CN112962321A - Lavender essence microcapsule finishing liquid - Google Patents
Lavender essence microcapsule finishing liquid Download PDFInfo
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- CN112962321A CN112962321A CN202110267287.4A CN202110267287A CN112962321A CN 112962321 A CN112962321 A CN 112962321A CN 202110267287 A CN202110267287 A CN 202110267287A CN 112962321 A CN112962321 A CN 112962321A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses a lavender essence microcapsule finishing liquid, and relates to the technical field of functional finishing liquids and application thereof. The lavender essence microcapsule comprises: core material prepared from lavender essence; the wall material is prepared from modified melamine resin; wherein, the core-wall ratio in the microcapsule structure is 1-1.5: 1. the finishing liquid specifically comprises: the lavender essence microcapsule, the cross-linking agent and water. The microcapsule finishing liquid prepared by the invention is used for finishing the fabric, so that the soaping resistance, the brushing resistance and the wear resistance of the fabric can be effectively improved, the fragrance release is delayed, the fragrance retention time is prolonged, and the health care effect is enhanced. The added value of the textile is greatly improved, the finished fabric can be used as home textile products such as pillowcase and sheet, and can also be used as underwear and children's clothes, and the like, and the fabric is safe, environment-friendly, fragrant and pleasant and has wide market space.
Description
Technical Field
The invention belongs to the technical field of functional finishing liquid and application thereof, and particularly relates to lavender essence microcapsule finishing liquid.
Background
In recent years, with the increasing living standard of people, the demands on textiles are not limited to warm keeping, comfort and beauty, but have wider demands on functionality and safety. The fragrance finishing is to extract essence from natural plants to prepare microcapsules, and the microcapsules are organically combined with textile fibers through a special process, so that the textile is endowed with various fragrances, has health care functions of pleasure mood, pressure relief, tranquilization and the like, is beneficial to physical and mental health, and has fruit fragrance, such as apples, lemons and the like, at home and abroad by using a wide fragrance finishing technology at present; fresh scent, such as jasmine, rose, etc., lavender is more popular with the public due to its unique medicinal value and faint scent!
Lavender (Latin school name:Lavandula angustifolia Mill vanilla, also known as "aromatic herb", is a plant with sedative, soothing, hypnotic effects, is suitable for any skin, and has the functions of promoting cell regeneration, relieving stress, relaxing nerves, helping sleep, relieving tension and anxiety, and calming the mind. The whole plant has light fragrance with wood sweet taste, fresh fragrance and pleasant fragrance, is widely applied to various daily cosmetics such as perfume, perfumed soap, floral water and the like, and is one of important natural essential oils in the perfume industry.
The microcapsule technology is a microcapsule technology which utilizes a high polymer material to embed active substances to form a microcapsule with semi-permeability or a sealed capsule membrane. It can improve the physical property of the coated substance, isolate the active ingredient from the external environment, enhance stability, reduce volatility, prolong shelf life, and control release. However, the essence microcapsules sold on the market at present often have the defects of low essence wrapping rate, low mechanical strength of capsule walls, short aroma retention time, low affinity with textile fibers, difficult adhesion and the like.
Disclosure of Invention
The invention aims to provide a lavender essence microcapsule finishing liquid, which is used for finishing a fabric, can effectively improve the soaping resistance, the brushing resistance and the wear resistance of the fabric, delay the fragrance release, prolong the fragrance retention time, enhance the health care effect and has excellent antibacterial performance.
The technical scheme adopted by the invention for realizing the purpose is as follows:
the application of modified melamine resin in the preparation of plant essence microcapsules is characterized in that the modified melamine resin is prepared by grafting the epristerine with the melamine resin. The modified melamine resin is used as the wall material of the microcapsule, and the antibacterial performance of the microcapsule can be effectively enhanced and the coating rate of the microcapsule can be improved after the modified epristeride is adopted for modification; meanwhile, the existence of the epristeride effectively improves the slow release performance of the microcapsule. After the finishing liquor is used for finishing the fabric, the soaping resistance, the brushing resistance and the wear resistance of the fabric are obviously improved, the fragrance retention time is obviously prolonged, and the health care effect is enhanced.
Preferably, the preparation method of the modified melamine resin specifically comprises the following steps: dissolving melamine resin and epristerine in DMF, slowly dropwise adding DMAP under the condition of ice water bath, reacting for 10-15 min, adding EDC, naturally heating to 22-25 ℃, and reacting for 18-20 h; drying overnight, filtering, separating by silica gel column chromatography, distilling under reduced pressure, and vacuum drying to obtain modified melamine resin.
Preferably, the mass ratio of melamine to epristeride is 1: 2.5-3; the mass ratio of the DMAP to the melamine resin is 1-1.2: 1; the mass ratio of the EDC to the melamine resin is 1-1.1: 1.
a lavender essence microcapsule, comprising:
core material prepared from lavender essence;
wall materials made from the modified melamine resin of claim;
wherein the core-wall ratio (mass ratio) in the microcapsule structure is 1-1.5: 1. the microcapsule structure has certain protection and slow release effects on the lavender essence core material, and after the microcapsule structure is used as plant essence microcapsule finishing liquid to treat fabrics, the defects that the microcapsule structure is directly applied to skin and the like can be avoided. The modified melamine resin is used as the wall material of the microcapsule, and the lavender essence is used as the core material to prepare the microcapsule, so that the coating rate of the microcapsule can be obviously improved; meanwhile, the existence of the epristeride effectively improves the slow release performance of the microcapsule.
A preparation method of lavender essence microcapsules specifically comprises the following steps:
s1: weighing lavender essence, adding a high-molecular emulsifier and distilled water, and emulsifying under stirring to obtain an emulsion;
s2: adjusting the pH value of the emulsion by using acetic acid, adding the trimethylol melamine at the same stirring speed, reducing the stirring speed, reacting at constant temperature, and performing single-layer wall building;
s3: after the reaction is finished, cooling to normal temperature, adding the modified melamine resin while stirring, and preserving the temperature for a period of time at constant temperature; and cooling to room temperature, adding a dispersant NNO, and adjusting the pH value to obtain the lavender essence microcapsule.
Preferably, in the step S1, the using amount of the emulsifier is 13.6-16.4% of the total mass of the lavender essence; the emulsifying time is 10-15 min; the stirring speed is 14000 to 16000 r/min.
Preferably, the pH value of the emulsion is adjusted to 4.5-5.5 by using acetic acid in the step S2; the constant temperature is 60-65 ℃, and the heat preservation is carried out for 1-1.5 h.
Preferably, in the step S3, the constant temperature is 70-80 ℃, the temperature is kept for 1.5-2 hours, and the pH value is adjusted to 7-8.
Preferably, the average particle size of the microcapsule prepared by the preparation method is 2.5-3 μm, and the particle size distribution is 0.5-3.5 μm; the coating rate of the microcapsule is more than 90 percent.
A lavender essence microcapsule finishing liquid comprises: the lavender essence microcapsule, the cross-linking agent and the water are contained, wherein the mass of the lavender essence microcapsule is 0.4-0.8% of that of the water, and the mass of the cross-linking agent is 1.5-2.4% of that of the water. After the fabric is finished by the finishing liquid prepared from the lavender essence microcapsules, the soaping resistance, the brushing resistance and the wear resistance of the fabric are obviously improved, the fragrance retention time is obviously prolonged, and the health care effect is enhanced. Most raw materials are biodegradable, the whole preparation and finishing processes are green and environment-friendly, and the environmental load is not increased; the microcapsule finishing liquid can synergistically inhibit bacteria and fungi, and has a lasting antibacterial effect.
Preferably, the crosslinker is an epoxy silane crosslinker.
A finishing method of fabric specifically comprises the following steps: pretreating a fabric, immersing the fabric into the lavender essence microcapsule finishing liquid, padding, rolling under the roller pressure of 3-4 kg, the liquid carrying rate of 82-92% and the vehicle speed of 20-26 m/min, drying and baking to obtain the lavender fragrance fabric. The fabric after the fragrance finishing is baked at a specific temperature, and the soaping resistance, the scouring resistance and the friction resistance of the fabric can be effectively improved to a certain extent.
Preferably, the fabric pretreatment specifically comprises: the fabric is cleaned firstly, so that the water absorption of the fabric is less than or equal to 2 seconds, the pH value of the fabric surface is weak acidity of 6-7, and then the fabric is dried and shaped at the temperature of 115-125 ℃.
Preferably, the drying temperature is 110-120 ℃, and the time is 1-2 min;
preferably, the baking temperature is 135-150 ℃ and the baking time is 1-2 min.
Preferably, in the fabric pretreatment process, after the fabric is cleaned, the fabric is soaked in an aqueous solution of phellodendron amurense bark extract for 10-20 min, wherein the concentration of the aqueous solution of phellodendron amurense bark extract is 1-2%. When the fabric is pretreated, the phellodendron amurense bark extract aqueous solution is adopted for soaking, so that the lavender essence microcapsule finishing liquid is favorable for functionally finishing the fabric, the fragrance retention time of the fabric is prolonged, and the health care effect is enhanced; and can effectively improve the softness of the fabric.
Compared with the prior art, the invention has the following beneficial effects:
the modified melamine resin is used as the wall material of the microcapsule, and the lavender essence is used as the core material to prepare the microcapsule, so that the coating rate of the microcapsule can be obviously improved; meanwhile, the existence of the epristeride effectively improves the slow release performance of the microcapsule. After the fabric is finished by the finishing liquid prepared from the lavender essence microcapsules, the soaping resistance, the brushing resistance and the wear resistance of the fabric can be obviously improved, the fragrance retention time is effectively prolonged, and the health care effect is enhanced. In addition, when the fabric is pretreated, the phellodendron amurense bark extract aqueous solution is adopted for soaking, so that the lavender essence microcapsule finishing liquid is favorable for functionally finishing the fabric, the fragrance retention time of the fabric is prolonged, and the health care effect is enhanced; and can effectively improve the softness of the fabric. The microcapsule prepared by the invention has the advantages that part of raw materials can be biologically degraded, the whole preparation and finishing processes are green and environment-friendly, and the environmental load cannot be increased.
Therefore, the lavender essence microcapsule finishing liquid provided by the invention is used for finishing the fabric, so that the soaping resistance, the brushing resistance and the wear resistance of the fabric can be effectively improved, the fragrance release is delayed, the fragrance retaining time is prolonged, the health care effect is enhanced, and the lavender essence microcapsule finishing liquid has excellent antibacterial performance.
Drawings
FIG. 1 shows the results of the infrared test in test example 1 of the present invention;
FIG. 2 is a schematic diagram showing the results of the sustained-release performance test in Experimental example 2 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
the organic chelated tin used in the embodiment of the invention is chelated tin KRA-1 which is purchased from Kary chemical technology Co., Ltd, Changzhou; the polymer emulsifier is purchased from Shanghai technical service company; the cortex Phellodendri bark extract is obtained from Xian Qingzhi biotechnology, Inc., cat # 310; the crosslinking agent used was XR-500.
Example 1:
preparation of modified melamine resin:
weighing melamine resin and epristeride (the mass ratio of the melamine resin to the epristeride is 1: 2.8), dissolving the melamine resin and the epristeride in DMF (the solid-liquid ratio of the melamine resin to the DMF is 1: 17 g/mL), slowly dripping DMAP (the mass ratio of the DMAP to the melamine resin is 1.2: 1) under the condition of ice-water bath, reacting for 10min, adding EDC (the mass ratio of the melamine resin to the EDC is 1: 1.1), naturally heating to 23 ℃, and reacting for 20 h. Thin Layer Chromatography (TLC) was used to check if the reaction was complete. Pouring the reactant into water, respectively extracting with ethyl acetate and washing with saturated saline water, drying the organic phase with anhydrous sodium sulfate overnight, filtering, separating with silica gel column chromatography (eluent is ethyl acetate and petroleum ether with volume ratio of 1: 2), distilling under reduced pressure, and vacuum drying to obtain the modified melamine resin.
Preparation of a lavender essence microcapsule: (microcapsule structure core wall ratio of 1: 1)
S1: weighing lavender essence, adding a high molecular emulsifier (15.6% of the total mass of the lavender essence) and a proper amount of distilled water, and emulsifying at 15500r/min for 15min to obtain an emulsion;
s2: adjusting the pH value of the solution to 5.0 by using acetic acid, and pouring the solution into a three-neck flask to react at the same stirring speed; then adding the trimethylol melamine, properly reducing the stirring speed to 12000r/min, and preserving the temperature of the reaction solution at 65 ℃ for 1.5h to carry out single-layer wall building;
s3: after the reaction is finished, cooling to normal temperature, adding the modified melamine resin while stirring, and preserving heat for 2 hours at 80 ℃; and cooling to room temperature, adding a dispersant NNO, and adjusting the pH value to 7.5 by using ammonia water to obtain the lavender essence microcapsule. The average particle size of the prepared microcapsule is 2.8 mu m, and the particle size distribution is 0.8-3.2 mu m.
The finishing liquid is: 0.7 percent of lavender essence microcapsule (calculated by the weight of water), 1.8 percent of cross-linking agent (calculated by the weight of water) and water.
The finishing liquid is used for lavender fragrance finishing of the fabric, the fabric is pretreated, soaked in the lavender fragrance microcapsule finishing liquid, padded, the roller pressure is 3.6 kilograms, the liquid carrying rate is 90 percent, the vehicle speed is 24m/min, the fabric is dried at 115 ℃ for 1min, and the fabric is baked at 142 ℃ for 1min to obtain the lavender fragrance fabric.
The pretreatment of the fabric specifically comprises the following steps: the fabric is cleaned firstly, so that the water absorption of the fabric is less than or equal to 2 seconds, the pH value of the fabric surface is faintly acid 6.5, and then the fabric is dried and shaped at 120 ℃.
Example 2:
the preparation of the modified melamine resin differs from example 1 in that: the mass ratio of the melamine resin to the epristeride is 1: 2.5, fine adjustment is carried out on other conditions according to the actual reaction condition;
the difference between the preparation of the lavender essence microcapsule and the preparation of the lavender essence microcapsule in example 1 is that:
the core-wall ratio in the microcapsule structure is 1.1: 1;
in the step S1, the using amount of the high molecular emulsifier is 14.1 percent of the total mass of the lavender essence; the emulsifying time is 12 min; the stirring speed is 14500 r/min;
adjusting the pH value of the emulsion to 4.5 by using acetic acid in step S2; the constant temperature is 60 ℃, and the temperature is kept for 1 h.
The average grain diameter of the prepared microcapsule is 3.0 mu m, and the grain diameter distribution is 1.0-3.5 mu m.
The finishing liquid is: 0.5 percent of lavender essence microcapsule (calculated by the weight of water), 1.9 percent of cross-linking agent (calculated by the weight of water) and water.
The finishing liquid is used for the lavender fragrance finishing of the fabric, the fabric is pretreated, soaked in the lavender fragrance microcapsule finishing liquid, padded, the roller pressure is 3.8 kg, the liquid carrying rate is 89%, the vehicle speed is 25m/min, the fabric is dried at 112 ℃ for 1.5min, and the fabric is baked at 138 ℃ for 2min to obtain the lavender fragrance fabric;
the pretreatment of the fabric specifically comprises the following steps: the fabric is cleaned firstly, so that the water absorption of the fabric is less than or equal to 2 seconds, the pH value of the fabric surface is weak acidity of 6.4, and then the fabric is dried and shaped at 115 ℃.
Example 3:
the preparation of the modified melamine resin differs from example 1 in that: the mass ratio of the melamine resin to the epristeride is 1: 2.6, fine adjustment is carried out on other conditions according to the actual reaction condition;
the difference between the preparation of the lavender essence microcapsule and the preparation of the lavender essence microcapsule in example 1 is that:
the core-wall ratio in the microcapsule structure is 1.4: 1;
in the step S1, the dosage of the high molecular emulsifier is 14.7 percent of the total mass of the lavender essence; emulsifying for 10 min; the stirring speed is 14000 r/min;
adjusting the pH value of the emulsion to 5.0 by using acetic acid in step S2; the constant temperature is 63 ℃, and the temperature is kept for 1.5 h.
The average grain diameter of the prepared microcapsule is 2.5 mu m, and the grain diameter distribution is 0.5-3.0 mu m.
The finishing liquid is: 0.6 percent of lavender essence microcapsule (calculated by the weight of water), 2.1 percent of cross-linking agent (calculated by the weight of water) and water.
The finishing liquid is used for lavender fragrance finishing of the fabric, the fabric is pretreated, soaked in the lavender fragrance microcapsule finishing liquid, padded, rolled under the roller pressure of 4 kg and the liquid carrying rate of 92 percent, the vehicle speed is 26m/min, the fabric is dried at 110 ℃ for 2min, and the fabric is baked at 148 ℃ for 1.5min to obtain the lavender fragrance fabric;
the pretreatment of the fabric specifically comprises the following steps: the fabric is cleaned firstly, so that the water absorption of the fabric is less than or equal to 2 seconds, the pH value of the fabric surface is faintly acid 6, and then the fabric is dried and shaped at 125 ℃.
Example 4:
the preparation of the modified melamine resin differs from example 1 in that: the mass ratio of the melamine resin to the epristeride is 1: 3, fine adjustment is carried out on other conditions according to the actual reaction condition;
the difference between the preparation of the lavender essence microcapsule and the preparation of the lavender essence microcapsule in example 1 is that:
the core-wall ratio in the microcapsule structure is 1.5: 1;
in the step S1, the dosage of the high molecular emulsifier is 15.9 percent of the total mass of the lavender essence; the emulsifying time is 13 min; the stirring speed is 15000 r/min;
adjusting the pH value of the emulsion to 4.5 by using acetic acid in step S2; the constant temperature is 60 ℃, and the temperature is kept for 1.5 h.
The average particle size of the prepared microcapsule is 2.9 mu m, and the particle size distribution is 0.9-3.4 mu m.
The finishing liquid is: 0.4 percent of lavender essence microcapsule (calculated by the weight of water), 1.6 percent of cross-linking agent (calculated by the weight of water) and water.
The finishing liquid is used for the lavender fragrance finishing of the fabric, the fabric is pretreated, soaked in the lavender fragrance microcapsule finishing liquid, padded, rolled under the roller pressure of 3 kg, the liquid carrying rate is 88%, the vehicle speed is 23m/min, the fabric is dried at 120 ℃ for 1.5min, and the fabric is baked at 140 ℃ for 1min to obtain the lavender fragrance fabric;
the pretreatment of the fabric specifically comprises the following steps: the fabric is cleaned firstly, so that the water absorption of the fabric is less than or equal to 2 seconds, the pH value of the fabric surface is faintly acid 6.2, and then the fabric is dried and shaped at 125 ℃.
Example 5:
the preparation of the modified melamine resin differs from example 1 in that: the mass ratio of the melamine resin to the epristeride is 1: 2.9, fine adjustment is carried out on other conditions according to the actual reaction condition;
the difference between the preparation of the lavender essence microcapsule and the preparation of the lavender essence microcapsule in example 1 is that:
the core-wall ratio in the microcapsule structure is 1.3: 1.
in the step S1, the dosage of the high molecular emulsifier is 15.2 percent of the total mass of the lavender essence; the emulsifying time is 14 min; the stirring speed is 15600 r/min;
adjusting the pH value of the emulsion to 5.5 by using acetic acid in step S2; the constant temperature is 65 ℃, and the temperature is kept for 1.5 h.
The average particle size of the prepared microcapsule is 2.7 mu m, and the particle size distribution is 0.6-3.0 mu m.
The finishing liquid is: 0.8 percent of lavender essence microcapsule (calculated by the weight of water), 2.2 percent of cross-linking agent (calculated by the weight of water) and water.
The finishing liquid is used for the lavender fragrance finishing of the fabric, the fabric is pretreated, immersed in the lavender fragrance microcapsule finishing liquid, padded, the roller pressure is 3.5 kg, the liquid carrying rate is 91%, the vehicle speed is 24m/min, the fabric is dried at 115 ℃ for 1min, and the fabric is baked at 135 ℃ for 2min to obtain the lavender fragrance fabric;
the pretreatment of the fabric specifically comprises the following steps: the fabric is cleaned firstly, so that the water absorption of the fabric is less than or equal to 2 seconds, the pH value of the fabric surface is weak acidity of 6.5, and then the fabric is dried and shaped at 115 ℃.
Example 6:
the preparation of the modified melamine resin differs from example 1 in that: the mass ratio of the melamine resin to the epristeride is 1: 2.7, fine adjustment is carried out on other conditions according to the actual reaction condition;
the difference between the preparation of the lavender essence microcapsule and the preparation of the lavender essence microcapsule in example 1 is that:
the core-wall ratio in the microcapsule structure is 1.2: 1;
in the step S1, the dosage of the high molecular emulsifier is 16.1 percent of the total mass of the lavender essence; the emulsifying time is 14 min; the stirring speed is 16000 r/min;
adjusting the pH value of the emulsion to 4.5 by using acetic acid in step S2; the constant temperature is 60 ℃, and the temperature is kept for 1.5 h.
The average particle size of the prepared microcapsule is 2.6 mu m, and the particle size distribution is 0.7-3.1 mu m.
The finishing liquid is: 0.5 percent of lavender essence microcapsule (calculated by the weight of water), 2.2 percent of cross-linking agent (calculated by the weight of water) and water.
The finishing liquid is used for lavender fragrance finishing of the fabric, the fabric is pretreated, soaked in the lavender fragrance microcapsule finishing liquid, padded, the roller pressure is 3.1 kg, the liquid carrying rate is 86%, the vehicle speed is 22m/min, drying is carried out at 119 ℃ for 1.5min, and baking is carried out at 145 ℃ for 1min, so that the lavender fragrance fabric is obtained;
the pretreatment of the fabric specifically comprises the following steps: the fabric is cleaned firstly, so that the water absorption of the fabric is less than or equal to 2 seconds, the pH value of the fabric surface is faintly acid 6.8, and then the fabric is dried and shaped at 122 ℃.
Example 7:
the preparation of the modified melamine resin was the same as in example 1.
A lavender essence microcapsule was prepared in the same manner as in example 1.
The finishing liquor was the same as in example 1.
The difference between the finishing liquor used for the lavender fragrance finishing of the fabric and the finishing liquor of example 1 is that: in the fabric pretreatment process, the fabric is soaked in an aqueous solution of the phellodendron amurense bark extract for 15min, and the concentration of the aqueous solution of the phellodendron amurense bark extract is 1.6%.
Comparative example 1:
the difference between the preparation of the lavender essence microcapsule and the preparation of the lavender essence microcapsule in example 1 is that: the modified melamine resin is replaced by melamine resin.
The finishing liquor was the same as in example 1.
The finish liquid was used for the lavender scent finish of the fabric as in example 1.
Comparative example 2:
the difference between the preparation of the lavender essence microcapsule and the preparation of the lavender essence microcapsule in example 1 is that: the modified melamine resin was replaced with hexamethylol melamine resin.
The finishing liquor was the same as in example 1.
The finish liquid was used for the lavender scent finish of the fabric as in example 1.
Comparative example 3:
a lavender essence microcapsule was prepared in the same manner as in example 1.
The finishing liquor was the same as in example 1.
The difference between the finishing liquor used for the lavender fragrance finishing of the fabric and the finishing liquor of example 1 is that: it was not baked.
Test example 1:
1. infrared Spectrometry (FT-IR)
After a sample is subjected to water removal treatment in a constant-temperature drying oven, a small amount of sample and potassium bromide are uniformly mixed in an agate mortar, ground and tabletted, and then the mixture is placed on a TENSOR 27 type infrared spectrometer for testing, wherein the scanning wave number range is 4000-500 cm-1Scanning resolution of 6cm-1The number of scans was 18.
The results of the above tests on melamine resin and the modified melamine resin obtained in example 1 are shown in FIG. 1. As can be seen from the figure, 3401cm in the spectrum of the melamine resin-1The absorption peaks of the near corresponding N-H bond and-OH stretching vibration are 2980cm-1Is located at C-H bond stretching vibration absorption peak, 1690cm-1Near C = N bond stretching vibration absorption peak, 1370cm-1Is treated as a C-N stretching vibration absorption peak of 1015cm-1Absorption peak of stretching vibration at C-O, 810cm-1Is an absorption peak of the melamine aromatic heterocycle; in the spectrum after modification, 2900cm is compared with that before modification-1The absorption peaks of methyl and methylene in the epristeride are nearby; 1590cm-1Has a C = O bond stretching vibration absorption peak of 1510cm-1Near C = C bond characteristic absorption peak 1389cm-1The vicinity is a characteristic absorption peak of C-H on the double bond. The above results show the success of the preparation of the epristeride modified melamine resin.
2. Measurement of microcapsule particle diameter
Sucking a small amount of the prepared essence microcapsule suspension (uniformly oscillating) in a small beaker by a dropper, diluting with appropriate amount of distilled water, and placing in an ultrasonic cleaner for oscillating to disperse into single particles. And then measuring the size and the distribution condition of the grain diameter of the essence microcapsule particles by using an LS13320 type laser particle size analyzer.
3. Measurement of coating ratio of microcapsules
The coating rate of the microcapsule refers to the ratio of the amount of the coated core to the original amount of the coated core after a certain amount of the core is subjected to microencapsulation. The test adopts an ultraviolet absorption photometry to measure the coating rate of the lavender essence microcapsules.
Adding a standard lavender essence-ethanol solution with a certain mass concentration into a quartz cuvette, carrying out ultraviolet scanning at the wavelength of 190-400 nm at the interval of 1nm, observing the wavelength with the maximum absorbance from a scanning map, and making a standard curve according to different mass concentrations corresponding to ultraviolet absorption under the condition of the wavelength. Washing the reacted sample with absolute ethyl alcohol, then washing with clear water, drying in vacuum, putting into a round-bottom flask filled with absolute ethyl alcohol solution, refluxing for 1h at 75 ℃, filtering, fixing the volume of the filtrate to 500mL with the ethyl alcohol solution, and measuring the absorbance. And finding out the essence concentration corresponding to the absorbance from the standard absorption curve of the essence so as to calculate the content of the essence coated in the sample.
The results of the above tests on the microcapsules prepared in comparative examples 1 to 2 and examples 1 to 6 are shown in Table 1:
TABLE 1 coating Rate test results
| Sample (I) | Coating rate/% |
| Comparative example 1 | 81.7 |
| Comparative example 2 | 82.3 |
| Example 1 | 96.4 |
| Example 2 | 95.3 |
| Example 3 | 97.3 |
| Example 4 | 96.1 |
| Example 5 | 98.4 |
| Example 6 | 96.6 |
From the analysis in table 1, it can be seen that the coating rate of the microcapsule prepared in example 1 is significantly higher than that of the microcapsules prepared in comparative examples 1-2, and the coating rate of the microcapsule can be significantly improved by modifying melamine resin with epristeramine.
4. Research on antibacterial property of microcapsules
Preparing broth recommended to American Standard AATCC-100, testing the antibacterial effect of the microcapsule on escherichia coli (gram negative bacteria) and staphylococcus aureus (gram positive bacteria) at a preparation concentration of 1.78 multiplied by 108CFU/mL bacterial liquid, and 20mL microcapsule dispersion liquid with concentration of 5g/L and 40g/L respectively. Inoculating 2mL of the bacterial liquid to each microcapsule dispersion sample, culturing for 24h in a biochemical incubator at the temperature of 37 ℃ and the shaking speed of 50rpm, accurately absorbing 200 mu L of supernatant of the cultured bacterial-microcapsule dispersion by using a pipette gun, and diluting to 10000 times by twice. Then, 200. mu.L of the diluted microcapsule-bacterium dispersion was pipetted onto the medium and cultured at a constant temperature of 37 ℃ for 12 hours. And then calculating the bacteriostasis rate by a counting method so as to characterize the antibacterial performance of the microcapsule.
Broth formula: yeast extract (B): 5g/L, tryptone: 10g/L, NaCl: 10 g/L;
the formula of the culture medium is as follows: yeast extract (B): 5g/L, tryptone: 10g/L, NaCl: 10g/L, agar: 15 g/L.
The formula for calculating the bacteriostasis rate is as follows:
η=（N1-N2）/N1×100%
wherein, eta-bacteriostasis rate; n is a radical of1-number of bacterial colonies of the blank sample; n is a radical of2Number of bacterial colonies of the microcapsule sample.
The results of the above tests on the microcapsules prepared in comparative examples 1 to 2 and examples 1 to 6 are shown in Table 2:
TABLE 2 results of the bacteriostatic ratio test
From the analysis in table 2, it can be seen that the bacteriostatic effect of the microcapsule prepared in example 1 is significantly better than that of comparative example 1 and comparative example 2, which indicates that the lavender essence capsule prepared by modifying melamine resin with epristeride has excellent antibacterial performance, the bacteriostatic rate is greater than 95% when the concentration of the microcapsule reaches 5g/L, and the bacteriostatic rate reaches 100% when the concentration of the microcapsule reaches 40g/L, and the bacteriostatic effect of the modified melamine resin can be significantly improved.
Test example 2:
performance testing of functionally finished fabrics
1. Soaping resistance test
Preparing 5g/L soap solution by using standard soap chips; putting 5 multiplied by 10cm of coated fabric into a soaping cup, wherein the bath ratio is 1: 50, covering the container, washing for 5min at 40 ℃, and soaping for 50 times; after washing, the sample is washed clean with running water, squeezed by hand to remove excess water, and hung to dry at normal temperature.
2. Scrub resistance test
About 250mL (bath ratio not less than 50: 1) of the prepared soap solution is placed in a 500mL beaker, the temperature is raised to 60 +/-2 ℃, and then a sample is put into the beaker to be immersed and fully moistened. After dipping for 1min, the sample was taken out, excess solution on the sample was squeezed off with a glass rod, and the sample was spread on a plate of a brushing color fastness apparatus, and both ends were fixed with a holder (to the extent that the sample did not loosen during brushing). The nylon brush is placed on the sample, the handle is shaken or the switch is started, the brush is used for brushing the sample in a reciprocating linear mode for 100 times along a 10CITI track, the time of brushing in a reciprocating mode is 1s, the downward pressure of the brush head is 9N, and after each brushing for 25 times, about 10mL of solution is added to the sample to enable the sample to be wetted. After the brushing is finished, the sample is taken down, the sample is fully cleaned by clear water, 5 multiplied by 10cm is cut off from the part brushed by the brush to be used as a sample to be measured, and the cleaned sample to be measured is hung at normal temperature and dried.
3. Abrasion resistance test
The test is used for simulating the friction condition of the fabric in the wearing process, and the method for testing the wear resistance of the finished fabric comprises the following steps: the sample was spread on a plate of a brush-wash fastness tester, and both ends were fixed with a holder (to the extent that the sample did not loosen during brush-wash). The nylon brush is placed on a sample, the handle is shaken or the switch is started, the brush is used for brushing the sample in a reciprocating linear mode for 100 times along a 10CITI track, the time of brushing is 1s every time of brushing in a reciprocating mode, and the downward pressure of a brushing head is 9N. After the brushing is finished, the sample is taken down, the sample is fully cleaned by clear water, 5 multiplied by 10cm is cut off from the part brushed by the brush to be used as a sample to be measured, and the cleaned sample to be measured is hung at normal temperature and dried.
Determination of essence content in sample
After the three treatments, the content of the essence contained in the sample is measured by an absorptiometry, the sample is put into a round-bottomed flask filled with absolute ethanol solution, the reflux is carried out for 1h at the temperature of 75 ℃ (after the test, the essence in the sample is completely melted into the ethanol solution), the filtration is carried out, the volume of the filtrate is reduced to 500mL by the ethanol solution, and the absorbance is measured. And finding out the essence concentration corresponding to the absorbance from the lavender essence concentration-absorbance standard absorption curve so as to calculate the content of the essence in the sample.
The results of the above tests on the fabrics finished in comparative examples 1 to 3 and examples 1 to 6 are shown in Table 3:
table 3 functional finished fabric performance test results
As can be seen from Table 3, after the fabric treated in example 1 is soaped for 50 times, the fragrance retention rate of the fabric is obviously higher than that of the fabric treated in comparative examples 1-2; after 100 times of washing, the fragrance retention rate of the fabric is still over 35 percent, which is obviously higher than that of the fabric in comparative examples 1-2; in the friction effect of the simulated fabric in the wearing process, after 100 times of friction, the fragrance retention rate of the fabric is more than 80 percent and is obviously higher than that of the fabric in comparative examples 1-2; the results show that after the finishing liquid prepared by modifying the melamine resin by using the epristeride is acted on the fabric, the soap washing resistance, the scrubbing resistance and the friction resistance of the fabric can be effectively improved. In addition, the properties of example 1 are significantly higher than those of comparative example 3, indicating that the soap wash resistance, the scrub resistance and the rub resistance of the fabric are improved to some extent by the baking treatment at a certain temperature during the finishing of the fabric.
4. Test of sustained Release Performance
Shearing a fabric with the length of 20 multiplied by 30cm, treating the fabric by the microcapsule finishing liquid, naturally placing the fabric, testing the essence content in the sample every other month (the testing method is the same as the above), and drawing the aroma release performance curve of the fabric.
The results of the above tests on the fabrics treated in comparative example 1, comparative example 2 and example 1 are shown in fig. 2. Analysis in the figure shows that the release rate of the essence of the fabric treated in the example 1 is obviously lower than that of the fabric treated in the comparative examples 1-2, and the result shows that the finishing liquid prepared by modifying the melamine resin by using the epristerine can effectively enhance the slow release effect of the essence after acting on the fabric, and after 10 months, the fabric still has about 2.4% of the essence and the light fragrance of the fabric is preserved.
5. Testing of crease recovery, stiffness, flexibility and drape
The stiffness and flexibility (bending length) were measured with a TNG02A type fabric stiffness meter; determining the crease recovery property (crease recovery angle) of the fabric by using a YG (B) 541D-II type fabric crease elasticity tester; the drape (drape coefficient) of the fabric was measured using a fabric drape style tester model M506-ii.
The results of the above tests on the fabrics treated in comparative examples 1 to 2 and examples 1 to 7 are shown in Table 4:
table 4 fabric wrinkle recovery, stiffness, flexibility and drape test results
| Sample (I) | Bending length/cm | Crumple return angle/° | Sag coefficient/% |
| Original cloth | 1.43 | 61.32 | 23.48 |
| Comparative example 1 | 1.73 | 70.93 | 29.43 |
| Comparative example 2 | 1.63 | 69.19 | 30.47 |
| Example 1 | 1.91 | 73.31 | 33.63 |
| Example 2 | 1.83 | 71.43 | 32.17 |
| Example 3 | 1.92 | 73.29 | 33.98 |
| Example 4 | 1.86 | 73.14 | 32.02 |
| Example 5 | 2.05 | 71.51 | 33.94 |
| Example 6 | 2.08 | 72.73 | 33.53 |
| Example 7 | 2.21 | 80.43 | 38.42 |
From the analysis in table 4, it is found that the fabric treated in example 1 has a certain improvement in the wrinkle recovery angle, an increase in the bending length, and a higher sag factor than the original fabric; the effect of example 1 is only slightly better than that of comparative examples 1-2, while the effect of example 7 is obviously better than that of example 1, which shows that the softness of the fabric can be effectively improved after the fabric is soaked in the phellodendron bark extract aqueous solution in the pretreatment of the fabric.
Test example 3:
fragrance retention time test for fragrant functional finished fabrics
Please refer to 40 volunteers, including 20 girls and 20 boys, with the age between 20 and 40 years old; the fragrance intensity of the essence microcapsule finished fabric was evaluated periodically and the average value was taken, which was divided into four groups (5 boys and 5 girls per group). "+ +++" indicates a strong scent, "+ ++" indicates a moderate scent, "+ + + +" indicates a light scent, and "-" indicates no scent
The results of the above tests on the fabrics treated in comparative examples 1 to 2, 1 and 7 are shown in Table 5:
table 5 fragrance test results
From the analysis in the table 5, the fragrance retention time of the fabric treated in the example 1 is obviously better than that of the fabric treated in the comparative examples 1-2, and the fragrance retention time of the fabric can be effectively enhanced after the finishing liquid prepared by modifying the melamine resin by using the epristeramine acts on the fabric; example 7 is more effective than example 1, showing that the pre-treatment of the fabric by soaking with an aqueous solution of cork tree bark extract has a synergistic enhancement effect. The lavender has faint scent, and can improve sleep, relieve stress and anxiety and calm mind, so the fabric treated by the embodiment of the invention has good health care effect.
Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The application of modified melamine resin in the preparation of plant essence microcapsules is characterized in that the modified melamine resin is prepared by grafting the epristerine with the melamine resin.
2. Use according to claim 1, characterized in that: the preparation method of the modified melamine resin specifically comprises the following steps: dissolving melamine resin and epristerine in DMF, slowly dropwise adding DMAP under the condition of ice water bath, reacting for 10-15 min, adding EDC, naturally heating to 22-25 ℃, and reacting for 18-20 h; drying overnight, filtering, separating by silica gel column chromatography, distilling under reduced pressure, and vacuum drying to obtain modified melamine resin.
3. Use according to claim 2, characterized in that: the mass ratio of the melamine resin to the epristeride is 1: 2.5-3; the mass ratio of the DMAP to the melamine resin is 1-1.2: 1; the mass ratio of the EDC to the melamine is 1-1.1: 1.
4. a lavender essence microcapsule, comprising:
core material prepared from lavender essence;
a wall material made of the modified melamine resin according to claim 1;
wherein the core-wall ratio of the microcapsule structure is 1-1.5: 1.
5. the method for preparing the lavender essence microcapsule according to claim 4, comprising the following steps:
s1: weighing lavender essence, adding a high-molecular emulsifier and distilled water, and emulsifying under stirring to obtain an emulsion;
s2: adjusting the pH value of the emulsion by using acetic acid, adding the trimethylol melamine at the same stirring speed, reducing the stirring speed, reacting at constant temperature, and performing single-layer wall building;
s3: after the reaction is finished, cooling to normal temperature, adding the modified melamine resin while stirring, and preserving the temperature for a period of time at constant temperature; and cooling to room temperature, adding a dispersant NNO, and adjusting the pH value to obtain the lavender essence microcapsule.
6. The preparation method of the lavender essence microcapsule according to claim 5, wherein the preparation method comprises the following steps: in the step S1, the using amount of the emulsifier is 13.6-16.4% of the total mass of the lavender essence; the emulsifying time is 10-15 min; the stirring speed is 14000 to 16000 r/min;
adjusting the pH value of the emulsion to 4.5-5.5 by using acetic acid in the step S2; keeping the constant temperature at 60-65 ℃ and keeping the temperature for 1-1.5 h;
in the step S3, the constant temperature is 70-80 ℃, the temperature is kept for 1.5-2 h, and the pH value is adjusted to 7-8.
7. The preparation method of the lavender essence microcapsule according to claim 5, wherein the preparation method comprises the following steps: the average particle size of the microcapsule prepared by the preparation method is 2.5-3 mu m, and the particle size distribution is 0.5-3.5 mu m; the coating rate of the microcapsule is more than 90%.
8. A lavender essence microcapsule finishing liquid comprises: the lavender essence microcapsule, the cross-linking agent and the water according to claim 4, wherein the mass of the lavender essence microcapsule is 0.4-0.8% of the mass of the water, and the mass of the cross-linking agent is 1.5-2.4% of the mass of the water.
9. A finishing method of fabric specifically comprises the following steps: pretreating a fabric, immersing the fabric into the lavender essence microcapsule finishing liquid of claim 8, padding, rolling under the roller pressure of 3-4 kg, the liquid carrying rate of 82-92% and the vehicle speed of 20-26 m/min, drying, and baking to obtain the lavender fragrance fabric.
10. A method of finishing a fabric according to claim 9, wherein: the fabric pretreatment specifically comprises the following steps: cleaning the fabric to ensure that the water absorption of the fabric is less than or equal to 2 seconds and the pH value of the fabric surface is faintly acid 6-7, drying at 115-125 ℃, and shaping;
the drying temperature is 110-120 ℃, and the time is 1-2 min;
the baking temperature is 135-150 ℃, and the baking time is 1-2 min.
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| WO2006092094A1 (en) * | 2005-03-04 | 2006-09-08 | Tianjin Yorkool International Trading Co., Ltd. | Fabric finishing liquor for expelling and killing mosquitoes, method of use and products thereof |
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| WO2006092094A1 (en) * | 2005-03-04 | 2006-09-08 | Tianjin Yorkool International Trading Co., Ltd. | Fabric finishing liquor for expelling and killing mosquitoes, method of use and products thereof |
| CN102268326A (en) * | 2010-12-30 | 2011-12-07 | 上海水星家用纺织品股份有限公司 | Slow-release controllable lavender essential oil microcapsule and preparation method thereof as well as finishing agent and application thereof |
| CN107904929A (en) * | 2017-12-20 | 2018-04-13 | 贺州宝兴新材料有限公司 | A kind of modified melamine resin essence microcapsule preparation method |
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