquid, the reaction time and softening degree of the parts can be adjusted, and the alkaline liquid after the reaction can be recycled by increasing the alkalinity. In addition, depending on the embodiment, sodium sulfide or anthraquinone may be used together with the alkali.

Step (2) is a step of bleaching the parts obtained in the step (1) using an oxidizing agent and a reducing agent. Since chlorine bleach is expensive and environmentally problematic, oxidizing agents and reducing agents other than chlorine bleach can be used in the present invention. The oxidizing agent may be hydrogen peroxide, peracetic acid, sodium percarbonate, ozone as the oxygen system, or sodium chlorite, chlorine dioxide, or sodium hypochlorite as the chlorine system, and the reducing agent may be sodium hydrogen sulfite, hydrosulfide, One or more selected from the group consisting of sulfurous acid gas, acidic sodium sulfite, sodium thiosulfate, sodium sulfite and FAS (Formamidine sulfinic acid) can be used. Preferably hydrogen peroxide and FAS can be used. According to one embodiment of the invention, step (2) may be reacted for at least 1 hour at a temperature of less than 100 ℃ using the oxidizing agent and the reducing agent. Preferably, it can be made to react 1 time or more in 5 hours or less. That is, bleaching can be performed in one stage and, if necessary, in multiple stages of bleaching. By going through this bleaching step, the parts are gradually changed into the form of bundles, which can remove the smell of the bundle of bundle fibers, brighten and clean the color of the bundles, and are environmentally friendly because they do not use chlorine bleach. By treating the bleach in multiple stages, the color of the bundle of bundle fibers can be greatly improved. The color of the bundle of bundle fibers is measured using a colorimeter. The stems and leaves of the bleached parts are not separated into each other, but rather can be in the form of a thin bundle of fibers. Such bundles of fibers can be controlled through improvements in reaction temperature and time, process and apparatus (heat supply method, capacity and mechanical agitation).

Step (3) is a step of making the bleached parts obtained in step (2) into bundles of bleached fibers adjusted to a length and width suitable for use of the biocomposite material. In the bleaching process of step (2), most of them are separated into bundles, but the length and width of the fiber bundles can be adjusted through additional mechanical treatment. As a method of controlling the length and width of the fiber bundle, a high concentration of pulp, calbitter, refiner, defibrillator or other cutting systems can be used.

The present invention provides a bundle of bleached fibers prepared through the above steps. 1 is a view showing a comparison of the shape of the raw material and pulp and bleached bundle of bundle fibers.

The present invention also provides a biocomposite material comprising a polymer matrix and using the fiber bleached fiber bundle as a reinforcing material. In other words, the fiber bundle of the bleached portion can be utilized as a reinforcing material of a biocomposite material prepared by high temperature compression molding by mixing with a polymer resin.

The shape of the reinforcement is important to improve the mechanical properties of the biocomposite. Tensile strength and flexural strength are greatly influenced by the length of reinforcing fibers, and composite materials are manufactured by compression molding without cutting the reinforcing fibers. In compression molding, the temperature, melting time and cooling time may vary depending on the properties of the polymer resin.

According to one embodiment of the invention, the polymer matrix is a biodegradable polymer, starch, polybutylene succinate, polyhydrobutylate, polyhydrobutylate, polylactic acid, polycaprolactone, polyglycolic acid, polylactic It consists of an acid, a polyorthoester, phosphazine, or a polypeptide, and may include one or more selected from the group consisting of blends and copolymers thereof. According to another embodiment, the polymer matrix may be a thermoplastic polymer resin or a thermosetting polymer resin as a non-biodegradable polymer. The thermoplastic polymer resin may include polyethylene, polypropylene, polyamide resin, polyvinyl chloride resin, vinyl acetate resin, polystyrene, ABS resin, acrylic resin, polybutylene terephthalate, celluloid resin, polyphenylene sulfide, or the like. The thermosetting polymer resin may include urea resin, melamine resin, alkyd resin, silicone resin, epoxy resin, urethane resin, polyester resin, or the like. According to another embodiment, the biocomposite may include mixing 10 to 70 wt% of the bleached fiber bundles and 30 to 90 wt% of the polymer matrix.

3 is a diagram illustrating a manufacturing process of a biocomposite using a bundle of bleached fibers. As shown in FIG. 3, the parts are collected, subjected to softening of the stems and leaves of the parts, and are mostly fiber bundles during the bleaching process, and if necessary, additional lengths and widths suitable for biocomposites by additional mechanical treatment. And a step of dehydrating and drying the manufactured bundle fiber bundle, mixing the dried bleached fiber bundle with a polymer resin, and performing a high temperature compression molding of the bleached fiber bundle mixed with the polymer resin. Through biocomposites can be prepared. Leaves and stems of the parts used in the present invention can be used to cut to about 30cm before the initial softening process, but is not limited to this, by maintaining the length of the parts themselves (1 ~ 2m) through the improvement of the process and apparatus It can also manufacture.

Biocomposites made using bleached bundles of fiber as reinforcements can replace composite materials reinforced with other natural fibers as well as interior or exterior materials, lightweight structures, and other glass and carbon fibers in cars. It is environmentally friendly from manufacture and use to disposal. In addition, it is possible to increase the added value by using parts that are very insignificant as a reinforcement material of the composite material.

Hereinafter, the present invention will be described in more detail with reference to Examples and Test Examples. However, the following examples and test examples are provided only to more easily understand the present invention, and the contents of the present invention are not limited by the following examples and test examples.

[ Example ]

Example 1 Preparation of Bleached Fiber Bundles

The parts used in the manufacture of the fiber bundles were used in the cultivation house of the Department of Horticulture, College of Agriculture and Life Sciences, Chungnam National University. At that time, the water content of the parts was about 8 to 10%. The leaves and stems were added 1: 1 to the reaction vessel and the liquid ratio was 1:10. The reaction was carried out at 16 ° C. for 16 hours with 16% activated alkali (24% sulfidation). The fibers were rubbed by hand once every 30 minutes for the fibrosis to occur effectively, and after the reaction, they were washed thoroughly with fresh water.

Partially fibrous bundle fibers were bleached with hydrogen peroxide and FAS. Hydrogen peroxide bleaching of 3% and 5% was performed, and FAS bleaching of 3% and 5% was performed secondly as needed. The pH was maintained at 10 to 11 at each bleaching process, and 1% Sodium Silicate was added to the hydrogen peroxide bleaching solution to maximize the bleaching performance. Bleached fiber bundles after bleaching no longer need to adjust their length and width, so remove moisture with a dehydrator and spread them wide and dry them for 1 to 2 days at room temperature or dry them for about 5 hours in a hot air dryer to reinforce the biocomposite material. Material was used.

[Test Example]

Test Example 1. Measurement of chromaticity of bundle fiber bundle by bleaching

In order to measure the chromaticity of the bleached bundle of bundle fibers, samples subjected to each bleaching step were pulverized using a domestic mixer, and then chromaticity was measured using a colorimeter (see FIG. 2). Table 1 shows the results of the change in chromaticity according to the bleaching step. As shown in Table 1, Sample A is a bundle of fiber bundles prepared by the P company using a chlorine bleach, and has a very weak strength. The B-L samples had very good strength properties compared to the A samples. In case of primary bleaching with 5% hydrogen peroxide and secondary bleaching with 3% FAS, (sample G) L ^* value is more than 80%, and a ^* value is less than 1, so that the A Compared to the excellent. In addition, it can be seen that even when the alkalinity is reduced from 16% to 10%, an excellent color can be expressed through redox bleaching.

The CIE LAB (L *, a *, b *) notation was developed by the CIE (International Lighting Commission) as a method of expressing color in a quantitative manner. a *, b *). At this time, if a is +, red is-, it is close to green, b is + is yellow, and-is close to blue.

The foregoing description of the present invention is intended for illustration, and it will be understood by those skilled in the art that the present invention may be easily modified in other specific forms without changing the technical spirit or essential features of the present invention. will be. Therefore, it should be understood that the examples and test examples described above are exemplary in all respects and not limiting.

Claims (19)

Method for producing a bleached fiber bundle comprising the following steps:
(1) softening the stems and leaves of the parts by an alkali treatment process; And
(2) bleaching the softened parts using an oxidizing agent other than a chlorine system and a reducing agent.
The method of claim 1,
And mechanically adjusting the length and width of the fiber bundles.
The method of claim 1,
Said wealth is one or more selected from the group consisting of perennial herb belonging to the wealth family and mixtures thereof.
The method of claim 1,
Wherein said parts are moths, baby parts, or large parts.
The method of claim 1,
The step of softening the parts of step (1) comprises drying the stems and leaves of the dried parts to 5% to 30% activated alkali in a liquid ratio of 1: 4 to 1:10, the temperature of 0.5 to 50 to 100 ℃ The process which consists of processing for 5 hours.
The method of claim 1,
Method of using sodium sulfide or anthraquinone with alkali in the step (1).
delete The method of claim 1,
The reducing agent of step (2) is characterized in that at least one selected from the group consisting of sodium hydrogen sulfite, hydrosulfide, sulfite gas, acidic sodium sulfite, sodium thiosulfate, sodium sulfite and FAS (Formamidine sulfinic acid).
The method of claim 1,
The bleaching step of step (2) is to react at least once 5 hours or less at a temperature of 100 ℃ or less using an oxidizing agent and a reducing agent.
The method of claim 2,
Method for controlling the length and width of the fiber bundle using a high concentration of pulper, calbiter, refiner, defibrillator, or cutter system.
Bleached fiber bundles produced by the method of any one of claims 1 to 10.
Comprising a polymer matrix,
A biocomposite material using the bleached fiber bundle of claim 11 as a reinforcing material.
The method of claim 12,
The polymer matrix is a biodegradable polymer, such as starch, polybutylene succinate, polyhydrobutylate, polyhydrobutylate, polylactic acid, polycaprolactone, polyglycolic acid, polylactic acid, polyorthoester, phos Biocomposite, at least one selected from the group consisting of phages, polypeptides and mixtures thereof.
The method of claim 12,
The polymer matrix is a non-biodegradable polymer, a thermoplastic polymer resin or a thermosetting polymer resin, a biocomposite material.
The method of claim 14,
The thermoplastic polymer resin may be polyethylene, polypropylene, polyamide resin, polyvinyl chloride resin, vinyl acetate resin, polystyrene, ABS resin, acrylic resin, polybutylene terephthalate, celluloid resin, or polyphenylene sulfide .
The method of claim 14,
The thermosetting polymer resin is a urea resin, melamine resin, alkyd resin, silicone resin, epoxy resin, urethane resin, or polyester resin, bio-composite material.
The method of claim 12,
The biocomposite includes 10 to 70 wt% of the bleached fiber bundles and 30 to 90 wt% of the polymer matrix.
The method of claim 12,
The biocomposite material, characterized in that used as a vehicle interior or exterior material, biocomposite material.
Biocomposite manufacturing method comprising the following steps:
(1) softening the stems and leaves of the parts by an alkali treatment process;
(2) bleaching the softened parts using an oxidizing agent other than a chlorine system and a reducing agent;
(3) dewatering, drying, and controlling the length and width of the bleached fiber bundles;
(4) mixing the dried bleached fiber bundles with a polymer resin; And
(5) a step of producing a biocomposite material by high-temperature compression molding the bundle of bleached fiber fibers mixed with the polymer resin.

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