CN116240753A - Lasting fragrance-releasing adhesive film paper with sleep-aiding effect for artificial board veneers - Google Patents
Lasting fragrance-releasing adhesive film paper with sleep-aiding effect for artificial board veneers Download PDFInfo
- Publication number
- CN116240753A CN116240753A CN202211547992.0A CN202211547992A CN116240753A CN 116240753 A CN116240753 A CN 116240753A CN 202211547992 A CN202211547992 A CN 202211547992A CN 116240753 A CN116240753 A CN 116240753A
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- Prior art keywords
- poss
- sleep
- releasing
- film paper
- adhesive film
- Prior art date
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- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 3
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- D21H21/54—Additives of definite length or shape being spherical, e.g. microcapsules, beads
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Abstract
The invention relates to a lasting fragrance-releasing microcapsule with sleep-aiding effect and adhesive film paper using the same for artificial board veneers, wherein the microcapsule is coated with lavender compound essential oil with the sleep-aiding effect through a polyurea wall layer modified by cage Polysilsesquioxane (POSS). The invention adopts the wall layer structure of the POSS grafted modified polyurea microcapsule, enhances the wall layer strength of the microcapsule, ensures the integrity of the wall layer structure in the hot pressing process and secondary adsorption of the wall layer structure through the cage-shaped structure when the fragrance is released in high concentration, reduces the release rate of the fragrance, and realizes the long-term fragrance release of the artificial board product.
Description
Technical Field
The invention belongs to the field of high polymer resin compositions and application of the high polymer resin compositions in the technical field of functional paper products, and particularly relates to lasting fragrance-releasing adhesive film paper with sleep-aiding effect for artificial board veneers.
Background
Along with the improvement of living standard and environmental protection consciousness of people, the requirements on the health and safety of the air environment of the living room are higher and higher. Although the improvement of the technology for preparing the artificial board makes the formaldehyde control far lower than the national standard, the artificial board products such as the wardrobe, the floor and the like have little unpleasant smell due to the wood itself or the processing technology and the like, and are frequently complained by consumers. Odor problems have become an important research direction in the field of wood materials for home decoration. Many aromatic odors can bring pleasant mood to people, and have certain functions of regulating spirit and emotion, for example, the lavender compound essential oil can play roles of relieving nerves, relaxing mind and body, soothing nerves and aiding sleep; the peppermint essential oil has the effects of refreshing and restoring consciousness and reducing the pressure; the rose essential oil has the functions of relieving anxiety and injury, soothing emotion and improving mood. Therefore, the development of the functional fragrance-releasing artificial board not only can solve the problem of indoor odor, but also can improve the life quality of people and meet the great health requirements of people.
At present, the fragrance of the fragrance-releasing artificial board is realized by two ways: firstly, by adding plant fiber powder with fragrance to the fiber board (CN 112677257A); and secondly, adding essence and perfume into melamine resin for facing paper in the forms of microcapsule coating, emulsification and the like (CN 112900146 A;CN 113134879A). The two methods have the defects that firstly, perfume is directly used for perfuming in the process of plate making, the finished plate is obtained after high temperature and high pressure, the perfume is released too quickly and too strongly in the hot pressing process, the production environment is affected, and the perfume of the finished plate is almost completely lost after the finished plate is placed for a few days. Secondly, the aim of slow release of fragrance can be achieved through coating of the microcapsules, but the microcapsule wall layer structure is mostly made of polymer or biological base such as polyurea, cyclodextrin and the like, under the process of manufacturing the artificial board at high temperature and high pressure, the wall layer structure of the microcapsules is broken, even the phase change is directly softened at high temperature, the structure is seriously damaged, a large amount of encapsulated essential oil is separated out, a large amount of heat-sensitive substances in the essence and the spice can be released instantly at high temperature, the fragrance of the artificial board is too strong in the early stage, the fragrance of the artificial board is too low in the later stage, and the slow release effect is poor.
Therefore, the essence microcapsules used in the artificial board veneer must have dual properties of pressure resistance and temperature resistance. The microcapsule system with inorganic mesoporous silica as a wall material solves the problem of temperature and pressure resistance of the microcapsule, but the method has obvious disadvantages: firstly, the perfume and essence wrapped by the surface adsorption effect is far lower than the microcapsule encapsulation capacity, the fragrance release durability is poor, and the requirements of the artificial board product on service life as long as several years or even more than ten years are difficult to meet; secondly, unsaturated residual bonds exist on the surface of silicon dioxide, the polarity is strong, a three-dimensional network structure is easily formed through hydrogen bonds, the agglomeration phenomenon is easy to occur among silicon dioxide particles, the silicon dioxide particles are difficult to well disperse into melamine impregnated adhesive, the appearance of the adhesive film paper veneered artificial board is easy to influence, wrinkles, bubbles, white spots, stains, cracks and the like are easy to occur on the surface of the adhesive film paper, and defects such as dry flowers, scratches, indentation, bubbling, layering, corrugation and the like on the surface of the artificial board are easy to cause after the surface is faced.
Polyhedral oligomeric silsesquioxane (POSS for short) is a nano cage-shaped organic silicon material with a shell-core structure, and has a structural general formula (RSiO) 1.5 ) n N=4, 6,8,10,12, etc., the inner shells of the material are connected by silicon peaks, the material has good heat resistance and mechanical property, peripheral R active groups can initiate monomer polymerization, and the material plays a role of reinforcing microcapsule wall material polymers through organic-inorganic hybridization. In addition, the cage-shaped structure of the POSS is not only beneficial to the release of the essence and the spice, but also can carry out secondary adsorption on the excessive released essence and spice through adsorption, so that the fragrance is released permanently and uniformly.
Disclosure of Invention
The invention aims to provide lasting fragrance-releasing adhesive film paper with sleep-aiding effect for artificial board veneers, which is prepared by wrapping compound essential oil with sleep-aiding effect by adopting POSS grafted polyurea microcapsule wall materials to form an aromatic microcapsule auxiliary agent, has the characteristics of high temperature resistance and high pressure resistance, can realize stable and slow-release fragrance release, and is prepared by dispersing the aromatic microcapsule auxiliary agent in melamine resin adhesive.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
in a first aspect, the invention provides a lasting fragrance-releasing adhesive film paper with sleep-aiding effect for artificial board veneers, which comprises a lasting fragrance-releasing microcapsule auxiliary agent with sleep-aiding effect, melamine resin and paper, wherein the lasting fragrance-releasing microcapsule auxiliary agent with sleep-aiding effect comprises a POSS modified polyurea microcapsule wall layer and compound essential oil with sleep-aiding effect, and the compound essential oil with sleep-aiding effect is fully or partially encapsulated in the POSS modified polyurea microcapsule wall layer;
the raw material components of the microcapsule auxiliary agent with sleep-aiding effect and lasting fragrance release are 5.0-45.0% of compound essential oil, 2.0-5.0% of polyisocyanate, 0.5-1% of POSS, 1.0-3.5% of polyamine, 0.5-2.5% of emulsifier, 0.5-2.0% of stabilizer, 40.0-85.0% of deionized water, and the total mass percentage of the whole components is 100%; the preparation method comprises the following steps:
(1) Uniformly mixing lavender, sweet orange, ylang and agilawood essential oil according to a mass ratio to obtain compound essential oil, mixing isocyanate and the compound essential oil, and rapidly and uniformly stirring to obtain an oil phase;
(2) Mixing an emulsifying agent and deionized water, and rapidly and uniformly stirring to obtain a water phase;
(3) Adding the water phase in the step (2) into the oil phase in the step (1), homogenizing and stirring at a high speed, and emulsifying to obtain an oil-in-water emulsion;
(4) Dripping POSS (polyhedral oligomeric silsesquioxane) into the oil-in-water emulsion in the step (3), adding a tin catalyst, stirring at uniform speed for reacting for a certain time at a certain temperature, wherein the POSS is selected from hydroxyl-terminated POSS and/or amino-terminated POSS, isocyanate can perform better crosslinking reaction with the POSS, and a better capsule wall layer network structure is obtained, so that good pressure resistance, temperature resistance and long-term stable slow-release fragrance effect are shown.
(5) And (3) dropwise adding polyamine substances and a stabilizer into the product obtained in the step (4) at the temperature of 30-40 ℃ for reaction for 1.5h, heating to 50-60 ℃, and stirring at constant temperature for 1-3 h to obtain the POSS grafted and modified durable fragrance-releasing polyurea microcapsule auxiliary agent with sleep-aiding effect.
In some embodiments, the compound essential oil comprises lavender, sweet orange, ylang and agilawood essential oil, wherein the mass ratio is (2-4): (0.5-2): (0.5-1.5), preferably 3:1:1:1.
In some embodiments, the isocyanate is one containing at least two isocyanate groups; preferably, the compound contains at least three isocyanate groups, at least three isocyanate groups are contained, three or more isocyanate groups can perform better crosslinking reaction with POSS, and a better capsule wall layer network structure is obtained, so that the compound has good effects of pressure resistance, temperature resistance and long-term stable slow-release aroma.
In some embodiments, the isocyanate contains at least three isocyanate groups; further preferably, the isocyanate is at least one selected from toluene diisocyanate and its trimethylolpropane adduct, hexamethylene diisocyanate and its trimer, isophorone diisocyanate and its trimer, hexamethylene diisocyanate and its trimethylolpropane adduct, hexamethylene diisocyanate biuret; still more preferably, the isocyanate is selected from hexamethylene diisocyanate biuret and toluene diisocyanate trimethylolpropane adducts, and the compound essential oil is compounded in a mass ratio of (2-5): 5-45, preferably 4 (20-36).
In some embodiments, the emulsifier comprises an anionic surfactant comprising sodium dodecyl sulfonate and a nonionic surfactant such as at least one selected from polyethylene oxide, polyethylene, tween-80, span-80; preferably, the mass percentage of the emulsifying agent is 2%, the emulsifying in the step (3) is performed by a high-speed homogenizer for shearing and emulsifying, the emulsifying rate is 5000-15000rpm, and the time is 3-5 min.
In some embodiments, the POSS is selected from at least one of octahydroxybutyl POSS, amino POSS, N-methylaminopropyl isobutyl POSS, N-phenylaminopropyl POSS; in some embodiments, the POSS is selected from the group consisting of octahydroxybutyl POSS and amino POSS; the mass of POSS is 10-50% of the isocyanate consumption, and is preferably 25-30%.
In some embodiments, the tin-based catalyst comprises dibutyl tin dilaurate, stannous octoate, dibutyl tin di (dodecylsulfide), dibutyl tin diacetate. In some embodiments, the tin-based catalyst is dibutyl tin dilaurate; the tin catalyst accounts for 0.5 percent of the weight of the isocyanate.
In some embodiments, in step (4), the POSS and isocyanate are reacted at a temperature of 30 to 50 ℃, preferably 40 ℃, for a period of 1 to 2 hours, preferably 1.5 hours.
In some embodiments, the stabilizer is selected from polyvinyl alcohol and/or cellulose derivatives; in some embodiments, the cellulose derivative is selected from at least one of hydroxyethyl cellulose, polyethylene oxide, acrylamide, preferably polyvinyl alcohol and hydroxyethyl cellulose. In some embodiments, the polyamine comprises amine compounds of at least two amino groups, including ethylenediamine, guanidine, 1, 2-diaminopropane, 1, 2-diaminoethane, diethylenetriamine, tris (2-aminoethyl) amine, tetrakis (3-aminopropyl) -1, 4-butanediamine, bis (3-aminopropyl) -ethylenediamine. In some embodiments, the polyamine is selected from ethylenediamine, diethylenetriamine; the polyamine is used in an amount of 50% to 70%, preferably 55% to 65% of the isocyanate.
In some embodiments, the sustained release coated paper is obtained by a process comprising:
(A) Preparing a lasting fragrance-releasing microcapsule auxiliary agent with sleep-aiding effect, and adding the microcapsule auxiliary agent into melamine resin;
(B) Immersing paper in urea-formaldehyde resin adhesive, controlling gum dipping amount by roll coating, and then drying to obtain primary gum dipping and drying adhesive film paper;
(C) And (C) dipping the adhesive film paper subjected to primary dipping and drying into the sleep-aiding effect lasting fragrance-releasing melamine resin adhesive obtained in the step (A), controlling the dipping amount through roll coating, and then drying to obtain the sleep-aiding effect lasting fragrance-releasing adhesive film paper.
In some embodiments, the weight ratio of the sustained release microcapsule adjunct to the melamine resin is no greater than 1/100.
In some specific embodiments, the solid content of the microcapsule auxiliary agent is 0.5-2 wt%, preferably 0.7-1 wt%, and the microcapsule auxiliary agent is stirred for 1-2 min at 800-1200 rpm, the gum dipping amount is controlled to be 110-150% of the weight of the adhesive film paper by roll coating, and then the microcapsule auxiliary agent is dried for 5-10 min at 110-130 ℃.
In a second aspect, the invention provides a pressure-resistant high-temperature-resistant aroma slow-release microcapsule auxiliary agent, which comprises the following raw material components of an oil phase and a water phase, wherein the oil phase is compound essential oil, polyisocyanate and POSS; the water phase is emulsifier, stabilizer, polyamine and deionized water; specifically, the aromatic microcapsule auxiliary agent comprises the following raw materials in parts by weight: 5.0 to 45.0 percent of compound essential oil, 2.0 to 5.0 percent of polyisocyanate, 0.5 to 1 percent of POSS, 1.0 to 3.5 percent of polyamine, 0.5 to 2.5 percent of emulsifier, 0.5 to 2.0 percent of stabilizer and 40.0 to 85.0 percent of deionized water. The sum of the mass percentages of the whole components is 100 percent.
In some embodiments, the polyisocyanate comprises a polymer comprising at least two isocyanate groups, preferably at least three isocyanate groups, which can undergo a good crosslinking reaction with POSS and achieve a good network structure of capsule wall layers, thereby exhibiting good pressure, temperature and long-term stable slow-release aroma.
In some embodiments, the polyisocyanate includes toluene diisocyanate and its trimethylolpropane adducts, hexamethylene diisocyanate and its trimers, isophorone diisocyanate and its trimers, hexamethylene diisocyanate and its trimethylolpropane adducts, hexamethylene diisocyanate biuret, and various isocyanate mixtures. Hexamethylene diisocyanate biuret and toluene diisocyanate trimethylolpropane adducts are preferred.
In some embodiments, the POSS includes hydroxyl-terminated POSS and amino-terminated POSS, including, but not limited to, octahydroxybutyl POSS, amino POSS, N-methylaminopropyl isobutyl POSS, N-phenylaminopropyl POSS, preferably octahydroxybutyl POSS and amino POSS.
In some embodiments, the emulsifier includes an anionic surfactant such as sodium dodecyl sulfonate and a nonionic surfactant such as polyethylene oxide, polyethylene, tween-80, span-80, and the like, preferably a nonionic surfactant.
In some embodiments, the stabilizers include polyvinyl alcohol, cellulose derivatives such as hydroxyethyl cellulose, polyethylene oxide, acrylamide, and various mixtures, preferably polyvinyl alcohol and hydroxyethyl cellulose.
In some embodiments, the polyamine comprises an amine compound of at least two amino groups, including ethylenediamine, guanidine, 1, 2-diaminopropane, 1, 2-diaminoethane, diethylenetriamine, tris (2-aminoethyl) amine, tetrakis (3-aminopropyl) -1, 4-butanediamine, bis (3-aminopropyl) -ethylenediamine, preferably ethylenediamine, diethylenetriamine.
In some embodiments, the present invention provides a method of preparing a sustained release fragrance microcapsule adjunct having sleep-aiding efficacy comprising:
(1) Mixing Lavender, fructus Citri sinensis, ylang and lignum Aquilariae Resinatum essential oil at a certain weight ratio to obtain compound essential oil, mixing isocyanate and compound essential oil, and rapidly stirring to obtain oil phase.
(2) Mixing the emulsifier with deionized water, and rapidly and uniformly stirring to obtain a water phase.
(3) Adding the water phase in the step (2) into the oil phase in the step (1), homogenizing and stirring at a high speed, and emulsifying to obtain the oil-in-water emulsion. (4) Dripping POSS into the oil-in-water emulsion in the step (3), adding tin catalysts, and stirring at uniform speed for reacting for a certain time at a certain temperature.
(5) And (3) dropwise adding polyamine substances and a stabilizer into the product obtained in the step (4) at the temperature of 30-40 ℃ for reaction for 1.5h, heating to 50-60 ℃, and stirring at constant temperature for 1-3 h to obtain the POSS grafted and modified durable fragrance-releasing polyurea microcapsule auxiliary agent with sleep-aiding effect.
In some embodiments, the compound essential oil in the step (1) includes lavender, sweet orange, ylang and agilawood essential oil, and the mass ratio is (2-4): (0.5-2): (0.5-1.5), preferably 3:1:1:1.
In some embodiments, the compound mass ratio of the isocyanate and the compound essential oil in the step (1) is (2-5): 5-45, preferably 4 (20-36)
In some embodiments, the emulsifier in step (2) is 2% by mass.
In some embodiments, the emulsifying in step (3) is performed by shearing and emulsifying with a high-speed homogenizer at a speed of 5000-15000rpm for 3-5 min.
In some embodiments, the mass of POSS in step (4) is 10% to 50%, preferably 25% to 30% of the isocyanate amount.
In some embodiments, the tin-based catalyst in step (4) comprises dibutyl tin dilaurate, stannous octoate, dibutyl tin di (dodecylsulfide), dibutyl tin diacetate, preferably dibutyl tin dilaurate; the tin catalyst accounts for 0.5 percent of the weight of the isocyanate.
In some embodiments, the reaction temperature in step (4) is 30 to 50 ℃, preferably 40 ℃, and the reaction time is 1 to 2 hours, preferably 1.5 hours.
In some embodiments, the polyamine amount in step (5) is 50% to 70%, preferably 55% to 65% of the isocyanate amount.
In a third aspect, the present invention uses the sleep-aiding sustained-release coated paper for artificial boards.
Compared with the prior art, the invention has the following beneficial effects:
firstly, the sleep-assisting effect is realized by adopting the compound plant extract through synergistic compounding, the lavender is a recognized plant extract with the sleep-assisting effect, the lavender belongs to high-volatility essential oil, and the lavender has the characteristics of easy volatilization and strong smell, if a single lavender plant extract is adopted to prepare the lasting fragrance-releasing microcapsule auxiliary agent, the microcapsule auxiliary agent is extremely easy to volatilize under heat in the preparation process of the fragrance-releasing plate, so that the smell of a production workshop is too strong, and the fragrance-releasing time of a finished product of the fragrance-releasing plate is shorter in the use process. Based on the above, the inventor of the invention compounds the lavender essential oil with sweet orange with moderate volatilizing ability, ylang essential oil and agilawood essential oil with difficult volatilizing ability, firstly, the agilawood essential oil is also helpful for sleeping, and the aroma of the sweet orange and ylang essential oil can be adjusted more pleasant; secondly, the sweet orange, the ylang essential oil and the agilawood essential oil can prolong the fragrance releasing time of the lavender essential oil, and the slow releasing effect is improved. In some embodiments of the present invention, after the above-mentioned compound essential oil is replaced by a single lavender essential oil, the inventor of the present invention attaches the corresponding perfume releasing adhesive film paper to the artificial board, and the result of the perfume releasing test shows that the perfume releasing time is shortened from 360h (15 days) to 240h (10 days), which proves that the compound essential oil prolongs the perfume releasing time of the perfume releasing board, and the slow releasing effect is increased.
Secondly, hydroxyl POSS and amino POSS are selected to react with isocyanate through organic-inorganic hybridization, so that the wall layer structure can be enhanced, the wall layer structure is prevented from being broken under hot pressure, the secondary adsorption and supersaturation slow release effects of aroma molecules are realized through the cage-shaped structure of the POSS, and the slow release performance is improved; in addition, hydroxyl and amino are more active groups, so that the hydroxyl and amino are extremely easy to react with isocyanate groups of isocyanate, and the crosslinking reaction can be realized at a low temperature. In some specific embodiments of the invention, if POSS is not added in the preparation process of the lasting fragrance-releasing microcapsule auxiliary agent, the fragrance-releasing and slow-releasing time of the artificial board compounded with the lasting fragrance-releasing microcapsule auxiliary agent is shortened from 720 hours to 480 hours, and the fragrance-releasing content is reduced by times. In other embodiments, isooctyl POSS is added in the preparation process of the lasting fragrance-releasing microcapsule auxiliary agent, and the result shows that the fragrance-releasing and slow-releasing time of the artificial board compounded with the isooctyl POSS is shortened from 720 hours to 600 hours, and the fragrance-releasing content is reduced by times. The above proves that only hydroxyl-terminated POSS and/or amino-terminated POSS can generate better crosslinking reaction with isocyanate, the wall layer structure can be enhanced, and the wall layer structure is prevented from being broken under the action of heat, so that the coated essence is protected to be slowly released, the POSS of the wall layer presents a cage-shaped structure, and fragrance molecules can be adsorbed in the POSS cage-shaped structure again when being greatly overflowed under the influence of high temperature during hot pressing, so that the secondary adsorption and supersaturation slow release effect of the fragrance molecules are realized, and the slow release performance is improved.
In the third aspect, experiments prove that as the addition amount of the perfume-releasing polyurea microcapsule auxiliary agent is increased, the essential oil loading rate is increased, and the perfume releasing time is longer. However, when the addition amount of the perfume-releasing polyurea microcapsule auxiliary agent is too large, the perfume at the earlier stage of the perfume-releasing board is too high, and the experience is poor. Further apparent performance test experiments of the adhesive film paper show that when the dosage of the microcapsule auxiliary agent is too large (the weight ratio of the microcapsule auxiliary agent to the melamine resin adhesive is more than 1/50), tiny rubber powder, rubber bubbles and white spots are easy to appear on the surface of the adhesive film paper, the number of cracks is also increased, and dry flowers, surface scratches and indentations, uneven gloss and slight surface waves appear on the ecological plate. In addition, through the surface bonding strength test of the finished product fragrance-releasing joinery board, the inventor of the invention discovers that the fragrance-releasing joinery board microcapsule auxiliary agent does not influence the surface bonding strength of the joinery board; however, with further optimization testing, it is shown that as the amount of the microcapsule auxiliary agent added increases, the surface bonding strength tends to decrease, and in some specific embodiments, when the weight ratio of the microcapsule auxiliary agent to the melamine resin adhesive is 1/50, the bonding degree is reduced from 1.1MPa to 0.6/MPa, which proves that the excessive amount of the microcapsule auxiliary agent added causes bonding strength; it is therefore preferred in the present invention that the weight ratio of the microcapsule auxiliary to the melamine resin adhesive is not more than 1/100.
Drawings
FIG. 1 is a POSS modified fragrance-releasing polyurea microcapsule obtained in preparation example 3;
FIG. 2 is a polyurea microcapsule without POSS modification obtained in comparative preparation 2.
Detailed Description
In the present invention, all preparation materials/components are commercially available products well known to those skilled in the art unless specified otherwise.
The invention has no special requirements on the specific type of the impregnated bond paper.
The above technical solutions provided by the present invention are described in detail below in conjunction with examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
PREPARATION EXAMPLE 1 preparation of POSS graft modified sleep-aiding sustained-release fragrance polyurea microcapsule auxiliary
(1) Mixing Lavender, fructus Citri sinensis, ylang and lignum Aquilariae Resinatum essential oil at a mass ratio of 2:0.5:0.5:0.5, mixing hexamethylene diisocyanate biuret 2g and compound essential oil 10g, and rapidly stirring to obtain oil phase.
(2) 85g of sodium dodecyl sulfate aqueous solution with the mass fraction of 1% is prepared and is rapidly and uniformly stirred to obtain a water phase.
(3) Adding the water phase in the step (2) into the oil phase in the step (1) for emulsification at a speed of 5000rpm for 5min to obtain the oil-in-water emulsion.
(4) 0.2g of octahydroxybutyl POSS was added dropwise to the oil-in-water emulsion of (3), 0.01g of dibutyltin dilaurate was added as a catalyst, and the mixture was reacted at 30℃for 2 hours.
(5) And (3) dropwise adding 1g of ethylenediamine and 0.5g of polyvinyl alcohol into the product in the step (4) at the temperature of 30 ℃, heating to 50 ℃, and stirring at constant temperature for 3 hours to obtain the POSS grafted and modified sustained-release polyurea microcapsule auxiliary agent with sleep-aiding effect.
Example 1 preparation of film paper
1) Dipping ordinary paper (with the thickness of 0.15mm and the gram weight of 90 g/square meter) into urea-formaldehyde resin adhesive (urea-formaldehyde resin is purchased from Zhejiang sublimation Yunfeng New Material Co., ltd., molecular weight is 10000, solid content is 48%, pH value is 7-7.5, viscosity is 10-12 mPa.s, and curing time is 180 s), controlling the dipping amount to 150% of the paper weight through roll coating, and then drying at 130 ℃ for 10min to obtain adhesive film paper I after primary dipping and drying;
2) 5 parts of POSS grafted and modified durable fragrance-releasing polyurea microcapsule auxiliary agent with sleep-aiding effect is added into 1000 parts of melamine resin adhesive (purchased from Zhejiang sublimate Yunfeng New material Co., ltd., solid content of 55%, viscosity of 19-21 mPa.s, pH value of 8-9.5, melamine molecular weight of 126 g/mol), and stirring for 2min at 1200 r/min to obtain the sleep-aiding durable fragrance-releasing melamine resin composition.
3) Dipping the adhesive film paper subjected to primary dipping and drying in the sleep-aiding lasting fragrance-releasing melamine resin composition obtained in the step 2), controlling the dipping amount to be 130% of the weight of the adhesive film paper I through roll coating, and then drying at 130 ℃ for 10min.
PREPARATION EXAMPLE 2 preparation of POSS graft modified sleep-aiding sustained-release fragrance polyurea microcapsule auxiliary
(1) Uniformly mixing lavender, sweet orange, ylang and agilawood essential oil according to the mass ratio of 4:2:2:1.5, taking 5g of isophorone diisocyanate trimer, mixing 45g of compound essential oil, and rapidly and uniformly stirring to obtain an oil phase.
(2) 45g of polyethylene oxide aqueous solution with mass fraction of 3% is prepared, and the mixture is rapidly and uniformly stirred to obtain a water phase.
(3) Adding the water phase in (2) into the oil phase in (1) to emulsify at a speed of 15000rpm for 3min to obtain the oil-in-water emulsion.
(4) 2.5. 2.5g N-methyl amino propyl isobutyl POSS was added dropwise to the oil-in-water emulsion in (3), and 0.01g of stannous octoate was added as a catalyst to react at 50℃for 1 hour.
(5) Cooling to 40 ℃, dropwise adding 3.5g of tri (2-aminoethyl) amine and 2g of acrylamide into the product in the step (4), heating to 60 ℃, and stirring at constant temperature for 1h to obtain the POSS grafted and modified durable fragrance-releasing polyurea microcapsule auxiliary agent with sleep-aiding effect.
Example 2 preparation of film paper
1) Paper (thickness 0.15mm, gram weight 90 g/square meter) is immersed in urea-formaldehyde resin adhesive (urea-formaldehyde resin is purchased from Zhejiang sublimation Yunfeng New materials Co., ltd., molecular weight 10000, solid content 48%, pH value 7-7.5, viscosity 10-12 mPa.s, curing time 180 s), the gum dipping amount is controlled to be 120% of the paper weight through roll coating, and then the paper is dried for 5min at 110 ℃ to obtain the adhesive film paper I after primary gum dipping and drying.
2) 20 parts of POSS grafted and modified long-lasting fragrance-releasing polyurea microcapsule auxiliary agent with sleep-aiding effect is added into 1000 parts of melamine resin adhesive (purchased from Zhejiang sublimation Yunfeng New Material Co., ltd., solid content of 55%, viscosity of 19-21 mPa.s, pH value of 8-9.5, curing time of 600s, melamine molecular weight of 126 g/mol) and stirred for 2min at 1000 revolutions/min to obtain the sleep-aiding long-lasting fragrance-releasing melamine resin composition.
3) The gum paper after primary gum dipping and drying is immersed in the sleep-aiding lasting fragrance-releasing melamine resin composition obtained in preparation example 2, the gum dipping amount is controlled to be 115% of the weight of the gum paper I through roll coating, and then the gum paper is dried for 5min at 110 ℃.
PREPARATION EXAMPLE 3 preparation of POSS graft modified sleep-aiding sustained-release fragrance polyurea microcapsule auxiliary
(1) Mixing Lavender, fructus Citri sinensis, ylang and lignum Aquilariae Resinatum essential oil at a mass ratio of 3:1:1:1, mixing toluene diisohydrogen ester trimethylolpropane 3g and compound essential oil 30g, and rapidly stirring to obtain oil phase.
(2) Preparing tween-80 and span-80 with mass fraction of 2% with mass ratio of 1:1, and rapidly and uniformly stirring to obtain a water phase.
(3) Adding the water phase in (2) into the oil phase in (1), emulsifying at 10000rpm for 4min to obtain the oil-in-water emulsion.
(4) 0.825g of amino POSS was added dropwise to the oil-in-water emulsion of (3), and 0.01g of sodium acetate dibutyltin as a catalyst was added to react at 40℃for 1.5 hours.
(5) Dripping 1.8g of diethylenetriamine and 1g of hydroxyethyl cellulose into the product obtained in the step (4), heating to 55 ℃, and stirring at constant temperature for 2 hours to obtain the POSS grafted and modified sustained-release polyurea microcapsule auxiliary agent with sleep-aiding effect; FIG. 1 shows the POSS modified perfume-releasing polyurea microcapsule obtained in preparation example 3, which has uniform size, about 1 μm, and a rough convex structure on the surface, wherein the size of the convex structure is about 1-3nm, and accords with the original size of POSS, and the POSS is grafted on the microcapsule wall layer.
Example 3 preparation of film paper
1) Immersing paper (thickness 0.15mm, gram weight 90 g/square meter) in urea-formaldehyde resin adhesive (urea-formaldehyde resin is purchased from Zhejiang sublimation Yunfeng New materials Co., ltd., molecular weight 10000, solid content 48%, pH value 7-7.5, viscosity 10-12 mPa.s, curing time 180 s), controlling the gum dipping amount to 120% of the paper weight by roll coating, and then drying at 120 ℃ for 8min to obtain adhesive film paper I after primary gum dipping and drying;
2) 10 parts of POSS grafted and modified durable fragrance-releasing polyurea microcapsule auxiliary agent with sleep-aiding effect is added into 1000 parts of melamine resin adhesive (purchased from Zhejiang sublimate Yunfeng New material Co., ltd., solid content of 55%, viscosity of 19-21 mPa.s, pH value of 8-9.5, curing time of 600s, melamine molecular weight of 126 g/mo) and stirred for 1.5min at 1000 revolutions/min to obtain the sleep-aiding durable fragrance-releasing melamine resin composition.
The adhesive film paper after primary dipping and drying is immersed in the sleep-aiding lasting fragrance-releasing melamine resin composition obtained in the preparation example 3, the adhesive film paper after primary dipping and drying is immersed in a secondary dipping adhesive system, the dipping amount is controlled to be 130% of the weight of the adhesive film paper I through roll coating, and then the adhesive film paper is dried for 7min at 120 ℃.
Comparative preparation example 1 preparation of POSS graft modified sleep-aiding sustained-release fragrance polyurea microcapsule auxiliary
The other conditions were the same as in preparation example 3, except that the essential oil was lavender single essential oil.
Comparative example 1 preparation of bond paper
Other conditions were the same as in example 3, except that the POSS graft modified sleep-aiding sustained-release polyurea microcapsule auxiliary obtained in comparative preparation example 1 was used instead of the POSS graft modified sleep-aiding sustained-release polyurea microcapsule auxiliary obtained in preparation example 3.
Comparative preparation example 2 preparation of sleep-aiding sustained-release fragrance polyurea microcapsule auxiliary agent
Other conditions were the same as in preparation example 3, except that step (4) was omitted and POSS was not added; FIG. 2 shows that the perfume-releasing polyurea microcapsules without POSS modification are about 1-5 μm in size and are uneven, and the surface of the perfume-releasing polyurea microcapsules is obviously smooth.
Comparative example 2 preparation of bond paper
Other conditions were the same as in example 3 except that the sleep-aiding sustained-release fragrance polyurea microcapsule auxiliary obtained in comparative preparation 2 was used instead of the sleep-aiding sustained-release fragrance polyurea microcapsule auxiliary obtained in preparation 3.
Comparative preparation example 3 preparation of POSS graft modified sleep-aiding sustained-release fragrance polyurea microcapsule auxiliary
The other conditions were the same as in preparation example 3 except that isooctyl POSS was used in place of amino POSS in step (4).
Comparative example 3 preparation of bond paper
Other conditions were the same as in example 3, except that the sleep-aiding sustained-release polyurea microcapsule auxiliary obtained in comparative preparation 2 was used instead of the POSS graft-modified sleep-aiding sustained-release polyurea microcapsule auxiliary obtained in preparation 3.
Test example 1
The sleeping-aid fragrance-releasing adhesive film paper veneers prepared in examples 1 to 3 and comparative examples 1 to 3 were hot-pressed for 7min at 130 ℃ and then placed in a blast oven at 50 ℃ for a period of time, smelling was taken out in different periods of time, and the smelling was scored (0-5 min) according to the smell size according to the following scoring criteria:
5, the method comprises the following steps: obvious smell can be smelled 10cm away from the tested object, and the smell is obvious after the nose paste board is stuck
4, the following steps: the smell is very obvious after the nose paste board is smelled slightly 10cm away from the tested object
3, the method comprises the following steps: smell can be smelled 5cm away from the tested object, and the smell is obvious after the nose paste board is attached
2, the method comprises the following steps: the smell is low when the distance from the object to be measured is 5cm, and the smell is obvious after the nose paste board is attached
1, the method comprises the following steps: the smell can not be detected when the distance from the detected object is 5cm, and the smell is obvious after the nose paste board is attached
0.5 point: the smell of the nose paste board is suitable
0.3 point: the smell behind the nose paste board is weaker
0.1 point: the smell behind the nose patch is very weak
0 point: no smell after nose paste
TABLE 1 fragrance release test results table for fragrance releasing artificial board
| Sequence number | 0h | 120h | 240h | 360h | 480h | 600h | 720h |
| Example 1 | 3.5 | 1.5 | 1 | 0.3 | 0 | 0 | 0 |
| Example 2 | 5 | 4 | 3 | 2 | 1.5 | 1.5 | 1 |
| Example 3 | 4.5 | 2.5 | 1.5 | 1 | 0.5 | 0.5 | 0.5 |
| Comparative example 1 | 2 | 1 | 0.3 | 0 | 0 | 0 | 0 |
| Comparative example 2 | 2.5 | 1.5 | 1 | 0.3 | 0.1 | 0 | 0 |
| Comparative example 3 | 2.5 | 1.5 | 1 | 0.5 | 0.3 | 0.1 | 0 |
As can be seen from the data in Table 1, as the amount of the additive for the perfume-releasing polyurea microcapsules increases, the essential oil loading increases, but the amount of the additive is too large (example 2), the early-stage perfume is too high, and the experience is poor. Comparative example 1 illustrates that the release of the unilateral lavender essential oil is too rapid and the loss is large mainly in the hot pressing process. Comparative example 2 shows that the perfume releasing microcapsule which is not modified by POSS grafting has a certain slow release effect, but the slow release time is short, mainly because the microcapsule breaks in the hot pressing process to cause excessive loss of perfume molecules. In the comparative example, the POSS end group is isooctyl, the group can hardly react with isocyanate, a large amount of POSS can not participate in the formation of the microcapsule wall layer, even if a small amount of POSS is coated in the wall layer structure, the phenomenon of maldistribution exists in the microcapsule, and the function of supporting the microcapsule wall layer structure is not achieved.
Test example 2
The fragrance releasing impregnated bond papers prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to hot pressing and veneering to prepare ecological plates, the apparent properties of the bond papers were measured according to the appearance quality requirements of GB/T28995-2012 (Table 2), and the apparent masses of the ecological plates were measured according to the appearance quality requirements of GB/T34722-2017 (Table 3).
TABLE 2 apparent property test results of bond paper
| Sequence number | Folding wrinkles | Cracking of | Rubber bubble | Rubber powder | Glue leakage | White point | Stain spots |
| Example 1 | Without any means for | 0-1 | Very small | Very small | Without any means for | Without any means for | Without any means for |
| Example 2 | Micro-scale | 2-3 | Micro-scale | Micro-scale | Without any means for | Micro-scale | Micro-scale |
| Example 3 | Without any means for | 0-1 | Without any means for | Without any means for | Without any means for | Without any means for | Without any means for |
| Comparative example 1 | Without any means for | 0-1 | Without any means for | Without any means for | Without any means for | Without any means for | Without any means for |
| Comparative example 2 | Without any means for | 0-1 | Without any means for | Micro-scale | Without any means for | Without any means for | Without any means for |
| Comparative example 3 | Without any means for | 0-1 | Without any means for | Micro-scale | Without any means for | Micro-scale | Micro-scale |
TABLE 3 results of the apparent Performance test of ecological plates
As can be seen from the data in tables 2-3, the perfume-releasing impregnated bond paper prepared in examples 1-3 and comparative example completely meets the requirements of GB/T28995-2012 on appearance quality, and the prepared ecological plate meets the requirements of GB/T34722-2017 on appearance quality. The results of examples 1-3 show that when the amount of the microcapsule auxiliary agent is too large, tiny rubber powder, rubber bubbles and white spots are easy to appear on the surface of the adhesive film paper, the number of cracks is also increased, and dry flowers, surface scratches and indentations, uneven gloss and slight surface waves appear on the ecological plate.
In addition, as can be seen from examples 1 to 3 and comparative examples, the single lavender essential oil and the composite essential oil have little difference in the easy surface properties of the coated paper. Compared with isooctyl POSS, the amino POSS has remarkable improvement on the final aroma release performance and remarkable advantage on the apparent performance, and the adhesive film paper provided in the comparative example 3 has the conditions of indentation and uneven gloss, and the adhesive film paper in the example 3 has no defects.
Test example 3
The fragrance releasing adhesive film papers prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to hot press facing to prepare joinery boards, and the surface adhesion strength was measured according to GB/T5849-2016 standard requirements of joinery boards (Table 4).
TABLE 4 test of surface adhesion Strength of fragrance releasing core-board
| Sequence number | Surface bonding strength/MPa |
| Example 1 | 1.1 |
| Example 2 | 0.6 |
| Example 3 | 1.05 |
| Comparative example 1 | 1.02 |
| Comparative example 2 | 1.1 |
| Comparative example 3 | 0.95 |
As can be seen from the data of table 4, the surface bonding strength of the fragrance releasing joinery boards prepared in examples 1 to 3 and comparative example is far higher than the standard, but when the amount of the microcapsule auxiliary agent is too large, the surface bonding strength is significantly reduced because the amount of the microcapsule auxiliary agent needs to be controlled in order to achieve both fragrance releasing performance and bonding strength.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
Claims (10)
1. The lasting fragrance-releasing adhesive film paper with the sleep-aiding effect for the artificial board veneers is characterized by comprising a sleep-aiding effect lasting fragrance-releasing microcapsule auxiliary agent, melamine resin and paper, wherein the sleep-aiding effect lasting fragrance-releasing microcapsule auxiliary agent comprises a POSS modified polyurea microcapsule wall layer and compound essential oil with the sleep-aiding effect, and the compound essential oil with the sleep-aiding effect is fully or partially encapsulated in the POSS modified polyurea microcapsule wall layer;
the raw material components of the microcapsule auxiliary agent with sleep-aiding effect and lasting fragrance release are 5.0-45.0% of compound essential oil, 2.0-5.0% of polyisocyanate, 0.5-1% of POSS, 1.0-3.5% of polyamine, 0.5-2.5% of emulsifier, 0.5-2.0% of stabilizer, 40.0-85.0% of deionized water, and the total mass percentage of the whole components is 100%; the preparation method comprises the following steps:
(1) Uniformly mixing lavender, sweet orange, ylang and agilawood essential oil according to a mass ratio to obtain compound essential oil, mixing isocyanate and the compound essential oil, and rapidly and uniformly stirring to obtain an oil phase;
(2) Mixing an emulsifying agent and deionized water, and rapidly and uniformly stirring to obtain a water phase;
(3) Adding the water phase in the step (2) into the oil phase in the step (1), homogenizing and stirring at a high speed, and emulsifying to obtain an oil-in-water emulsion;
(4) Dropwise adding POSS (polyhedral oligomeric silsesquioxane) into the oil-in-water emulsion in the step (3), adding a tin catalyst, and uniformly stirring at a certain temperature for reacting for a certain time, wherein the POSS is selected from hydroxyl-terminated POSS and/or amino-terminated POSS;
(5) And (3) dropwise adding polyamine substances and a stabilizer into the product obtained in the step (4) at the temperature of 30-40 ℃ for reaction for 1.5h, heating to 50-60 ℃, and stirring at constant temperature for 1-3 h to obtain the POSS grafted and modified durable fragrance-releasing polyurea microcapsule auxiliary agent with sleep-aiding effect.
2. The lasting fragrance releasing adhesive film paper according to claim 1, wherein the compound essential oil comprises lavender, sweet orange, ylang and agilawood essential oil, and the mass ratio is (2-4): (0.5-2): (0.5-1.5), preferably 3:1:1:1.
3. The lasting fragrance film paper according to claim 1, wherein the isocyanate is one containing at least two isocyanate groups; preferably, the isocyanate contains at least three isocyanate groups; further preferably, the isocyanate is at least one selected from toluene diisocyanate and its trimethylolpropane adduct, hexamethylene diisocyanate and its trimer, isophorone diisocyanate and its trimer, hexamethylene diisocyanate and its trimethylolpropane adduct, hexamethylene diisocyanate biuret; still more preferably, the isocyanate is selected from hexamethylene diisocyanate biuret and toluene diisocyanate trimethylolpropane adducts, and the compound essential oil is compounded in a mass ratio of (2-5): 5-45, preferably 4 (20-36).
4. The lasting fragrance film paper according to claim 2, wherein the emulsifier comprises an anionic surfactant comprising sodium dodecyl sulfonate and a nonionic surfactant such as at least one selected from polyethylene oxide, polyethylene, tween-80, span-80;
preferably, the mass percentage of the emulsifying agent is 2%, the emulsifying in the step (3) is performed by a high-speed homogenizer for shearing and emulsifying, the emulsifying rate is 5000-15000rpm, and the time is 3-5 min.
5. The lasting fragrance releasing adhesive film paper according to claim 2, wherein the POSS is at least one selected from the group consisting of octahydroxybutyl POSS, amino POSS, N-methylaminopropyl isobutyl POSS, N-phenylaminopropyl POSS; preferably, the POSS is selected from the group consisting of octahydroxybutyl POSS and amino POSS; the mass of POSS is 10-50% of the isocyanate consumption, and is preferably 25-30%.
6. The lasting fragrance releasing adhesive film paper according to claim 2, wherein the tin-based catalyst is at least one selected from the group consisting of dibutyltin dilaurate, stannous octoate, dibutyltin dilaurate, dibutyltin diacetate; preferably, the tin catalyst is dibutyl tin dilaurate; the tin catalyst accounts for 0.5 percent of the weight of the isocyanate.
7. The lasting fragrance releasing adhesive film paper according to claim 2, wherein in the step (4), the reaction temperature of POSS and isocyanate is 30-50 ℃, preferably 40 ℃, and the reaction time is 1-2 hours, preferably 1.5 hours.
8. A sustained-release adhesive film paper according to claim 2, wherein the stabilizer is selected from polyvinyl alcohol and/or cellulose derivatives; preferably, the cellulose derivative is at least one selected from hydroxyethyl cellulose, polyethylene oxide and acrylamide, preferably polyvinyl alcohol and hydroxyethyl cellulose.
9. The lasting glue film paper according to claim 2, wherein the polyamine comprises amine compounds of at least two amino groups; further preferably, the polyamine comprises ethylenediamine, guanidine, 1, 2-diaminopropane, 1, 2-diaminoethane, diethylenetriamine, tris (2-aminoethyl) amine, tetrakis (3-aminopropyl) -1, 4-butanediamine, bis (3-aminopropyl) -ethylenediamine, still further preferably, the polyamine is selected from ethylenediamine and diethylenetriamine; the polyamine is used in an amount of 50% to 70%, preferably 55% to 65% of the isocyanate.
10. The lasting fragrance releasing adhesive film paper according to claim 1, wherein the lasting fragrance releasing adhesive film paper is obtained by the following preparation method:
(A) Preparing a lasting fragrance-releasing microcapsule auxiliary agent with sleep-aiding effect, and adding the microcapsule auxiliary agent into melamine resin;
(B) Immersing paper in urea-formaldehyde resin adhesive, controlling gum dipping amount by roll coating, and then drying to obtain primary gum dipping and drying adhesive film paper;
(C) Dipping the adhesive film paper subjected to primary dipping and drying in the sleep-assisting effect lasting fragrance-releasing melamine resin adhesive obtained in the step (A), controlling the dipping amount through roll coating, and then drying to obtain the sleep-assisting effect lasting fragrance-releasing adhesive film paper;
the weight ratio of the lasting fragrance-releasing microcapsule auxiliary agent to the melamine resin is not more than 1/100;
preferably, the solid content of the microcapsule auxiliary agent is 0.5-2 wt%, preferably 0.7-1 wt%, and the microcapsule auxiliary agent is stirred for 1-2 min at 800-1200 r/min, the gum dipping amount is controlled to be 110-150% of the weight of the adhesive film paper by roll coating, and then the microcapsule auxiliary agent is dried for 5-10 min at 110-130 ℃.
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