CN111608011B - Preparation method of high-permeability and bacterium-resistant type dialysis base paper - Google Patents

Preparation method of high-permeability and bacterium-resistant type dialysis base paper Download PDF

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CN111608011B
CN111608011B CN202010357638.6A CN202010357638A CN111608011B CN 111608011 B CN111608011 B CN 111608011B CN 202010357638 A CN202010357638 A CN 202010357638A CN 111608011 B CN111608011 B CN 111608011B
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paper
pulp
mass
drying
berberine
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CN111608011A (en
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黄学英
戴贤中
周晓光
张�诚
刘祥波
孙兵
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Xianhe Co ltd
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
    • D21F1/00—Wet end of machines for making continuous webs of paper
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
    • D21F3/00—Press section of machines for making continuous webs of paper
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
    • D21F5/00—Dryer section of machines for making continuous webs of paper
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/18—Reinforcing agents
    • D21H21/20—Wet strength agents
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
    • D21H25/04—Physical treatment, e.g. heating, irradiating
    • D21H25/06—Physical treatment, e.g. heating, irradiating of impregnated or coated paper

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Abstract

The invention relates to the technical field of papermaking, and discloses a preparation method of high-permeability and high-resistance bacteria type dialysis base paper, which comprises the following steps of (1) pulping: the pulp comprises 70-80% of bleached natural softwood pulp and 20-30% of bleached hardwood pulp; (2) modifying the slurry: adding modified berberine with the mass of 15-25% of the slurry into the slurry, stirring and reacting at 60-70 ℃ for 30-60 min, adding a PAE wet strength agent, intra-slurry glue and AKD, and stirring uniformly to obtain modified slurry; (3) manufacturing paper with pulp; (4) squeezing and pre-drying; (5) and (3) obtaining the high-permeability bacteria-resistant dialysis base paper after surface sizing, drying and calendaring. According to the invention, the modified berberine is used for modifying the paper pulp fibers in the pulping process, so that the original hydrogen bond structure between the fibers can be reduced, the air permeability of the paper sheet is improved, the bacteria-resistant effect of the paper sheet can be improved through the antibacterial property of the berberine, and the prepared dialysis base paper can have high air permeability and bacteria resistance.

Description

Preparation method of high-permeability and bacterium-resistant type dialysis base paper
Technical Field
The invention relates to the technical field of papermaking, in particular to a preparation method of high-permeability and high-resistance bacteria type dialysis base paper.
Background
Dialysis paper is generally made into a paper-plastic bag after being coated, printed (printed with ink) and subjected to heat sealing or glue sealing with film materials such as PE or PP and the like, and is used for packaging medical instruments for sterilization, and the bacteria resistance and the air permeability are the two most important indexes. The bacteria resistance refers to the property that the dialysis paper can prevent bacteria in the external environment from permeating, so as to avoid bacterial infection in the sterilization process or after sterilization of medical instruments, and the quality of the bacteria resistance of the dialysis paper is particularly important for the effective storage of sterilized products. The air permeability is that the sterilization mode of the medical apparatus is mainly an ETO ethylene oxide sterilization method and a high-temperature damp-heat steam method, so the dialysis paper needs to have certain air permeability, ethylene oxide gas or steam is allowed to permeate, and the aim of sterilizing the medical apparatus and articles of the package is fulfilled.
In the prior art, the dialyzing paper is generally made to have bacteria-resisting property by sizing, for example, in the Chinese patent document, "a heat-seal self-adhesive type medical dialyzing paper producing method", which is disclosed in publication No. CN110939009A, comprising the following steps: crushing the slurry; pulping; preparing materials; molding on the net; squeezing and dewatering; drying and surface sizing; drying and transfer coating; calendaring and coiling; rewinding and packaging to obtain a finished product. The method can complete the production of the base paper and the adhesive layer in one step in the paper machine, and can be directly used for manufacturing the plastic bag of the medical packaging paper, thereby saving equipment, labor and transportation cost and greatly improving efficiency.
However, in the dialysis paper production process in the prior art, air permeability and bacteria resistance are two contradictory indexes, the larger the glue application amount is, the fewer the pores among the fibers are, the better the bacteria resistance is, but the air permeability is reduced at the same time. Therefore, the dialyzing paper in the prior art is difficult to have good bacteria resistance and air permeability at the same time, so that the prepared packaging material is difficult to ensure that the packaged medical instruments can be effectively sterilized and the sterilized instruments can be effectively stored.
Disclosure of Invention
The invention provides a preparation method of high-permeability and bacteria-resistant type dialysis base paper, aiming at overcoming the problems that in the production process of dialysis paper in the prior art, air permeability and bacteria resistance are two contradictory indexes, the larger the glue application amount is, the fewer the pores among fibers are, the better the bacteria resistance is, but the air permeability is reduced, and the dialysis paper is difficult to have good bacteria resistance and air permeability at the same time.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-permeability and bacterium-resistant dialysis base paper comprises the following steps:
(1) pulping: pulping and then mixing pulp to obtain pulp, wherein the pulp comprises 70-80% of bleached natural softwood pulp and 20-30% of bleached hardwood pulp;
(2) modifying the slurry: adding modified berberine with the mass of 15-25% of the slurry into the slurry, stirring and reacting at 60-70 ℃ for 30-60 min, adding a PAE wet strength agent, intra-slurry glue and AKD, and stirring uniformly to obtain modified slurry;
(3) manufacturing paper: screening the modified pulp on a net to make paper to obtain wet paper sheets;
(4) pressing and pre-drying: squeezing and pre-drying the wet paper sheet to obtain a pre-dried paper sheet;
(5) surface sizing and drying: and (3) carrying out surface sizing, drying and calendaring on the paper sheet after the paper sheet is dried by using a surface sizing agent to obtain the high-permeability and bacterium-resistant dialysis base paper.
When the dialysis paper is prepared, the proper proportion of the pulp is adopted, and the pulp is modified by using the modified berberine, so that the air permeability of the dialysis base paper can be improved, and the bacteria resistance of the paper can be ensured. The berberine is a natural quaternary ammonium alkaloid separated from traditional Chinese medicine coptis, has excellent antibacterial performance and wide antibacterial spectrum, has an antibacterial effect on various gram positive and negative bacteria in vitro, can effectively prevent bacteria in the external environment from permeating by utilizing the antibacterial performance of the berberine added into dialysis paper, and avoids causing bacterial infection in the sterilization process or after sterilization of packaged medical instruments. Meanwhile, as the berberine is a quaternary ammonium base, after the modified berberine is added into the slurry, OH in the modified berberine-Can form hydrogen bonds with the hydroxyl of cellulose molecules in the pulp through the action of the hydrogen bonds, replace the hydrogen bonds of the cellulose molecules, and simultaneously, the positively charged quaternary ammonium salt groups approach the cellulose molecules through the electrostatic action to separate the cellulose molecular chains, so that the fiber structure becomes loose, the content of fine fibers is reduced, the basic structure of the fibers is not damaged, and the permeation is effectively improvedThe air permeability of the paper ensures that ethylene oxide gas or steam can effectively permeate during sterilization, thereby achieving the purpose of sterilizing medical appliances and articles of packages.
At the same time, the mechanical properties of the paper are reduced by loosening the fiber structure, so that the PAE wet strength agent is added into the pulp to improve the mechanical properties of the paper. The PAE wet strength agent is composed of polyamide epichlorohydrin, and can be added into the pulp to crosslink with fiber to form a net structure, thereby improving the mechanical strength of the paper. After the berberine is added, quaternary ammonium salt groups of the berberine enter the space between cellulose molecular chains, and berberine molecules have no reactive groups, so that the crosslinking between PAE and fibers can be influenced.
Preferably, the preparation method of the modified berberine comprises the following steps:
A) dissolving berberine in N, N-dimethylformamide, reacting for 15-20 min under microwave radiation, adding water with the mass of 1-2 times of that of the solution, diluting, refrigerating at 0-4 ℃ for 10-20 h, filtering and drying to obtain red crystals;
B) dissolving the red crystal in N, N-dimethylformamide, adding dibromoethane and potassium carbonate, stirring and reacting for 20-24 h at 70-80 ℃ under the protection of nitrogen, adding diethyl ether, standing for 8-10 h, filtering and drying in vacuum to obtain yellow powder;
C) dissolving the yellow powder in methanol, adding supersaturated ammonium chloride and 25-28% by mass of ammonia water, carrying out sealed stirring reaction for 8-12 h at 75-85 ℃, carrying out reduced pressure evaporation on the solution after reaction, washing the product with dichloromethane, filtering, evaporating the filtrate, adding the product into 5-8% by mass of sodium hydroxide solution, carrying out stirring reaction for 1-2 h at 75-85 ℃, and evaporating the solution to dryness to obtain the modified berberine.
The invention firstly adopts the step A) to make berberine react under microwave radiation to generate berberberrubine red crystal; then reacting with dibromoethane to obtain bromoethyl berberine through the step B); and finally, the berberine is reacted with ammonia water to obtain aminoethyl modified berberine, so that amino groups are introduced to the surface of the berberine to serve as reaction groups, the berberine can react with hydroxyl groups on the surface of the fiber, chlorine in a PAE wet strength agent and other reaction groups to carry out crosslinking, and the mechanical strength of the paper sheet is improved.
Preferably, the mass-to-volume ratio of the flavonolignans to the N, N-dimethylformamide in the step A) is 1 g: (20-30 mL) and microwave power of 400-500W.
Preferably, the mass-to-volume ratio of the red crystals to the N, N-dimethylformamide in step B) is 1 g: (90-100 mL), the ratio of the dibromoethane, the potassium carbonate and the red crystal added is (10-15 mL): (0.5-0.6 g): 1g, the volume ratio of the added diethyl ether to the N, N-dimethylformamide is (2-3): 1.
preferably, the mass-to-volume ratio of the yellow powder to the methanol and the ammonia water in the step C) is (12-15 g): 1mL of: (12-13 mL), the mass-to-volume ratio of the product added into the sodium hydroxide solution to the sodium hydroxide solution is 1 g: (20-50 mL).
Preferably, in the step (1), the beating degree of the bleached softwood pulp is 21-25 DEG SR, the wet weight is 10-12 g, the beating degree of the bleached hardwood pulp is 30-35 DEG SR, and the wet weight is 2.0-4.0 g.
Preferably, the sizing agent in the step (2) is cationic starch, and the dosage of each ton of paper is 5-10 kg; the solid content of the PAE wet strength agent is 12-15%, the dosage of each ton of paper is 10-15 kg, and the dosage of AKD each ton of paper is 10-20 kg.
Preferably, the moisture content of the paper sheet after the pre-drying in the step (4) is 5-8%.
Preferably, the surface sizing agent raw material in the step (5) comprises a raw material with a mass ratio of 1: (5-6) the cassava starch and the PVA, wherein the mass concentration of the PVA in the surface sizing agent is 1-3%, and the sizing amount is 1-2 g/m2。
Therefore, the invention has the following beneficial effects:
(1) the modified berberine is used for modifying the slurry, so that bacteria in the external environment can be effectively prevented from permeating by utilizing the antibacterial performance of the berberine, and bacterial infection of packaged medical equipment in the sterilization process or after sterilization is avoided;
(2) because berberine is a quaternary ammonium base, the OH in berberine is added into the slurry-Hydrogen bonds can be formed with hydroxyl groups of cellulose molecules in the pulp through the action of the hydrogen bonds to replace the hydrogen bonds of the cellulose molecules, and meanwhile, the positively charged quaternary ammonium salt groups approach the cellulose molecules through the electrostatic action to separate the cellulose molecular chains, so that the fiber structure becomes loose, the content of fine fibers is reduced, and the air permeability of the dialyzing paper is effectively improved;
(3) the berberine is modified, and the amine group is introduced to the surface of the berberine to serve as a reaction group, so that the berberine can react with the fiber and the reaction group in the PAE wet strength agent to carry out co-crosslinking, the influence on crosslinking between the PAE and the fiber after the berberine is added is avoided, and the mechanical strength of the paper sheet is improved.
Detailed Description
The invention is further described with reference to specific embodiments.
The reagents used in the present invention are commercially available or commonly used in the art unless otherwise specified.
Example 1:
a preparation method of high-permeability and bacterium-resistant dialysis base paper comprises the following steps:
(1) pulping: pulping and then mixing pulp to obtain pulp, wherein the pulp comprises 75% of bleached natural color softwood pulp and 25% of bleached hardwood pulp, the beating degree of the bleached natural color softwood pulp is 22 DEG SR, the wet weight is 11g, the beating degree of the bleached hardwood pulp is 32 DEG SR, and the wet weight is 3.0 g;
(2) modifying the slurry: adding modified berberine with the mass of 20% of the pulp into the pulp, stirring and reacting for 40min at 65 ℃, adding 12kg of PAE wet strength agent (with the solid content of 15%) per ton of paper, 8kg of cationic starch and 15kg of AKD, and uniformly stirring to obtain modified pulp;
the preparation method of the modified berberine comprises the following steps:
A) dissolving berberine in N, N-dimethylformamide, wherein the mass-volume ratio of the berberine to the N, N-dimethylformamide is 1 g: reacting for 18min under 450W microwave radiation by 25mL, adding water with the mass of 1.5 times of that of the solution, diluting, refrigerating at 4 ℃ for 12h, filtering and drying to obtain red crystals;
B) dissolving the red crystal in N, N-dimethylformamide, wherein the mass-volume ratio of the red crystal to the N, N-dimethylformamide is 1 g: 95mL, adding 12mL of red crystal: 0.55 g: 1g of dibromoethane and potassium carbonate, stirring and reacting for 22h at 75 ℃ under the protection of nitrogen, and adding the mixture to N, N-dimethylformamide in a volume ratio of 2.5: 1, standing for 9 hours, filtering and drying in vacuum to obtain yellow powder;
C) dissolving the yellow powder in methanol, adding supersaturated ammonium chloride and 28% ammonia water by mass, wherein the mass-volume ratio of the yellow powder to the methanol and the ammonia water is 13 g: 1mL of: 12.5mL, reacting for 10h under sealed stirring at 80 ℃, drying the reacted solution under reduced pressure, washing the product with dichloromethane, filtering, drying the filtrate by distillation, adding the obtained product into a sodium hydroxide solution with the mass fraction of 6%, reacting for 1.5h under stirring at 80 ℃, and drying the solution by distillation to obtain the modified berberine;
(3) manufacturing paper: screening the modified pulp on a net to make paper to obtain wet paper sheets;
(4) pressing and pre-drying: squeezing and pre-drying the wet paper to obtain a pre-dried paper sheet, wherein the moisture content of the pre-dried paper sheet is 6.2%;
(5) surface sizing and drying: carrying out film transfer surface sizing on the paper sheet after the paper sheet is dried by using a surface sizing agent, wherein the surface sizing agent comprises the following raw materials in mass ratio of 1: 5.5 of cassava starch and PVA, wherein the mass concentration of the PVA in the surface sizing agent is 2 percent, and the sizing amount is 1.5g/m2And drying and calendaring the sized paper to obtain the high-permeability bacteria-resistant dialysis base paper.
Example 2:
(1) pulping: pulping and then mixing pulp to obtain pulp, wherein the pulp comprises 70% of bleached natural color softwood pulp and 30% of bleached hardwood pulp, the beating degree of the bleached natural color softwood pulp is 21 DEG SR, the wet weight is 10g, the beating degree of the bleached hardwood pulp is 30 DEG SR, and the wet weight is 2.0 g;
(2) modifying the slurry: adding modified berberine with the mass of 15% of the pulp into the pulp, stirring and reacting for 30min at 60 ℃, adding 10kg of PAE wet strength agent (with the solid content of 12%) with the dosage of 10kg per ton of paper, 5kg of cationic starch and 20kg of AKD, and uniformly stirring to obtain modified pulp;
the preparation method of the modified berberine comprises the following steps:
A) dissolving berberine in N, N-dimethylformamide, wherein the mass-volume ratio of the berberine to the N, N-dimethylformamide is 1 g: 20mL, reacting for 20min under 400W microwave radiation, adding water with the mass of 1 time of that of the solution, diluting, refrigerating at 0 ℃ for 10h, filtering and drying to obtain red crystals;
B) dissolving the red crystal in N, N-dimethylformamide, wherein the mass-volume ratio of the red crystal to the N, N-dimethylformamide is 1 g: 90mL, adding 10mL of red crystal: 0.5 g: 1g of dibromoethane and potassium carbonate, stirring and reacting for 20 hours at 70 ℃ under the protection of nitrogen, and adding the mixture to N, N-dimethylformamide in a volume ratio of 2: 1, standing for 8 hours, filtering and drying in vacuum to obtain yellow powder;
C) dissolving the yellow powder in methanol, adding supersaturated ammonium chloride and 25% by mass of ammonia water, wherein the mass-volume ratio of the yellow powder to the methanol to the ammonia water is 12 g: 1mL of: 12mL, hermetically stirring and reacting at 75 ℃ for 8h, evaporating the solution after reaction under reduced pressure, washing the product with dichloromethane, filtering, evaporating the filtrate to dryness, adding the obtained product into a sodium hydroxide solution with the mass fraction of 5%, stirring and reacting at 75 ℃ for 1h, and evaporating the solution to dryness to obtain the modified berberine;
(3) manufacturing paper: screening the modified pulp on a net to make paper to obtain wet paper sheets;
(4) pressing and pre-drying: squeezing and pre-drying the wet paper to obtain a pre-dried paper sheet, wherein the moisture content of the pre-dried paper sheet is 5.1%;
(5) surface sizing and drying: carrying out film transfer surface sizing on the paper sheet after the paper sheet is dried by using a surface sizing agent, wherein the surface sizing agent comprises the following raw materials in mass ratio of 1: 5 cassava starch and PVA, the PVA mass concentration in the surface sizing agent is 1 percent, and the sizing amount is 1g/m2And drying and calendaring the sized paper to obtain the high-permeability bacteria-resistant dialysis base paper.
Example 3:
(1) pulping: pulping and then mixing pulp to obtain pulp, wherein the pulp comprises 80% of bleached natural color softwood pulp and 20% of bleached hardwood pulp, the beating degree of the bleached natural color softwood pulp is 25 DEG SR, the wet weight is 12g, the beating degree of the bleached hardwood pulp is 35 DEG SR, and the wet weight is 4.0 g;
(2) modifying the slurry: adding modified berberine with the mass of 25% of the pulp into the pulp, stirring and reacting for 60min at 70 ℃, adding 15kg of PAE wet strength agent (with the solid content of 12%) per ton of paper, 10kg of cationic starch and 10kg of AKD, and uniformly stirring to obtain modified pulp;
the preparation method of the modified berberine comprises the following steps:
A) dissolving berberine in N, N-dimethylformamide, wherein the mass-volume ratio of the berberine to the N, N-dimethylformamide is 1 g: 30mL of the red crystal is reacted for 15min under 500W of microwave radiation, then water with the mass 2 times of that of the solution is added for dilution, and the mixture is refrigerated for 20h at 4 ℃, filtered and dried to obtain the red crystal;
B) dissolving the red crystal in N, N-dimethylformamide, wherein the mass-volume ratio of the red crystal to the N, N-dimethylformamide is 1 g: 100mL, adding 15mL of red crystals: 0.6 g: 1g of dibromoethane and potassium carbonate, stirring and reacting for 24 hours at 80 ℃ under the protection of nitrogen, and adding the mixture to N, N-dimethylformamide in a volume ratio of 3: 1, standing for 8 hours, filtering and drying in vacuum to obtain yellow powder;
C) dissolving the yellow powder in methanol, adding supersaturated ammonium chloride and 25% by mass of ammonia water, wherein the mass-volume ratio of the yellow powder to the methanol to the ammonia water is 15 g: 1mL of: 13mL, hermetically stirring and reacting at 85 ℃ for 12h, drying the solution after reaction under reduced pressure, washing the product with dichloromethane, filtering, drying the filtrate by distillation, adding the obtained product into a sodium hydroxide solution with the mass fraction of 8%, stirring and reacting at 85 ℃ for 2h, and drying the solution by distillation to obtain the modified berberine;
(3) manufacturing paper: screening the modified pulp on a net to make paper to obtain wet paper sheets;
(4) pressing and pre-drying: squeezing and pre-drying the wet paper to obtain a pre-dried paper sheet, wherein the moisture content of the pre-dried paper sheet is 7.8%;
(5) surface sizing and drying: carrying out film transfer surface sizing on the paper sheet after the front drying by using a surface sizing agent, wherein the surface sizing agent raw material bagThe mass ratio of the components is 1: 6 cassava starch and PVA, the PVA mass concentration in the surface sizing agent is 3 percent, and the sizing amount is 2g/m2And drying and calendaring the sized paper to obtain the high-permeability bacteria-resistant dialysis base paper.
Comparative example 1 (without addition of modified berberine):
a preparation method of dialysis base paper comprises the following steps:
(1) pulping: pulping and then mixing pulp to obtain pulp, wherein the pulp comprises 75% of bleached natural color softwood pulp and 25% of bleached hardwood pulp, the beating degree of the bleached natural color softwood pulp is 22 DEG SR, the wet weight is 11g, the beating degree of the bleached hardwood pulp is 32 DEG SR, and the wet weight is 3.0 g;
(2) adding 12kg of PAE wet strength agent (solid content is 15%) per ton of paper, 8kg of cationic starch and 15kg of AKD into the pulp, and uniformly stirring to obtain pulp for papermaking;
(3) manufacturing paper: screening the papermaking pulp to obtain wet paper sheets;
(4) pressing and pre-drying: squeezing and pre-drying the wet paper to obtain a pre-dried paper sheet, wherein the moisture content of the pre-dried paper sheet is 6.2%;
(5) surface sizing and drying: carrying out film transfer surface sizing on the paper sheet after the paper sheet is dried by using a surface sizing agent, wherein the surface sizing agent comprises the following raw materials in mass ratio of 1: 5.5 of cassava starch and PVA, wherein the mass concentration of the PVA in the surface sizing agent is 2 percent, and the sizing amount is 1.5g/m2And drying and calendaring the sized paper to obtain the dialysis base paper.
Comparative example 2 (varying the amount of modified berberine):
a preparation method of high-permeability and bacterium-resistant dialysis base paper comprises the following steps:
(1) pulping: pulping and then mixing pulp to obtain pulp, wherein the pulp comprises 75% of bleached natural color softwood pulp and 25% of bleached hardwood pulp, the beating degree of the bleached natural color softwood pulp is 22 DEG SR, the wet weight is 11g, the beating degree of the bleached hardwood pulp is 32 DEG SR, and the wet weight is 3.0 g;
(2) modifying the slurry: adding modified berberine with the mass of 30% of the pulp into the pulp, stirring and reacting for 40min at 65 ℃, adding 12kg of PAE wet strength agent (with the solid content of 15%) per ton of paper, 8kg of cationic starch and 15kg of AKD, and uniformly stirring to obtain modified pulp;
the preparation method of the modified berberine comprises the following steps:
A) dissolving berberine in N, N-dimethylformamide, wherein the mass-volume ratio of the berberine to the N, N-dimethylformamide is 1 g: reacting for 18min under 450W microwave radiation by 25mL, adding water with the mass of 1.5 times of that of the solution, diluting, refrigerating at 4 ℃ for 12h, filtering and drying to obtain red crystals;
B) dissolving the red crystal in N, N-dimethylformamide, wherein the mass-volume ratio of the red crystal to the N, N-dimethylformamide is 1 g: 95mL, adding 12mL of red crystal: 0.55 g: 1g of dibromoethane and potassium carbonate, stirring and reacting for 22h at 75 ℃ under the protection of nitrogen, and adding the mixture to N, N-dimethylformamide in a volume ratio of 2.5: 1, standing for 9 hours, filtering and drying in vacuum to obtain yellow powder;
C) dissolving the yellow powder in methanol, adding supersaturated ammonium chloride and 28% ammonia water by mass, wherein the mass-volume ratio of the yellow powder to the methanol and the ammonia water is 13 g: 1mL of: 12.5mL, reacting for 10h under sealed stirring at 80 ℃, drying the reacted solution under reduced pressure, washing the product with dichloromethane, filtering, drying the filtrate by distillation, adding the obtained product into a sodium hydroxide solution with the mass fraction of 6%, reacting for 1.5h under stirring at 80 ℃, and drying the solution by distillation to obtain the modified berberine;
(3) manufacturing paper: screening the modified pulp on a net to make paper to obtain wet paper sheets;
(4) pressing and pre-drying: squeezing and pre-drying the wet paper to obtain a pre-dried paper sheet, wherein the moisture content of the pre-dried paper sheet is 6.2%;
(5) surface sizing and drying: carrying out film transfer surface sizing on the paper sheet after the paper sheet is dried by using a surface sizing agent, wherein the surface sizing agent comprises the following raw materials in mass ratio of 1: 5.5 of cassava starch and PVA, wherein the mass concentration of the PVA in the surface sizing agent is 2 percent, and the sizing amount is 1.5g/m2And drying and calendaring the sized paper to obtain the high-permeability bacteria-resistant dialysis base paper.
Comparative example 3 (no berberine modification):
a preparation method of high-permeability and bacterium-resistant dialysis base paper comprises the following steps:
(1) pulping: pulping and then mixing pulp to obtain pulp, wherein the pulp comprises 75% of bleached natural color softwood pulp and 25% of bleached hardwood pulp, the beating degree of the bleached natural color softwood pulp is 22 DEG SR, the wet weight is 11g, the beating degree of the bleached hardwood pulp is 32 DEG SR, and the wet weight is 3.0 g;
(2) modifying the slurry: adding berberine accounting for 20% of the mass of the pulp into the pulp, stirring and reacting for 40min at 65 ℃, adding 12kg of PAE wet strength agent (with solid content of 15%) per ton of paper, 8kg of cationic starch and 15kg of AKD, and uniformly stirring to obtain modified pulp;
(3) manufacturing paper: screening the modified pulp on a net to make paper to obtain wet paper sheets;
(4) pressing and pre-drying: squeezing and pre-drying the wet paper to obtain a pre-dried paper sheet, wherein the moisture content of the pre-dried paper sheet is 6.2%;
(5) surface sizing and drying: carrying out film transfer surface sizing on the paper sheet after the paper sheet is dried by using a surface sizing agent, wherein the surface sizing agent comprises the following raw materials in mass ratio of 1: 5.5 of cassava starch and PVA, wherein the mass concentration of the PVA in the surface sizing agent is 2 percent, and the sizing amount is 1.5g/m2And drying and calendaring the sized paper to obtain the high-permeability bacteria-resistant dialysis base paper.
The properties of the dialysis base papers obtained in the above examples and comparative examples were measured, and the results are shown in table 1.
Table 1: and (5) testing the performance of the dialysis base paper.
Figure BDA0002474023100000081
(wherein, the bacterium resistance is detected by adopting an agar contact attack test method according to ISO11607-2006 and DIN58953-6-1987, and the specific steps are as follows:
(1) culturing bacillus subtilis strains: 3g of beef extract, 5g of peptone, 5g of sodium chloride, 15g of agar, 1000mL of distilled water and 5mg of MnSO4·H2Adjusting the pH value to 7.0 by O, and culturing for 24 h);
(2) diluting the cultured strain to 107cfu/mL for later use;
(3) cutting the prepared dialyzing paper into square paper patterns with the side length of 50mm, and sterilizing for later use (5 paper patterns in each group are used as parallel samples);
(4) transferring the sterilized dialyzing paper to a sterile plate, and taking 0.5mL of 107Uniformly dripping cfu/mL bacillus subtilis solution on the outer surface of the dialyzing paper, and drying for 10 hours at the temperature of 25 ℃ and under the relative humidity of 45%;
(5) spreading the inner surface of the dried bacteria-contaminated sample paper on the surface of an agar culture medium, and discarding the sample paper after 5-6 s; the nutrient medium is cultured for 24h at 37 ℃, and the growth condition of the bacteria is observed. )
As can be seen from Table 1, the dialysis base papers prepared by the method of the present invention in examples 1 to 3 are good in air permeability, bacteria resistance and mechanical properties; in the comparative example 1, the pulp is not modified by the modified berberine, so that the air permeability and the bacteria resistance of the prepared dialysis paper are reduced, and the modified berberine is proved to be capable of effectively improving the air permeability and the bacteria resistance of the paper; the addition amount of the modified berberine in the comparative example 2 is beyond the range of the invention, the mechanical property of the dialyzing paper is obviously reduced, the use requirement is not met, probably because the cellulose is dissolved when the addition amount of the modified berberine is too much, and the cellulose structure is damaged; in comparative example 3, the mechanical properties of berberine were not modified and decreased, demonstrating that the addition of berberine affects the mechanical properties of paper.

Claims (8)

1. A preparation method of high-permeability bacteria-resistant dialysis base paper is characterized by comprising the following steps:
(1) pulping: pulping and then mixing pulp to obtain pulp, wherein the pulp comprises 70-80% of bleached natural softwood pulp and 20-30% of bleached hardwood pulp;
(2) modifying the slurry: adding modified berberine with the mass of 15-25% of the slurry into the slurry, stirring and reacting at 60-70 ℃ for 30-60 min, adding a PAE wet strength agent, intra-slurry glue and AKD, and stirring uniformly to obtain modified slurry;
(3) manufacturing paper: screening the modified pulp on a net to make paper to obtain wet paper sheets;
(4) pressing and pre-drying: squeezing and pre-drying the wet paper sheet to obtain a pre-dried paper sheet;
(5) surface sizing and drying: carrying out surface sizing, drying and calendaring on the paper sheet after the paper sheet is dried by using a surface sizing agent to obtain the high-permeability bacteria-resistant dialysis base paper;
the preparation method of the modified berberine comprises the following steps:
A) dissolving berberine in N, N-dimethylformamide, reacting for 15-20 min under microwave radiation, adding water with the mass of 1-2 times of that of the solution, diluting, refrigerating at 0-4 ℃ for 10-20 h, filtering and drying to obtain red crystals;
B) dissolving the red crystal in N, N-dimethylformamide, adding dibromoethane and potassium carbonate, stirring and reacting for 20-24 h at 70-80 ℃ under the protection of nitrogen, adding diethyl ether, standing for 8-10 h, filtering and drying in vacuum to obtain yellow powder;
C) dissolving the yellow powder in methanol, adding supersaturated ammonium chloride and 25-28% by mass of ammonia water, carrying out sealed stirring reaction for 8-12 h at 75-85 ℃, carrying out reduced pressure evaporation on the solution after reaction, washing the product with dichloromethane, filtering, evaporating the filtrate, adding the product into 5-8% by mass of sodium hydroxide solution, carrying out stirring reaction for 1-2 h at 75-85 ℃, and evaporating the solution to dryness to obtain the modified berberine.
2. The preparation method of the dialysis base paper with high permeability and bacterium resistance of claim 1, wherein the mass-to-volume ratio of the flavonolignans to the N, N-dimethylformamide in the step A) is 1 g: (20-30 mL) and microwave power of 400-500W.
3. The method for preparing the dialysis base paper with high permeability and bacteria resistance as claimed in claim 1, wherein the mass-to-volume ratio of the red crystal to the N, N-dimethylformamide in the step B) is 1 g: (90-100 mL), the ratio of the dibromoethane, the potassium carbonate and the red crystal added is (10-15 mL): (0.5-0.6 g): 1g, the volume ratio of the added diethyl ether to the N, N-dimethylformamide is (2-3): 1.
4. the preparation method of the dialysis base paper with high permeability and bacteria resistance as claimed in claim 1, wherein the mass volume ratio of the yellow powder to the methanol and the ammonia water in the step C) is (12-15 g): 1mL of: (12-13 mL), the mass-to-volume ratio of the product added into the sodium hydroxide solution to the sodium hydroxide solution is 1 g: (20-50 mL).
5. The preparation method of the high-permeability and bacteria-resistant type dialysis base paper as claimed in claim 1, wherein in the step (1), the beating degree of the bleached natural color softwood pulp is 21-25oSR, the wet weight is 10-12 g, and the beating degree of the bleached hardwood pulp is 30-35oSR, wet weight 2.0-4.0 g.
6. The method for preparing the dialysis base paper with high permeability and bacteria resistance according to claim 1 or 2, wherein the sizing agent in the step (2) is cationic starch, and the dosage of each ton of paper is 5-10 kg; the solid content of the PAE wet strength agent is 12-15%, the dosage of each ton of paper is 10-15 kg, and the dosage of AKD each ton of paper is 10-20 kg.
7. The method for preparing the dialysis base paper with high permeability and bacteria resistance as claimed in claim 1, wherein the moisture content of the paper sheet after pre-drying in the step (4) is 5-8%.
8. The method for preparing the dialysis base paper with high permeability and bacteria resistance as claimed in claim 1, wherein the surface sizing agent raw material in the step (5) comprises the following components in a mass ratio of 1: (5-6) the cassava starch and the PVA, wherein the mass concentration of the PVA in the surface sizing agent is 1-3%, and the sizing amount is 1-2 g/m2。
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