CN111793989A - Dyeing and finishing method for spandex fabric of mint-fragrant cool regenerated cellulose fiber - Google Patents
Dyeing and finishing method for spandex fabric of mint-fragrant cool regenerated cellulose fiber Download PDFInfo
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- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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Abstract
The invention discloses a dyeing and finishing method of a spandex fabric of mint-fragrant cool regenerated cellulose fibers, which comprises the following steps: preparing a prepolymerization emulsion containing a polymerizable anionic surfactant and peppermint oil, a monomer pre-emulsion containing a polymerizable ester monomer, a polymerizable carboxylic acid monomer and graphene powder prepared by a redox method, an ammonium persulfate oxidant solution and a vitamin C solution in sequence; then, under the condition of room temperature, 1/3 oxidant solution and reducing agent solution are simultaneously dripped into the pre-polymerization emulsion while stirring, and capsule seed emulsion is prepared; and adding the rest oxidant solution, simultaneously dropwise adding the monomer pre-emulsion and the rest reducing agent solution to prepare the mint essential oil microcapsule emulsion, and diluting the mint essential oil microcapsule emulsion to prepare the fabric made of 90% of regenerated cellulose fiber yarns and 10% of spandex fibers. 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 dyeing and finishing, and particularly relates to a dyeing and finishing method of a spandex fabric of mint-fragrant cool regenerated cellulose fibers.
Background
In summer, the clothes to be worn have cool, cool and excellent ventilation effects. The cool fabric in the current market is mostly processed by the following two methods: one is realized by adopting ice-feeling raw yarn, and the ice-feeling raw yarn is obtained by adding cool-feeling materials such as jade and the like in the spinning process and then spinning. The method has the advantages that the fabric is good in washability, but the cool feeling materials such as jade are hidden inside the fibers, so that the cool feeling effect is poor after the fabric is contacted with the skin. The other method is to adopt ice feeling auxiliary agents such as mint microcapsules and the like, and the ice feeling auxiliary agents are realized by a later-stage padding mode, but the binding force of the mint microcapsules on the fabric is limited, and in order to increase the binding force, the mint microcapsules need to be fixed at the temperature of more than 100 ℃ after padding finishing, so that the stability of the mint microcapsules is poor, the release is fast, and the cool feeling durability of the fabric is influenced.
Disclosure of Invention
In order to overcome the problems in the background art, the invention provides a dyeing and finishing method of a spandex fabric of mint-fragrant cool regenerated cellulose fibers. The method can enhance the adhesion effect of the mint microcapsules on the fabric, avoid high-temperature adhesion and better ensure the stability of the mint microcapsules.
In order to realize the purpose of the invention, the adopted technical scheme is as follows: a dyeing and finishing method of a spandex fabric of mint-fragrant cool regenerated cellulose fibers comprises the following steps:
step 1, dissolving peregal O-30 in deionized water, and then adding a polymerizable anionic surfactant and peppermint oil to prepare a prepolymerization emulsion, wherein the mass percentage of each component is as follows: 10-15% of polymerizable anionic surfactant, 10-20% of peppermint oil, 1-5% of peregal O-30 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 nano 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 1/3 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 finished within 5-10min, controlling the dripping speed of the reducing agent solution to be finished within 1.5-3h, and continuing to react for 30-60min after finishing dripping; 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 to 3 hours, and continuing to react for 0.5 to 1.5 hours after the dropwise adding is finished to prepare the mint essential oil microcapsule emulsion;
and 5, diluting the mint essential oil microcapsule emulsion prepared in the step 4 with deionized water, then soaking a fabric made of 90% of regenerated cellulose fiber yarns and 10% of spandex fibers into the diluted microcapsule emulsion, performing dip finishing, and then drying at the temperature lower than 80 ℃.
Further, 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.
Further, the polymerizable carboxylic acid monomer is any one of acrylic acid and methacrylic acid.
Further, the polymerizable anionic surfactant is any one of ABM, MAPM, MAEM, VBM or VBS, and the structural formula is as follows:
ABM CH2=CHCOO(CH2)4OCOCH=CHCOOH
MAPM CH2=CH(CH3)COOCH2CH(CH3)OCOCH=CHCOOH
MAEM CH2=CH(CH3)COO(CH2)2OCOCH=CHCOOH
VBM CH2=CH6H4CH2OCOCH=CHCOOH
VBS CH2=CHC6H4CH2OCOCH2CH2COOH
compared with the prior art, the invention has the following technical effects:
the microcapsule preparation reaction temperature is room temperature, the reaction temperature is low, and the volatilization loss of the peppermint oil is reduced.
The acrylic adhesive is introduced to the surface of the microcapsule, so that the adhesive force of the acrylic adhesive on the surface of the fiber is improved, the high-temperature fixation is not needed in the later dyeing and finishing, the microcapsule structure is not damaged, and the stability and the durability of the microcapsule 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, the release rate of the peppermint oil in the microcapsule can be reduced, and the graphene can also improve the mechanical strength of the microcapsule and enhance the adhesive force of the microcapsule on the surface of the fiber, so that the service life of the microcapsule on the surface of the fiber is prolonged; in addition, the antibacterial ability of the fabric can be improved by adding the graphene.
The finished fabric has the original hand feeling of the regenerated cellulose fiber (bamboo): comfortable, soft and good drapability, and has the characteristics of mint fragrance and cool wearing. Meanwhile, due to the use of a slow release technology of the microcapsule, the mint fragrance is high in fixation fastness and lasting in fragrance, and the cool feeling durability of the fabric is good.
Drawings
Fig. 1 is a graph of the sustained release performance of the mint essential oil microcapsules prepared in the embodiments of the present invention.
Fig. 2 is a diagram showing the water washing resistance of the mint essential oil microcapsules prepared in the embodiments of the present invention.
Detailed Description
The invention is described in more detail below with reference to the following examples:
example 1
A dyeing and finishing method of a spandex fabric of mint-fragrant cool regenerated cellulose fibers comprises the following steps:
step 1, dissolving peregal O-30 in deionized water, and then adding a polymerizable anionic surfactant and peppermint oil to prepare a prepolymerization emulsion, wherein the mass percentage of each component is as follows: 10% of polymerizable anionic surfactant, 15% of peppermint oil, 1% of peregal O-30 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: 45% of polymerizable ester monomer, 3% of polymerizable carboxylic acid monomer, 0.05% of graphene powder, 1% 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 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 0.1 percent of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer;
step 4, simultaneously dripping 1/3 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 finished within 5min, controlling the dripping speed of the reducing agent solution to be finished within 2h, and continuing to react for 60min after finishing dripping; 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 oxidant solution, completing dropwise adding within 3h, and continuing to react for 0.5h after the dropwise adding is finished to obtain the mint essential oil microcapsule emulsion;
and 5, diluting the mint essential oil microcapsule emulsion prepared in the step 4 by using deionized water until the mass concentration is 15%, then soaking a fabric made of 90% of regenerated cellulose fiber yarns and 10% of spandex fibers into the diluted microcapsule emulsion, performing padding finishing, and drying, wherein the mass ratio of the fabric to the diluted mint essential oil microcapsule emulsion is 3%, and the rolling residual rate is controlled to be 90%.
The polymerizable ester monomer is ethyl methacrylate, propyl methacrylate, methyl acrylate and hydroxypropyl acrylate in a mass ratio of 1:1:1:1, the polymerizable carboxylic acid monomer is acrylic acid, and the polymerizable anionic surfactant is ABM.
Example 2
A dyeing and finishing method of a spandex fabric of mint-fragrant cool regenerated cellulose fibers comprises the following steps:
step 1, dissolving peregal O-30 in deionized water, and then adding a polymerizable anionic surfactant and peppermint oil to prepare a prepolymerization emulsion, wherein the mass percentage of each component is as follows: 15% of polymerizable anionic surfactant, 10% of peppermint oil, 3% of peregal O-30 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% of polymerizable ester monomer, 10% of polymerizable carboxylic acid monomer, 0.1% of graphene powder, 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 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 0.01 percent of the total mole number of the polymerizable anionic surfactant, the polymerizable ester monomer and the polymerizable carboxylic acid monomer;
step 4, simultaneously dripping 1/3 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 finished within 10min, controlling the dripping speed of the reducing agent solution to be finished within 1.5, and continuing to react for 30min after finishing dripping; 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 oxidant solution, completing dropwise adding within 2 hours, and continuing to react for 1 hour after the dropwise adding is finished to obtain the mint essential oil microcapsule emulsion;
and 5, diluting the mint essential oil microcapsule emulsion prepared in the step 4 to the mass concentration of 15% by using deionized water, then soaking a fabric made of 90% of regenerated cellulose fiber yarns and 10% of spandex fibers into the diluted microcapsule emulsion, performing padding finishing, and then drying, wherein the mass ratio of the fabric to the diluted mint essential oil microcapsule emulsion is 3%, and the rolling residual rate is controlled to be 90%.
The polymerizable ester monomer is propyl methacrylate, butyl methacrylate, methyl acrylate, ethyl acrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate in a mass ratio of 1:1:2:2:1, the polymerizable carboxylic acid monomer is methacrylic acid, and the polymerizable anionic surfactant is MAPM.
Example 3
A dyeing and finishing method of a spandex fabric of mint-fragrant cool regenerated cellulose fibers comprises the following steps:
step 1, dissolving peregal O-30 in deionized water, and then adding a polymerizable anionic surfactant and peppermint oil to prepare a prepolymerization emulsion, wherein the mass percentage of each component is as follows: 12% of polymerizable anionic surfactant, 20% of peppermint oil, 5% of peregal O-30 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: 30% of polymerizable ester monomer, 5% of polymerizable carboxylic acid monomer, 0.1% of graphene powder, 2% 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 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;
step 4, simultaneously dripping 1/3 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 finished within 8min, controlling the dripping speed of the reducing agent solution to be finished within 3h, and continuing to react for 40min after finishing dripping; 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 oxidant solution, completing dropwise adding within 3h, and continuing to react for 1h after the dropwise adding is finished to obtain the mint essential oil microcapsule emulsion;
and 5, diluting the mint essential oil microcapsule emulsion prepared in the step 4 to the mass concentration of 15% by using deionized water, then soaking a fabric made of 90% of regenerated cellulose fiber yarns and 10% of spandex fibers into the diluted microcapsule emulsion, performing padding finishing, and then drying, wherein the mass ratio of the fabric to the diluted mint essential oil microcapsule emulsion is 3%, and the rolling residual rate is controlled to be 90%.
The polymerizable ester monomer is ethyl methacrylate and methyl acrylate in a mass ratio of 2:1, the polymerizable carboxylic acid monomer is acrylic acid, and the polymerizable anionic surfactant is VBS.
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.
Examples of effects
And (3) determining the encapsulation rate: reference to journal literature: royal jelly, xiao gang, xu xiao ying determination of slow release property of microencapsulated peppermint oil [ J ]. food and fermentation industry, 1999,26(2):28-31. first determine the total oil content of the microcapsules, then determine the surface oil content of the microcapsules, the encapsulation rate (total oil content of the microcapsules-surface oil content of the microcapsules)/total oil content of the microcapsules x 100%, and the encapsulation rates of the peppermint essential oil microcapsules prepared in examples 1, 2 and 3 and comparative example 1 were determined to be 97.1%, 97.7%, 98% and 98.5%, respectively.
Testing the slow release performance of the dyed and finished fabric by using the mint essential oil microcapsules: the mint essential oil microcapsule dyeing and finishing material obtained in each of the above examples and comparative example 1 was placed in an oven at 100 ℃ to test the amount of mint essential oil contained in the fabric after 0, 2, 4, 6, 8 and 10 hours. The specific test method is as follows: taking 1g of the dyed and finished fabric of the mint essential oil microcapsules, cutting into pieces, placing the cut fabric 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, taking supernatant, and performing gas chromatography analysis under the gas chromatography conditions: GC-950 type gas chromatography, carrier gas: nitrogen gas; sample inlet temperature: 250 ℃, sample introduction: 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 3 min; FID temperature: at 250 ℃ to obtain a mixture. 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 water washing resistance of the fabric after dyeing and finishing by the mint essential oil microcapsules is as follows: according to the standard test of GB/T8629-: GC-950 type gas chromatography, carrier gas: nitrogen gas; sample inlet temperature: 250 ℃, sample introduction: 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 3 min; 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 the water washing resistance of the microcapsule is obviously improved after the graphene powder is added.
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 (4)
1. A dyeing and finishing method of a spandex fabric of mint-fragrant cool regenerated cellulose fibers is characterized by comprising the following steps: the method comprises the following steps:
step 1, dissolving peregal O-30 in deionized water, and then adding a polymerizable anionic surfactant and peppermint oil to prepare a prepolymerization emulsion, wherein the mass percentage of each component is as follows: 10-15% of polymerizable anionic surfactant, 10-20% of peppermint oil, 1-5% of peregal O-30 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 1/3 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 finished within 5-10min, controlling the dripping speed of the reducing agent solution to be finished within 1.5-3h, and continuing to react for 30-60min after finishing dripping; 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 to 3 hours, and continuing to react for 0.5 to 1.5 hours after the dropwise adding is finished to prepare the mint essential oil microcapsule emulsion;
and 5, diluting the mint essential oil microcapsule emulsion prepared in the step 4 with deionized water, soaking a fabric made of 90% of regenerated cellulose fiber yarns and 10% of spandex fibers in the diluted microcapsule emulsion, performing padding finishing, and drying.
2. The dyeing and finishing method of the spandex fabric of the mint-scented cool regenerated cellulose fiber as claimed in claim 1, characterized in that: 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. The dyeing and finishing method of the spandex fabric of the mint-scented cool regenerated cellulose fiber as claimed in claim 1, characterized in that: the polymerizable carboxylic acid monomer is any one of acrylic acid and methacrylic acid.
4. The dyeing and finishing method of the spandex fabric of the mint-scented cool regenerated cellulose fiber as claimed in claim 1, characterized in that: the polymerizable anionic surfactant is any one of ABM, MAPM, MAEM, VBM or VBS.
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