CN117569007A - High-cleanness non-stimulation cotton soft towel and preparation method thereof - Google Patents

High-cleanness non-stimulation cotton soft towel and preparation method thereof Download PDF

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Publication number
CN117569007A
CN117569007A CN202311250815.0A CN202311250815A CN117569007A CN 117569007 A CN117569007 A CN 117569007A CN 202311250815 A CN202311250815 A CN 202311250815A CN 117569007 A CN117569007 A CN 117569007A
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cotton
melt
modified
antistatic agent
irritating
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薛浩锴
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Jiangyin Yunzhi Medical Non Woven Products Co ltd
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Jiangyin Yunzhi Medical Non Woven Products Co ltd
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    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D04H1/43835Mixed fibres, e.g. at least two chemically different fibres or fibre blends
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/425Cellulose series
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4282Addition polymers
    • D04H1/4291Olefin series
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/542Adhesive fibres
    • D04H1/544Olefin series
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/56Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06CFINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
    • D06C23/00Making patterns or designs on fabrics
    • D06C23/04Making patterns or designs on fabrics by shrinking, embossing, moiréing, or crêping
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/77Treating 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 silicon or compounds thereof
    • D06M11/79Treating 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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/83Treating 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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/192Polycarboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46Compounds containing quaternary nitrogen atoms
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic

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

Abstract

The invention discloses a high-cleaning non-irritating cotton soft towel which comprises the following raw materials in parts by weight: functional cotton fibers, PP melt blown cotton; the preparation process of the functional cotton fiber comprises the following steps: adding succinic acid modified cotton fibers and an antistatic agent into a reaction kettle, and reacting to obtain antistatic agent modified cotton fibers; the preparation method comprises the steps of magnetically stirring modified silicon dioxide, triethylamine and tetrahydrofuran in a three-neck flask, adding antistatic agent modified cotton fiber at 0 ℃, then adding 4-dimethylaminopyridine, adding N, N' -dicyclohexylcarbodiimide after reaction liquid is clarified, and reacting to obtain the functional antioxidant; and the cotton soft towel has good softness, is not easy to generate stimulation when in use, and the addition of the antistatic agent can prevent the cotton soft towel from generating electrostatic stimulation when in use.

Description

High-cleanness non-stimulation cotton soft towel and preparation method thereof
Technical Field
The invention relates to the technical field of cotton soft towels, in particular to a high-cleaning non-irritating cotton soft towel and a preparation method thereof.
Background
Chinese patent CN112853615A discloses a disposable cotton soft towel and a preparation process thereof, wherein the disposable cotton soft towel comprises wood pulp fibers and PP melt-blown cotton as raw materials, the wood pulp fibers and the PP melt-blown cotton are mixed and formed, the forming process is simple, the wood pulp fibers and the PP melt-blown cotton are mutually combined by means of self viscosity in the melting process, the good liquid absorption performance of the disposable cotton soft towel is ensured in a reasonable proportion, the mechanical performance of the disposable cotton soft towel is improved, the disposable cotton soft towel is not easy to break after being immersed, and the water absorption performance is effectively improved.
In the prior art, the cotton soft towel is relatively poor in antibacterial property when in use, so that bacteria and the like are bred, the cleanliness of the cotton soft towel is affected, and the irritation exists in the use process of the cotton soft towel material, so that the use effect of a product is affected.
Disclosure of Invention
The invention aims to provide a high-cleaning non-irritating cotton soft towel and a preparation method thereof, which solve the following technical problems: when the cotton soft towel is used, bacteria and the like are bred due to relatively poor antibacterial performance, so that the cleanliness of the cotton soft towel is affected, and the material of the cotton soft towel has irritation in the use process, so that the use effect of the product is affected.
The aim of the invention can be achieved by the following technical scheme:
the high-cleanness non-irritating cotton soft towel comprises the following raw materials in parts by weight: 50-100 parts of functional cotton fiber and 10-20 parts of PP melt blown cotton;
wherein, the preparation process of the functional cotton fiber comprises the following steps:
step 1: preparing succinic acid modified cotton fibers;
step 2: mixing 2, 2-dimethylolbutyric acid, triethylamine and tetrahydrofuran under the protection of nitrogen, adding dimethylaminopropylamine and 4-dimethylaminopyridine at 0 ℃, stirring, adding N, N' -dicyclohexylcarbodiimide, heating to 25 ℃, reacting for 3-4h, concentrating to 1/3 of the original volume, washing, extracting and steaming to obtain an intermediate 1;
mixing the intermediate 1, 4-dibromobutane and isopropanol, carrying out reflux reaction for 4-6h, and carrying out reduced pressure distillation and recrystallization after the reaction is finished to obtain an antistatic agent;
step 3: adding succinic acid modified cotton fibers and an antistatic agent into a reaction kettle, stirring at a rotating speed of 300-500r/min, adding concentrated sulfuric acid, and reacting at a temperature of 80-90 ℃ for 2-3h to obtain antistatic agent modified cotton fibers;
step 3: mixing polysuccinimide with DMSO, adding triethylamine and silver-loaded silicon dioxide under the protection of nitrogen, stirring at 60 ℃ for reaction for 24 hours, adding unsaturated tertiary amino derivative, reacting for 14-16 hours under heat preservation, carrying out suction filtration, washing and drying a filter cake to obtain an intermediate product, stirring and reacting the intermediate product, anhydrous THF and 1, 3-propane sultone at 40 ℃ for 14-16 hours, and carrying out rotary evaporation to obtain modified silicon dioxide;
step 4: and magnetically stirring modified silicon dioxide, triethylamine and tetrahydrofuran in a three-neck flask, adding antistatic agent modified cotton fiber at 0 ℃, then adding 4-dimethylaminopyridine, adding N, N' -dicyclohexylcarbodiimide after the reaction liquid is clarified, heating to 25 ℃, and reacting for 3 hours to obtain the functional antioxidant.
As a further scheme of the invention: the preparation process of the succinic acid modified cotton fiber comprises the following steps:
placing cotton fiber in an aqueous solution containing 5.0 g per liter of anionic detergent and 2.0 g per liter of sodium carbonate at room temperature under stirring, treating for 30 minutes under boiling condition, taking out cotton fiber, washing with water for 3 times, and drying at 100deg.C to obtain pretreated cotton fiber;
the pretreated cotton fibers were modified with an aqueous solution containing succinic acid at a concentration of 11.8 grams per liter to 82.6 grams per liter and 50 grams per liter of sodium dihydrogen phosphate.
As a further scheme of the invention: the dosage ratio of 2, 2-dimethylolbutyric acid, tetrahydrofuran, dimethylaminopropylamine, 4-dimethylaminopyridine and N, N' -dicyclohexylcarbodiimide was 0.1mol:68-72mL:0.1mol:0.4-0.6g:0.3-0.5g, and the amount of triethylamine is 3-5% of the mass of the 2, 2-dihydroxymethyl butyric acid.
As a further scheme of the invention: the dosage ratio of the intermediate 1, 4-dibromobutane and isopropanol is 0.1mol l:0.05mol:68.7-72.4mL.
As a further scheme of the invention: the molar ratio of the succinic acid modified cotton fiber to the antistatic agent is 1:1.2, the amount of the concentrated sulfuric acid is 20% of the volume of the antistatic agent, and the mass fraction of the concentrated sulfuric acid is 95%.
As a further scheme of the invention: the dosage ratio of polysuccinimide, DMSO, triethylamine, silver-loaded silicon dioxide and unsaturated tertiary amino derivative is 0.3-0.5g:40-50mL:3.5-4.4mL:5.4-6.7g:2.5-3.1g, the ratio of intermediate, anhydrous THF and 1, 3-propane sultone being 3.5-4.1g:40-50mL:0.45-0.61g.
As a further scheme of the invention: controlling the mole ratio of the modified silicon dioxide, the triethylamine, the modified cotton fiber, the 4-dimethylaminopyridine and the N, N' -dicyclohexyl carbon to be 1:0.01-0.03:1:1-5:1-6.
A preparation method of a high-cleanness non-stimulation cotton soft towel comprises the following steps:
mixing the PP melt-blown cotton passing through a fiber extruder and in a melt-blown state, and then drafting the PP melt-blown cotton and the PP melt-blown cotton on a receiving device by high-pressure hot air; wherein the heating temperature of the melt-blowing die head is 160-350 ℃; wherein the melt-blowing die head assembly comprises two melt-blowing die heads, the two melt-blowing die heads are installed at an angle of 90 degrees, and the discharge port of the fiber extruder is positioned between the two melt-blowing die heads;
the receiving device adsorbs the functional cotton fibers and the PP melt-blown cotton into a net through the suction device; embossing by hot rolling bars; and the working temperature is 80-230 ℃; the high-cleanness non-irritating cotton soft towel is obtained.
The invention has the beneficial effects that:
the small-molecule antistatic agent contains a biquaternary ammonium salt structure, an F-C bond, a hydroxyl-terminated group and a long carbon chain, has amphipathy, has a skin-seeking function of an F atom, can enable the small-molecule antistatic agent to quickly migrate to the surface of a non-woven fabric, has the biquaternary ammonium salt structure and the hydroxyl-terminated group as hydrophilic groups, can absorb trace moisture in the environment, and forms a conductive layer because water is liquid with high dielectric constant; the hydroxyl of the small-molecule antistatic agent reacts with carboxyl of the succinic acid modified cotton fiber to obtain the antistatic agent modified cotton fiber, so that the surface resistance of the cotton fiber can be reduced, and the antistatic agent modified cotton fiber has good antistatic property;
the modified silicon dioxide of the invention exerts double antibacterial performance, and combines the characteristics of inorganic antibacterial agent and organic antibacterial property, wherein the inorganic antibacterial property is characterized in that the inorganic antibacterial agent can slowly release nano silver, the protein is deactivated by combining with the protein, so that the structure of cell walls is changed and the nuclear membrane is broken to cause bacterial death, the organic antibacterial property is characterized in that quaternary ammonium salt grafted on the surface of the inorganic antibacterial agent can be combined with negatively charged phospholipid on bacterial cell membranes to damage the integrity of the cell membranes, and cause the overall disturbance of the cell membranes and the leakage of intracellular liquid to cause bacterial death; on the other hand, the modified silicon dioxide plays a strong hydrophilic role, the amino group and the hydroxyl group on the surface of the modified silicon dioxide endow certain hydrophilic performance,
reacting the amino group of the modified silica with the other carboxyl group of the succinic acid modified cotton fiber to obtain the silica modified cotton fiber; the cotton fiber has good antibacterial effect and hydrophilic performance;
in conclusion, the cotton soft towel prepared from the functional cotton fibers has good antibacterial performance, so that the cotton soft towel has good cleaning performance and is not easy to produce dirt; and the cotton soft towel has good softness, is not easy to generate stimulation when in use, and the addition of the antistatic agent can prevent the cotton soft towel from generating electrostatic stimulation when in use.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The invention relates to a high-cleaning non-irritating cotton soft towel which comprises the following raw materials in parts by weight: 50 parts of functional cotton fiber and 10 parts of PP melt-blown cotton;
wherein, the preparation process of the functional cotton fiber comprises the following steps:
step 1: placing cotton fiber in an aqueous solution containing 5.0 g per liter of anionic detergent and 2.0 g per liter of sodium carbonate at room temperature under stirring, treating for 30 minutes under boiling condition, taking out cotton fiber, washing with water for 3 times, and drying at 100deg.C to obtain pretreated cotton fiber;
carrying out modification treatment on the pretreated cotton fiber by using an aqueous solution containing 11.8 g/L to 82.6 g/L succinic acid and 50 g/L sodium dihydrogen phosphate through a rolling and baking combined system to obtain succinic acid modified cotton fiber;
step 2: mixing 2, 2-dimethylolbutyric acid, triethylamine and tetrahydrofuran under the protection of nitrogen, adding dimethylaminopropylamine and 4-dimethylaminopyridine at 0 ℃, stirring, adding N, N' -dicyclohexylcarbodiimide, heating to 25 ℃, reacting for 3-4h, concentrating to 1/3 of the original volume, washing, extracting and steaming to obtain an intermediate 1;
mixing the intermediate 1, 4-dibromobutane and isopropanol, carrying out reflux reaction for 4-6h, and carrying out reduced pressure distillation and recrystallization after the reaction is finished to obtain an antistatic agent;
wherein, the dosage ratio of the 2, 2-dimethylolbutyric acid, tetrahydrofuran, dimethylaminopropylamine, 4-dimethylaminopyridine and N, N' -dicyclohexylcarbodiimide is 0.1mol:68 mL:0.1mol:0.4 g:0.3g, the amount of triethylamine is 3% of the mass of the 2, 2-dimethylolbutyric acid; the dosage ratio of the intermediate 1, 4-dibromobutane and isopropanol is 0.1mol l:0.05mol:68.7 mL;
step 3: adding succinic acid modified cotton fibers and an antistatic agent into a reaction kettle, stirring at a rotating speed of 300-500r/min, adding concentrated sulfuric acid, and reacting at a temperature of 80-90 ℃ for 2-3 hours to obtain antistatic agent modified cotton fibers (the molar ratio of the succinic acid modified cotton fibers to the antistatic agent is 1:1.2, the volume of the antistatic agent is 20%, and the mass fraction of the concentrated sulfuric acid is 95%);
step 3: mixing polysuccinimide with DMSO, adding triethylamine and silver-loaded silicon dioxide under the protection of nitrogen, stirring at 60 ℃ for reaction for 24 hours, adding unsaturated tertiary amino derivative, reacting for 14 hours under heat preservation, filtering, washing and drying a filter cake to obtain an intermediate product, stirring and reacting the intermediate product, anhydrous THF and 1, 3-propane sultone at 40 ℃ for 14 hours, and performing rotary evaporation to obtain modified silicon dioxide;
wherein the dosage ratio of polysuccinimide, DMSO, triethylamine, silver-loaded silicon dioxide and unsaturated tertiary amino derivative is 0.3g:40mL:3.5mL:5.4g:2.5g, the ratio of intermediate, anhydrous THF and 1, 3-propane sultone being 3.5g:40mL:0.45g;
step 4: magnetically stirring modified silicon dioxide, triethylamine and tetrahydrofuran in a three-neck flask, adding antistatic agent modified cotton fiber at 0 ℃, then adding 4-dimethylaminopyridine, adding N, N' -dicyclohexylcarbodiimide after the reaction liquid is clarified, heating to 25 ℃, reacting for 3 hours, concentrating the reaction liquid under reduced pressure, washing with 5% sodium bicarbonate solution and 1 mmo/L hydrochloric acid solution in molar volume, and drying with anhydrous sodium sulfate and concentrating under reduced pressure to obtain the functional antioxidant;
wherein, the mole ratio of the modified silicon dioxide, the triethylamine, the modified cotton fiber, the 4-dimethylaminopyridine and the N, N' -dicyclohexyl carbodiimide is controlled to be 1:0.01:1:1:1.
Example 2
The invention relates to a high-cleaning non-irritating cotton soft towel which comprises the following raw materials in parts by weight: 80 parts of functional cotton fiber and 15 parts of PP melt-blown cotton;
wherein, the preparation process of the functional cotton fiber comprises the following steps:
step 1: placing cotton fiber in an aqueous solution containing 5.0 g per liter of anionic detergent and 2.0 g per liter of sodium carbonate at room temperature under stirring, treating for 30 minutes under boiling condition, taking out cotton fiber, washing with water for 3 times, and drying at 100deg.C to obtain pretreated cotton fiber;
carrying out modification treatment on the pretreated cotton fiber by using an aqueous solution containing 11.8 g/L to 82.6 g/L succinic acid and 50 g/L sodium dihydrogen phosphate through a rolling and baking combined system to obtain succinic acid modified cotton fiber;
step 2: mixing 2, 2-dimethylolbutyric acid, triethylamine and tetrahydrofuran under the protection of nitrogen, adding dimethylaminopropylamine and 4-dimethylaminopyridine at 0 ℃, stirring, adding N, N' -dicyclohexylcarbodiimide, heating to 25 ℃, reacting for 3-4h, concentrating to 1/3 of the original volume, washing, extracting and steaming to obtain an intermediate 1;
mixing the intermediate 1, 4-dibromobutane and isopropanol, carrying out reflux reaction for 4-6h, and carrying out reduced pressure distillation and recrystallization after the reaction is finished to obtain an antistatic agent;
wherein, the dosage ratio of the 2, 2-dimethylolbutyric acid, tetrahydrofuran, dimethylaminopropylamine, 4-dimethylaminopyridine and N, N' -dicyclohexylcarbodiimide is 0.1mol: 70mL:0.1 mol: 0.5g:0.4g, the amount of triethylamine is 4% of the mass of the 2, 2-dimethylolbutyric acid; the dosage ratio of the intermediate 1, 4-dibromobutane and isopropanol is 0.1mol l:0.05mol: 69.4mL;
step 3: adding succinic acid modified cotton fibers and an antistatic agent into a reaction kettle, stirring at a rotating speed of 300-500r/min, adding concentrated sulfuric acid, and reacting at a temperature of 80-90 ℃ for 2-3 hours to obtain antistatic agent modified cotton fibers (the molar ratio of the succinic acid modified cotton fibers to the antistatic agent is 1:1.2, the volume of the antistatic agent is 20%, and the mass fraction of the concentrated sulfuric acid is 95%);
step 3: mixing polysuccinimide with DMSO, adding triethylamine and silver-loaded silicon dioxide under the protection of nitrogen, stirring at 60 ℃ for reaction for 24 hours, adding unsaturated tertiary amino derivative, reacting for 14-16 hours under heat preservation, carrying out suction filtration, washing and drying a filter cake to obtain an intermediate product, stirring and reacting the intermediate product, anhydrous THF and 1, 3-propane sultone at 40 ℃ for 14-16 hours, and carrying out rotary evaporation to obtain modified silicon dioxide;
wherein the dosage ratio of polysuccinimide, DMSO, triethylamine, silver-loaded silicon dioxide and unsaturated tertiary amino derivative is 0.4g:40-50mL:3.9mL:5.9g:2.8g, the ratio of intermediate, anhydrous THF and 1, 3-propane sultone being 3.9g:45mL:0.55g;
step 4: magnetically stirring modified silicon dioxide, triethylamine and tetrahydrofuran in a three-neck flask, adding antistatic agent modified cotton fiber at 0 ℃, then adding 4-dimethylaminopyridine, adding N, N' -dicyclohexylcarbodiimide after the reaction liquid is clarified, heating to 25 ℃, reacting for 3 hours, concentrating the reaction liquid under reduced pressure, washing with 5% sodium bicarbonate solution and 1 mmo/L hydrochloric acid solution in molar volume, and drying with anhydrous sodium sulfate and concentrating under reduced pressure to obtain the functional antioxidant;
wherein, the mole ratio of the modified silicon dioxide, the triethylamine, the modified cotton fiber, the 4-dimethylaminopyridine and the N, N' -dicyclohexyl carbodiimide is controlled to be 1:0.02:1:3:4.
Example 3
The invention relates to a high-cleaning non-irritating cotton soft towel which comprises the following raw materials in parts by weight: 100 parts of functional cotton fiber and 20 parts of PP melt-blown cotton;
wherein, the preparation process of the functional cotton fiber comprises the following steps:
step 1: placing cotton fiber in an aqueous solution containing 5.0 g per liter of anionic detergent and 2.0 g per liter of sodium carbonate at room temperature under stirring, treating for 30 minutes under boiling condition, taking out cotton fiber, washing with water for 3 times, and drying at 100deg.C to obtain pretreated cotton fiber;
carrying out modification treatment on the pretreated cotton fiber by using an aqueous solution containing 11.8 g/L to 82.6 g/L succinic acid and 50 g/L sodium dihydrogen phosphate through a rolling and baking combined system to obtain succinic acid modified cotton fiber;
step 2: mixing 2, 2-dimethylolbutyric acid, triethylamine and tetrahydrofuran under the protection of nitrogen, adding dimethylaminopropylamine and 4-dimethylaminopyridine at 0 ℃, stirring, adding N, N' -dicyclohexylcarbodiimide, heating to 25 ℃, reacting for 3-4h, concentrating to 1/3 of the original volume, washing, extracting and steaming to obtain an intermediate 1;
mixing the intermediate 1, 4-dibromobutane and isopropanol, carrying out reflux reaction for 4-6h, and carrying out reduced pressure distillation and recrystallization after the reaction is finished to obtain an antistatic agent;
wherein, the dosage ratio of the 2, 2-dimethylolbutyric acid, tetrahydrofuran, dimethylaminopropylamine, 4-dimethylaminopyridine and N, N' -dicyclohexylcarbodiimide is 0.1mol: 72mL:0.1mol: 0.6g:0.5g, the amount of triethylamine is 5% of the mass of the 2, 2-dimethylolbutyric acid; the dosage ratio of the intermediate 1, 4-dibromobutane and isopropanol is 0.1mol l:0.05mol: 72.4mL;
step 3: adding succinic acid modified cotton fibers and an antistatic agent into a reaction kettle, stirring at a rotating speed of 300-500r/min, adding concentrated sulfuric acid, and reacting at a temperature of 80-90 ℃ for 2-3 hours to obtain antistatic agent modified cotton fibers (the molar ratio of the succinic acid modified cotton fibers to the antistatic agent is 1:1.2, the volume of the antistatic agent is 20%, and the mass fraction of the concentrated sulfuric acid is 95%);
step 3: mixing polysuccinimide with DMSO, adding triethylamine and silver-loaded silicon dioxide under the protection of nitrogen, stirring at 60 ℃ for reaction for 24 hours, adding unsaturated tertiary amino derivative, reacting for 14-16 hours under heat preservation, carrying out suction filtration, washing and drying a filter cake to obtain an intermediate product, stirring and reacting the intermediate product, anhydrous THF and 1, 3-propane sultone at 40 ℃ for 14-16 hours, and carrying out rotary evaporation to obtain modified silicon dioxide;
wherein the dosage ratio of polysuccinimide, DMSO, triethylamine, silver-loaded silicon dioxide and unsaturated tertiary amino derivative is 0.5g:50mL:4.4mL:6.7g:3.1g, the ratio of intermediate, anhydrous THF and 1, 3-propane sultone being 4.1g:50mL:0.61g;
step 4: magnetically stirring modified silicon dioxide, triethylamine and tetrahydrofuran in a three-neck flask, adding antistatic agent modified cotton fiber at 0 ℃, then adding 4-dimethylaminopyridine, adding N, N' -dicyclohexylcarbodiimide after the reaction liquid is clarified, heating to 25 ℃, reacting for 3 hours, concentrating the reaction liquid under reduced pressure, washing with 5% sodium bicarbonate solution and 1 mmo/L hydrochloric acid solution in molar volume, and drying with anhydrous sodium sulfate and concentrating under reduced pressure to obtain the functional antioxidant;
wherein, the mole ratio of the modified silicon dioxide, the triethylamine, the modified cotton fiber, the 4-dimethylaminopyridine and the N, N' -dicyclohexyl carbodiimide is controlled to be 1:0.03:1:5:6.
Example 4
The invention relates to a preparation method of a high-cleanness non-stimulation cotton soft towel, which comprises the following steps:
mixing the PP melt-blown cotton passing through a fiber extruder and in a melt-blown state, and then drafting the PP melt-blown cotton and the PP melt-blown cotton on a receiving device by high-pressure hot air; wherein the heating temperature of the melt-blowing die head is 160-350 ℃; wherein the melt-blowing die head assembly comprises two melt-blowing die heads, the two melt-blowing die heads are installed at an angle of 90 degrees, and the discharge port of the fiber extruder is positioned between the two melt-blowing die heads;
the receiving device adsorbs the functional cotton fibers and the PP melt-blown cotton into a net through the suction device; embossing by hot rolling bars; and the working temperature is 80-230 ℃; the high-cleanness non-irritating cotton soft towel is obtained.
Comparative example 1
Comparative example 1 used a cotton towel of chinese patent No. CN112853615 a;
the performance test was conducted on examples 1 to 3 and comparative example 1, and the test results were as follows:
from the table, the high-cleaning non-irritating cotton soft towel prepared by the invention has good antibacterial performance.
The foregoing describes one embodiment of the present invention in detail, but the description is only a preferred embodiment of the present invention and should not be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the present invention are intended to be covered by the present invention.

Claims (8)

1. The high-cleanness non-irritating cotton soft towel is characterized by comprising the following raw materials in parts by weight: 50-100 parts of functional cotton fiber and 10-20 parts of PP melt blown cotton;
wherein, the preparation process of the functional cotton fiber comprises the following steps:
step 1: preparing succinic acid modified cotton fibers;
step 2: mixing 2, 2-dimethylolbutyric acid, triethylamine and tetrahydrofuran under the protection of nitrogen, adding dimethylaminopropylamine and 4-dimethylaminopyridine at 0 ℃, stirring, adding N, N' -dicyclohexylcarbodiimide, heating to 25 ℃, reacting for 3-4h, concentrating to 1/3 of the original volume, washing, extracting and steaming to obtain an intermediate 1;
mixing the intermediate 1, 4-dibromobutane and isopropanol, carrying out reflux reaction for 4-6h, and carrying out reduced pressure distillation and recrystallization after the reaction is finished to obtain an antistatic agent;
step 3: adding succinic acid modified cotton fibers and an antistatic agent into a reaction kettle, stirring at a rotating speed of 300-500r/min, adding concentrated sulfuric acid, and reacting at a temperature of 80-90 ℃ for 2-3h to obtain antistatic agent modified cotton fibers;
step 3: mixing polysuccinimide with DMSO, adding triethylamine and silver-loaded silicon dioxide under the protection of nitrogen, stirring at 60 ℃ for reaction for 24 hours, adding unsaturated tertiary amino derivative, reacting for 14-16 hours under heat preservation, carrying out suction filtration, washing and drying a filter cake to obtain an intermediate product, stirring and reacting the intermediate product, anhydrous THF and 1, 3-propane sultone at 40 ℃ for 14-16 hours, and carrying out rotary evaporation to obtain modified silicon dioxide;
step 4: and magnetically stirring modified silicon dioxide, triethylamine and tetrahydrofuran in a three-neck flask, adding antistatic agent modified cotton fiber at 0 ℃, then adding 4-dimethylaminopyridine, adding N, N' -dicyclohexylcarbodiimide after the reaction liquid is clarified, heating to 25 ℃, and reacting for 3 hours to obtain the functional antioxidant.
2. The high-cleaning non-irritating cotton towel according to claim 1, wherein the preparation process of the succinic acid modified cotton fibers comprises the following steps:
placing cotton fiber in an aqueous solution containing 5.0 g per liter of anionic detergent and 2.0 g per liter of sodium carbonate at room temperature under stirring, treating for 30 minutes under boiling condition, taking out cotton fiber, washing with water for 3 times, and drying at 100deg.C to obtain pretreated cotton fiber;
the pretreated cotton fibers were modified with an aqueous solution containing succinic acid at a concentration of 11.8 grams per liter to 82.6 grams per liter and 50 grams per liter of sodium dihydrogen phosphate.
3. The high cleaning non-irritating cotton towel according to claim 1, characterized in that the dosage ratio of 2, 2-dimethylolbutyric acid, tetrahydrofuran, dimethylaminopropylamine, 4-dimethylaminopyridine and N, N' -dicyclohexylcarbodiimide is 0.1mol:68-72mL:0.1mol:0.4-0.6g:0.3-0.5g, and the amount of triethylamine is 3-5% of the mass of the 2, 2-dihydroxymethyl butyric acid.
4. The high-cleaning non-irritating cotton soft towel according to claim 1, wherein the dosage ratio of the intermediate 1, 4-dibromobutane and isopropanol is 0.1mol:0.05mol:68.7-72.4mL.
5. The high-cleaning non-irritating cotton soft towel according to claim 1, wherein the molar ratio of the succinic acid modified cotton fibers to the antistatic agent is 1:1.2, the amount of concentrated sulfuric acid is 20% by volume of the antistatic agent, and the mass fraction of the concentrated sulfuric acid is 95%.
6. The high cleaning non-irritating cotton towel according to claim 1, characterized in that the usage ratio of polysuccinimide, DMSO, triethylamine, silver-loaded silica, unsaturated tertiary amine derivatives is 0.3-0.5g:40-50mL:3.5-4.4mL:5.4-6.7g:2.5-3.1g, the ratio of intermediate, anhydrous THF and 1, 3-propane sultone being 3.5-4.1g:40-50mL:0.45-0.61g.
7. The high cleaning non-irritating cotton towel according to claim 1, wherein the molar ratio of modified silica, triethylamine, modified cotton fibers, 4-dimethylaminopyridine and N, N' -dicyclohexyl-carbon-diimine is controlled to be 1:0.01-0.03:1:1-5:1-6.
8. The preparation method of the high-cleanness non-stimulation cotton soft towel is characterized by comprising the following steps of:
mixing the PP melt-blown cotton passing through a fiber extruder and in a melt-blown state, and then drafting the PP melt-blown cotton and the PP melt-blown cotton on a receiving device by high-pressure hot air; wherein the heating temperature of the melt-blowing die head is 160-350 ℃; wherein the melt-blowing die head assembly comprises two melt-blowing die heads, the two melt-blowing die heads are installed at an angle of 90 degrees, and the discharge port of the fiber extruder is positioned between the two melt-blowing die heads;
the receiving device adsorbs the functional cotton fibers and the PP melt-blown cotton into a net through the suction device; embossing by hot rolling bars; and the working temperature is 80-230 ℃; the high-cleanness non-irritating cotton soft towel is obtained.
CN202311250815.0A 2023-09-26 2023-09-26 High-cleanness non-stimulation cotton soft towel and preparation method thereof Pending CN117569007A (en)

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