KR102554401B1 - Fragrance and its manufacturing method with excellent persistence of incense - Google Patents

Abstract

The fragrance according to the present invention activates the pore structure of the carrier through a means for simultaneously activating the micropores and impregnating the fragrance, thereby forming finer pores and further improving the porosity, as well as having a very fine size. As the impregnation of the fragrance can be maximized up to the pores of the fragrance, there is a remarkably excellent effect of fragrance persistence and fragrance strength.

Description

Fragrance and its manufacturing method with excellent persistence of fragrance {Fragrance and its manufacturing method with excellent persistence of incense}

The present invention relates to an air freshener with excellent fragrance persistence and a method for preparing the same.

Fragrances impregnated with synthetic resins can be widely used in various indoor accessories, accessories, air filters, etc., and are very useful in that they can emit fragrance without a separate spice storage box. In addition, the fragrance has excellent processability during manufacture, and thus has the advantage of being able to develop various fragrance products.

However, in the conventional method of impregnating a fragrance component into a synthetic resin, there is a problem in that the intensity or persistence of the fragrance is weak, and thus the range of use is limited. Specifically, as a conventional method, there is a method of mixing a small amount of solid perfume with synthetic resin before molding and then molding together, a method of mixing a small amount of liquid perfume with synthetic resin and molding. In this way, it is possible to emit fragrance from the synthetic resin, but since it is not possible to use a sufficient amount of fragrance due to deterioration of moldability, the fragrance temporarily emits strongly and only a small amount of fragrance is emitted shortly after, significantly shortening the use time of the fragrance. There is a limit to falling.

As such, the problem of fragrance persistence of air fresheners is a very important matter in this technical field, and various studies have been conducted on plastic air fresheners in the past to improve this.

For example, in Korean Patent Publication No. 10-1998-034312, EVA (ethylene-vinyl acetate) copolymer particles having a vinyl acetate content of 20 to 30% are impregnated with a liquid fragrance, and the particles and low-density polyethylene and Disclosed is a method for producing a fragrance lasting synthetic resin, characterized in that high-density polyethylene is mixed in a weight ratio of 20 to 30:50 to 60:10 to 20. However, when the synthetic resin is impregnated during the manufacturing process, vaporization of the liquid fragrance is rapid at high temperatures, resulting in a large loss of fragrance components, and at low temperatures, the molecular activity of the liquid fragrance is lowered, so that impregnation is not effectively performed.

In addition, Korean Patent Registration No. 10-1682074 discloses a method for preparing a plastic air freshener in which EVA particles are impregnated with a mixture including a foaming agent and a liquid fragrance and then injected and foam-molded. However, the liquid fragrance is not smoothly impregnated into the micropores formed during injection and foam molding, and in particular, the liquid fragrance is impregnated into the micropores formed relatively small among the pores in the final product. There is a problem in that it is difficult to remain. .

Korean Patent Publication No. 10-1998-034312 (Publication date: 1998.08.05) Korean Registered Patent Publication No. 10-1682074 (registration date: 2016.11.28)

An object of the present invention is to provide a fragrance that can significantly improve fragrance persistence and fragrance strength by effectively impregnating a carrier with fragrance and a method for manufacturing the same.

A specific object of the present invention is to activate the pore structure of the carrier during the manufacturing process to form finer pores and further improve the porosity, as well as to maximize the impregnation of spices to very fine pores, fragrance persistence and fragrance It is to provide a fragrance with excellent strength and a method for producing the same.

A method for producing a fragrance-sustaining fragrance according to the present invention includes a mixing step of preparing a mixture comprising a liquid fragrance and an ethylene-vinylacetate copolymer carrier; and a pore activation step of activating micropores inside the carrier by applying ultrasonic waves to the mixture, wherein in the pore activation step, activation of micropores by application of ultrasonic waves and perfume impregnation into the micropores are simultaneously performed. characterized by

In one example of the present invention, in the mixing step, the carrier may be a porous foam carrier.

In one example of the present invention, the ethylene-vinyl acetate copolymer of the carrier may have a vinyl acetate content of less than 25% by weight based on the total weight of the copolymer.

In one example of the present invention, in the pore activation step, the micropores inside the carrier are activated on an extrusion device equipped with a die, and ultrasonic waves are applied on the die to extrude the carrier through the extrusion device, thereby micropores are activated. Stomata can be activated.

In one example of the present invention, the extruding device includes a hopper into which a mixture including the carrier and the liquid spice is introduced; an extrusion unit into which the mixture is introduced from the hopper and is extruded by applying physical pressure by a screw extruder; a die through which the mixture extruded from the extrusion part is discharged; and an ultrasonic wave applicator adjacent to the die and applying ultrasonic waves to the mixture discharged from the die, wherein the carrier impregnated with the liquid flavoring into micropores activated by the physical pressure and the ultrasonic waves. can be obtained from the die.

In one example of the present invention, the ultrasonic applying unit, a power supply unit for converting the supplied current into a high-frequency current; a converter that converts the high-frequency current supplied from the power supply into ultrasonic waves; a booster for first adjusting the amplitude of ultrasonic waves from the converter; and a horn spaced apart from the die to secondly adjust the first-adjusted amplitude of ultrasonic waves from the booster and to apply ultrasonic waves to the mixture discharged from the die.

In one example of the present invention, the separation distance between the horn of the ultrasonic application unit and the die may be 0.5 to 5 mm.

In one example of the present invention, the pressure of the extrusion unit may be controlled to 500 to 2,000 kgf/cm ² .

In one example of the present invention, in the pore activation step, the temperature of the mixture when pressure and ultrasonic waves are applied may be controlled to 30 to 80 °C.

The manufacturing method of the fragrance lasting air freshener according to an embodiment of the present invention may further include, after the pore activation step, an impregnation step of further mixing and re-impregnating the carrier in which the micropores are activated with a liquid fragrance.

The manufacturing method of the fragrance lasting fragrance according to an embodiment of the present invention may further include a drying step of removing the solvent of the liquid perfume impregnated in the carrier after the pore activation step or the impregnation step.

In one example of the present invention, the micropore size activated through the pore activation step of the carrier may be 0.3 to 300 μm.

In one example of the present invention, the carrier may have a size of 1 to 30 mm.

The fragrance according to the present invention effectively impregnates the carrier with the fragrance, so that the fragrance persistence and strength are remarkably excellent.

The manufacturing method of the fragrance according to the present invention activates the pore structure of the carrier during the manufacturing process to form finer pores, further improves the porosity, and has the effect of maximizing the impregnation of the fragrance to very fine pores. there is

1 is a conceptual diagram schematically illustrating an ultrasonic/extrusion device according to the present invention.

Hereinafter, an air freshener with excellent fragrance persistence and a method for manufacturing the same according to the present invention will be described in detail with reference to the accompanying drawings.

The drawings described in this specification are provided as examples to sufficiently convey the spirit of the present invention to those skilled in the art. Therefore, the present invention may be embodied in other forms without being limited to the drawings presented, and the drawings may be exaggerated to clarify the spirit of the present invention.

Unless otherwise defined, the technical and scientific terms used in this specification have meanings commonly understood by those of ordinary skill in the art to which this invention belongs, and the gist of the present invention in the following description and accompanying drawings Descriptions of known functions and configurations that may unnecessarily obscure are omitted.

Singular forms of terms used in this specification may be construed as including plural forms unless otherwise indicated.

Numerical ranges, as used herein, include lower and upper limits and all values within that range, increments logically derived from the form and breadth of the range being defined, all values defined therein, and the upper and lower limits of the numerical range defined in different forms. includes all possible combinations of Unless otherwise specifically defined in the specification of the present invention, values outside the numerical range that may occur due to experimental errors or rounding of values are also included in the defined numerical range.

'Includes' referred to in this specification is an open description having the same meaning as expressions such as 'includes', 'includes', 'has', and 'characterized', and elements not additionally listed, No materials or processes are excluded.

In this specification, the unit of % used without particular notice means weight % unless otherwise defined.

The term "layer" or "film" referred to herein means that each material forms a continuum and has a relatively small dimension in thickness compared to width and length. Accordingly, the term "layer" or "film" in this specification should not be interpreted as a two-dimensional flat plane.

The method for producing a fragrance lasting fragrance according to the present invention provides a method for producing a fragrance with significantly increased fragrance time by effectively impregnating a liquid fragrance into an ethylene-vinylacetate copolymer carrier.

A method for producing a fragrance-sustaining fragrance of the present invention for implementing the above effects includes a mixing step of preparing a mixture including a liquid fragrance and an ethylene-vinylacetate copolymer carrier; and a pore activation step of activating micropores in the carrier by applying ultrasonic waves to the mixture. At this time, in the pore activation step, the activation of the micropores by the application of ultrasonic waves and the impregnation of the fragrance into the micropores are performed simultaneously.

In the mixing step, the carrier preferably has a porous structure in which pores are formed, and may be, for example, a porous foam carrier prepared by foaming with a chemical/physical foaming agent. Since the foaming process of a polymer is widely known in the art, it is okay to refer to known literature or use a commercially available polymer foam.

As a specific example, a porous foam carrier may be prepared by foaming a masterbatch composition including an ethylene-vinyl acetate copolymer and a foaming agent at high temperature and high pressure.

The mixing weight ratio of the ethylene-vinyl acetate copolymer and the foaming agent is not particularly limited, and for example, 0.1 to 10 parts by weight of the foaming agent may be used with respect to 100 parts by weight of the copolymer. However, this is only described as a specific example, and the present invention is not construed as being limited thereto.

The blowing agent serves to form internal pores of the ethylene-vinyl acetate copolymer, and is, for example, sodium bicarbonate, ammonium carbonate, ammonium bicarbonate, ammonium nitrite, sodium borohydride, azodicarbonamide, dinitropenta methylenetetramine , It may include any one or two or more selected from oxybisbenzenesulfonyl hydroxide, toluenesulfonyl hydroxide, and the like. However, this is only described as a specific example, and the present invention is not construed as being limited thereto.

By using such a carrier having a porous structure, pore activation such as pore refinement, porosity increase, and pore size increase is performed through a pore activation step in the subsequent step, and at the same time, the pores are impregnated with spices.

As described above, in the step of activating the pores, the physical pressure and ultrasonic waves are applied to the carrier to simultaneously activate the pores of the carrier and impregnate the carrier with the spice. Even if ultrasonic waves are applied to a mixture containing a carrier and a liquid flavoring agent, the ultrasonic waves may affect the carrier, but since the ultrasonic wave is transmitted to the inside of the carrier and activation of pores cannot be expected, physical pressure and ultrasonic waves must be applied at the same time. That is, by applying ultrasonic waves in a state where physical pressure is applied to the carrier, pore refining, porosity increase, and pore activation such as formation of expanded micropores are effectively performed, and at the same time, perfume impregnation into the pores can be properly performed.

As a preferred means of applying physical pressure and ultrasonic waves to the carrier, micropores are activated inside the carrier on an extrusion device equipped with a die 30, and ultrasonic waves are applied on the die 30 to pass through the extrusion device. As the carrier is extruded, the micropores may be activated.

As a preferred example, an ultrasonic/extrusion device as shown in FIG. 1 may be used as the extrusion device. The ultrasonic / extrusion device includes a hopper (Hopper) 10 into which a mixture including the carrier and the liquid fragrance is introduced; an extrusion unit 20 into which the mixture is introduced from the hopper 10 and extruded by a physical pressure applied by a screw extruder 21 to extrude the mixture; a die 30 through which the mixture extruded from the extrusion part 20 is discharged; and an ultrasonic wave applicator 40 adjacent to the die 30 and applying ultrasonic waves to the mixture discharged from the die 30 . The screw extruder 21 may be driven by a motor 22 located at one end of the extruder 20. Using such an extrusion device, the carrier impregnated with the liquid fragrance into micropores activated by physical pressure and ultrasonic waves can be obtained from the die 30 .

As a specific example, the ultrasonic applying unit 40 may include a power supply unit (Ultrasonic power supply) 41 that converts supplied current into high-frequency current; a converter 42 that converts the high-frequency current supplied from the power supply 41 into ultrasonic waves; a booster (43) for first adjusting the amplitude of ultrasonic waves from the converter (42); and a horn 44 spaced apart from the die 30 so as to secondly adjust the first-adjusted amplitude of the ultrasonic waves from the booster 43 and apply ultrasonic waves to the mixture discharged from the die 30 );

The horn 44 of the ultrasonic applying unit 40 serves to apply ultrasonic waves adjacent to the carrier discharged from the die 30 of the extruding unit 20, and the horn 44 of the ultrasonic applying unit 40 ) and the die 30 is preferably 0.5 to 5 mm, specifically 1 to 3 mm. If this is satisfied, ultrasound can be effectively applied to the carrier positioned on the die 30 of the extrusion unit 20, so that pores can be activated and flavor impregnation can be better induced.

The intensity of the ultrasonic waves applied to the carrier may be controlled as long as the above effect can be realized, and may be controlled to, for example, 5 to 100 kHz, specifically 10 to 40 kHz.

The pressure of the extruding unit 20 may be applied as long as it is applied with ultrasonic waves to the extent that pores can be activated and flavor impregnated into the carrier, for example, 500 to 2,000 kgf/cm ² It may be preferable to control.

The extrusion speed of the extrusion unit 20 may be sufficient as long as the extrudate can be properly subjected to ultrasonic treatment, and, for example, 5 to 100 rpm, specifically 10 to 50 rpm is preferable in terms of effectively applying ultrasonic waves. can do.

The size of activated micropores of the carrier prepared through the pore activation step may be, for example, 0.3 to 300 μm.

The carrier is an ethylene-vinyl acetate copolymer, and the content of vinyl acetate is preferably less than 25% by weight, more preferably 20% by weight or less, based on the total weight of the copolymer. In addition, the carrier may preferably have tensile strength and elongation of 143 kg/cm ² or more and 870% or less, specifically, 145 kg/cm ² or more and 850% or less (ASTM D638). If this is satisfied, as the carrier has higher strength, microstructuring and formation of expanded micropores can be implemented more effectively when pores are activated by applying pressure and ultrasonic waves. In addition, when the ethylene-vinyl acetate copolymer satisfies the above-mentioned range of vinyl acetate content, tensile strength, elongation, etc., there is an effect of having higher durability and structural stability, which may occur during the manufacturing process, post-manufacturing transportation process, etc. Performance deterioration due to structural collapse due to external impact can be minimized.

In the ethylene-vinyl acetate copolymer, other specific details not mentioned may be used, for example, a melt index of 1.5 to 180 g / 10 min (ASTM D1238), a Vicat softening point of 40 to 90 ° C (ASTM D1525 ), those having a weight average molecular weight of 10,000 to 300,000 g/mol may be used. However, this is only described as a specific example, and the present invention is not construed as being limited thereto.

The size of the carrier may be appropriately adjusted according to the specific use, and may be, for example, 1 to 30 mm. However, this is only described as a specific example, and the present invention is not construed as being limited thereto.

The shape of the carrier may be appropriately adjusted according to the specific use, and may have various shapes such as spherical shape, rod shape, flake shape, polygonal shape, etc., of course.

As the liquid fragrance, various kinds of liquid type fragrances known in the field of fragrance technology may be used, and for example, herbal fragrances such as lavender, mint, and jasmine, flower fragrances such as roses, lilies, and lilacs, lemon, strawberry, Fruit flavors such as banana, apple, grape, etc., synthetic flavors such as chocolate, coffee, vanilla, and the like can be used. However, this is only described as a specific example, and the present invention is not construed as being limited thereto.

The manufacturing method of the fragrance lasting air freshener according to an embodiment of the present invention may further include, after the pore activation step, an impregnation step of further mixing 44 and re-impregnating the liquid fragrance into the carrier in which the micropores are activated. . Sufficient impregnation is ensured even in the pore activation step, but if an impregnation step of re-impregnating the liquid fragrance is further performed after the pore activation step, the fragrance duration can be further increased.

In the pore activation step, the temperature of the mixture when pressure and ultrasonic waves are applied, that is, the temperature of the carrier may be preferably controlled to 30 to 80 °C. If this is satisfied, it is possible to increase the impregnation rate while minimizing vaporization of the spice.

In addition, the mixing step 44 or the impregnation step may be controlled at a predetermined temperature, for example, 30 to 80 °C. In addition, the impregnation step may be performed at normal pressure or high pressure, for example, at a high pressure of 1.5 to 10 bar. If this is satisfied, it is possible to increase the impregnation rate while minimizing vaporization of the spice.

The manufacturing method of the fragrance lasting fragrance according to an embodiment of the present invention may further include a drying step of removing the solvent of the liquid perfume impregnated in the carrier after the pore activation step or the impregnation step. In the drying step, the drying temperature is not particularly limited, and may be performed in various temperature ranges, such as low-temperature drying, normal temperature drying, and high-temperature drying, for example.

Hereinafter, the present invention will be described in detail through examples, but these are for explaining the present invention in more detail, and the scope of the present invention is not limited by the following examples.

<Manufacture of porous foam carrier>

0.5 kg of azodicarbonamide as a foaming agent and 10 kg of ethylene-vinyl acetate copolymer (EVA 1315, Hanwha Solutions) having a vinyl acetate content of 15% by weight were mixed, and pressurized at 4 k/cm ³ at 60 ° C. After blending for 5 minutes, the mixture was aged at room temperature for 24 hours to prepare a masterbatch composition.

The masterbatch composition was put into an extruder (Cylinder: 150, Press Gage: 500 bar, 108 kW), melted and kneaded at 30 ° C. for 7 minutes, and extruded under a pressure of 110 bar. The prepared extrudate was heated at 110 ° C. for 30 seconds, heated at 130 ° C. for 20 seconds, heated at 155 ° C. for 15 seconds, and heated at 145 ° C. for 10 seconds. A porous foam carrier of the form was prepared.

<pore activation>

Pressure and ultrasonic waves are applied to a mixture of liquid fragrance (jasmine extract) and the porous foam carrier in the following manner through an ultrasonic/extrusion device as shown in FIG. Impregnated with spices. The mixture was introduced into the hopper of an ultrasonic/extrusion device, and the mixture was introduced into an extruder and extruded at an extrusion speed of 30 rpm at 60° C. while the liquid fragrance remained on the surface of the carrier through a screw extruder. Here, when the extrudate is discharged to the die located at the end of the extrusion unit, the horn of the ultrasonic application unit is located 2 mm apart from the die as shown in FIG. 1, and ultrasonic waves are applied at an intensity of 20 kHz to the extrudate located on the die It activates the micropores of the extruded carrier. Therefore, the porosity of the carrier is increased, the micropores are expanded, and more micropores are formed, and at the same time, the liquid fragrance is effectively impregnated to the deep and micropores.

<Liquid fragrance re-impregnation and drying>

In addition, the extrudate was immersed in a sufficient amount of the liquid fragrance, re-impregnated for 2 hours, and then sufficiently dried at room temperature to prepare an EVA fragrance impregnated with the liquid fragrance.

In Example 1, in the same manner as in Example 1, except that the vinyl acetate (VA) content of 26% by weight of the ethylene-vinyl acetate copolymer (EVA 1315, Hanwha Solutions) was used (EVA 1326, Hanwha Solutions). An EVA fragrance impregnated with a liquid fragrance was prepared.

In Example 1, an EVA fragrance impregnated with a liquid fragrance was prepared in the same manner as in Example 1, except that the distance between the die of the extrusion part and the ultrasonic applying part was adjusted to 6 mm.

[Comparative Example 1]

In Example 1, without pore activation, the porous foam carrier was soaked in liquid fragrance, impregnated, and then dried to prepare an EVA fragrance impregnated with liquid fragrance.

[Experimental Example 1] Orientation duration test

Samples in which equal amounts of EVA fragrances impregnated with fragrances prepared in Examples 1 to 3 and Comparative Example 1 were loaded into containers were placed in a space maintained at 15°C. In addition, the time required until the fragrance impregnated with the fragrance is no longer released to the outside was measured, and the results are shown in Table 1 below.

Example 1 Example 2 Example 3 Comparative Example 1 VA content of EVA Co-polymer (wt%) 15 26 15 15 stomatal activation ○ ○ ○ × Distance between die and horn (mm) 2 2 6 Perfume release duration (hours) 76 68 52 44

Referring to Table 1, Comparative Example 1, which did not undergo the pore activation step, had a significantly reduced fragrance release duration compared to Example 1. This difference is considered to be due to the fact that in the case of Example 1, pore activation and liquid fragrance impregnation were performed simultaneously, so that even very fine pores were effectively impregnated with liquid fragrance.

Comparing Example 1 and Example 2, when the vinyl acetate (VA) content of the ethylene-vinyl acetate copolymer was 15% by weight, the fragrance release duration was better than that when the content was 26% by weight. This difference is thought to be due to better microstructuring during pore activation by application of pressure and ultrasonic waves as the carrier has higher strength due to lower content of vinyl acetate.

Comparing Example 1 and Example 3, when the separation distance between the die and the horn is too far beyond 5 mm, as in Example 3, the ultrasound is not properly transmitted to the carrier, so the pore activation does not occur well, and the fragrance release duration It can be seen that this is significantly reduced.

10 : Hopper
20: extrusion part
21: screw extruder
22: motor
30: die
40: ultrasonic application unit
41: power supply
42: converter
43 : Booster
44: Horn

Claims (6)

A mixing step of preparing a mixture comprising a liquid perfume and an ethylene-vinylacetate copolymer carrier; and
A pore activation step of activating micropores in the carrier by applying ultrasonic waves to the mixture; includes,
In the pore activation step, activation of the micropores and perfume impregnation into the micropores are simultaneously performed by applying ultrasonic waves,
After the pore activation step, an impregnation step of re-impregnating the carrier in which the micropores are activated by further mixing a liquid fragrance; and
After the pore activation step or the impregnation step, a drying step of removing the solvent of the liquid perfume impregnated in the carrier; Method for producing a fragrance lasting fragrance further comprising. According to claim 1,
In the mixing step, the carrier is a porous foam carrier,
The ethylene-vinyl acetate copolymer of the carrier has a vinyl acetate content of less than 25% by weight of the total weight of the copolymer,
In the pore activation step, the temperature of the mixture when pressure and ultrasonic waves are applied is controlled to 30 to 80 ° C. Method for producing a fragrance lasting fragrance. According to claim 1,
In the pore activation step, the micropores are activated in the carrier on an extrusion device equipped with a die, and ultrasonic waves are applied on the die to extrude the carrier through the extrusion device to activate the micropores,
The extrusion device,
a hopper into which a mixture including the carrier and the liquid fragrance is introduced;
an extrusion unit into which the mixture is introduced from the hopper and is extruded by applying physical pressure by a screw extruder;
a die through which the mixture extruded from the extrusion part is discharged; and
An ultrasonic/extrusion device including an ultrasonic wave applicator adjacent to the die and applying ultrasonic waves to the mixture discharged from the die,
A method for producing a fragrance lasting fragrance, wherein the carrier impregnated with the liquid fragrance in micropores activated by the pressure and the ultrasonic waves is obtained from the die. According to claim 3,
The ultrasonic application unit,
a power supply unit that converts the supplied current into a high-frequency current;
a converter that converts the high-frequency current supplied from the power supply into ultrasonic waves;
a booster for first adjusting the amplitude of ultrasonic waves from the converter; and
A horn spaced apart from the die to secondly adjust the amplitude of the first-adjusted ultrasonic wave from the booster and to apply the ultrasonic wave to the mixture discharged from the die;
The method for producing a fragrance lasting air freshener wherein the distance between the horn of the ultrasonic applying unit and the die is 0.5 to 5 mm. delete According to claim 1,
The size of the activated micropores of the carrier through the pore activation step is 0.3 to 300 μm,
The size of the carrier is a method for producing a fragrance lasting fragrance of 1 to 30 mm.

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