CN113930967A - Lignin-containing composite emulsion for sun-blocking clothes and preparation method and application thereof - Google Patents

Lignin-containing composite emulsion for sun-blocking clothes and preparation method and application thereof Download PDF

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CN113930967A
CN113930967A CN202111346477.1A CN202111346477A CN113930967A CN 113930967 A CN113930967 A CN 113930967A CN 202111346477 A CN202111346477 A CN 202111346477A CN 113930967 A CN113930967 A CN 113930967A
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lignin
sun
emulsion
clothes
water
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CN113930967B (en
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杨永生
冯宇琴
李海波
马文霞
余韵滋
张钢
杨铭
吴雅琪
周凡雨
彭雄义
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Wuhan Textile University
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Wuhan Textile University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/248Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
    • D06M13/256Sulfonated compounds esters thereof, e.g. sultones
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a preparation method of lignin-containing composite emulsion for sun-blocking clothes. The lignin composite emulsion for sun-blocking clothes can be prepared by the following steps: firstly, performing acetylation treatment on alkali lignin, and preparing the acetylated alkali lignin into an oil-in-water emulsion containing lignin; preparing a polyacrylate emulsion, and compounding the lignin-containing oil-in-water emulsion with the polyacrylate emulsion to obtain the lignin/polyacrylate composite emulsion, namely the lignin composite emulsion for sun protection clothes. The emulsion is used for sun-blocking clothes with polyester fiber as fabric, and the sun-blocking clothes have good ultraviolet resistance after being finished. The UPF value of the sun-blocking clothes prepared by the invention reaches above 68, and is obviously higher than that of purchased sun-blocking clothes; after 10 times of washing, the UPF value of the sun-blocking clothes prepared by the invention is not obviously reduced, which shows that the uvioresistant performance of the sun-blocking clothes is not weakened after multiple times of washing.

Description

Lignin-containing composite emulsion for sun-blocking clothes and preparation method and application thereof
Technical Field
The invention belongs to the technical field of emulsion, and particularly relates to lignin-containing composite emulsion for sun-blocking clothes, and a preparation method and application thereof.
Background
Lignin is a degradable natural polymer material, which is the second most abundant natural resource on earth. At present, the waste water is mainly used as a byproduct of industrial pulping and is discharged along with waste water. If the waste water is not recycled, the environment is seriously polluted, and the material resources are greatly wasted. Thus, the commercial application of lignin has been the subject of research by scientists, especially in today's ever-increasing awareness of the energy crisis. The lignin has a complex structure, can be reduced to be utilized by micromolecules, and can also be directly utilized by macromolecules. The lignin structure contains a plurality of functional groups and chemical bonds such as methoxy, phenolic hydroxyl, carboxyl, carboxymethyl and the like, so that the lignin has strong reaction activity, and the possibility is provided for chemical modification and comprehensive utilization of the lignin. The lignin has the advantages of good thermal stability, no toxicity, weather resistance and the like, and the biomass-based high polymer material prepared by using the lignin is widely applied to various fields.
The sun-blocking clothes mainly have the function of preventing direct irradiation of solar ultraviolet rays, have the same function as a sun shade, and prevent the skin from being blackened by the irradiation of the sun, which is a necessary repair course for a plurality of beauty-loving girls. Of course, sun protection is not just for girls. All people in outdoor activities should take good care of themselves and take care of the sun. Sunscreen garments first began to prevail in the united states in 2007, and then entered china. At first, most of the clothes are applied to outdoor products, and the application of common clothes is less, and then the clothes are favored by a plurality of girls.
The sun-proof clothes are made of high-quality polyester fiber materials, and the sun-proof coefficients of various fibers are as follows: polyester fiber, cotton fiber and artificial cotton and silk. Most sun-proof clothes are ultraviolet-proof clothes with sun-proof auxiliary agents added in the clothes, and a sun-proof coating is smeared on the inner layer of the clothes, just like a sun umbrella. A piece of sun-blocking clothing can isolate 95% of the uv light. However, after such sun protection clothes are soaked or washed several times, the sun protection effect is weakened until it disappears. And part of the high-grade sun-proof clothes cloth is formed by combining sun-proof ceramic fibers and polyester fibers, so that the reflection and scattering effects of the surface of the clothes on ultraviolet rays are increased, and the ultraviolet rays are prevented from penetrating through the fabric to damage the skin of a human body. The sun-proof clothes are less affected by water immersion and washing, and the sun-proof function can be kept for a long time. When the clothes with the ultraviolet-proof function are worn in hot seasons, sweat can be quickly led out from the surface of the skin to the surface of the fabric and is dried quickly, and the trouble of sweat wetting is avoided.
In view of the special molecular structure of lignin, researches show that the lignin has better ultraviolet resistance and has good prospects when being used in the field of sun protection clothes. However, the lignin has stable performance, so that the lignin is difficult to apply to textiles.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides lignin-containing composite emulsion for sun protection clothes and a preparation method and application thereof.
The invention aims to provide lignin-containing composite emulsion for sun-blocking clothes, which is used for sun-blocking clothes with fabric made of polyester fibers, and the sun-blocking clothes have good ultraviolet resistance after being finished. The lignin-containing composite emulsion for sun-blocking clothes in the invention can be prepared by the following steps: firstly, performing acetylation treatment on alkali lignin, and preparing the acetylated alkali lignin into an oil-in-water emulsion containing lignin; preparing a polyacrylate emulsion, and compounding the lignin-containing oil-in-water emulsion with the polyacrylate emulsion to obtain the lignin/polyacrylate composite emulsion, namely the lignin-containing composite emulsion for sun protection clothes.
Another object of the present invention is to provide a method for preparing a lignin-containing composite emulsion for sun-blocking clothes, comprising the steps of:
(1) acetylation treatment of alkali lignin: adding alkali lignin into a round-bottom flask containing an acetylation reagent, sealing, heating and stirring at 50-60 ℃ for 2-4 h, and quickly evaporating a solvent in a rotary evaporator after the reaction is finished to obtain a solid, namely the acetylated alkali lignin.
Preferably, in the step (1), the acetylating reagent consists of acetyl bromide and glacial acetic acid, and the volume ratio of the acetyl bromide to the glacial acetic acid is as follows: 1: 9-11.
Preferably, the ratio of alkali lignin (g) to acetylating agent (mL) in step (1) is: 1: 90-110.
(2) Preparation of oil-in-water emulsion: dissolving acetylated alkali lignin in dichloromethane to prepare an oil phase; dissolving sodium dodecyl sulfate and span 60 in water to prepare a water phase; and dropwise adding the oil phase into the water phase under stirring to prepare the lignin-containing oil-in-water emulsion.
Preferably, the ratio of acetylated alkali lignin (g) to methylene chloride (mL) in step (2) is: 1: 10-20;
preferably, the ratio of sodium dodecyl sulfonate (g), span 60(g) and water (mL) in the step (2) is: 1: 1-2: 100-200;
preferably, the volume ratio of the oil phase to the water phase in the step (2) is: 1: 9-11.
(3) Preparation of polyacrylate emulsion: weighing sodium p-toluenesulfonate, a Tween 80 emulsifier, acrylic acid, ethyl acrylate and ammonium persulfate, dissolving all the sodium p-toluenesulfonate, the Tween 80 emulsifier and 1/2 total acrylic acid, ethyl acrylate and ammonium persulfate initiator in a proper amount of deionized water, uniformly stirring, controlling the temperature to be 75-85 ℃, and stirring for 1-2 hours; then, dissolving the rest 1/2 of acrylic acid, ethyl acrylate and ammonium persulfate initiator in a proper amount of deionized water, and then dropwise adding the deionized water into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2-3 h, and after the dropwise adding is finished, keeping the temperature for 2-3 h; the emulsion is placed for one month, and the polyacrylate emulsion can be prepared without layering or precipitation.
Preferably, in the step (3), the mass-to-volume ratio of the sodium p-toluenesulfonate (g), the tween 80 emulsifier (g), the acrylic acid (mol), the ethyl acrylate (mol) and the ammonium persulfate (g) is as follows: 0.5-1: 1-2: 0.1-0.2: 0.5-1.
(4) Mixing the emulsion: and (3) mixing the oil-in-water emulsion containing the lignin prepared in the step (2) with the polyacrylate emulsion prepared in the step (3), and stirring the mixed solution on a high-speed dispersion homogenizer for 1-2 hours at the stirring temperature of 70-80 ℃ to obtain the lignin/polyacrylate composite emulsion, namely the lignin-containing composite emulsion for sun-blocking clothes.
Preferably, the volume ratio of the oil-in-water emulsion containing lignin prepared in the step (2) in the step (4) to the polyacrylate emulsion prepared in the step (3) is 1: 5-7.
Still another object of the present invention is to provide an application of the lignin-containing composite emulsion for sun-blocking clothes, the application method comprising the steps of:
the sun-blocking clothes are tightened on a stretching frame, the emulsion is diluted and then is uniformly coated on the sun-blocking clothes by a scraper, and the dry weight of the coating is 15-20 g/m2Drying at 90 ℃ for 3 minutes and baking at 140-170 ℃ for 4 minutes.
Preferably, the sun-blocking clothes are made of polyester fiber fabric.
The invention has the following remarkable advantages:
(1) the lignin has the function of absorbing ultraviolet, and the invention prepares the lignin into emulsion which contains the lignin and can absorb the ultraviolet in the sunlight, thereby having good sun-proof performance.
(2) The UPF value of the sun-blocking clothes prepared by the invention reaches above 68, and is obviously higher than that of purchased sun-blocking clothes; after 10 times of washing, the UPF value of the sun-blocking clothes prepared by the invention is not obviously reduced, which shows that the uvioresistant performance of the sun-blocking clothes is not weakened after multiple times of washing. The oil-in-water emulsion containing lignin only has weak binding force with the fabric, and the inventor of the application unexpectedly finds that the oil-in-water emulsion containing lignin is compounded with the polyacrylate emulsion, and the firm loading of the lignin on the surface of the fabric is realized by relying on the characteristic that the binding force of the polyacrylate emulsion and the fabric is strong.
(3) The lignin-containing composite emulsion for sun-blocking clothes prepared by the invention has the advantages of simple preparation method, wide raw material source and good application prospect.
Detailed Description
The examples described below illustrate the invention in detail.
Example 1
In this embodiment, a lignin-containing composite emulsion for sun-blocking clothes is prepared by the following steps:
(1) acetylation treatment of alkali lignin: adding 10g of alkali lignin into a round-bottom flask containing 1000mL of acetylation reagent, sealing, heating and stirring at 55 ℃ for 3h, and quickly evaporating the solvent to dryness in a rotary evaporator after the reaction is finished to obtain solid, namely acetylated alkali lignin; the acetylation reagent consists of 100mL of acetyl bromide and 900mL of glacial acetic acid.
(2) Preparation of oil-in-water emulsion: dissolving 1g of acetylated alkali lignin in 15mL of dichloromethane to prepare an oil phase; dissolving 1g of sodium dodecyl sulfate and 1.5g of span 60 in 150mL of water to prepare a water phase; and dropwise adding the oil phase into the water phase under stirring to prepare the lignin-containing oil-in-water emulsion.
(3) Preparation of polyacrylate emulsion: weighing 0.75g of sodium p-toluenesulfonate, 1.5g of Tween 80 emulsifier, 0.15mol of acrylic acid, 0.15mol of ethyl acrylate and 0.75g of ammonium persulfate, dissolving all the sodium p-toluenesulfonate, the Tween 80 emulsifier and 1/2 of acrylic acid, ethyl acrylate and ammonium persulfate initiator in 200mL of deionized water, uniformly stirring, controlling the temperature to be 80 ℃, and stirring for 1.5 h; then, dissolving the rest 1/2 of acrylic acid, ethyl acrylate and ammonium persulfate initiator in 200mL of deionized water, and then dropwise adding the solution into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2.5h, and after the dropwise adding is finished, keeping the temperature for 2.5 h; the emulsion is placed for one month, and the polyacrylate emulsion can be prepared without layering or precipitation.
(4) Mixing the emulsion: and (3) mixing 10mL of the lignin-containing oil-in-water emulsion prepared in the step (2) with 60mL of the polyacrylate emulsion prepared in the step (3), and stirring the mixed solution on a high-speed dispersion homogenizer for 1.5h at the stirring temperature of 75 ℃ to obtain the lignin/polyacrylate composite emulsion, namely the lignin-containing composite emulsion for sun protection clothes.
Use of a lignin-containing composite emulsion for sun protection clothing, the method of application comprising the steps of:
the sun-proof clothes are tightened on a stretching frame, the emulsion is diluted and then is evenly coated on the sun-proof clothes of the polyester fiber fabric by a scraper, and the dry weight of the coating weight is 18.4g/m2Oven-drying at 90 deg.C for 3 min, and baking at 150 deg.C for 4 min.
Example 2
In this embodiment, a lignin-containing composite emulsion for sun-blocking clothes is prepared by the following steps:
(1) acetylation treatment of alkali lignin: adding 10g of alkali lignin into a round-bottom flask containing 900mL of acetylation reagent, sealing, heating and stirring at 55 ℃ for 3h, and quickly evaporating the solvent to dryness in a rotary evaporator after the reaction is finished to obtain solid, namely acetylated alkali lignin; the acetylation reagent consists of 90mL of acetyl bromide and 810mL of glacial acetic acid.
(2) Preparation of oil-in-water emulsion: dissolving 1g of acetylated alkali lignin in 10mL of dichloromethane to prepare an oil phase; dissolving 1g of sodium dodecyl sulfate and 1g of span 60 in 100mL of water to prepare a water phase; and dropwise adding the oil phase into the water phase under stirring to prepare the lignin-containing oil-in-water emulsion.
(3) Preparation of polyacrylate emulsion: weighing 0.75g of sodium p-toluenesulfonate, 1.5g of Tween 80 emulsifier, 0.15mol of acrylic acid, 0.15mol of ethyl acrylate and 0.75g of ammonium persulfate, dissolving all the sodium p-toluenesulfonate, the Tween 80 emulsifier and 1/2 of acrylic acid, ethyl acrylate and ammonium persulfate initiator in 200mL of deionized water, uniformly stirring, controlling the temperature to be 80 ℃, and stirring for 1.5 h; then, dissolving the rest 1/2 of acrylic acid, ethyl acrylate and ammonium persulfate initiator in 200mL of deionized water, and then dropwise adding the solution into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2.5h, and after the dropwise adding is finished, keeping the temperature for 2.5 h; the emulsion is placed for one month, and the polyacrylate emulsion can be prepared without layering or precipitation.
(4) Mixing the emulsion: and (3) mixing 10mL of the lignin-containing oil-in-water emulsion prepared in the step (2) with 50mL of the polyacrylate emulsion prepared in the step (3), and stirring the mixed solution on a high-speed dispersion homogenizer for 1.5h at the stirring temperature of 75 ℃ to obtain the lignin/polyacrylate composite emulsion, namely the lignin-containing composite emulsion for sun protection clothes.
Use of a lignin-containing composite emulsion for sun protection clothing, the method of application comprising the steps of:
the sun-proof clothes are tightened on a stretching frame, the emulsion is diluted and then is evenly coated on the sun-proof clothes of the polyester fiber fabric by a scraper, and the dry weight of the coating weight is 17.5g/m2Oven-drying at 90 deg.C for 3 min, and baking at 140 deg.C for 4 min.
Example 3
In this embodiment, a lignin-containing composite emulsion for sun-blocking clothes is prepared by the following steps:
(1) acetylation treatment of alkali lignin: adding 10g of alkali lignin into a round-bottom flask containing 1100mL of acetylation reagent, sealing, heating and stirring at 55 ℃ for 3h, and quickly evaporating the solvent to dryness in a rotary evaporator after the reaction is finished to obtain solid, namely acetylated alkali lignin; the acetylation reagent consists of 100mL of acetyl bromide and 1000mL of glacial acetic acid.
(2) Preparation of oil-in-water emulsion: dissolving 1g of acetylated alkali lignin in 20mL of dichloromethane to prepare an oil phase; dissolving 1g of sodium dodecyl sulfate and 2g of span 60 in 200mL of water to prepare a water phase; and dropwise adding the oil phase into the water phase under stirring to prepare the lignin-containing oil-in-water emulsion.
(3) Preparation of polyacrylate emulsion: weighing 0.75g of sodium p-toluenesulfonate, 1.5g of Tween 80 emulsifier, 0.15mol of acrylic acid, 0.15mol of ethyl acrylate and 0.75g of ammonium persulfate, dissolving all the sodium p-toluenesulfonate, the Tween 80 emulsifier and 1/2 of acrylic acid, ethyl acrylate and ammonium persulfate initiator in 200mL of deionized water, uniformly stirring, controlling the temperature to be 80 ℃, and stirring for 1.5 h; then, dissolving the rest 1/2 of acrylic acid, ethyl acrylate and ammonium persulfate initiator in 200mL of deionized water, and then dropwise adding the solution into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2.5h, and after the dropwise adding is finished, keeping the temperature for 2.5 h; the emulsion is placed for one month, and the polyacrylate emulsion can be prepared without layering or precipitation.
(4) Mixing the emulsion: and (3) mixing 10mL of the lignin-containing oil-in-water emulsion prepared in the step (2) with 70mL of the polyacrylate emulsion prepared in the step (3), and stirring the mixed solution on a high-speed dispersion homogenizer for 1.5h at the stirring temperature of 75 ℃ to obtain the lignin/polyacrylate composite emulsion, namely the lignin-containing composite emulsion for sun protection clothes.
Use of a lignin-containing composite emulsion for sun protection clothing, the method of application comprising the steps of:
the sun-proof clothes are tightened on a stretching frame, the emulsion is diluted and then is evenly coated on the sun-proof clothes of the polyester fiber fabric by a scraper, and the dry weight of the coating weight is 16.8g/m2Oven-drying at 90 deg.C for 3 min, and baking at 150 deg.C for 4 min.
Comparative example 1
In this example, instead of preparing a lignin-containing oil-in-water emulsion, only a polyacrylate emulsion was prepared, referring to the preparation method of example 1, comprising the steps of:
preparation of polyacrylate emulsion: weighing 0.75g of sodium p-toluenesulfonate, 1.5g of Tween 80 emulsifier, 0.15mol of acrylic acid, 0.15mol of ethyl acrylate and 0.75g of ammonium persulfate, dissolving all the sodium p-toluenesulfonate, the Tween 80 emulsifier and 1/2 of acrylic acid, ethyl acrylate and ammonium persulfate initiator in 200mL of deionized water, uniformly stirring, controlling the temperature to be 80 ℃, and stirring for 1.5 h; then, dissolving the rest 1/2 of acrylic acid, ethyl acrylate and ammonium persulfate initiator in 200mL of deionized water, and then dropwise adding the solution into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2.5h, and after the dropwise adding is finished, keeping the temperature for 2.5 h; the emulsion is placed for one month, and the polyacrylate emulsion can be prepared without layering or precipitation.
Use of a polyacrylate emulsion, said use comprising the steps of:
the sun-proof clothes are tightened on a stretching frame, the emulsion is diluted and then is evenly coated on the sun-proof clothes of the polyester fiber fabric by a scraper, and the dry weight of the coating weight is 18.4g/m2Oven-drying at 90 deg.C for 3 min, and baking at 150 deg.C for 4 min.
And (3) application performance testing:
the sun-blocking clothes obtained by finishing the above specific examples 1 to 3 and comparative example 1 of the present invention and purchased sun-blocking clothes were used. According to the standard of the sunlight ultraviolet protection performance of EU textiles, RrEN13758-2001, an HB902 ultraviolet transmittance tester is adopted, the ultraviolet protection coefficient (UPF value) and the ultraviolet transmittance of the textiles are measured within the range of 250-450nm, each sample is tested for 3 times, and the average value is taken. The smaller the transmittance is, the larger the UPF value is, and the better the ultraviolet-proof effect is. UPF values of the sun-blocking clothes prepared in examples 1 to 3 and comparative example 1 were measured. The fabric to be tested is subjected to standard washing by referring to a washing method of a GB/T20944.1-2007 color fastness to washing tester, the uvioresistant performance of different washing times is tested, and the test result is shown in Table 1.
Table 1 results of evaluation of uv resistance of sun-blocking clothes obtained after finishing of examples 1 to 3 and comparative example 1
Number of washes Example 1 Example 2 Example 3 Comparative example 1 Purchased sun-proof clothes
0 68.8 68.5 68.8 21.1 63.2
10 67.3 67.4 67.5 20.3 62.4
The higher the UPF value is, the better the uvioresistant performance of the fabric is, and the better the sun protection performance of the fabric is. As can be seen from table 1: when the sun-blocking clothes are not washed, the UPF value of the sun-blocking clothes prepared by the invention reaches above 68 and is obviously higher than that of purchased sun-blocking clothes; after 10 times of washing, the UPF value of the sun-blocking clothes prepared by the invention is not obviously reduced, which shows that the uvioresistant performance of the sun-blocking clothes is not weakened after multiple times of washing.

Claims (8)

1. A preparation method of lignin-containing composite emulsion for sun-blocking clothes is characterized by comprising the following steps:
(1) acetylation treatment of alkali lignin: adding alkali lignin into a round-bottom flask containing an acetylation reagent, sealing, heating and stirring at 50-60 ℃ for 2-4 h, and quickly evaporating a solvent in a rotary evaporator after the reaction is finished to obtain a solid, namely acetylated alkali lignin;
(2) preparation of oil-in-water emulsion: dissolving acetylated alkali lignin in dichloromethane to prepare an oil phase; dissolving sodium dodecyl sulfate and span 60 in water to prepare a water phase; dripping the oil phase into the water phase under stirring to prepare an oil-in-water emulsion containing lignin;
(3) preparation of polyacrylate emulsion: weighing sodium p-toluenesulfonate, a Tween 80 emulsifier, acrylic acid, ethyl acrylate and ammonium persulfate, dissolving all the sodium p-toluenesulfonate, the Tween 80 emulsifier and 1/2 total acrylic acid, ethyl acrylate and ammonium persulfate initiator in a proper amount of deionized water, uniformly stirring, controlling the temperature to be 75-85 ℃, and stirring for 1-2 hours; then, dissolving the rest 1/2 of acrylic acid, ethyl acrylate and ammonium persulfate initiator in a proper amount of deionized water, and then dropwise adding the deionized water into the mixed solution which is just stirred, wherein the dropwise adding time is controlled to be 2-3 h, and after the dropwise adding is finished, keeping the temperature for 2-3 h; the emulsion is placed for one month, and the polyacrylate emulsion can be prepared without layering or precipitation;
(4) mixing the emulsion: and (3) mixing the oil-in-water emulsion containing the lignin prepared in the step (2) with the polyacrylate emulsion prepared in the step (3), and stirring the mixed solution on a high-speed dispersion homogenizer for 1-2 hours at the stirring temperature of 70-80 ℃ to obtain the lignin/polyacrylate composite emulsion, namely the lignin-containing composite emulsion for sun-blocking clothes.
2. The method for preparing lignin-containing composite emulsion for sun protection clothes according to claim 1, wherein the acetylation reagent in step (1) consists of acetyl bromide and glacial acetic acid, and the volume ratio of acetyl bromide to glacial acetic acid is: 1: 9-11; the ratio of alkali lignin to acetylating agent is: 1g to (90-110) mL.
3. The method for preparing lignin-containing composite emulsion for sun blocking clothes according to claim 1, wherein the ratio of acetylated alkali lignin to dichloromethane in the step (2) is: 1g to (10-20) mL; the ratio of sodium dodecyl sulfate, span 60 and water is: 1g, (1-2) g, (100-200) mL; the volume ratio of the oil phase to the water phase is as follows: 1: 9-11.
4. The method for preparing the lignin-containing composite emulsion for sun blocking clothes according to claim 1, wherein the mass volume ratio of the sodium p-toluenesulfonate, the tween 80 emulsifier, the acrylic acid, the ethyl acrylate and the ammonium persulfate in the step (3) is as follows: (0.5-1) g, (1-2) g, (0.1-0.2) mol and (0.5-1) g.
5. The method for preparing the lignin-containing composite emulsion for sun-blocking clothes according to claim 1, wherein the volume ratio of the lignin-containing oil-in-water emulsion prepared in the step (2) in the step (4) to the polyacrylate emulsion prepared in the step (3) is 1: 5-7.
6. A lignin-containing composite emulsion for sun-blocking clothes, which is characterized by being prepared by the method for preparing the lignin-containing composite emulsion for sun-blocking clothes according to any one of claims 1 to 5.
7. Use of the lignin-containing composite emulsion according to claim 6 for sun protection clothing, said method of application comprising the steps of: the sun-blocking clothes are tightened on a stretching frame, the emulsion is diluted and then is uniformly coated on the sun-blocking clothes by a scraper, and the dry weight of the coating is 15-20 g/m2Drying at 90 ℃ for 3 minutes and baking at 140-170 ℃ for 4 minutes.
8. The use of the lignin-containing composite emulsion for sun protection clothing according to claim 7, wherein the sun protection clothing material is a polyester fiber fabric.
CN202111346477.1A 2021-11-15 2021-11-15 Lignin-containing composite emulsion for sun-blocking clothes and preparation method and application thereof Active CN113930967B (en)

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US20180344590A1 (en) * 2015-11-30 2018-12-06 Centre National De La Recherche Scientifique Control of evaporation of emulsions stabilized with lignin
CN110607690A (en) * 2019-08-28 2019-12-24 武汉纺织大学 Polyacrylate-polyurethane composite emulsion with ultraviolet resistance function and preparation method and application thereof
US10682304B1 (en) * 2019-11-26 2020-06-16 King Saud University Lignin-zinc oxide nanohybrid emulsion for UV protection
CN113355914A (en) * 2021-06-29 2021-09-07 武汉纺织大学 Wool fabric shrink-proof finishing liquid containing lignin, and preparation method and application thereof
CN113529210A (en) * 2021-06-28 2021-10-22 武汉纺织大学 Lignin fiber for textile material and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180344590A1 (en) * 2015-11-30 2018-12-06 Centre National De La Recherche Scientifique Control of evaporation of emulsions stabilized with lignin
CN110607690A (en) * 2019-08-28 2019-12-24 武汉纺织大学 Polyacrylate-polyurethane composite emulsion with ultraviolet resistance function and preparation method and application thereof
US10682304B1 (en) * 2019-11-26 2020-06-16 King Saud University Lignin-zinc oxide nanohybrid emulsion for UV protection
CN113529210A (en) * 2021-06-28 2021-10-22 武汉纺织大学 Lignin fiber for textile material and preparation method thereof
CN113355914A (en) * 2021-06-29 2021-09-07 武汉纺织大学 Wool fabric shrink-proof finishing liquid containing lignin, and preparation method and application thereof

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