CN111851079B - Microencapsulated wormwood essential oil-containing mosquito-repellent fabric finishing agent and mosquito-repellent fabric finishing method - Google Patents
Microencapsulated wormwood essential oil-containing mosquito-repellent fabric finishing agent and mosquito-repellent fabric finishing method Download PDFInfo
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Abstract
The invention discloses a microencapsulated blumea essential oil-containing mosquito repellent fabric finishing agent, which is prepared by the following method: sequentially preparing Arabic gum, a pre-polymerization emulsion containing a polymerizable anionic surfactant, wormwood essential oil, cinnamon oil and mint oil, a monomer pre-emulsion containing a polymerizable ester monomer, a polymerizable carboxylic acid monomer and graphene powder prepared by a redox method, and preparing a capsule seed emulsion from the pre-polymerization emulsion in a redox catalysis system at room temperature; and then dropwise adding the monomer pre-emulsion and the residual reducing agent solution to prepare the microencapsulated mosquito repellent fabric finishing agent containing the wormwood essential oil, and finishing the fabric modified by cations after dilution. The finished fabric is not required to be fixed at high temperature in the later period, the microcapsule structure is not damaged, and the stability and the durability of the microcapsule are ensured.
Description
Technical Field
The invention belongs to the technical field of textile finishing, and particularly relates to a microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent and a mosquito repellent fabric finishing method.
Background
In summer, the weather is hot and the mosquitoes are more, in order to prevent the mosquitoes from biting, the clothing fabric with the mosquito repelling effect is developed, but the mosquito repelling fabric in the prior art is mostly of a multilayer structure and comprises a base fabric layer, a fabric layer and a mosquito repelling layer arranged between the base fabric layer and the fabric layer, for example, a mosquito repelling and moisture absorbing fabric is disclosed in Chinese patent literature (application No. 201410428554.1), and then, for example, an antibacterial mosquito repelling fabric with good effect and a preparation method thereof are disclosed in Chinese patent literature (application No. 201510284983.0), and the defects of multiple material layers, vapor permeability difficulty, sultry and water fastness exist.
Disclosure of Invention
In order to overcome the problems in the background art, the invention provides a microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent and a mosquito repellent fabric finishing method. According to the method, the argy wormwood leaf essential oil is microencapsulated, and the cinnamon oil and the mint oil are introduced simultaneously to obtain the mosquito-repellent fabric finishing agent, so that the fabric can be endowed with the mosquito-repellent and itching-relieving functions, the fabric can be increased in coolness and comfort, and the fabric finishing agent is particularly suitable for clothes in summer.
In order to realize the purpose of the invention, the adopted technical scheme is as follows: a microencapsulated blumea essential oil-containing mosquito repellent fabric finishing agent is prepared by the following steps:
step 1, dissolving Arabic gum in deionized water, and then adding a polymerizable anionic surfactant, peppermint oil, wormwood essential oil and cinnamon oil to prepare a prepolymerization emulsion, wherein the mass percentages of the components are as follows: 5-10% of polymerizable anionic surfactant, 15-20% of wormwood essential oil, 2-5% of peppermint oil, 2-5% of cinnamon oil, 5-10% of Arabic gum and the balance of deionized water;
dissolving ammonium persulfate in deionized water to prepare an oxidant solution, wherein the use amount of the ammonium persulfate is 1-3% of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer; dissolving vitamin C in deionized water to prepare a reducing agent solution, wherein the dosage of the vitamin C is 0.01-0.1% of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer;
Further, in the step 2, the polymerizable ester monomer is any one or more of ethyl methacrylate, propyl methacrylate, butyl methacrylate, methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate.
Further, in the step 2, the polymerizable carboxylic acid monomer is any one of acrylic acid and methacrylic acid.
Further, in step 1, the polymerizable anionic surfactant is any one of ABM, MAPM, MAEM, VBM or VBS, and the structural formula is as follows:
ABM CH 2 =CHCOO(CH 2 ) 4 OCOCH=CHCOOH
MAPM CH 2 =CH(CH 3 )COOCH 2 CH(CH 3 )OCOCH=CHCOOH
MAEM CH 2 =CH(CH 3 )COO(CH 2 ) 2 OCOCH=CHCOOH
VBM CH 2 =CHC 6 H 4 CH 2 OCOCH=CHCOOH
VBS CH 2 =CHC 6 H 4 CH 2 OCOCH 2 CH 2 COOH。
a finishing method of mosquito repellent fabric comprises the following steps:
step a, soaking the fabric into a solution containing bis (3-chloro-2-hydroxypropyl) tetramethylethylenediamine dichloride, then drying, soaking into a sodium hydroxide solution, and cooling after baking to obtain a cation modified fabric;
and b, diluting the microencapsulated mosquito repellent fabric finishing agent containing the wormwood essential oil with deionized water, soaking the cation modified fabric prepared in the step a into the diluted microencapsulated mosquito repellent fabric finishing agent containing the wormwood essential oil, and dehydrating and drying after soaking to prepare the mosquito repellent fabric.
Further, the fabric is made of yarns of 70% of regenerated cellulose fibers, 20% of cotton fibers and 10% of spandex fibers.
Compared with the prior art, the invention has the following technical effects:
preparing essential oil seed emulsion from prepolymerization emulsion containing Arabic gum and polymerizable anionic surfactant in an oxidation-reduction system, wrapping the Arabic gum on the surface of the essential oil in the seed emulsion for primary encapsulation, combining the anionic surfactant to promote compatibility, and further forming the microencapsulated mosquito repellent fabric finishing agent containing the wormwood essential oil.
The microencapsulated mosquito-repellent fabric finishing agent containing the argy wormwood essential oil is prepared at room temperature, the reaction temperature is low, the loss of effective components of the argy wormwood essential oil is reduced, and the freshness and the mosquito-repellent effect of the argy wormwood essential oil are maintained.
The acrylic monomer is introduced, so that the microencapsulated mosquito repellent fabric finishing agent containing the wormwood essential oil can be endowed with the adhesive property, and is combined with the quaternary ammonium salt cations on the surface of the fabric, the attachment rate and the adhesive force of the finishing agent on the fabric are greatly improved, the high-temperature fixation is not needed in later finishing, the microcapsule structure cannot be damaged, and the stability of the microcapsule and the lasting mosquito repellent and itching relieving effects are ensured.
The graphene prepared by the redox method has a small amount of defects on the surface, has reaction activity at double bonds near the defects, and can participate in free radical polymerization reaction so as to be grafted to the microcapsule. By introducing the graphene, the shielding property of the microcapsule wall can be improved, and the release rate of the peppermint oil in the microcapsule can be reduced. The mechanical strength of the microcapsule can be improved by the graphene, and the residual carboxyl groups on the surface of the graphene can be combined with the quaternary ammonium salt grafted on the fabric to form chemical bonds, so that the adhesive force of the graphene on the fabric is enhanced, and the service life of the graphene on the surface of the fiber is prolonged; in addition, the antibacterial ability of the fabric can be improved by adding the graphene.
The finishing agent disclosed by the invention contains carboxyl and other anionic groups and cationic groups grafted on the fabric to form chemical bonds, so that the attachment density of the finishing agent on the fabric is improved, and the fabric is ensured to have good mosquito repelling and itching relieving effects, good air permeability and cooling comfort.
Drawings
Fig. 1 is a slow release performance diagram of the fabric finished by the microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent prepared in each embodiment of the invention.
Fig. 2 is a water washing resistance chart of the fabric finished by the microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent prepared in each embodiment of the invention.
Detailed Description
The invention is described in further detail below with reference to examples:
example 1
A microencapsulated mosquito repellent fabric finishing agent containing wormwood essential oil is prepared by the following steps:
step 1, dissolving Arabic gum in deionized water, and then adding a polymerizable anionic surfactant, peppermint oil, wormwood essential oil and cinnamon oil to prepare a prepolymerization emulsion, wherein the mass percentage of each component is as follows: 7% of polymerizable anionic surfactant, 15% of wormwood essential oil, 5% of mint essential oil, 5% of cinnamon oil, 7% of Arabic gum and the balance of deionized water.
step 3, dissolving ammonium persulfate in deionized water to prepare an oxidant solution, wherein the using amount of the ammonium persulfate is 1.5 percent of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer; dissolving vitamin C in deionized water to prepare a reducing agent solution, wherein the using amount of the vitamin C is 0.08 percent of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer;
The polymerizable ester monomer is ethyl methacrylate, propyl methacrylate, methyl acrylate and hydroxypropyl acrylate with the mass ratio of 1.
A finishing method of mosquito repellent fabric comprises the following steps:
step a, soaking the fabric into a solution containing bis (3-chloro-2-hydroxypropyl) tetramethylethylenediamine dichloride, then drying, soaking into a sodium hydroxide solution, and cooling after baking to obtain a cation modified fabric;
and b, diluting the microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent with deionized water until the mass content of the microcapsules is 15%, then soaking the cation modified fabric prepared in the step a in the diluted microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent, and after the cation modified fabric is soaked in the diluted wormwood essential oil-containing mosquito repellent fabric finishing agent, dehydrating and drying the fabric to obtain the mosquito repellent fabric. The mass ratio of the fabric to the diluted microencapsulated blumea essential oil-containing mosquito repellent fabric finishing agent is 3%, and the rolling residual rate is controlled to be 90%. The fabric is made of yarns of 70% of regenerated cellulose fibers, 20% of cotton fibers and 10% of spandex fibers.
Example 2
A finishing method of a spandex fabric of mint-fragrant cool regenerated cellulose fibers comprises the following steps:
step 1, dissolving Arabic gum in deionized water, and then adding a polymerizable anionic surfactant, peppermint oil, wormwood essential oil and cinnamon oil to prepare a prepolymerization emulsion, wherein the mass percentage of each component is as follows: 5% of polymerizable anionic surfactant, 18% of wormwood essential oil, 4% of peppermint oil, 3% of cinnamon oil, 8% of acacia senegal and the balance of deionized water;
dissolving ammonium persulfate in deionized water to prepare an oxidant solution, wherein the using amount of the ammonium persulfate is 1.5 percent of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer; dissolving vitamin C in deionized water to prepare a reducing agent solution, wherein the using amount of the vitamin C is 0.03 percent of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer;
a finishing method of mosquito repellent fabric comprises the following steps:
step a, soaking the fabric into a solution containing bis (3-chloro-2-hydroxypropyl) tetramethyldiammonium ethylene dichloride, then drying, soaking into a sodium hydroxide solution, and cooling after baking to obtain a cation modified fabric;
and b, diluting the emulsion containing the microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent with deionized water until the mass concentration of the microcapsules is 15%, soaking the cation modified fabric prepared in the step a in the diluted microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent, and dehydrating and drying after the fabric is soaked to obtain the mosquito repellent fabric. The mass ratio of the fabric to the diluted microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent is 3%, and the rolling residual rate is controlled to be 90%. The fabric is made of yarns of 70% of regenerated cellulose fibers, 20% of cotton fibers and 10% of spandex fibers.
The polymerizable ester monomer is propyl methacrylate, butyl methacrylate, methyl acrylate, ethyl acrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate in a mass ratio of 1.
Example 3
A microencapsulated mosquito repellent fabric finishing agent containing wormwood essential oil is prepared by the following steps:
step 1, dissolving Arabic gum in deionized water, and then adding a polymerizable anionic surfactant, peppermint oil, wormwood essential oil and cinnamon oil to prepare a prepolymerization emulsion, wherein the mass percentage of each component is as follows: 10% of polymerizable anionic surfactant, 18% of wormwood essential oil, 2% of peppermint oil, 5% of cinnamon oil, 10% of Arabic gum and the balance of deionized water;
step 3, dissolving ammonium persulfate in deionized water to prepare an oxidant solution, wherein the using amount of the ammonium persulfate is 3% of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer; dissolving vitamin C in deionized water to prepare a reducing agent solution, wherein the using amount of the vitamin C is 0.05 percent of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer;
a finishing method of mosquito repellent fabric comprises the following steps:
step a, soaking the fabric into a solution containing bis (3-chloro-2-hydroxypropyl) tetramethylethylenediamine dichloride, then drying, soaking into a sodium hydroxide solution, and cooling after baking to obtain a cation modified fabric;
and b, diluting the emulsion containing the microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent with deionized water until the mass concentration of the microcapsules is 15%, soaking the cation modified fabric prepared in the step a in the diluted microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent, and dehydrating and drying after the fabric is soaked to obtain the mosquito repellent fabric. The mass ratio of the fabric to the diluted microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent is 3%, and the rolling residual rate is controlled to be 90%. The fabric is made of yarns containing 70% of regenerated cellulose fibers, 20% of cotton fibers and 10% of spandex fibers.
The polymerizable ester monomer is ethyl methacrylate and methyl acrylate with the mass ratio of 2.
Comparative example 1
The difference from example 1 is that the content of graphene powder in the monomer pre-emulsion is 0, the polymerizable carboxylic acid monomer is 3.05%, and the rest is the same as example 1.
Comparative example 2
The difference from example 1 is that the finished face fabric is not cationically modified, and the rest is the same as example 1.
Effects of the invention
And (3) determining the encapsulation rate: reference to journal literature: xylonite, xiaogang, xu Shi Ying, determination of slow release performance of microencapsulated peppermint oil [ J ] food and fermentation industry, 1999,26 (2): 28-31. First, the total oil content of the microcapsules is determined, then, the surface oil content of the microcapsules is determined, and the encapsulation rate = (the total oil content of the microcapsules-the surface oil content of the microcapsules)/the total oil content of the microcapsules x 100%, and the encapsulation rates of the microencapsulated mosquito repellent fabric finishing agents containing wormwood essential oil prepared in examples 1, 2 and 3 and comparative example 1 are respectively 96.5%, 95.9%, 96.3% and 96.4% after determination.
The slow release performance of the fabric finished by the microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent is tested as follows: after the materials finished by the microencapsulated mosquito repellent fabric finishing agent containing wormwood essential oil in each of the above examples and comparative example 1 are placed in an oven at 100 ℃, the residual percentage content of the wormwood essential oil on the fabric after 0, 2, 4, 6, 8 and 10 hours is respectively tested. The specific test method is as follows: taking 1g of the fabric finished by the microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent in the above examples and comparative examples, cutting the fabric into pieces, placing the cut fabric pieces into a four-neck flask, adding 5mL of 0.809mol/L HCl solution, stirring at 65 ℃ for 30min, adding 15mL of ethyl acetate, stirring for 90min, centrifuging at 4000r/min for 2min, and taking the supernatant to perform gas chromatography analysis under the gas chromatography conditions: GC-950 type gas chromatography, carrier gas: nitrogen gas; sample inlet temperature: 250 ℃, sample size: 0.2 μ L, sample injection mode: shunting; column temperature: keeping at 80 deg.C for 1min, heating to 150 deg.C at 20 deg.C/min, and keeping for 3min; FID temperature: at 250 deg.c. The test result is shown in fig. 1, and it can be seen from fig. 1 that the slow release performance of the microcapsule added with the graphene powder is obviously improved.
The fabric after being finished by the microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent has the advantages of water washing resistance and mosquito repellent effect: according to the standard test of GB/T8629-2017 household washing and drying program for textile test, the fabric after the finishing agent of the microencapsulated wormwood essential oil-containing mosquito repellent fabric in each example and comparative example 1 is washed for 0, 2, 4, 6, 8 and 10 times, the amount of the wormwood essential oil remained in the fabric and the mosquito repellent effect of the fabric are respectively determined. And (3) measuring the residual argy wormwood leaf essential oil amount of the fabric by adopting a gas chromatography, wherein the gas chromatography conditions are as follows: GC-950 type gas chromatography, carrier gas: nitrogen gas; sample inlet temperature: 250 ℃, sample size: 0.2 μ L, sample injection mode: shunting; column temperature: maintaining at 80 deg.C for 1min, heating to 150 deg.C at 20 deg.C/min, and maintaining for 3min; FID temperature: at 250 ℃ to obtain a mixture. The test result is shown in fig. 2, and it can be seen from fig. 2 that after the graphene powder is added, the water washing resistance of the microencapsulated wormwood essential oil-containing finishing agent for mosquito repellent fabric is obviously improved. The mosquito repelling test method of the mosquito repelling fabric comprises the following specific steps: 300 prepared female culex fatigues are placed in 6 mosquito cages of 300mm × 300mm × 300mm, 3 persons are selected, the prepared fabrics (the fabrics washed by water for 0 time, 6 times and 10 times respectively) are laid on the palm of the left hand, then the left hand and the right hand are stretched into 2 mosquito cages for 5min respectively, the palm of the hand is upward, the number of mosquitoes staying and sucking blood before is observed and recorded, the right hand is used as a blank control hand, more than 30 mosquitoes come before, that is, the mosquito attack force is judged to be qualified, the mosquito repelling effect of the fabric on the left hand is effective, the room temperature is 26-27 ℃ in the experimental process, the relative humidity is 60-70%, and the experimental results are shown in table 1:
TABLE 1 mosquito repellent Effect test
As can be seen from table 1, the mosquito repellent fabrics obtained in examples 1 to 3 still have mosquito repellent effect after being washed for ten times, and the mosquito repellent effect of comparative example 1 and comparative example 2 is significantly reduced.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and their concepts should be equivalent or changed within the technical scope of the present invention.
Claims (6)
1. A microencapsulated mosquito repellent fabric finishing agent containing wormwood essential oil is characterized in that: the finishing agent is prepared by the following steps:
step 1, dissolving Arabic gum in deionized water, and then adding a polymerizable anionic surfactant, peppermint oil, wormwood essential oil and cinnamon oil to prepare a prepolymerization emulsion, wherein the mass percentage of each component is as follows: 5-10% of polymerizable anionic surfactant, 15-20% of wormwood essential oil, 2-5% of peppermint oil, 2-5% of cinnamon oil, 5-10% of Arabic gum and the balance of deionized water;
step 2, dissolving peregal O-30 in deionized water, and then adding a polymerizable ester monomer, a polymerizable carboxylic acid monomer and graphene powder prepared by a redox method to prepare a monomer pre-emulsion, wherein the monomer pre-emulsion comprises the following components in percentage by mass: 25-45% of polymerizable ester monomer, 3-10% of polymerizable carboxylic acid monomer, 0.05-0.2% of graphene powder, 1-6% of peregal O-30 and the balance of deionized water; the sheet diameter of the graphene powder is less than 1 mu m, and the number of layers is less than 5;
dissolving ammonium persulfate in deionized water to prepare an oxidant solution, wherein the use amount of the ammonium persulfate is 1-3% of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer; dissolving vitamin C in deionized water to prepare a reducing agent solution, wherein the dosage of the vitamin C is 0.01-0.1% of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer;
step 4, simultaneously dripping 1/5 of the oxidant solution and the reducing agent solution prepared in the step 3 into the pre-polymerization emulsion prepared in the step 1 while stirring at room temperature, controlling the dripping speed of the oxidant solution to be completely dripped within 5-10min, controlling the dripping speed of the reducing agent solution to be completely dripped within 30-60min, and continuously reacting for 10-30min after the dripping is finished; and after the heat preservation is finished, adding the residual oxidant solution, dropwise adding the monomer pre-emulsion and the residual reducing agent solution into the mixture, completing the dropwise adding within 1.5-3h, and continuing to react for 0.5-1.5h after the dropwise adding is finished to prepare the microencapsulated mosquito repellent fabric finishing agent containing the wormwood essential oil.
2. A microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent as claimed in claim 1, characterized in that: in the step 2, the polymerizable ester monomer is any one or more of ethyl methacrylate, propyl methacrylate, butyl methacrylate, methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate or hydroxypropyl methacrylate.
3. A microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent as claimed in claim 1, characterized in that: the polymerizable carboxylic acid monomer in the step 2 is any one of acrylic acid and methacrylic acid.
4. A microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent as claimed in claim 1, characterized in that: in the step 1, the polymerizable anionic surfactant is any one of ABM, MAPM, MAEM, VBM or VBS.
5. A finishing method of mosquito repellent fabric is characterized by comprising the following steps: the method comprises the following steps:
step a, soaking the fabric into a solution containing bis (3-chloro-2-hydroxypropyl) tetramethylethylenediamine dichloride, then drying, soaking into a sodium hydroxide solution, and cooling after baking to obtain a cation modified fabric;
step b, diluting the microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent of any one of claims 1 to 4 with deionized water, then soaking the cation modified fabric prepared in the step a in the diluted microencapsulated wormwood essential oil-containing mosquito repellent fabric finishing agent, and dehydrating and drying after soaking to prepare the mosquito repellent fabric.
6. A finishing method of a mosquito repellent fabric according to claim 5, characterized in that: the fabric is made of yarns containing 70% of regenerated cellulose fibers, 20% of cotton fibers and 10% of spandex fibers.
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