CN112779620A - Process for manufacturing surgical cap material - Google Patents
Process for manufacturing surgical cap material Download PDFInfo
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- CN112779620A CN112779620A CN202110003381.9A CN202110003381A CN112779620A CN 112779620 A CN112779620 A CN 112779620A CN 202110003381 A CN202110003381 A CN 202110003381A CN 112779620 A CN112779620 A CN 112779620A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- A—HUMAN NECESSITIES
- A42—HEADWEAR
- A42B—HATS; HEAD COVERINGS
- A42B1/00—Hats; Caps; Hoods
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- A—HUMAN NECESSITIES
- A42—HEADWEAR
- A42C—MANUFACTURING OR TRIMMING HEAD COVERINGS, e.g. HATS
- A42C1/00—Manufacturing hats
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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Abstract
The invention discloses a process for preparing a surgical cap material, which comprises the steps of mixing butanediol terephthalate, trifluoroacetic acid and dichloromethane to prepare a polyester solution, adding an antibacterial agent for ultrasonic treatment to prepare a spinning solution, and spinning to prepare the surgical cap material.
Description
Technical Field
The invention relates to the technical field of new material preparation, in particular to a process for manufacturing an operation cap material.
Background
Nonwoven fabrics have been rapidly developed in recent years as medical fabrics, and nonwoven fabrics are used in many cases. The non-woven fabric formed by randomly arranging the fibers has the holes with the sizes and the shapes distributed in the non-woven fabric, is favorable for the attachment of microorganisms, becomes a good parasitic place for the survival and the propagation of the microorganisms, and is a transfer station for the secondary propagation of pathogenic bacteria. The antibacterial cloth endows the cloth with antibacterial performance, so that the cloth can efficiently kill or inhibit bacteria, fungi and mould on the fabric, prevent bacteria from regenerating and propagating, reduce the risk of secondary propagation, and improve the safety of normal use and waste treatment of the cloth.
The existing operation cap can generate a large amount of sweat due to long-time operation in the use process of a doctor, the operation cap can absorb the sweat and breed bacteria, the breeding of the bacteria enables the operation environment to be reduced, the wound of a patient can be infected, and the success rate of the operation is reduced.
Disclosure of Invention
The invention aims to provide a manufacturing process of an operation cap material.
The technical problems to be solved by the invention are as follows:
the existing operation cap can generate a large amount of sweat due to long-time operation in the use process of a doctor, the operation cap can absorb the sweat and breed bacteria, the breeding of the bacteria enables the operation environment to be reduced, the wound of a patient can be infected, and the success rate of the operation is reduced.
The purpose of the invention can be realized by the following technical scheme:
a manufacturing process of an operation cap material specifically comprises the following steps:
step S1: adding butylene terephthalate, trifluoroacetic acid and dichloromethane into a stirring kettle, and stirring for 1-1.5h under the condition that the rotating speed is 500-800r/min to prepare a polyester solution;
step S2: adding the antibacterial agent and the polyester solution prepared in the step S1 into a stirring kettle, stirring for 5-10min under the condition that the rotating speed is 800-1000r/min, and then carrying out ultrasonic treatment for 1-1.5h under the condition that the frequency is 5-8MHz to prepare spinning solution;
step S3: adding the spinning solution into an electrostatic spinning instrument, and spinning under the conditions that the pushing speed is 0.001-0.003mm/s, the spinning voltage is 22-25kV, and the receiving distance is 5-8cm to obtain the surgical cap material.
Furthermore, the mass ratio of the using amount of the butylene terephthalate, the trifluoroacetic acid and the dichloromethane in the step S1 is 1:8:2, and the using amount of the antibacterial agent and the polyester solution in the step S2 is 1g:20 mL.
Further, the antibacterial agent is prepared by the following steps:
step A1: adding 2, 6-dimethylphenol and a sodium hydroxide solution into a reaction kettle, stirring the 2, 6-dimethylphenol to completely dissolve under the conditions that the rotation speed is 200-35 ℃ and the temperature is 30-35 ℃, adding dimethyl sulfate to react for 2-4h to prepare an intermediate 1, adding the intermediate 1, deionized water and potassium permanganate into the reaction, performing reflux reaction for 4-5h under the condition that the temperature is 110-120 ℃ to prepare an intermediate 2, adding the intermediate 2, methanol and concentrated sulfuric acid into the reaction kettle, and reacting for 3-5h under the conditions that the rotation speed is 150-200r/min and the temperature is 70-80 ℃ to prepare an intermediate 3;
the reaction process is as follows:
step A2: adding the intermediate 3, dimethylaminoethanol, hydroquinone and tetrabutyl titanate into a reaction kettle, reacting for 4-6h at the rotation speed of 200-300r/min and the temperature of 65-70 ℃ to obtain an intermediate 4, adding the intermediate 4, acetonitrile and hydroquinone into the reaction kettle, stirring and adding bromohexadecane at the rotation speed of 150-200r/min and the temperature of 45-50 ℃ to react for 10-15h to obtain an intermediate 5, dissolving the intermediate 5 in medium tetrahydrofuran, adding boron tribromide at the temperature of 70-80 ℃ below zero, reacting for 10-15h at the temperature of 25-30 ℃ after the addition is finished to obtain an intermediate 6, dissolving cyanuric chloride in acetone, reacting at the rotation speed of 200-300r/min and the temperature of 0-5 ℃, adding the intermediate 6 and sodium acetate, and reacting for 5-8h to obtain an intermediate 7;
the reaction process is as follows:
step A3: adding 5, 5-dimethylhydantoin, potassium carbonate and acetone into a reaction kettle, refluxing for 30-35min at the rotation speed of 150-;
the reaction process is as follows:
step A4: adding graphite powder, sodium nitrate and concentrated sulfuric acid into a reaction kettle, stirring and adding potassium permanganate under the conditions that the rotating speed is 120-minus one year (r/min) and the temperature is 0-3 ℃, after stirring for 3-5min, heating to the temperature of 30-40 ℃, reacting for 1-1.5h, adding deionized water, reacting for 15-20min under the temperature of 95-98 ℃, adding hydrogen peroxide, reacting for 5-10min, filtering to remove filtrate, and drying a filter cake to obtain graphene oxide;
step A5: adding chitosan and acetic acid solution into a stirring kettle, stirring for 1-1.5h under the condition of the rotation speed of 200-300r/min to prepare chitosan colloidal solution, adding graphene oxide and deionized water into the stirring kettle, stirring for 1-1.5h under the condition of the rotation speed of 200-300r/min to prepare graphene oxide colloidal solution, mixing the chitosan colloidal solution and the graphene oxide colloidal solution, adding magnesium carbonate, butyl titanate, ethanol and deionized water, stirring for 3-5h under the condition of the rotation speed of 400-500r/min, adding silver nitrate solution, continuously stirring for 3-5h, adding ethylenediamine and 1-hydroxybenzotriazole, reacting for 3-5h under the condition of the temperature of 35-40 ℃, adding an intermediate 10, and reacting at the temperature of 80-90 ℃, after reacting for 5-8h, distilling to remove the solvent, and obtaining the antibacterial agent.
Further, the mass ratio of the 2, 6-dimethylphenol, the sodium hydroxide solution and the dimethyl sulfate in the step A1 is 4.8:40:27.3, the mass fraction of the sodium hydroxide solution is 25%, the mass ratio of the intermediate 1, the deionized water and the potassium permanganate is 1.8g:50mL:4.5g, and the mass ratio of the intermediate 2, the methanol and the concentrated sulfuric acid is 0.25mol:0.25mol:10 mL.
Further, the molar ratio of the intermediate 3, the dimethylaminoethanol, the hydroquinone and the tetrabutyl titanate in the step A2 is 5:15:0.04:0.3, the molar ratio of the intermediate 4, the acetonitrile, the hydroquinone and the bromohexadecane is 0.055mol:30mL:0.004mol:0.05mol, the molar ratio of the intermediate 5 and the boron tribromide is 1g:3mL, and the molar ratio of the cyanuric chloride, the intermediate 6 and the sodium acetate is 0.25mol:0.25mol:0.3 g.
Further, the amount ratio of 5, 5-dimethylhydantoin, potassium carbonate, acetone, 1, 3-dibromopropane described in step A3 is 3.05g:12.07g:200mL:13.62g, the amount ratio of ciprofloxacin, intermediate 8, triethylamine, potassium iodide, tetrabutyl, dichloromethane, and ethanol is 6mmol:6.5mmol:6mmol: 0.1g:30mL:10mL, and the amount ratio of intermediate 7, intermediate 9, and sodium acetate is 0.5mol:0.5mol:1 g.
Further, the using amount ratio of the graphite powder, the sodium nitrate, the concentrated sulfuric acid, the potassium permanganate, the deionized water and the hydrogen peroxide in the step A4 is 1g to 0.5g to 25mL to 3g to 20mL to 10mL, the mass fraction of the concentrated sulfuric acid is 80%, and the mass fraction of the hydrogen peroxide is 25%.
Further, the dosage ratio of the chitosan to the acetic acid solution in the step A5 is 1g:100mL, the mass fraction of the acetic acid solution is 1%, the dosage ratio of the graphene oxide to the deionized water is 1g:50mL, and the dosage ratio of the chitosan colloidal solution, the graphene oxide colloidal solution, the magnesium carbonate, the butyl titanate, the ethanol, the deionized water, the silver nitrate solution, the ethylenediamine, the 1-hydroxybenzotriazole and the intermediate 10 is 100mL:100mL:1g:15mL:10mL:50mL:50mL:12mL:2.5 g.
The invention has the beneficial effects that: the invention discloses an antibacterial agent prepared in the process of preparing an operation cap material, which takes 2, 6-dimethylphenol as a raw material, dimethyl sulfate is firstly used for hydroxyl protection to prepare an intermediate 1, the intermediate 1 is oxidized by potassium permanganate to prepare an intermediate 2, the intermediate 2 is subjected to esterification reaction with methanol to prepare an intermediate 3, the intermediate 3 is subjected to reaction with dimethylaminoethanol to prepare an intermediate 4, the intermediate 4 is reacted with bromohexadecane to prepare an intermediate 5, the intermediate 5 is subjected to deprotection to prepare an intermediate 6, the intermediate 6 is reacted with cyanuric chloride, the reaction is carried out with one chlorine atom site of the cyanuric chloride under the control of temperature to prepare an intermediate 7, the 5, 5-dimethylhydantoin is reacted with 1, 3-dibromopropane to prepare an intermediate 8, and the intermediate 8 is reacted with ciprofloxacin, preparing an intermediate 9, reacting the intermediate 9 and the intermediate 7 with a chlorine atom site on the intermediate 7 through temperature control to prepare an intermediate 10, oxidizing graphite powder to prepare graphene oxide, mixing chitosan colloidal solution and graphene colloidal solution, hydrolyzing butyl titanate to generate nano titanium dioxide, adding magnesium carbonate and silver nitrate to enable a large amount of silver ions to be attached to the surface of the nano titanium dioxide, adding ethylenediamine and the graphene oxide to react, condensing carboxyl on the surface of the graphene oxide and an amino on the ethylenediamine, adding the intermediate 10, distilling the residual chlorine atom site on the intermediate 10 and the residual amino on the ethylenediamine to remove a solvent after the reaction, and preparing an antibacterial agent, wherein the antibacterial agent can destroy a phospholipid bilayer of bacterial cells to damage cell membranes and simultaneously cause proton and proton of the cells, Nucleic acid and protein are oxidized to destroy cell membranes to inhibit the growth and reproduction of bacteria, the antibacterial agent is quaternary ammonium salt, positive charges act with head groups of acidic phospholipid in the cell membranes of the bacteria to reduce the permeability of the cell membranes, bacterial cell sap leaks to cause bacterial cell death, and meanwhile, the antibacterial agent molecules can denature bacterial protein to prevent bacterial metabolism and further kill the bacteria, so that the prepared operating cap is not easy to breed the bacteria.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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
A manufacturing process of an operation cap material specifically comprises the following steps:
step S1: adding butylene terephthalate, trifluoroacetic acid and dichloromethane into a stirring kettle, and stirring for 1h at the rotating speed of 500r/min to prepare a polyester solution;
step S2: adding the antibacterial agent and the polyester solution prepared in the step S1 into a stirring kettle, stirring for 5min at the rotation speed of 800r/min, and then carrying out ultrasonic treatment for 1h at the frequency of 5MHz to prepare a spinning solution;
step S3: and adding the spinning solution into an electrostatic spinning instrument, and spinning under the conditions that the pushing speed is 0.001mm/s, the spinning voltage is 22kV and the receiving distance is 5cm to obtain the surgical cap material.
The antibacterial agent is prepared by the following steps:
step A1: adding 2, 6-dimethylphenol and a sodium hydroxide solution into a reaction kettle, stirring to completely dissolve the 2, 6-dimethylphenol at the rotation speed of 200r/min and the temperature of 30 ℃, adding dimethyl sulfate, reacting for 2 hours to obtain an intermediate 1, adding the intermediate 1, deionized water and potassium permanganate into the reaction, performing reflux reaction for 4 hours at the temperature of 110 ℃ to obtain an intermediate 2, adding the intermediate 2, methanol and concentrated sulfuric acid into the reaction kettle, and reacting for 3 hours at the rotation speed of 150r/min and the temperature of 70 ℃ to obtain an intermediate 3;
step A2: adding the intermediate 3, dimethylaminoethanol, hydroquinone and tetrabutyl titanate into a reaction kettle, reacting for 4 hours at the rotating speed of 200r/min and the temperature of 65 ℃ to obtain an intermediate 4, adding the intermediate 4, acetonitrile and hydroquinone into the reaction kettle, stirring and adding bromohexadecane to react for 10 hours at the rotating speed of 150r/min and the temperature of 45 ℃ to obtain an intermediate 5, dissolving cyanuric chloride in acetone, adding the intermediate 5 and sodium acetate to react for 5 hours at the rotating speed of 200r/min and the temperature of 0 ℃ to obtain an intermediate 6;
step A3: adding 5, 5-dimethylhydantoin, potassium carbonate and acetone into a reaction kettle, refluxing for 30min at the rotation speed of 150r/min and the temperature of 60 ℃, adding 1, 3-dibromopropane, continuing to react for 3h to obtain an intermediate 7, adding ciprofloxacin, the intermediate 7, triethylamine, potassium iodide, tetrabutyl, dichloromethane and ethanol into the reaction kettle, refluxing for 18h at the rotation speed of 200r/min and the temperature of 40 ℃ to obtain an intermediate 8, adding the intermediate 6, the intermediate 8, sodium acetate and acetone into the reaction kettle, and reacting for 3h at the temperature of 40 ℃ to obtain an intermediate 9;
step A4: adding graphite powder, sodium nitrate and concentrated sulfuric acid into a reaction kettle, stirring and adding potassium permanganate under the conditions that the rotating speed is 120r/min and the temperature is 0 ℃, stirring for 3min, heating to 30 ℃, reacting for 1h, adding deionized water, reacting for 15min under the condition that the temperature is 95 ℃, adding hydrogen peroxide, reacting for 5min, filtering to remove filtrate, and drying a filter cake to obtain graphene oxide;
step A5: adding chitosan and acetic acid solution into a stirring kettle, stirring for 1h at the rotation speed of 200r/min to prepare chitosan colloidal solution, adding graphene oxide and deionized water into the stirring kettle, stirring for 1h at the rotation speed of 200r/min to prepare graphene oxide colloidal solution, mixing the chitosan colloidal solution and the graphene oxide colloidal solution, adding magnesium carbonate, butyl orthotitanate, ethanol and deionized water, stirring for 3h at the rotation speed of 400r/min, adding silver nitrate solution, continuously stirring for 3h, adding ethylenediamine and 1-hydroxybenzotriazole, reacting for 3h at the temperature of 35 ℃, adding an intermediate 9, reacting for 5h at the temperature of 80 ℃, and distilling to remove the solvent to prepare the antibacterial agent.
Example 2
A manufacturing process of an operation cap material specifically comprises the following steps:
step S1: adding butanediol terephthalate, trifluoroacetic acid and dichloromethane into a stirring kettle, and stirring for 1.5h under the condition that the rotating speed is 500r/min to prepare a polyester solution;
step S2: adding the antibacterial agent and the polyester solution prepared in the step S1 into a stirring kettle, stirring for 10min at the rotation speed of 800r/min, and then carrying out ultrasonic treatment for 1.5h at the frequency of 5MHz to prepare a spinning solution;
step S3: and adding the spinning solution into an electrostatic spinning instrument, and spinning under the conditions that the pushing speed is 0.001mm/s, the spinning voltage is 25kV and the receiving distance is 5cm to obtain the surgical cap material.
The antibacterial agent is prepared by the following steps:
step A1: adding 2, 6-dimethylphenol and a sodium hydroxide solution into a reaction kettle, stirring to completely dissolve the 2, 6-dimethylphenol under the conditions of the rotating speed of 300r/min and the temperature of 30 ℃, adding dimethyl sulfate, reacting for 4 hours to obtain an intermediate 1, adding the intermediate 1, deionized water and potassium permanganate into the reaction, performing reflux reaction for 5 hours under the temperature of 110 ℃ to obtain an intermediate 2, adding the intermediate 2, methanol and concentrated sulfuric acid into the reaction kettle, and reacting for 3 hours under the conditions of the rotating speed of 150r/min and the temperature of 80 ℃ to obtain an intermediate 3;
step A2: adding the intermediate 3, dimethylaminoethanol, hydroquinone and tetrabutyl titanate into a reaction kettle, reacting for 6 hours at the rotating speed of 300r/min and the temperature of 65 ℃ to obtain an intermediate 4, adding the intermediate 4, acetonitrile and hydroquinone into the reaction kettle, stirring and adding bromohexadecane to react for 10 hours at the rotating speed of 150r/min and the temperature of 50 ℃ to obtain an intermediate 5, dissolving cyanuric chloride in acetone, adding the intermediate 5 and sodium acetate to react for 8 hours at the rotating speed of 300r/min and the temperature of 0 ℃ to obtain an intermediate 6;
step A3: adding 5, 5-dimethylhydantoin, potassium carbonate and acetone into a reaction kettle, refluxing for 30min at the rotation speed of 150r/min and the temperature of 70 ℃, adding 1, 3-dibromopropane, continuing to react for 5h to prepare an intermediate 7, adding ciprofloxacin, the intermediate 7, triethylamine, potassium iodide, tetrabutyl, dichloromethane and ethanol into the reaction kettle, refluxing for 18h at the rotation speed of 200r/min and the temperature of 50 ℃ to prepare an intermediate 8, adding the intermediate 6, the intermediate 8, sodium acetate and acetone into the reaction kettle, and reacting for 3-5h at the temperature of 50 ℃ to prepare an intermediate 9;
step A4: adding graphite powder, sodium nitrate and concentrated sulfuric acid into a reaction kettle, stirring and adding potassium permanganate under the conditions that the rotating speed is 120r/min and the temperature is 3 ℃, stirring for 3min, heating to 40 ℃, reacting for 1h, adding deionized water, reacting for 15min under the condition that the temperature is 98 ℃, adding hydrogen peroxide, reacting for 10min, filtering to remove filtrate, and drying a filter cake to obtain graphene oxide;
step A5: adding chitosan and acetic acid solution into a stirring kettle, stirring for 1.5h at the rotation speed of 200r/min to prepare chitosan colloidal solution, adding graphene oxide and deionized water into the stirring kettle, stirring for 1.5h at the rotation speed of 200r/min to prepare graphene oxide colloidal solution, mixing the chitosan colloidal solution and the graphene oxide colloidal solution, adding magnesium carbonate, butyl orthotitanate, ethanol and deionized water, stirring for 5h at the rotation speed of 400r/min, adding silver nitrate solution, continuously stirring for 3h, adding ethylenediamine and 1-hydroxybenzotriazole, reacting for 3h at the temperature of 40 ℃, adding the intermediate 9, reacting for 5h at the temperature of 90 ℃, and distilling to remove the solvent to prepare the antibacterial agent.
Example 3
A manufacturing process of an operation cap material specifically comprises the following steps:
step S1: adding butanediol terephthalate, trifluoroacetic acid and dichloromethane into a stirring kettle, and stirring for 1h at the rotating speed of 800r/min to prepare a polyester solution;
step S2: adding the antibacterial agent and the polyester solution prepared in the step S1 into a stirring kettle, stirring for 5min at the rotation speed of 1000r/min, and then carrying out ultrasonic treatment for 1h at the frequency of 8MHz to prepare a spinning solution;
step S3: and adding the spinning solution into an electrostatic spinning instrument, and spinning under the conditions that the pushing speed is 0.003mm/s, the spinning voltage is 22kV and the receiving distance is 8cm to obtain the surgical cap material.
The antibacterial agent is prepared by the following steps:
step A1: adding 2, 6-dimethylphenol and a sodium hydroxide solution into a reaction kettle, stirring to completely dissolve the 2, 6-dimethylphenol under the conditions of the rotating speed of 200r/min and the temperature of 35 ℃, adding dimethyl sulfate, reacting for 2 hours to obtain an intermediate 1, adding the intermediate 1, deionized water and potassium permanganate into the reaction, performing reflux reaction for 4 hours under the condition of the temperature of 120 ℃ to obtain an intermediate 2, adding the intermediate 2, methanol and concentrated sulfuric acid into the reaction kettle, and reacting for 5 hours under the conditions of the rotating speed of 200r/min and the temperature of 70 ℃ to obtain an intermediate 3;
step A2: adding the intermediate 3, dimethylaminoethanol, hydroquinone and tetrabutyl titanate into a reaction kettle, reacting for 4 hours at the rotation speed of 200r/min and the temperature of 70 ℃ to obtain an intermediate 4, adding the intermediate 4, acetonitrile and hydroquinone into the reaction kettle, stirring and adding bromohexadecane at the rotation speed of 200r/min and the temperature of 45 ℃ to react for 15 hours to obtain an intermediate 5, dissolving cyanuric chloride in acetone, adding the intermediate 5 and sodium acetate at the rotation speed of 200r/min and the temperature of 5 ℃ to react for 5 hours to obtain an intermediate 6;
step A3: adding 5, 5-dimethylhydantoin, potassium carbonate and acetone into a reaction kettle, refluxing for 35min at the rotation speed of 200r/min and the temperature of 60 ℃, adding 1, 3-dibromopropane, continuing to react for 3h to prepare an intermediate 7, adding ciprofloxacin, the intermediate 7, triethylamine, potassium iodide, tetrabutyl, dichloromethane and ethanol into the reaction kettle, refluxing for 25h at the rotation speed of 300r/min and the temperature of 40 ℃ to prepare an intermediate 8, adding the intermediate 6, the intermediate 8, sodium acetate and acetone into the reaction kettle, and reacting for 5h at the temperature of 40 ℃ to prepare an intermediate 9;
step A4: adding graphite powder, sodium nitrate and concentrated sulfuric acid into a reaction kettle, stirring and adding potassium permanganate under the conditions that the rotating speed is 120r/min and the temperature is 3 ℃, stirring for 3min, heating to 40 ℃, reacting for 1h, adding deionized water, reacting for 15min under the condition that the temperature is 98 ℃, adding hydrogen peroxide, reacting for 10min, filtering to remove filtrate, and drying a filter cake to obtain graphene oxide;
step A5: adding chitosan and acetic acid solution into a stirring kettle, stirring for 1.5h at the rotation speed of 200r/min to prepare chitosan colloidal solution, adding graphene oxide and deionized water into the stirring kettle, stirring for 1.5h at the rotation speed of 200r/min to prepare graphene oxide colloidal solution, mixing the chitosan colloidal solution and the graphene oxide colloidal solution, adding magnesium carbonate, butyl orthotitanate, ethanol and deionized water, stirring for 5h at the rotation speed of 400r/min, adding silver nitrate solution, continuously stirring for 3h, adding ethylenediamine and 1-hydroxybenzotriazole, reacting for 3h at the temperature of 40 ℃, adding the intermediate 9, reacting for 5h at the temperature of 90 ℃, and distilling to remove the solvent to prepare the antibacterial agent.
Example 4
A manufacturing process of an operation cap material specifically comprises the following steps:
step S1: adding butanediol terephthalate, trifluoroacetic acid and dichloromethane into a stirring kettle, and stirring for 1.5h under the condition that the rotating speed is 800r/min to prepare a polyester solution;
step S2: adding the antibacterial agent and the polyester solution prepared in the step S1 into a stirring kettle, stirring for 10min at the rotation speed of 1000r/min, and then carrying out ultrasonic treatment for 1.5h at the frequency of 8MHz to prepare a spinning solution;
step S3: and adding the spinning solution into an electrostatic spinning instrument, and spinning under the conditions that the pushing speed is 0.003mm/s, the spinning voltage is 25kV and the receiving distance is 8cm to obtain the surgical cap material.
The antibacterial agent is prepared by the following steps:
step A1: adding 2, 6-dimethylphenol and a sodium hydroxide solution into a reaction kettle, stirring to completely dissolve the 2, 6-dimethylphenol under the conditions of the rotating speed of 300r/min and the temperature of 35 ℃, adding dimethyl sulfate, reacting for 4 hours to obtain an intermediate 1, adding the intermediate 1, deionized water and potassium permanganate into the reaction, performing reflux reaction for 5 hours under the condition of the temperature of 120 ℃ to obtain an intermediate 2, adding the intermediate 2, methanol and concentrated sulfuric acid into the reaction kettle, and reacting for 5 hours under the conditions of the rotating speed of 200r/min and the temperature of 80 ℃ to obtain an intermediate 3;
step A2: adding the intermediate 3, dimethylaminoethanol, hydroquinone and tetrabutyl titanate into a reaction kettle, reacting for 6 hours at the rotation speed of 300r/min and the temperature of 70 ℃ to obtain an intermediate 4, adding the intermediate 4, acetonitrile and hydroquinone into the reaction kettle, stirring and adding bromohexadecane at the rotation speed of 200r/min and the temperature of 50 ℃ to react for 15 hours to obtain an intermediate 5, dissolving cyanuric chloride in acetone, adding the intermediate 5 and sodium acetate at the rotation speed of 300r/min and the temperature of 5 ℃ to react for 8 hours to obtain an intermediate 6;
step A3: adding 5, 5-dimethylhydantoin, potassium carbonate and acetone into a reaction kettle, refluxing for 35min at the rotation speed of 200r/min and the temperature of 70 ℃, adding 1, 3-dibromopropane, continuing to react for 5h to prepare an intermediate 7, adding ciprofloxacin, the intermediate 7, triethylamine, potassium iodide, tetrabutyl, dichloromethane and ethanol into the reaction kettle, refluxing for 25h at the rotation speed of 300r/min and the temperature of 50 ℃ to prepare an intermediate 8, adding the intermediate 6, the intermediate 8, sodium acetate and acetone into the reaction kettle, and reacting for 5h at the temperature of 50 ℃ to prepare an intermediate 9;
step A4: adding graphite powder, sodium nitrate and concentrated sulfuric acid into a reaction kettle, stirring and adding potassium permanganate under the conditions that the rotating speed is 150r/min and the temperature is 3 ℃, stirring for 5min, heating to 40 ℃, reacting for 1.5h, adding deionized water, reacting for 20min under the condition that the temperature is 98 ℃, adding hydrogen peroxide, reacting for 10min, filtering to remove filtrate, and drying a filter cake to obtain graphene oxide;
step A5: adding chitosan and acetic acid solution into a stirring kettle, stirring for 1.5h at the rotation speed of 300r/min to prepare chitosan colloidal solution, adding graphene oxide and deionized water into the stirring kettle, stirring for 1.5h at the rotation speed of 300r/min to prepare graphene oxide colloidal solution, mixing the chitosan colloidal solution and the graphene oxide colloidal solution, adding magnesium carbonate, butyl orthotitanate, ethanol and deionized water, stirring for 5h at the rotation speed of 500r/min, adding silver nitrate solution, continuously stirring for 5h, adding ethylenediamine and 1-hydroxybenzotriazole, reacting for 5h at the temperature of 40 ℃, adding an intermediate 9, reacting for 8h at the temperature of 90 ℃, and distilling to remove the solvent to prepare the antibacterial agent.
Comparative example
The comparative example is a common surgical cap material in the market.
The performance of the surgical cap materials prepared in examples 1 to 4 and the comparative example was tested, and the test results are shown in table 1 below;
TABLE 1
As can be seen from Table 1 above, the antibacterial rates of Staphylococcus aureus of the surgical cap materials prepared in examples 1-4 are 99.13-99.62%, Candida albicans are 98.95-99.42%, and Escherichia coli is 99.27-99.63%, while the antibacterial rates of Staphylococcus aureus of the surgical cap materials prepared in the comparative examples are 90.5%, Candida albicans are 89.25%, and Escherichia coli is 91.25%, indicating that the present invention has a good antibacterial effect.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (8)
1. A process for manufacturing an operation cap material is characterized in that: the method specifically comprises the following steps:
step S1: adding butylene terephthalate, trifluoroacetic acid and dichloromethane into a stirring kettle, and stirring for 1-1.5h under the condition that the rotating speed is 500-800r/min to prepare a polyester solution;
step S2: adding the antibacterial agent and the polyester solution prepared in the step S1 into a stirring kettle, stirring for 5-10min under the condition that the rotating speed is 800-1000r/min, and then carrying out ultrasonic treatment for 1-1.5h under the condition that the frequency is 5-8MHz to prepare spinning solution;
step S3: adding the spinning solution into an electrostatic spinning instrument, and spinning under the conditions that the pushing speed is 0.001-0.003mm/s, the spinning voltage is 22-25kV, and the receiving distance is 5-8cm to obtain the surgical cap material.
2. The process for manufacturing a surgical cap material according to claim 1, wherein: the mass ratio of the using amount of the butylene terephthalate, the trifluoroacetic acid and the dichloromethane in the step S1 is 1:8:2, and the using amount of the antibacterial agent and the polyester solution in the step S2 is 1g:20 mL.
3. The process for manufacturing a surgical cap material according to claim 1, wherein: the antibacterial agent is prepared by the following steps:
step A1: adding 2, 6-dimethylphenol and a sodium hydroxide solution into a reaction kettle, stirring the 2, 6-dimethylphenol to completely dissolve under the conditions that the rotation speed is 200-35 ℃ and the temperature is 30-35 ℃, adding dimethyl sulfate to react for 2-4h to prepare an intermediate 1, adding the intermediate 1, deionized water and potassium permanganate into the reaction, performing reflux reaction for 4-5h under the condition that the temperature is 110-120 ℃ to prepare an intermediate 2, adding the intermediate 2, methanol and concentrated sulfuric acid into the reaction kettle, and reacting for 3-5h under the conditions that the rotation speed is 150-200r/min and the temperature is 70-80 ℃ to prepare an intermediate 3;
step A2: adding the intermediate 3, dimethylaminoethanol, hydroquinone and tetrabutyl titanate into a reaction kettle, reacting for 4-6h at the rotation speed of 200-300r/min and the temperature of 65-70 ℃ to obtain an intermediate 4, adding the intermediate 4, acetonitrile and hydroquinone into the reaction kettle, stirring and adding bromohexadecane at the rotation speed of 150-200r/min and the temperature of 45-50 ℃ to react for 10-15h to obtain an intermediate 5, dissolving the intermediate 5 in medium tetrahydrofuran, adding boron tribromide at the temperature of 70-80 ℃ below zero, reacting for 10-15h at the temperature of 25-30 ℃ after the addition is finished to obtain an intermediate 6, dissolving cyanuric chloride in acetone, reacting at the rotation speed of 200-300r/min and the temperature of 0-5 ℃, adding the intermediate 6 and sodium acetate, and reacting for 5-8h to obtain an intermediate 7;
step A3: adding 5, 5-dimethylhydantoin, potassium carbonate and acetone into a reaction kettle, refluxing for 30-35min at the rotation speed of 150-;
step A4: adding graphite powder, sodium nitrate and concentrated sulfuric acid into a reaction kettle, stirring and adding potassium permanganate under the conditions that the rotating speed is 120-minus one year (r/min) and the temperature is 0-3 ℃, after stirring for 3-5min, heating to the temperature of 30-40 ℃, reacting for 1-1.5h, adding deionized water, reacting for 15-20min under the temperature of 95-98 ℃, adding hydrogen peroxide, reacting for 5-10min, filtering to remove filtrate, and drying a filter cake to obtain graphene oxide;
step A5: adding chitosan and acetic acid solution into a stirring kettle, stirring for 1-1.5h under the condition of the rotation speed of 200-300r/min to prepare chitosan colloidal solution, adding graphene oxide and deionized water into the stirring kettle, stirring for 1-1.5h under the condition of the rotation speed of 200-300r/min to prepare graphene oxide colloidal solution, mixing the chitosan colloidal solution and the graphene oxide colloidal solution, adding magnesium carbonate, butyl titanate, ethanol and deionized water, stirring for 3-5h under the condition of the rotation speed of 400-500r/min, adding silver nitrate solution, continuously stirring for 3-5h, adding ethylenediamine and 1-hydroxybenzotriazole, reacting for 3-5h under the condition of the temperature of 35-40 ℃, adding an intermediate 10, and reacting at the temperature of 80-90 ℃, after reacting for 5-8h, distilling to remove the solvent, and obtaining the antibacterial agent.
4. The process for manufacturing a surgical cap material according to claim 3, wherein: the mass ratio of the 2, 6-dimethylphenol, the sodium hydroxide solution and the dimethyl sulfate in the step A1 is 4.8:40:27.3, the mass fraction of the sodium hydroxide solution is 25%, the mass ratio of the intermediate 1, the deionized water and the potassium permanganate is 1.8g:50mL:4.5g, and the mass ratio of the intermediate 2, the methanol and the concentrated sulfuric acid is 0.25mol:0.25mol:10 mL.
5. The process for manufacturing a surgical cap material according to claim 3, wherein: the molar ratio of the intermediate 3, the dimethylaminoethanol, the hydroquinone and the tetrabutyl titanate in the step A2 is 5:15:0.04:0.3, the molar ratio of the intermediate 4, the acetonitrile, the hydroquinone and the bromohexadecane is 0.055mol:30mL:0.004mol:0.05mol, the molar ratio of the intermediate 5 and the boron tribromide is 1g:3mL, and the molar ratio of the cyanuric chloride, the intermediate 6 and the sodium acetate is 0.25mol:0.25mol:0.3 g.
6. The process for manufacturing a surgical cap material according to claim 3, wherein: the dosage ratio of the 5, 5-dimethylhydantoin, the potassium carbonate, the acetone and the 1, 3-dibromopropane in the step A3 is 3.05g to 12.07g, 200mL to 13.62g, the dosage ratio of the ciprofloxacin, the intermediate 8, the triethylamine, the potassium iodide, the tetrabutyl, the dichloromethane and the ethanol is 6mmol to 6.5mmol to 6mmol to 0.1g to 30mL to 10mL, and the dosage ratio of the intermediate 7, the intermediate 9 and the sodium acetate is 0.5mol to 1 g.
7. The process for manufacturing a surgical cap material according to claim 3, wherein: the using amount ratio of the graphite powder, the sodium nitrate, the concentrated sulfuric acid, the potassium permanganate, the deionized water and the hydrogen peroxide in the step A4 is 1g to 0.5g to 25mL to 3g to 20mL to 10mL, the mass fraction of the concentrated sulfuric acid is 80%, and the mass fraction of the hydrogen peroxide is 25%.
8. The process for manufacturing a surgical cap material according to claim 3, wherein: the dosage ratio of the chitosan to the acetic acid solution in the step A5 is 1g to 100mL, the mass fraction of the acetic acid solution is 1%, the dosage ratio of the graphene oxide to the deionized water is 1g to 50mL, and the dosage ratio of the chitosan colloidal solution, the graphene oxide colloidal solution, the magnesium carbonate, the butyl titanate, the ethanol, the deionized water, the silver nitrate solution, the ethylenediamine, the 1-hydroxybenzotriazole and the intermediate 10 is 100mL to 1g to 15mL to 10mL to 50mL to 12mL to 2.5 g.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512331A (en) * | 2021-07-27 | 2021-10-19 | 浙江精筑环保科技有限公司 | Mildew-proof and bacteria-removing coating and preparation method thereof |
| CN113862854A (en) * | 2021-11-04 | 2021-12-31 | 江苏金銮纺织科技股份有限公司 | Production process of antibacterial nanofiber yarn |
| CN115679547A (en) * | 2022-09-08 | 2023-02-03 | 河南省安邦卫材有限公司 | Antibacterial non-woven fabric for preparing protective clothing |
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2021
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512331A (en) * | 2021-07-27 | 2021-10-19 | 浙江精筑环保科技有限公司 | Mildew-proof and bacteria-removing coating and preparation method thereof |
| CN113862854A (en) * | 2021-11-04 | 2021-12-31 | 江苏金銮纺织科技股份有限公司 | Production process of antibacterial nanofiber yarn |
| CN115679547A (en) * | 2022-09-08 | 2023-02-03 | 河南省安邦卫材有限公司 | Antibacterial non-woven fabric for preparing protective clothing |
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Application publication date: 20210511 |