CN115045110A - Preparation method of antibacterial environment-friendly shopping bag based on waste textiles - Google Patents
Preparation method of antibacterial environment-friendly shopping bag based on waste textiles Download PDFInfo
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- D—TEXTILES; PAPER
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating 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 nitrogen
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
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- C07C209/10—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms with formation of amino groups bound to carbon atoms of six-membered aromatic rings or from amines having nitrogen atoms bound to carbon atoms of six-membered aromatic rings
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- C07C209/32—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups
- C07C209/36—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst
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- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/02—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols
- C07C319/12—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols by reactions not involving the formation of mercapto groups
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- C07C323/51—Thiols, sulfides, hydropolysulfides or polysulfides substituted by halogen, oxygen or nitrogen atoms, or by sulfur atoms not being part of thio groups containing thio groups and carboxyl groups bound to the same carbon skeleton having the sulfur atoms of the thio groups bound to acyclic carbon atoms of the carbon skeleton
- C07C323/60—Thiols, sulfides, hydropolysulfides or polysulfides substituted by halogen, oxygen or nitrogen atoms, or by sulfur atoms not being part of thio groups containing thio groups and carboxyl groups bound to the same carbon skeleton having the sulfur atoms of the thio groups bound to acyclic carbon atoms of the carbon skeleton with the carbon atom of at least one of the carboxyl groups bound to nitrogen atoms
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Abstract
The invention relates to the field of recycling of waste textiles, solves the problems that the existing shopping bags made of regenerated textiles have poor antibacterial and bacteriostatic properties and are easy to breed bacteria, and particularly relates to a preparation method of bacteriostatic environment-friendly shopping bags based on waste textiles; according to the preparation method, firstly, the antibacterial agent is prepared, a large number of quaternary ammonium groups contained in the molecular structure of the antibacterial agent are positively charged and can be adsorbed to bacterial cell walls with negative charges, so that intracellular substances are leaked, and finally cells die, and therefore, the antibacterial, bacteriostatic and bactericidal effects are achieved.
Description
Technical Field
The invention relates to the field of recycling of waste textiles, in particular to a preparation method of a bacteriostatic environment-friendly shopping bag based on the waste textiles.
Background
Shopping bags, as the name implies, are used when packing and carrying articles during shopping, such as supermarket shopping bags, online shopping bags and the like. Wherein, the shopping bags are divided into plastic shopping bags, paper shopping bags and non-woven fabric shopping bags according to different materials.
As is well known, plastic bags are not easy to degrade and are easy to bring great pressure to the subsequent treatment of environmental pollution. The strength of the paper packaging bag is far from insufficient and the paper packaging bag is not durable; and the range of use is limited and some liquid or damp objects cannot be packed. Therefore, the non-woven fabric shopping bag is widely used due to the advantages of environmental protection, durability and the like.
In recent years, people's living standard has increased, and consumers have been increasingly demanding from the basic requirements of textiles to the appearance. The former styles are less, and now, personalization is pursued more and more, which means that consumers can buy more clothes, bed sheets, quilt covers and the like under the drive of the fashion trend, the updating speed is faster and faster, and a large amount of waste textiles are generated.
The existing waste textile recovery treatment generally adopts incineration and burying, which causes environmental pollution and resource waste, so that the non-woven fabric shopping bag prepared by recycling the waste textile is an excellent method with environmental protection and energy saving, but the existing regenerated textile shopping bag has a large amount of bacteria after long-time use and recovery, which causes poor antibacterial and bacteriostatic properties of the shopping bag and is easy to breed bacteria to cause harm to human bodies.
How to improve the problem that the existing regenerated textile shopping bag is poor in antibacterial and bacteriostatic performance and easy to breed bacteria is the key of the invention, so that a preparation method of an antibacterial environment-friendly shopping bag based on waste textiles is urgently needed to solve the problems.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a preparation method of a bacteriostatic environment-friendly shopping bag based on waste textiles, which comprises the following steps: through washing old and useless fabrics, the drying, obtain the preliminary treatment fabrics, smash the preliminary treatment fabrics, later open, the decoloration, obtain old and useless fibre, wash old and useless fibre, the drying, later weaving shaping, obtain regeneration weaving cloth, add the antiseptic into deionized water, prepare into antibacterial liquid, impregnate regeneration weaving cloth in antibacterial liquid, later take out and dry, obtain antibiotic regeneration cloth, tailor antibiotic regeneration cloth, the stamp, it is sewed up to sew up, obtain this antibacterial environmental protection shopping bag, the problem of current regeneration fabrics shopping bag antibiotic antibacterial property not good has been solved, easily breed the bacterium.
The purpose of the invention can be realized by the following technical scheme:
the preparation method of the bacteriostatic environment-friendly shopping bag based on the waste textiles comprises the following steps:
the method comprises the following steps: washing and drying the waste textile to obtain a pretreated textile;
step two: crushing the pretreated textile, and then opening and decoloring to obtain waste fibers;
step three: washing and drying the waste fibers, and then spinning and forming to obtain regenerated textile cloth;
step four: adding the antibacterial agent into deionized water to prepare antibacterial liquid with the concentration of 50-100 g/L;
step five: soaking the regenerated textile cloth in an antibacterial solution for 1-2h, taking out and drying, soaking in the antibacterial solution for 1-2h again, and repeatedly soaking for 2-3 times to obtain the antibacterial regenerated cloth;
step six: and cutting, printing and sewing the antibacterial regenerated cloth to obtain the antibacterial environment-friendly shopping bag.
As a further scheme of the invention: the antibacterial agent is prepared by the following steps:
a1: adding p-chloronitrobenzene, p-nitroaniline, anhydrous potassium carbonate, toluene and N, N-dimethylformamide into a three-neck flask provided with a stirrer, a thermometer and a gas-guide tube, introducing nitrogen for protection, stirring and reacting for 5-6h under the conditions that the temperature is 130-;
the reaction principle is as follows:
a2: adding the intermediate 1, 10% palladium carbon and acetone into a four-neck flask provided with a stirrer, a thermometer, a gas-guide tube, a constant-pressure dropping funnel and a reflux condenser tube, introducing nitrogen for protection, stirring for 30-40min under the conditions that the temperature is 20-25 ℃ and the stirring speed is 450-550r/min, then heating to reflux, controlling the heating speed to be 2-3 ℃/min, then dropwise adding a hydrazine hydrate solution while stirring, controlling the dropwise adding speed to be 1-2 drops/s, continuously stirring for reacting for 6-8h after the dropwise adding is finished, filtering a reaction product while the reaction is hot after the reaction is finished, adding a filtrate into ice water, separating out a precipitate, carrying out vacuum filtration, washing a filter cake with distilled water for 2-3 times, then placing in a vacuum drying box, drying for 4-6h under the condition that the temperature is 60-70 ℃, obtaining an intermediate 2;
the reaction principle is as follows:
a3: adding the intermediate 2, mercaptopropionic acid, p-toluenesulfonic acid and toluene into a four-neck flask provided with a stirrer, a thermometer, a gas-guide tube, a constant-pressure dropping funnel and a reflux condenser tube, introducing nitrogen for protection, heating to reflux while stirring under the condition that the stirring speed is 450-550r/min, controlling the heating rate to be 2-3 ℃/min, then continuing stirring for reaction for 6-8h, dropwise adding a sodium hydroxide solution while stirring, controlling the dropwise adding rate to be 1-2 drops/s until the pH value is 7, washing a reaction product with distilled water for 2-3 times after the reaction is finished, standing for layering, drying an organic phase with anhydrous sodium sulfate, then carrying out vacuum filtration, and carrying out rotary evaporation on a filtrate to remove a solvent to obtain an intermediate 3;
the reaction principle is as follows:
a4: adding methyl acrylate, N-dimethylethanolamine, hydroquinone and tetrabutyl titanate into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, heating to 85-90 ℃ while stirring under the condition that the stirring speed is 450-550r/min, controlling the heating speed to 2-3 ℃/min, then continuously stirring for reacting for 2-3h, heating to 110-120 ℃ while stirring, continuously stirring for reacting for 6-8h, and rotationally evaporating a reaction product to remove a solvent after the reaction is finished to obtain an intermediate 4;
the reaction principle is as follows:
a5: adding the intermediate 4, monobromododecane and anhydrous acetonitrile into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 20-30h under the conditions that the temperature is 45-50 ℃ and the stirring rate is 450-550r/min, cooling a reaction product to room temperature after the reaction is finished, then adding the reaction product into anhydrous ether, separating out a precipitate, carrying out vacuum filtration, washing a filter cake with the anhydrous ether for 2-3 times, then placing the filter cake into a vacuum drying box, and drying for 4-6h under the condition that the temperature is 30-35 ℃ to obtain an intermediate 5;
the reaction principle is as follows:
a6: adding the intermediate 3, the intermediate 5 and toluene into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 8-10h under the conditions that the temperature is 55-60 ℃ and the stirring rate is 450-550r/min, cooling a reaction product to room temperature after the reaction is finished, then adding the reaction product into anhydrous ether, separating out a precipitate, carrying out vacuum filtration, washing a filter cake for 2-3 times by using the anhydrous ether, then placing the filter cake into a vacuum drying box, and drying for 10-15h under the condition that the temperature is 50-55 ℃ to obtain the antibacterial agent.
The reaction principle is as follows:
as a further scheme of the invention: the dosage ratio of the p-chloronitrobenzene, the p-nitroaniline, the anhydrous potassium carbonate, the toluene and the N, N-dimethylformamide in the step A1 is 0.21-0.23 mol: 0.1 mol: 0.15-0.2 mol: 60-70 mL: 200 and 250 mL.
As a further scheme of the invention: the dosage ratio of the intermediate 1, 10% palladium carbon, acetone and hydrazine hydrate solution in the step A2 is 0.1 mol: 1.8-3.6 g: 100-120 mL: 40-50mL, wherein the mass fraction of the hydrazine hydrate solution is 60-64%.
As a further scheme of the invention: the user quantity ratio of the intermediate 2, the mercaptopropionic acid, the p-toluenesulfonic acid and the toluene in the step A3 is 0.1 mol: 0.33-0.35 mol: 0.8-1.5 g: 80-100mL, wherein the mass fraction of the sodium hydroxide solution is 10-15%.
As a further scheme of the invention: the dosage ratio of the methyl acrylate, the N, N-dimethylethanolamine, the hydroquinone and the tetrabutyl titanate in the step A4 is 0.1 mol: 0.1 mol: 0.3-0.5 g: 5.2-6.8 g.
As a further scheme of the invention: the intermediate 4, monobromododecane and anhydrous acetonitrile in the step A5 are used in a ratio of 0.11-0.13 mol: 0.1 mol: 40-50 mL.
As a further scheme of the invention: the dosage ratio of the intermediate 3, the intermediate 5 and the toluene in the step A6 is 0.1 mol: 0.33-0.36 mol: 50-60 mL.
The invention has the beneficial effects that:
the preparation method of the bacteriostatic environment-friendly shopping bag based on the waste textiles comprises the steps of washing and drying the waste textiles to obtain pretreated textiles, crushing the pretreated textiles, then opening and decoloring to obtain waste fibers, washing and drying the waste fibers, then carrying out spinning forming to obtain regenerated textile cloth, adding an antibacterial agent into deionized water to prepare an antibacterial solution, dipping the regenerated textile cloth into the antibacterial solution, taking out and airing to obtain antibacterial regenerated cloth, cutting, printing and sewing the antibacterial regenerated cloth to obtain the bacteriostatic environment-friendly shopping bag; firstly, chlorine atoms on p-chloronitrobenzene and amino groups on p-nitroaniline are subjected to nucleophilic substitution reaction, a large amount of nitro groups are introduced to obtain an intermediate 1, then the intermediate 1 is subjected to reduction of the nitro groups into amino groups under the action of hydrazine hydrate to obtain an intermediate 2, then the amino groups on the intermediate 2 and carboxyl groups on mercaptopropionic acid are subjected to amidation reaction, a large amount of mercapto groups are introduced to obtain an intermediate 3, then ester exchange reaction is carried out between ester groups on methyl acrylate and hydroxyl groups on N, N-dimethylethanolamine to generate new ester groups, tertiary amine groups are introduced to obtain an intermediate 4, then the tertiary amine groups on the intermediate 4 and bromine atoms on monobromododecane are subjected to nucleophilic substitution reaction to form quaternary ammonium groups to obtain an intermediate 5, and then the alkenyl groups on the intermediate 5 and the mercapto groups on the intermediate 3 are subjected to mercaptan-olefin click reaction, introduce a large amount of quaternary ammonium groups, obtain the antibacterial agent, a large amount of quaternary ammonium groups that this antibacterial agent molecular structure contains are positive, can adsorb on the bacterium cell wall of negative charge, lead to the intracellular material to leak, finally lead to the cell death, thereby play antibiotic, antibacterial and bactericidal effect, with this antibacterial agent attached to on the antibacterial environmental protection shopping bag, can restrain bacterial growing on the antibacterial environmental protection shopping bag, thereby give the good antibacterial effect of antibacterial environmental protection shopping bag, thereby promote the sanitary safety nature of antibacterial environmental protection shopping bag.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
this embodiment is a method for preparing an antimicrobial agent, comprising the steps of:
a1: adding 0.21mol of p-chloronitrobenzene, 0.1mol of p-nitroaniline, 0.15mol of anhydrous potassium carbonate, 60mL of toluene and 200mLN, N-dimethylformamide into a three-neck flask provided with a stirrer, a thermometer and an air duct, introducing nitrogen for protection, stirring and reacting for 5h under the conditions that the temperature is 130 ℃ and the stirring speed is 450r/min, then continuously stirring and reacting for 5h under the condition that the temperature is increased to 150 ℃, then pouring into distilled water under the condition that the temperature is reduced to 100 ℃, precipitating and filtering out precipitates, then carrying out vacuum filtration, washing a filter cake for 2 times by using distilled water and anhydrous ethanol in sequence, then placing the filter cake into a vacuum drying oven, and drying for 4h under the condition that the temperature is 60 ℃ to obtain an intermediate 1;
a2: adding 0.1mol of intermediate 1, 1.8g of 10% palladium carbon and 100mL of acetone into a four-neck flask provided with a stirrer, a thermometer, a gas-guide tube, a constant-pressure dropping funnel and a reflux condenser, introducing nitrogen for protection, stirring for 30min under the conditions that the temperature is 20 ℃ and the stirring speed is 450r/min, then heating to reflux, controlling the heating rate to be 2 ℃/min, then dropwise adding 40mL of 60% hydrazine hydrate solution while stirring, controlling the dropwise adding rate to be 1 drop/s, continuing stirring for reaction for 6h after the dropwise adding is finished, filtering a reaction product after the reaction is finished, adding filtrate into ice water, precipitating and performing vacuum filtration, washing a filter cake with distilled water for 2 times, then placing in a vacuum drying box, and drying for 4h under the condition that the temperature is 60 ℃ to obtain an intermediate 2;
a3: adding 0.1mol of intermediate 2, 0.33mol of mercaptopropionic acid, 0.8g of p-toluenesulfonic acid and 80mL of toluene into a four-neck flask provided with a stirrer, a thermometer, a gas-guide tube, a constant-pressure dropping funnel and a reflux condenser tube, introducing nitrogen for protection, heating to reflux while stirring under the condition of a stirring rate of 450r/min, controlling the heating rate to be 2 ℃/min, continuing to stir for 6 hours, then dropwise adding a sodium hydroxide solution with the mass fraction of 10% while stirring, controlling the dropwise adding rate to be 1 drop/s until the pH is 7, washing a reaction product with distilled water for 2 times after the reaction is finished, standing for layering, drying an organic phase with anhydrous sodium sulfate, then carrying out vacuum filtration, and carrying out rotary evaporation on a filtrate to remove a solvent to obtain an intermediate 3;
a4: adding 0.1mol of methyl acrylate, 0.1mol of N, N-dimethylethanolamine, 0.3g of hydroquinone and 5.2g of tetrabutyl titanate into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, heating to 85 ℃ while stirring at a stirring speed of 450r/min, controlling the heating rate to be 2 ℃/min, continuing to stir for 2h, heating to 110 ℃ while stirring for 6h, and rotationally evaporating a reaction product to remove a solvent after the reaction is finished to obtain an intermediate 4;
a5: adding 0.11mol of intermediate 4, 0.1mol of monobromododecane and 40mL of anhydrous acetonitrile into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 20h at the temperature of 45 ℃ and the stirring rate of 450r/min, cooling a reaction product to room temperature after the reaction is finished, adding the reaction product into anhydrous ether, separating out a precipitate, carrying out vacuum filtration, washing a filter cake for 2 times by using the anhydrous ether, then placing the filter cake into a vacuum drying box, and drying for 4h at the temperature of 30 ℃ to obtain an intermediate 5;
a6: adding 0.1mol of the intermediate 3, 0.33mol of the intermediate 5 and 50mL of toluene into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 8h under the conditions that the temperature is 55 ℃ and the stirring rate is 450r/min, cooling a reaction product to room temperature after the reaction is finished, adding the reaction product into anhydrous ether, separating out a precipitate, carrying out vacuum filtration, washing a filter cake with the anhydrous ether for 2 times, then placing the filter cake into a vacuum drying box, and drying for 10h under the condition that the temperature is 50 ℃ to obtain the antibacterial agent.
Example 2:
this embodiment is a method for preparing an antimicrobial agent, comprising the steps of:
a1: adding 0.22mol of p-chloronitrobenzene, 0.1mol of p-nitroaniline, 0.18mol of anhydrous potassium carbonate, 65mL of toluene and 225mLN, N-dimethylformamide into a three-neck flask provided with a stirrer, a thermometer and an air duct, introducing nitrogen for protection, stirring and reacting for 5.5h under the conditions that the temperature is 132 ℃ and the stirring speed is 500r/min, then continuously stirring and reacting for 5.5h under the condition that the temperature is increased to 152 ℃, then pouring into distilled water under the condition that the temperature is reduced to 105 ℃, precipitating and precipitating, then carrying out vacuum filtration, washing a filter cake for 2 times by using distilled water and anhydrous ethanol in sequence, then placing the filter cake into a vacuum drying oven, and drying for 5h under the condition that the temperature is 65 ℃ to obtain an intermediate 1;
a2: adding 0.1mol of intermediate 1, 2.7g of 10% palladium carbon and 110mL of acetone into a four-neck flask provided with a stirrer, a thermometer, a gas guide tube, a constant-pressure dropping funnel and a reflux condenser, introducing nitrogen for protection, stirring for 35min under the conditions that the temperature is 22 ℃ and the stirring speed is 500r/min, then heating to reflux, controlling the heating speed to be 2 ℃/min, then dropwise adding 45mL of 62% hydrazine hydrate solution while stirring, controlling the dropwise adding speed to be 1 drop/s, continuing stirring for reaction for 7h after the dropwise adding is finished, filtering a reaction product after the reaction is finished, adding filtrate into ice water, precipitating and performing vacuum filtration, washing a filter cake with distilled water for 2 times, then placing in a vacuum drying box, and drying for 5h under the condition that the temperature is 65 ℃ to obtain an intermediate 2;
a3: adding 0.1mol of intermediate 2, 0.34mol of mercaptopropionic acid, 1.2g of p-toluenesulfonic acid and 90mL of toluene into a four-neck flask provided with a stirrer, a thermometer, a gas-guide tube, a constant-pressure dropping funnel and a reflux condenser tube, introducing nitrogen for protection, heating to reflux while stirring under the condition of a stirring speed of 500r/min, controlling the heating rate to be 2 ℃/min, continuing to stir for reaction for 7h, then dropwise adding a sodium hydroxide solution with the mass fraction of 12% while stirring, controlling the dropwise adding rate to be 1 drop/s until the pH is 7, washing a reaction product with distilled water for 2 times after the reaction is finished, standing for layering, drying an organic phase with anhydrous sodium sulfate, then carrying out vacuum filtration, and carrying out rotary evaporation on a filtrate to remove a solvent to obtain an intermediate 3;
a4: adding 0.1mol of methyl acrylate, 0.1mol of N, N-dimethylethanolamine, 0.4g of hydroquinone and 6.0g of tetrabutyl titanate into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, heating to 87 ℃ while stirring at the stirring rate of 500r/min, controlling the heating rate to be 2 ℃/min, continuously stirring for reacting for 2 hours, heating to 115 ℃ while stirring for continuously reacting for 7 hours, and rotationally evaporating a reaction product to remove a solvent after the reaction is finished to obtain an intermediate 4;
a5: adding 0.12mol of the intermediate 4, 0.1mol of monobromododecane and 45mL of anhydrous acetonitrile into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 25h at 48 ℃ and a stirring speed of 500r/min, cooling a reaction product to room temperature after the reaction is finished, adding the reaction product into anhydrous ether, separating out a precipitate, carrying out vacuum filtration, washing a filter cake for 2 times by using the anhydrous ether, then placing the filter cake into a vacuum drying box, and drying for 5h at 32 ℃ to obtain an intermediate 5;
a6: adding 0.1mol of the intermediate 3, 0.34mol of the intermediate 5 and 55mL of toluene into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 9h under the conditions that the temperature is 58 ℃ and the stirring rate is 500r/min, cooling a reaction product to room temperature after the reaction is finished, adding the reaction product into anhydrous ether, separating out a precipitate, carrying out vacuum filtration, washing a filter cake with the anhydrous ether for 2 times, then placing the filter cake into a vacuum drying box, and drying for 12h under the condition that the temperature is 52 ℃ to obtain the antibacterial agent.
Example 3:
this embodiment is a method for preparing an antimicrobial agent, comprising the steps of:
a1: adding 0.23mol of p-chloronitrobenzene, 0.1mol of p-nitroaniline, 0.2mol of anhydrous potassium carbonate, 70mL of toluene and 250mLN, N-dimethylformamide into a three-neck flask provided with a stirrer, a thermometer and an air guide tube, introducing nitrogen for protection, stirring and reacting for 6h under the conditions that the temperature is 135 ℃ and the stirring speed is 550r/min, then continuously stirring and reacting for 6h under the condition that the temperature is raised to 155 ℃, then pouring into distilled water under the condition that the temperature is reduced to 110 ℃, precipitating, then carrying out vacuum filtration, washing a filter cake for 3 times by using distilled water and anhydrous ethanol in sequence, then placing the filter cake into a vacuum drying oven, and drying for 6h under the condition that the temperature is 70 ℃ to obtain an intermediate 1;
a2: adding 0.1mol of intermediate 1, 3.6g of 10% palladium carbon and 120mL of acetone into a four-neck flask provided with a stirrer, a thermometer, a gas guide tube, a constant-pressure dropping funnel and a reflux condenser, introducing nitrogen for protection, stirring for 40min at the temperature of 25 ℃ and the stirring speed of 550r/min, then heating to reflux, controlling the heating rate to be 3 ℃/min, then dropwise adding 50mL of hydrazine hydrate solution with the mass fraction of 64% while stirring, controlling the dropwise adding rate to be 2 drops/s, continuing stirring for reaction for 8h after the dropwise adding is finished, filtering a reaction product after the reaction is finished, adding filtrate into ice water, separating out a precipitate, carrying out vacuum filtration, washing a filter cake with distilled water for 3 times, then placing in a vacuum drying box, and drying for 6h at the temperature of 70 ℃ to obtain an intermediate 2;
a3: adding 0.1mol of intermediate 2, 0.35mol of mercaptopropionic acid, 1.5g of p-toluenesulfonic acid and 100mL of toluene into a four-neck flask provided with a stirrer, a thermometer, a gas-guide tube, a constant-pressure dropping funnel and a reflux condenser tube, introducing nitrogen for protection, heating to reflux while stirring under the condition of a stirring rate of 550r/min, controlling the heating rate to be 3 ℃/min, continuing to stir for 8 hours, then dropwise adding a sodium hydroxide solution with the mass fraction of 15% while stirring, controlling the dropwise adding rate to be 2 drops/s until the pH is 7, washing a reaction product with distilled water for 3 times after the reaction is finished, standing for layering, drying an organic phase with anhydrous sodium sulfate, then carrying out vacuum filtration, and carrying out rotary evaporation on a filtrate to remove a solvent to obtain an intermediate 3;
a4: adding 0.1mol of methyl acrylate, 0.1mol of N, N-dimethylethanolamine, 0.5g of hydroquinone and 6.8g of tetrabutyl titanate into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, heating to 90 ℃ while stirring at the stirring rate of 550r/min, controlling the heating rate to be 3 ℃/min, continuing to stir for reaction for 3h, heating to 120 ℃ while stirring for reaction for 8h, and rotationally evaporating a reaction product to remove a solvent after the reaction is finished to obtain an intermediate 4;
a5: adding 0.13mol of intermediate 4, 0.1mol of monobromododecane and 50mL of anhydrous acetonitrile into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 30h at the temperature of 50 ℃ and the stirring speed of 550r/min, cooling a reaction product to room temperature after the reaction is finished, adding the reaction product into anhydrous ether, separating out a precipitate, carrying out vacuum filtration, washing a filter cake with the anhydrous ether for 3 times, then placing the filter cake into a vacuum drying oven, and drying for 6h at the temperature of 35 ℃ to obtain an intermediate 5;
a6: adding 0.1mol of the intermediate 3, 0.36mol of the intermediate 5 and 60mL of toluene into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 10h under the conditions that the temperature is 60 ℃ and the stirring speed is 550r/min, cooling a reaction product to room temperature after the reaction is finished, adding the reaction product into anhydrous ether, separating out a precipitate, carrying out vacuum filtration, washing a filter cake with the anhydrous ether for 3 times, then placing the filter cake into a vacuum drying box, and drying the filter cake for 15h under the condition that the temperature is 55 ℃ to obtain the antibacterial agent.
Example 4:
the embodiment is a preparation method of a bacteriostatic environment-friendly shopping bag based on waste textiles, which comprises the following steps:
the method comprises the following steps: washing and drying the waste textile to obtain a pretreated textile; the waste textile is waste cotton clothes;
step two: crushing the pretreated textile, and then opening and decoloring to obtain waste fibers;
step three: washing and drying the waste fibers, and then spinning and forming to obtain regenerated textile cloth;
step four: adding the antibacterial agent from example 1 into deionized water to prepare an antibacterial solution with the concentration of 50 g/L;
step five: soaking the regenerated textile cloth in an antibacterial solution for 1h, taking out and drying, soaking in the antibacterial solution for 1h again, and repeating the soaking for 2 times to obtain the antibacterial regenerated cloth;
step six: and cutting, printing and sewing the antibacterial regenerated cloth to obtain the antibacterial environment-friendly shopping bag.
Example 5:
the embodiment is a preparation method of a bacteriostatic environment-friendly shopping bag based on waste textiles, which comprises the following steps:
the method comprises the following steps: washing and drying the waste textile to obtain a pretreated textile; the waste textile is a waste cotton bed sheet;
step two: crushing the pretreated textile, and then opening and decoloring to obtain waste fibers;
step three: washing and drying the waste fibers, and then spinning and forming to obtain regenerated textile cloth;
step four: adding the antibacterial agent from example 2 into deionized water to prepare an antibacterial solution with the concentration of 75 g/L;
step five: soaking the regenerated textile cloth in an antibacterial solution for 1.5h, taking out and drying, soaking in the antibacterial solution for 1.5h again, and repeating the soaking for 2 times to obtain the antibacterial regenerated cloth;
step six: and cutting, printing and sewing the antibacterial regenerated cloth to obtain the antibacterial environment-friendly shopping bag.
Example 6:
the embodiment is a preparation method of a bacteriostatic environment-friendly shopping bag based on waste textiles, which comprises the following steps:
the method comprises the following steps: washing and drying the waste textile to obtain a pretreated textile; the waste textile is a waste cotton quilt cover;
step two: crushing the pretreated textile, and then opening and decoloring to obtain waste fibers;
step three: washing and drying the waste fibers, and then spinning and forming to obtain regenerated textile cloth;
step four: adding the antibacterial agent from example 3 into deionized water to prepare an antibacterial solution with the concentration of 100 g/L;
step five: soaking the regenerated textile fabric in the antibacterial solution for 2 hours, then taking out and airing, soaking in the antibacterial solution for 2 hours again, and repeatedly soaking for 3 times to obtain the antibacterial regenerated fabric;
step six: and cutting, printing and sewing the antibacterial regenerated cloth to obtain the antibacterial environment-friendly shopping bag.
Comparative example 1:
the difference between the comparative example 1 and the example 6 is that the comparative example is a preparation method of the bacteriostatic environment-friendly shopping bag based on waste textiles, and the preparation method comprises the following steps:
the method comprises the following steps: washing and drying the waste textiles to obtain pretreated textiles;
step two: crushing the pretreated textile, and then opening and decoloring to obtain waste fibers;
step three: washing and drying the waste fibers, and then spinning and forming to obtain regenerated textile cloth;
step four: and cutting, printing and sewing the regenerated textile fabric to obtain the antibacterial environment-friendly shopping bag.
Comparative example 2:
the difference between the comparative example 2 and the example 6 is that the comparative example is a preparation method of the bacteriostatic environment-friendly shopping bag based on waste textiles, and the preparation method comprises the following steps:
the method comprises the following steps: washing and drying the waste textile to obtain a pretreated textile;
step two: crushing the pretreated textile, and then opening and decoloring to obtain waste fibers;
step three: washing and drying the waste fibers, and then spinning and forming to obtain regenerated textile cloth;
step four: sterilizing the regenerated textile cloth for 1-2h by ultraviolet rays to obtain antibacterial regenerated cloth;
step six: and cutting, printing and sewing the antibacterial regenerated cloth to obtain the antibacterial environment-friendly shopping bag.
Comparative example 3:
the difference between the comparative example 3 and the example 6 is that the comparative example is a preparation method of the bacteriostatic environment-friendly shopping bag based on waste textiles, and the preparation method comprises the following steps:
the method comprises the following steps: washing and drying the waste textile to obtain a pretreated textile;
step two: crushing the pretreated textile, and then opening and decoloring to obtain waste fibers;
step three: washing and drying the waste fibers, and then spinning and forming to obtain regenerated textile cloth;
step four: adding the intermediate 5 from example 3 into deionized water to prepare an antibacterial solution with the concentration of 100 g/L;
step five: soaking the regenerated textile fabric in the antibacterial solution for 2 hours, then taking out and airing, soaking in the antibacterial solution for 2 hours again, and repeatedly soaking for 3 times to obtain the antibacterial regenerated fabric;
step six: and cutting, printing and sewing the antibacterial regenerated cloth to obtain the antibacterial environment-friendly shopping bag.
The antibacterial performance of the bacteriostatic environment-friendly shopping bags in examples 4-6 and comparative examples 1-3 is detected according to an agar plate diffusion method in GB/T20944.1-2007 ' evaluation of textile antibacterial performance ' part I ', and the antibacterial rates of escherichia coli and staphylococcus aureus are calculated, and the results are shown in the following table:
| sample (I) | Antibacterial rate of Escherichia coli | Staphylococcus aureus bacteriostasis rate | Bacteriostasis rate of candida albicans |
| Example 4 | 98.0％ | 97.6％ | 98.3％ |
| Example 5 | 98.8％ | 98.3％ | 99.1％ |
| Example 6 | 99.8％ | 99.4％ | 99.9％ |
| Comparative example 1 | 45.8％ | 40.6％ | 47.2％ |
| Comparative example 2 | 75.4％ | 73.3％ | 77.8％ |
| Comparative example 3 | 85.6％ | 82.7％ | 87.5％ |
Referring to the data in the table, it can be seen that the antibacterial rate of the antibacterial environment-friendly shopping bag can be improved by adding the intermediate 5, the antibacterial agent and the ultraviolet disinfection treatment, and the antibacterial effect of the antibacterial agent is the best, according to the comparison between the example 6 and the comparative examples 1-3.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The preparation method of the bacteriostatic environment-friendly shopping bag based on the waste textiles is characterized by comprising the following steps of:
the method comprises the following steps: washing and drying the waste textile to obtain a pretreated textile;
step two: crushing the pretreated textile, and then opening and decoloring to obtain waste fibers;
step three: washing and drying the waste fibers, and then spinning and forming to obtain regenerated textile cloth;
step four: adding the antibacterial agent into deionized water to prepare antibacterial liquid with the concentration of 50-100 g/L;
step five: soaking the regenerated textile cloth in an antibacterial solution for 1-2h, taking out and drying, soaking in the antibacterial solution for 1-2h again, and repeatedly soaking for 2-3 times to obtain the antibacterial regenerated cloth;
step six: and cutting, printing and sewing the antibacterial regenerated cloth to obtain the antibacterial environment-friendly shopping bag.
2. The method for preparing bacteriostatic environment-friendly shopping bags based on waste textiles as claimed in claim 1, wherein the antibacterial agent is prepared by the following steps:
a1: adding p-chloronitrobenzene, p-nitroaniline, anhydrous potassium carbonate, toluene and N, N-dimethylformamide into a three-neck flask provided with a stirrer, a thermometer and a gas-guide tube, introducing nitrogen for protection, stirring and reacting for 5-6h under the conditions that the temperature is 130-;
a2: adding the intermediate 1, 10% palladium carbon and acetone into a four-neck flask provided with a stirrer, a thermometer, a gas-guide tube, a constant-pressure dropping funnel and a reflux condenser tube, introducing nitrogen for protection, stirring for 30-40min under the conditions that the temperature is 20-25 ℃ and the stirring speed is 450-550r/min, then heating to reflux, controlling the heating speed to be 2-3 ℃/min, then dropwise adding a hydrazine hydrate solution while stirring, controlling the dropwise adding speed to be 1-2 drops/s, continuously stirring for reacting for 6-8h after the dropwise adding is finished, filtering a reaction product while the reaction is hot after the reaction is finished, adding a filtrate into ice water, separating out a precipitate, carrying out vacuum filtration, washing a filter cake with distilled water for 2-3 times, then placing in a vacuum drying box, drying for 4-6h under the condition that the temperature is 60-70 ℃, obtaining an intermediate 2;
a3: adding the intermediate 2, mercaptopropionic acid, p-toluenesulfonic acid and toluene into a four-neck flask provided with a stirrer, a thermometer, a gas-guide tube, a constant-pressure dropping funnel and a reflux condenser tube, introducing nitrogen for protection, heating to reflux while stirring under the condition that the stirring speed is 450-550r/min, controlling the heating rate to be 2-3 ℃/min, then continuing stirring for reaction for 6-8h, dropwise adding a sodium hydroxide solution while stirring, controlling the dropwise adding rate to be 1-2 drops/s until the pH value is 7, washing a reaction product with distilled water for 2-3 times after the reaction is finished, standing for layering, drying an organic phase with anhydrous sodium sulfate, then carrying out vacuum filtration, and carrying out rotary evaporation on a filtrate to remove a solvent to obtain an intermediate 3;
a4: adding methyl acrylate, N-dimethylethanolamine, hydroquinone and tetrabutyl titanate into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, heating to 85-90 ℃ while stirring under the condition that the stirring speed is 450-550r/min, controlling the heating speed to 2-3 ℃/min, then continuously stirring for reacting for 2-3h, heating to 110-120 ℃ while stirring, continuously stirring for reacting for 6-8h, and rotationally evaporating a reaction product to remove a solvent after the reaction is finished to obtain an intermediate 4;
a5: adding the intermediate 4, monobromododecane and anhydrous acetonitrile into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 20-30h under the conditions that the temperature is 45-50 ℃ and the stirring rate is 450-550r/min, cooling a reaction product to room temperature after the reaction is finished, then adding the reaction product into anhydrous ether, separating out a precipitate, carrying out vacuum filtration, washing a filter cake with the anhydrous ether for 2-3 times, then placing the filter cake into a vacuum drying box, and drying for 4-6h under the condition that the temperature is 30-35 ℃ to obtain an intermediate 5;
a6: adding the intermediate 3, the intermediate 5 and toluene into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 8-10h under the conditions that the temperature is 55-60 ℃ and the stirring rate is 450-550r/min, cooling a reaction product to room temperature after the reaction is finished, then adding the reaction product into anhydrous ether, separating out a precipitate, carrying out vacuum filtration, washing a filter cake for 2-3 times by using the anhydrous ether, then placing the filter cake into a vacuum drying box, and drying for 10-15h under the condition that the temperature is 50-55 ℃ to obtain the antibacterial agent.
3. The method for preparing bacteriostatic environment-friendly shopping bags based on waste textiles as claimed in claim 2, wherein the dosage ratio of p-chloronitrobenzene, p-nitroaniline, anhydrous potassium carbonate, toluene and N, N-dimethylformamide in step A1 is 0.21-0.23 mol: 0.1 mol: 0.15-0.2 mol: 60-70 mL: 200 and 250 mL.
4. The method for preparing bacteriostatic environment-friendly shopping bags based on waste textiles as claimed in claim 2, wherein the dosage ratio of the intermediate 1, 10% palladium on carbon, acetone and hydrazine hydrate solution in step A2 is 0.1 mol: 1.8-3.6 g: 100-120 mL: 40-50mL, wherein the mass fraction of the hydrazine hydrate solution is 60-64%.
5. The method for preparing bacteriostatic environment-friendly shopping bags based on waste textiles as claimed in claim 2, wherein the user amount ratio of the intermediate 2, mercaptopropionic acid, p-toluenesulfonic acid and toluene in step A3 is 0.1 mol: 0.33-0.35 mol: 0.8-1.5 g: 80-100mL, wherein the mass fraction of the sodium hydroxide solution is 10-15%.
6. The method for preparing bacteriostatic environment-friendly shopping bags based on waste textiles as claimed in claim 2, wherein the amount ratio of the methyl acrylate, the N, N-dimethylethanolamine, the hydroquinone and the tetrabutyl titanate in the step A4 is 0.1 mol: 0.1 mol: 0.3-0.5 g: 5.2-6.8 g.
7. The method for preparing bacteriostatic environment-friendly shopping bags based on waste textiles as claimed in claim 2, wherein the amount ratio of the intermediate 4, monobromododecane and anhydrous acetonitrile in step A5 is 0.11-0.13 mol: 0.1 mol: 40-50 mL.
8. The method for preparing bacteriostatic environment-friendly shopping bags based on waste textiles as claimed in claim 2, wherein the amount ratio of the intermediate 3, the intermediate 5 and toluene in step A6 is 0.1 mol: 0.33-0.36 mol: 50-60 mL.
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