CN107974831B - Calcium alginate modified polypropylene fiber non-woven fabric and preparation method thereof - Google Patents
Calcium alginate modified polypropylene fiber non-woven fabric and preparation method thereof Download PDFInfo
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- CN107974831B CN107974831B CN201610935936.2A CN201610935936A CN107974831B CN 107974831 B CN107974831 B CN 107974831B CN 201610935936 A CN201610935936 A CN 201610935936A CN 107974831 B CN107974831 B CN 107974831B
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- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 212
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 208
- -1 polypropylene Polymers 0.000 title claims abstract description 208
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 208
- 239000000835 fiber Substances 0.000 title claims abstract description 147
- 235000010410 calcium alginate Nutrition 0.000 title claims abstract description 56
- 239000000648 calcium alginate Substances 0.000 title claims abstract description 56
- 229960002681 calcium alginate Drugs 0.000 title claims abstract description 56
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 71
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 71
- 239000000661 sodium alginate Substances 0.000 claims abstract description 71
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- LIRDHUDRLFDYAI-UHFFFAOYSA-H iron(3+);trisulfite Chemical compound [Fe+3].[Fe+3].[O-]S([O-])=O.[O-]S([O-])=O.[O-]S([O-])=O LIRDHUDRLFDYAI-UHFFFAOYSA-H 0.000 claims description 2
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- LMDZBCPBFSXMTL-UHFFFAOYSA-N 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide Chemical compound CCN=C=NCCCN(C)C LMDZBCPBFSXMTL-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
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- HTTJABKRGRZYRN-UHFFFAOYSA-N Heparin Chemical compound OC1C(NC(=O)C)C(O)OC(COS(O)(=O)=O)C1OC1C(OS(O)(=O)=O)C(O)C(OC2C(C(OS(O)(=O)=O)C(OC3C(C(O)C(O)C(O3)C(O)=O)OS(O)(=O)=O)C(CO)O2)NS(O)(=O)=O)C(C(O)=O)O1 HTTJABKRGRZYRN-UHFFFAOYSA-N 0.000 description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 229920000669 heparin Polymers 0.000 description 2
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- 235000010408 potassium alginate Nutrition 0.000 description 2
- 239000000737 potassium alginate Substances 0.000 description 2
- MZYRDLHIWXQJCQ-YZOKENDUSA-L potassium alginate Chemical compound [K+].[K+].O1[C@@H](C([O-])=O)[C@@H](OC)[C@H](O)[C@H](O)[C@@H]1O[C@@H]1[C@@H](C([O-])=O)O[C@@H](O)[C@@H](O)[C@H]1O MZYRDLHIWXQJCQ-YZOKENDUSA-L 0.000 description 2
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- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 description 1
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/13—Alginic acid or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/155—Halides of elements of Groups 2 or 12 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The application relates to a calcium alginate modified polypropylene fiber non-woven fabric and a preparation method thereof in the field of high polymer materials. The method comprises two steps of polypropylene fiber non-woven fabric grafting and calcium chloride treatment. Firstly, taking sodium alginate as a grafting monomer, initiating free radical polymerization by an initiator, and grafting the sodium alginate monomer to the surface of the polypropylene non-woven fabric. And then, washing the polypropylene fiber non-woven fabric with deionized water, soaking in a calcium chloride aqueous solution, washing with deionized water, and drying by blowing to obtain the hydrophilic polypropylene fiber non-woven fabric with the surface grafted with calcium alginate. The method for chemically grafting the calcium alginate on the surface of the polypropylene fiber non-woven fabric is adopted, so that the hydrophilicity of the polypropylene fiber non-woven fabric is more stable. The preparation method is simple in process, easy to operate and suitable for large-scale production.
Description
Technical Field
The application relates to a hydrophilic polypropylene fiber non-woven fabric in the field of high polymer materials, and further relates to a calcium alginate modified polypropylene fiber non-woven fabric and a preparation method thereof.
Background
It is a current trend to modify nonwoven fabrics with natural polymers. The natural polymer is green and environment-friendly, has no harm to the environment and human body, and is most commonly used by chitosan, alginate, heparin, protein and the like. The natural polymer contains more groups capable of associating with water molecules, such as hydroxyl, carboxyl, carbonyl, amino, amide and the like, water molecules adsorbed by the hydrophilic groups firmly lean against the natural polymer by taking hydrogen bonds as attraction to form a directly adsorbed water molecule layer, and due to the polarity of the water molecules, the water molecules in the environment can be continuously adsorbed by the water molecules to form an indirectly adsorbed water molecule layer. Shenzhouran and the like adopt chitosan solution to dip and roll the polypropylene fiber non-woven fabric, and the modified polypropylene fiber non-woven fabric has certain hydrophilicity and antibacterial property. Lirong and the like initiate grafting of acrylic acid monomers on the polypropylene fiber non-woven fabric through low-temperature plasma pretreatment, and then react with heparin after being activated by EDC ([1- (3-dimethylaminopropyl) -3-ethylcarbodiimide ]), so that the hydrophilicity and blood compatibility of the obtained polypropylene fiber non-woven fabric are obviously improved. Chinese patent with application number CN200810120076.2 discloses a non-woven fabric with antibacterial and hydrophilic properties, which is characterized in that the non-woven fabric is soaked in fibroin and chitin finishing liquid, and after two soaking and two rolling, the non-woven fabric is baked at 160 ℃ and fixed. The method can endow the non-woven fabric with good hydrophilicity and antibacterial property, but the finishing method adopted by the patent belongs to physical modification, the combination of functional groups and the polypropylene non-woven fabric is not firm, and the hydrophilicity is unstable.
Alginate is a natural polymer extracted from marine algae, has a plurality of excellent performances, for example, strong hydrophilic carboxyl groups contained in the alginate can absorb exudate of wounds, a slightly acid wet environment is favorable for neutral granulocytes in human blood to play a role in accelerating the healing of skin wound surfaces, and metal ions in the alginate can react with human bodies to form a gel layer on the skin wound surfaces to play a role in protecting the wounds, so that the alginate modified non-woven fabrics and fabrics not only have improved hydrophilicity, but also can be applied to the field of medical care.
The polypropylene fiber non-woven fabric has high tensile strength, wear resistance, good air permeability and low price, and can be used for disposable medical and sanitary cloth, such as disinfectant wet tissues, wound dressings, hemostatic patches, bandages and the like; household sanitary cloths, such as baby diapers, sanitary napkins, tableware and cookware cleaning cloths, beauty wipes, and the like; in addition, the fabric can also be used in the fields of home decoration cloth, industrial cloth, sewage treatment membranes and the like. All these fields place high demands on the hydrophilicity of polypropylene nonwovens. The hydrophilic modification method of the polypropylene fiber non-woven fabric mainly comprises fiber macromolecular structure hydrophilization, graft copolymerization, hydrophilic finishing, porous structure, surface roughening and the like. The hydrophilic functional group is classified into a physical method in which van der waals force is combined and a chemical method in which chemical reaction occurs, according to the bond and property of the hydrophilic functional group to the polypropylene fiber matrix. The physical method has the advantages of flexibility, convenience and simple operation, but the hydrophilic agent and the polypropylene fiber non-woven fabric are physically combined, the binding force is weaker, the hydrophilic durability is poor, hydrophilic functional groups are easy to fall off after the polypropylene fiber non-woven fabric is used or washed, and the hydrophilicity is greatly reduced. The chemical hydrophilic modification can ensure that the polypropylene fiber non-woven fabric keeps a lasting hydrophilic effect and the hydrophilic performance is more stable. Most hydrophilic functional monomers used in the existing polypropylene chemical hydrophilic modification method are acrylic acid, polyethylene glycol, polyvinyl alcohol, polyether, vinyl pyrrolidone and the like, and compared with natural high-molecular alginate, the monomers have certain pollution to the environment, and in the prior art, the existing alginate hydrophilic modification of polypropylene mostly adopts a physical method.
The polypropylene fiber non-woven fabric is coated with polyvinyl alcohol crosslinked by glutaraldehyde such as Zhang wenqi to obtain the highly hydrophilic polypropylene fiber non-woven fabric which can be used in the field of sewage treatment membranes. The von ran adopts an atom transfer radical polymerization method, a layer of hydrophilic vinyl pyrrolidone is covered on the surface of polypropylene fiber non-woven fabric to prepare the sewage treatment membrane, the structure of the membrane is not changed, the hydrophilicity is improved, and the pollution resistance is obviously improved. Chinese patent application No. cn201120008896.x provides a hydrophilic non-woven fabric, specifically, 5% wt of hydrophilic agent solution is heated and then coated on the non-woven fabric, and then dried at high speed to form the fabric, the hydrophilic non-woven fabric is suitable for the medical health field with higher requirement on water absorbability. The method belongs to a physical method, and has the disadvantages that the hydrophilicity of the polypropylene nonwoven fabric is gradually lost with the time of use, and the hydrophilic agent adopted by the patent is particularly the model PHP37 manufactured by US manufacturers, and the preparation process of the hydrophilic agent is not disclosed in the patent. Chinese patent No. CN200910194726.2 provides a hydrophilic modification method suitable for polypropylene nonwoven fabrics, which comprises immersing nonwoven fabrics in an aqueous solution containing a water-soluble crosslinking agent and persulfate, and irradiating with ultraviolet light to obtain hydrophilic polypropylene nonwoven fabrics.
The Chinese patent with the application number of CN201310473945.0 provides a method for preparing constant-temperature non-woven fabric for sanitary products, which comprises the following steps: the polypropylene fiber non-woven fabric is coated with a microcapsule finishing liquid containing sodium alginate and chitosan on the surface and then dried at 75-85 ℃ to obtain the polypropylene fiber non-woven fabric, the sodium alginate and the chitosan endow the polypropylene fiber non-woven fabric with air permeability and skin-friendly hydrophilicity, and the human body feels constant temperature and comfortable feeling by absorbing water evaporated from the skin to disperse heat. However, the method belongs to a physical modification method, and no chemical bonding exists between the polypropylene non-woven fabric and the microcapsule finishing agent, so when the polypropylene non-woven fabric is subjected to external force or the service life of the polypropylene non-woven fabric is prolonged, functional microcapsule particles can be separated from the surface of the polypropylene non-woven fabric, and the hydrophilic function is lost. Chinese patent 201110120855.4 discloses a method for manufacturing a film containing alginate membrane, which comprises soaking a polypropylene nonwoven fabric in an aqueous solution of sodium alginate and potassium alginate to uniformly coat a layer of sodium alginate or potassium alginate on the surface, and then spraying a layer of salt solution containing divalent metal ions such as calcium ions on the surface of the nonwoven fabric by spraying. The method aims to make an alginate gel layer for use in the field of dressings and facial masks, and the soaking and spraying method adopted in this patent is a physical coating method. The surface of the polypropylene fiber non-woven fabric is not provided with groups which can form bonds with the alginate functional layer, so that the polypropylene fiber non-woven fabric and the alginate functional layer are only combined by physical force, and the alginate functional layer is easy to fall off in the using process.
Disclosure of Invention
In order to solve the problems in the prior art, the application provides a calcium alginate modified polypropylene fiber non-woven fabric. In particular to a calcium alginate modified polypropylene fiber non-woven fabric and a preparation method thereof. Namely, a polypropylene fiber non-woven fabric with a surface layer grafted with calcium alginate and a method for chemically grafting calcium alginate on the surface layer of the polypropylene fiber non-woven fabric. Compared with the existing hydrophilic modified polypropylene fiber non-woven fabric, the hydrophilic modified polypropylene fiber non-woven fabric solves the problem of unstable hydrophilicity of the polypropylene fiber non-woven fabric. The method of chemically grafting calcium alginate on the surface of the polypropylene non-woven fabric is adopted, so that the polypropylene non-woven fabric is more stable in hydrophilicity. The method has the advantages that the chemical initiator is adopted, the polypropylene non-woven fabric is fully soaked in the initiator solution, and the initiator fully acts on the surface of the polypropylene non-woven fabric to generate a large amount of free radicals. The alginate functional layer and the polypropylene fiber are combined by chemical bonds, and the alginate functional layer is not easy to fall off in the using process and has a lasting hydrophilic function. In addition, the hydrophilic functional layer of this application is calcium alginate, and calcium alginate belongs to natural macromolecular material, and green is harmless to environment and human body.
The application aims to provide a calcium alginate modified polypropylene fiber non-woven fabric and a preparation method thereof. The calcium alginate modified polypropylene fiber non-woven fabric is a polypropylene fiber non-woven fabric with the surface grafted with calcium alginate.
The calcium alginate modified polypropylene fiber non-woven fabric can be prepared by a preparation method comprising the following steps: the preparation method comprises the steps of taking sodium alginate as a grafting monomer, initiating the grafting reaction of the sodium alginate on the polypropylene fiber non-woven fabric by an initiator, dipping by using a calcium chloride aqueous solution, and drying to obtain the polypropylene fiber non-woven fabric.
Specifically, the preparation method of the calcium alginate modified polypropylene fiber non-woven fabric comprises two steps of a polypropylene fiber non-woven fabric grafting process and a calcium chloride treatment:
(1) polypropylene nonwoven grafting process:
dissolving a certain amount of sodium alginate powder in deionized water or distilled water, stirring, and standing for a period of time to obtain a transparent sodium alginate aqueous solution; immersing the polypropylene fiber non-woven fabric into a sodium alginate aqueous solution, and soaking for 10-30 minutes at 20-90 ℃, wherein the preferable temperature is 60-90 ℃; the bath ratio range is 1: 20-1: 1000, preferably 1: 100-1: 200 of a carrier;
dissolving an initiator in deionized water or distilled water to prepare an initiator aqueous solution, wherein the concentration of the initiator aqueous solution is not required, and the initiator is completely dissolved in the water.
Pouring an initiator aqueous solution into a sodium alginate aqueous solution soaked with the polypropylene non-woven fabric, uniformly stirring, standing the solution at room temperature to 90 ℃, preferably 40 to 60 ℃, and soaking the polypropylene non-woven fabric for 6 to 12 hours; setting grafting temperature, wherein the grafting temperature ranges from 20 ℃ to 90 ℃, the preferred temperature is 60-90 ℃, and the grafting time is 2-6 hours;
(2) calcium chloride treatment: after the grafting reaction is finished, taking out the polypropylene fiber non-woven fabric, cleaning the non-woven fabric by deionized water or distilled water, placing the non-woven fabric in a calcium chloride aqueous solution, and soaking the non-woven fabric for 0.5 to 24 hours at the temperature of between 20 and 90 ℃; and taking out the polypropylene fiber non-woven fabric, washing with deionized water or distilled water, and drying by air blasting to obtain the calcium alginate modified polypropylene fiber non-woven fabric.
Wherein, the functions of the components are as follows:
sodium alginate: the grafting monomer is grafted to the polypropylene under the action of an initiator; initiator: decomposing to generate free radicals in the grafting process, and initiating the grafting reaction; deionized water or distilled water: a solvent that dissolves the solid reactant; calcium chloride: and carrying out chemical reaction with the sodium alginate grafted to the polypropylene fiber in the previous step to generate calcium alginate, so that the polypropylene fiber is finally coated with a layer of calcium alginate, and the calcium alginate is a hydrophilic functional layer.
The concentration range of the sodium alginate in the sodium alginate aqueous solution is 0.5 to 2 percent (weight fraction) of the sodium alginate aqueous solution.
The initiator is at least one of ammonium ceric nitrate, ammonium ceric nitrate-nitric acid (a composite initiator consisting of ammonium ceric nitrate and nitric acid), ammonium persulfate-sodium bisulfite (a composite initiator consisting of ammonium persulfate and sodium bisulfite), potassium persulfate-sodium bisulfite (a composite initiator consisting of potassium persulfate and sodium bisulfite), and hydrogen peroxide-ferric sulfite (a composite initiator consisting of hydrogen peroxide and ferric sulfite).
The composite initiator is a water-soluble redox composite initiator, and free radicals are generated by redox reaction of an oxidant and a reducing agent to initiate grafting reaction.
The dosage of the initiator is 0.1 to 1 weight percent of the dosage of the sodium alginate.
The concentration range of calcium chloride in the calcium chloride aqueous solution is 4-10% (weight fraction) of the calcium chloride aqueous solution.
The hydrophilic functional layer adopted by the application is calcium alginate, the substance is a natural polymer material, the affinity with a human body is good, the substance is derived from algae, and the hydrophilic functional layer is green and environment-friendly and has no harm to the environment and the human body.
The chemical grafting method adopted by the application enables the bonding force between the polypropylene and the calcium alginate to be strong and the hydrophilic performance to be durable, thereby overcoming the defects that Van der Waals force exists between the polypropylene and the alginate hydrophilic layer caused by hydrophilic modification of alginate of the polypropylene by adopting a physical method in the prior art, the bonding force is weak, the alginate functional layer is easy to fall off and lose hydrophilicity in the using process, and the hydrophilic performance is not durable.
The method comprises two steps of polypropylene fiber non-woven fabric grafting and calcium chloride treatment. Firstly, taking sodium alginate as a grafting monomer, initiating free radical polymerization by an initiator, and grafting the sodium alginate monomer to the surface of the polypropylene non-woven fabric. And then cleaning the polypropylene fiber non-woven fabric with deionized water or distilled water, soaking in a calcium chloride aqueous solution, cleaning with deionized water or distilled water, and drying by blowing to obtain the hydrophilic polypropylene fiber non-woven fabric with the surface grafted with calcium alginate. The calcium alginate modified polypropylene fiber non-woven fabric can be used in the fields of disposable medical sanitary cloth, household sanitary cloth, industrial cloth, sewage treatment membranes and the like. The method for chemically grafting the calcium alginate on the surface of the polypropylene fiber non-woven fabric is adopted, so that the hydrophilicity of the polypropylene fiber non-woven fabric is more stable. The preparation method is simple in process, easy to operate and suitable for large-scale production.
Drawings
FIG. 1 is a scanning electron micrograph (2 ten thousand times magnified) of a calcium alginate-modified polypropylene nonwoven fabric of example 1;
FIG. 2 is a scanning electron micrograph (2 ten thousand times magnified) of a polypropylene nonwoven fabric treated by the method of comparative example 1;
FIG. 3 is an X-ray energy spectrum of the calcium alginate-modified polypropylene nonwoven fabric of example 1;
FIG. 4 is an X-ray energy spectrum of the polypropylene nonwoven fabric treated by the method of comparative example 1;
as can be seen from fig. 1 and 2, the surface of the polypropylene nonwoven fabric of example 1 was coated with calcium alginate, whereas the surface of the polypropylene nonwoven fabric of comparative example 1 was smooth and no calcium alginate was found.
As can be seen from fig. 3 and 4, the X-ray spectrum of example 1 shows the element Ca, while comparative example 1 does not detect the element Ca, confirming that calcium alginate can be grafted on the surface of the polypropylene nonwoven fabric by the method of the present application.
Detailed Description
The present application is further illustrated below with reference to examples. The present application is not limited by these examples. Example 1
Dissolving 1g of sodium alginate in 100g of deionized water, magnetically stirring for 2h at room temperature, and standing for 1h to obtain a clear and transparent sodium alginate aqueous solution; cutting polypropylene fiber non-woven fabric into 100mm × 100mm, placing into the above clear and transparent sodium alginate water solution, and soaking at 40 deg.C for 30 min; the bath ratio was 1: 100. 0.006g of ammonium ceric nitrate (the content is more than or equal to 98%) is put into 50g of deionized water, stirred until the solution is transparent, poured into the sodium alginate aqueous solution soaked with the polypropylene fiber non-woven fabric, stirred uniformly and then kept stand for 12 hours at 30 ℃; starting magnetic stirring, heating the solution to 60 ℃, and reacting for 4 hours; cooling to room temperature after the reaction is finished, taking out the polypropylene fiber non-woven fabric, soaking the polypropylene fiber non-woven fabric in deionized water, fully washing the polypropylene fiber non-woven fabric, and removing the surface layer of the polypropylene fiber non-woven fabric which is not grafted with sodium alginate; and (3) soaking the polypropylene fiber non-woven fabric into 100mL of 4% calcium chloride solution with weight fraction, reacting for 1h at 40 ℃, taking out, washing with deionized water, and drying by blowing at 60 ℃ to obtain the calcium alginate modified polypropylene fiber non-woven fabric.
Comparative example 1
Dissolving 1g of sodium alginate in 100g of deionized water, magnetically stirring for 2h at room temperature, and standing for 1h to obtain a clear and transparent sodium alginate solution; cutting polypropylene fiber non-woven fabric into 100mm multiplied by 100mm, putting the cut polypropylene fiber non-woven fabric into the sodium alginate solution, and soaking the cut polypropylene fiber non-woven fabric for 4 hours at the temperature of 60 ℃; then cooling to room temperature, taking out the polypropylene fiber non-woven fabric, and soaking and washing the polypropylene fiber non-woven fabric twice by using 200mL of deionized water; and then soaking the polypropylene non-woven fabric into 100mL of 4% calcium chloride solution with weight fraction at 40 ℃ for 1h, taking out, washing with deionized water, and drying by blowing at 60 ℃ to obtain the polypropylene non-woven fabric of the comparative example.
Example 2
Dissolving 1g of sodium alginate in 100g of deionized water, magnetically stirring for 2h at room temperature, and standing for 1h to obtain a clear and transparent sodium alginate aqueous solution; cutting polypropylene fiber non-woven fabric into 100mm × 100mm, placing into the above clear and transparent sodium alginate water solution, and soaking at 40 deg.C for 30 min; the bath ratio was 1: 100. 0.001g of ammonium ceric nitrate (the content is more than or equal to 98%) is put into 50g of deionized water, stirred until the solution is transparent, poured into the sodium alginate aqueous solution soaked with the polypropylene fiber non-woven fabric, stirred uniformly and then kept stand for 6 hours at 60 ℃; starting magnetic stirring, heating the solution to 60 ℃, and reacting for 6 hours; cooling to room temperature after the reaction is finished, taking out the polypropylene fiber non-woven fabric, soaking and washing the polypropylene fiber non-woven fabric by using deionized water, and removing the surface layer of the polypropylene fiber non-woven fabric which is not grafted with sodium alginate; and (3) soaking the cleaned polypropylene fiber non-woven fabric into 100mL of 4% calcium chloride solution with weight fraction, reacting for 1h at 40 ℃, taking out, cleaning with deionized water, and drying by blowing at 60 ℃ to obtain the calcium alginate modified polypropylene fiber non-woven fabric.
Example 3
Dissolving 1g of sodium alginate in 100g of deionized water, magnetically stirring for 2h at room temperature, and standing for 1h to obtain a clear and transparent sodium alginate aqueous solution; cutting polypropylene fiber non-woven fabric into 100mm × 100mm, placing into the above clear and transparent sodium alginate water solution, and soaking at 40 deg.C for 30 min; the bath ratio was 1: 100. 0.006g of ammonium ceric nitrate (the content is more than or equal to 98%) is put into 50g of deionized water, stirred until the solution is transparent, poured into the sodium alginate aqueous solution soaked with the polypropylene fiber non-woven fabric, stirred uniformly and then kept stand for 8 hours at 40 ℃; starting magnetic stirring, heating the solution to 90 ℃, and reacting for 3 hours; cooling to room temperature after the reaction is finished, taking out the polypropylene fiber non-woven fabric, soaking and washing the polypropylene fiber non-woven fabric by using deionized water, and removing the surface layer of the polypropylene fiber non-woven fabric which is not grafted with sodium alginate; and (3) soaking the cleaned polypropylene fiber non-woven fabric into 100mL of 4% calcium chloride solution by weight, reacting for 1h at 40 ℃, taking out, cleaning with deionized water, and drying by blowing at 60 ℃ to obtain the calcium alginate modified polypropylene fiber non-woven fabric.
Example 4
Dissolving 1g of sodium alginate in 100g of deionized water, magnetically stirring for 2h at room temperature, and standing for 1h to obtain a clear and transparent sodium alginate aqueous solution; cutting polypropylene fiber non-woven fabric into 100mm × 100mm, placing into the above clear and transparent sodium alginate water solution, and soaking at 40 deg.C for 30 min; the bath ratio was 1: 100. 0.006g of ammonium persulfate (the content is more than or equal to 99 percent) is taken and put into 50g of deionized water, stirred until the solution is transparent, poured into the sodium alginate aqueous solution soaked with the polypropylene fiber non-woven fabric, stirred uniformly and then kept stand for 6 hours at 90 ℃; starting magnetic stirring, heating the solution to 60 ℃, and reacting for 4 hours; cooling to room temperature after the reaction is finished, taking out the polypropylene fiber non-woven fabric, soaking and washing the polypropylene fiber non-woven fabric by using deionized water, and removing the surface layer of the polypropylene fiber non-woven fabric which is not grafted with sodium alginate; and (3) soaking the cleaned polypropylene fiber non-woven fabric into 100mL of 4% calcium chloride solution with weight fraction, reacting for 1h at 40 ℃, taking out, cleaning with deionized water, and drying by blowing at 60 ℃ to obtain the calcium alginate modified polypropylene fiber non-woven fabric.
Example 5
Dissolving 2g of sodium alginate in 100g of deionized water, magnetically stirring for 2h at room temperature, and standing for 1h to obtain a clear and transparent sodium alginate aqueous solution; cutting polypropylene fiber non-woven fabric into 100mm × 100mm, placing into the above clear and transparent sodium alginate water solution, and soaking at 40 deg.C for 30 min; the bath ratio was 1: 100. 0.01g of ammonium ceric nitrate (the content is more than or equal to 98%) is put into 50g of deionized water, stirred until the solution is transparent, poured into the sodium alginate aqueous solution soaked with the polypropylene fiber non-woven fabric, stirred uniformly and then kept stand for 12 hours at 25 ℃; starting magnetic stirring, heating the solution to 60 ℃, and reacting for 4 hours; cooling to room temperature after the reaction is finished, taking out the polypropylene fiber non-woven fabric, soaking and washing the polypropylene fiber non-woven fabric by using deionized water, and removing the surface layer of the polypropylene fiber non-woven fabric which is not grafted with sodium alginate; and (3) soaking the cleaned polypropylene fiber non-woven fabric into 100mlL 4% calcium chloride solution by weight fraction, reacting for 1h at 40 ℃, taking out, cleaning with deionized water, and drying by blowing at 60 ℃ to obtain the calcium alginate modified polypropylene fiber non-woven fabric.
Comparative example 2
Dissolving 2g of sodium alginate in 100g of deionized water, magnetically stirring for 2h at room temperature, and standing for 1h to obtain a clear and transparent sodium alginate aqueous solution; cutting polypropylene fiber non-woven fabric into 100mm × 100mm, placing into the above clear and transparent sodium alginate water solution, and soaking at 40 deg.C for 30 min; 0.01g of ammonium ceric nitrate (the content is more than or equal to 98%) is put into 50g of deionized water, stirred until the solution is transparent, poured into the sodium alginate solution soaked with the polypropylene fiber non-woven fabric, immediately started to stir by magnetic force, and the solution is heated to 60 ℃ to react for 4 hours; cooling to room temperature after the reaction is finished, taking out the polypropylene fiber non-woven fabric, soaking and washing the polypropylene fiber non-woven fabric by using deionized water, and removing the surface layer of the polypropylene fiber non-woven fabric which is not grafted with sodium alginate; and (3) soaking the cleaned polypropylene fiber non-woven fabric into 100mlL 4% calcium chloride solution by weight fraction, reacting for 1h at 40 ℃, taking out, cleaning with deionized water, and drying by blowing at 60 ℃ to obtain the calcium alginate modified polypropylene fiber non-woven fabric.
Comparative example 3
The comparative experiment was carried out according to the embodiment of chinese patent CN201310473945.0, as follows: preparing a certain amount of aqueous solution containing 2% (w/v) acetic acid and 0.6mol/L calcium chloride, namely a first mixed solution; adding 2% (w/v) chitosan with deacetylation degree of 60% into the first mixed solution, stirring thoroughly to dissolve, filtering, and standing the filtrate at room temperature overnight to obtain a second mixed solution; preparing a certain amount of 3% (w/v) sodium alginate aqueous solution, taking the aqueous solution as a water phase, and dripping 20% (v/v) paraffin and 1% (v/v) span 80 into the aqueous solution under the condition of 50 and standing for 10 minutes to obtain a water-in-oil emulsion; dropping 2500mL of the second mixed solution into 2500mL of the water-in-oil emulsion, dropping the second mixed solution into a whole-process stirring device, stirring at 600 revolutions per minute, continuing stirring for 30 minutes after dropping, and standing for 12 hours to obtain a microcapsule finishing liquid; adding 0.15% (w/v) carboxymethyl cellulose into the microcapsule finishing liquid in the last step, uniformly mixing, and attaching the mixture to the surface of a polypropylene non-woven fabric substrate in a roller coating mode at the roller speed of 90 revolutions per minute; and (3) drying the polypropylene fiber non-woven fabric substrate subjected to sizing treatment under the condition of 80 until the surface is dried to obtain the final hydrophilic polypropylene fiber non-woven fabric.
Water absorption test of polypropylene nonwoven fabric
Step 1: the polypropylene fiber nonwoven fabrics prepared in examples 1 to 5 and comparative examples 1 to 3 and the unmodified polypropylene fiber nonwoven fabrics were respectively cut into samples of 5cm × 5cm in size, the samples were left to stand at 20 ± 1 ℃ under a relative humidity of 65 ± 2% for 24 hours for temperature and humidity adjustment treatment, and the weight of the samples was measured to obtain a dry weight w1(g) In that respect And 2, step 2: placing the sample into a glass dish with the diameter of 15cm and containing 50mL of deionized water, placing the sample for 30 minutes at 20 ℃ under 1 standard atmosphere, clamping the sample by using tweezers, hanging the sample in the air at one corner for 30 seconds, and measuring the wet weight w of the sample2(g) In that respect And 3, step 3: the sample is placed back in the deionized water for 24 hours, and the above operation is repeated again to measure the wet weight w of the sample3(g) In that respect The water absorption of the sample per unit mass is (w)n-w1)/w1(n＝2，3)。
And (3) putting each polypropylene fiber non-woven fabric sample subjected to the step 1-3 into 5g/L soap solution for soaping for 5 minutes at the temperature of 40 ℃, washing with clean water, drying at the temperature of 40 ℃, and continuously repeating the step 1 and the step 3 for the water absorption test on the obtained sample.
The results are shown in Table 1.
TABLE 1 Water absorption test results of examples 1 to 5, comparative examples 1 to 3, and unmodified polypropylene nonwoven fabrics
As can be seen from table 1, compared with the unmodified polypropylene fiber nonwoven fabric, the water absorption of the modified polypropylene fiber nonwoven fabric in 30 minutes and 24 hours is improved by about 2-3 times; in comparative example 1, no initiator was added, the polypropylene nonwoven fabric was only soaked in the sodium alginate solution, and no graft polymerization reaction occurred between the polypropylene nonwoven fabric and the calcium alginate, but compared with the unmodified nonwoven fabric, the 24-hour water absorption of comparative example 1 was slightly improved, and it may be that the calcium alginate remaining between the nonwoven fabric gaps is acting; in comparative example 2, the step of soaking the polypropylene nonwoven fabric at room temperature to 90 ℃ with the initiator was not performed, so that the polypropylene nonwoven fabric had a low water absorption rate; comparative example 3 shows better water absorption result, but comparative example 3 shows significantly lower water absorption after soaping because the hydrophilicity is easily lost by the environment and external force by the physical modification method adopted in comparative example 3, and the result of water absorption of the present application is not much changed, indicating that the hydrophilic durability of the present application is better compared to comparative example 3.
Contact angle test of polypropylene nonwoven
Deionized water is used as a medium at room temperature, water drops are respectively and directly dripped on the surfaces of the polypropylene fiber non-woven fabrics and the unmodified polypropylene fiber non-woven fabrics prepared in the examples 1 to 5 and the comparative examples 1 to 3 through a needle tube, the static contact angle of the water drops is directly read and recorded through a computer measurement and calculation system, and the test result is shown in table 2.
TABLE 2 results of measuring static contact angles of examples 1 to 5, comparative examples 1 to 3 and unmodified polypropylene nonwoven fabrics
| Sample (I) | Static contact Angle [ deg ]] |
| Unmodified polypropylene non-woven fabric | 135.3 |
| Example 1 | 84.5 |
| Comparative example 1 | 105 |
| Example 2 | 86.5 |
| Example 3 | 85.3 |
| Example 4 | 84.8 |
| Example 5 | 77.2 |
| Comparative example 2 | 98.5 |
| Comparative example 3 | 85.6 |
As can be seen from table 2, the unmodified polypropylene nonwoven fabrics and comparative examples 1 to 3 have static contact angles of 135.3 degrees, 105 degrees, 98.5 degrees and 85.6 degrees, respectively, while the polypropylene nonwoven fabrics modified by the method of the present application have static contact angles of less than 90 degrees, and exhibit hydrophilicity.
X-ray energy spectrum of polypropylene nonwoven fabric
The calcium alginate-modified polypropylene nonwoven fabric prepared in example 1 and the comparative polypropylene nonwoven fabric prepared by the method of comparative example 1 were subjected to X-ray energy spectrum test analysis. The instrument used was FEI Inc., USA, NanoSEM 450 scanning electron microscope, and the results are shown in tables 3 and 4.
Table 3X-ray energy spectrum of calcium alginate modified polypropylene nonwoven fabric of example 1
| Element | Wt％ | At％ |
| C K | 86.31 | 90.78 |
| N K | 01.79 | 01.62 |
| O K | 07.64 | 06.03 |
| SiK | 01.12 | 00.51 |
| ClK | 01.80 | 00.64 |
| CaK | 01.34 | 00.42 |
Table 4X-ray energy spectrum of polypropylene nonwoven fabric prepared in comparative example 1
| Element | Wt％ | At％ |
| C K | 90.31 | 92.32 |
| N K | 04.91 | 04.30 |
| O K | 03.90 | 02.99 |
| SiK | 00.88 | 00.39 |
As can be seen from fig. 3 and 4, the X-ray energy spectrum of the calcium alginate-modified polypropylene nonwoven fabric of example 1 shows the element Ca, while the polypropylene nonwoven fabric prepared in comparative example 1 does not detect the element Ca, confirming that calcium alginate can be grafted on the surface of the polypropylene nonwoven fabric by the method of the present application.
Claims (12)
1. A calcium alginate modified polypropylene fiber non-woven fabric is characterized in that: the calcium alginate modified polypropylene fiber non-woven fabric is a polypropylene fiber non-woven fabric with the surface grafted with calcium alginate;
the calcium alginate modified polypropylene fiber non-woven fabric is prepared by a preparation method comprising the following steps: using sodium alginate as a grafting monomer, initiating the grafting reaction of the sodium alginate on the polypropylene fiber non-woven fabric by an initiator, and then performing dipping treatment and drying by using a calcium chloride aqueous solution to obtain the polypropylene fiber non-woven fabric;
the preparation method comprises the following steps:
dissolving sodium alginate in deionized water or distilled water to prepare sodium alginate aqueous solution; soaking the polypropylene fiber non-woven fabric into a sodium alginate aqueous solution for soaking;
dissolving an initiator in deionized water or distilled water to prepare an initiator aqueous solution, pouring the initiator aqueous solution into a sodium alginate aqueous solution soaked with the polypropylene non-woven fabric, uniformly stirring, standing the solution at room temperature to 90 ℃, and soaking the polypropylene non-woven fabric for 6-12 hours; then carrying out grafting reaction;
the initiator is at least one of a composite initiator consisting of ammonium ceric nitrate, ammonium ceric nitrate and nitric acid, a composite initiator consisting of ammonium persulfate, ammonium persulfate and sodium bisulfite, a composite initiator consisting of potassium persulfate, potassium persulfate and sodium bisulfite, and a composite initiator consisting of hydrogen peroxide and ferric sulfite.
2. The preparation method of the calcium alginate modified polypropylene fiber non-woven fabric as claimed in claim 1, which is characterized by comprising the following two steps of the polypropylene fiber non-woven fabric grafting process and the calcium chloride treatment:
(1) polypropylene nonwoven grafting process:
dissolving sodium alginate in deionized water or distilled water to prepare sodium alginate aqueous solution; immersing the polypropylene fiber non-woven fabric into a sodium alginate aqueous solution, and soaking at 20-90 ℃;
dissolving an initiator in deionized water or distilled water to prepare an initiator aqueous solution, pouring the initiator aqueous solution into a sodium alginate aqueous solution soaked with the polypropylene non-woven fabric, uniformly stirring, standing the solution at room temperature to 90 ℃, and soaking the polypropylene non-woven fabric for 6-12 hours; then carrying out grafting reaction;
(2) calcium chloride treatment: after the grafting reaction is finished, taking out the polypropylene fiber non-woven fabric, cleaning the polypropylene fiber non-woven fabric by deionized water or distilled water, and soaking the polypropylene fiber non-woven fabric in a calcium chloride aqueous solution; and then taking out the polypropylene fiber non-woven fabric, washing with deionized water or distilled water, and drying to obtain the calcium alginate modified polypropylene fiber non-woven fabric.
3. The preparation method of the calcium alginate modified polypropylene fiber non-woven fabric according to claim 2, which is characterized in that:
(1) and in the grafting process of the polypropylene fiber non-woven fabric, setting the soaking temperature to be 60-90 ℃.
4. The preparation method of the calcium alginate modified polypropylene fiber non-woven fabric according to claim 2, which is characterized in that:
(1) in the grafting process of the polypropylene non-woven fabric, pouring an initiator aqueous solution into a sodium alginate aqueous solution soaked in the polypropylene non-woven fabric, uniformly stirring, and standing the solution at 40-60 ℃.
5. The preparation method of the calcium alginate modified polypropylene fiber non-woven fabric according to claim 2, which is characterized in that:
(1) in the grafting process of the polypropylene fiber non-woven fabric, the grafting reaction temperature is set to be 20-90 ℃, and the grafting reaction time is 2-6 hours.
6. The preparation method of the calcium alginate modified polypropylene fiber non-woven fabric according to claim 5, wherein the preparation method comprises the following steps:
(1) and in the grafting process of the polypropylene non-woven fabric, setting the grafting reaction temperature to be 60-90 ℃.
7. The preparation method of the calcium alginate modified polypropylene fiber non-woven fabric according to claim 2, which is characterized in that:
the concentration range of the sodium alginate in the sodium alginate aqueous solution is 0.5 to 2 percent by weight of the sodium alginate aqueous solution.
8. The preparation method of the calcium alginate modified polypropylene fiber non-woven fabric according to claim 2, which is characterized in that:
(1) in the grafting process of the polypropylene fiber non-woven fabric, the polypropylene fiber non-woven fabric is immersed into a sodium alginate aqueous solution, and the bath ratio range is 1: 20-1: 1000.
9. the preparation method of the calcium alginate modified polypropylene fiber non-woven fabric according to claim 8, wherein the preparation method comprises the following steps:
the bath ratio range is 1: 100-1: 200.
10. the preparation method of the calcium alginate modified polypropylene fiber non-woven fabric according to claim 2, which is characterized in that:
the dosage of the initiator is 0.1 to 1 percent of the weight of the sodium alginate.
11. The preparation method of the calcium alginate modified polypropylene fiber non-woven fabric according to claim 2, which is characterized in that:
the concentration range of calcium chloride in the calcium chloride aqueous solution is 4-10% wt.
12. The preparation method of the calcium alginate modified polypropylene fiber non-woven fabric according to claim 2, which is characterized in that:
(2) in the calcium chloride treatment process: and after the grafting reaction is finished, taking out the polypropylene fiber non-woven fabric, cleaning the polypropylene fiber non-woven fabric by deionized water or distilled water, placing the polypropylene fiber non-woven fabric in a calcium chloride aqueous solution, and soaking the polypropylene fiber non-woven fabric for 0.5 to 24 hours at the temperature of between 20 and 90 ℃.
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| CN109235027A (en) * | 2018-10-17 | 2019-01-18 | 江苏阳光股份有限公司 | A kind of nano silver method for sorting of antibacterial wool fabric |
| CN110592808B (en) * | 2019-09-02 | 2020-11-24 | 中科纺织研究院（青岛）有限公司 | Alga modified PP spunbonded non-woven fabric |
| CN112095225A (en) * | 2020-09-16 | 2020-12-18 | 宿州衣尔雅无纺布有限公司 | Breathable dry non-woven fabric and production method thereof |
| CN112941926B (en) * | 2021-01-28 | 2022-05-27 | 美高怡生生物技术(北京)有限公司 | Calcium alginate-sodium polyacrylate modified composite membrane and preparation method thereof |
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