CN114032687A - Preparation method and application of moisture-proof and mildew-proof resin - Google Patents

Preparation method and application of moisture-proof and mildew-proof resin Download PDF

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Publication number
CN114032687A
CN114032687A CN202111339713.7A CN202111339713A CN114032687A CN 114032687 A CN114032687 A CN 114032687A CN 202111339713 A CN202111339713 A CN 202111339713A CN 114032687 A CN114032687 A CN 114032687A
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China
Prior art keywords
proof
mildew
moisture
padding
prepolymer
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CN202111339713.7A
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Chinese (zh)
Inventor
王海峰
王涛
徐杨
花玉成
彭佳钰
管永华
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Nantong C&t Textile Technology Co ltd
Nantong University
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Nantong C&t Textile Technology Co ltd
Nantong University
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Priority to CN202111339713.7A priority Critical patent/CN114032687A/en
Publication of CN114032687A publication Critical patent/CN114032687A/en
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    • 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
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters 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
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53Polyethers
    • 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
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/59Polyamides; Polyimides
    • 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
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters

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

Abstract

The invention discloses a preparation method and application of moisture-proof and mildew-proof resin. The water absorption rate of the distilled water is controlled between 40 and 50 times. After being treated in an environment with room temperature and relative humidity of 90% for 28d, no mold growth is found on the surface of the mildew-proof cloth sample. Especially, when the fabric is applied to rainy and humid areas, the fabric has good water absorption performance, can play a better role in preventing moisture and mildew, and effectively prevents wall cloth and walls from being damaged by mildew. The preparation method is simple, low in cost and high in safety, and can be applied to the fields of basement water absorption, moisture prevention and mildew prevention wall cloth and the like.

Description

Preparation method and application of moisture-proof and mildew-proof resin
Technical Field
The invention belongs to the field of resin prepolymers, and particularly relates to a preparation method and application of a moisture-proof and mildew-proof resin.
Background
With the development of society, the number of textile enterprises is greatly increased, the varieties of textiles are various, and most of the textiles are easy to mildew, such as cotton, hemp, wool, nylon, acrylic fibers and the like. Storage of textiles and their raw materials has thus become a problem for these enterprises. At present, the existing mildew preventive is easy to corrode textiles, reduces the quality of the textiles and has single performance. Therefore, how to overcome the defects of the prior art is a problem which needs to be solved in the technical field of the textile auxiliary at present.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the defects of the prior art, the invention provides a preparation method and application of moisture-proof and mildew-proof resin.
The technical scheme is as follows: a preparation method of a damp-proof and mildew-proof resin takes acrylic acid, NaOH and epsilon-polylysine as raw materials to synthesize a prepolymer of the damp-proof and mildew-proof resin, and comprises the following specific operation steps:
step one, adopting a polymerization building device of prepolymer, and matching and stably building a stirrer, a thermometer and a constant-pressure separating funnel with a three-necked flask; adding 300mL of deionized water, 200mL of acrylic acid and 1g of initiator potassium persulfate into a three-neck flask, placing the three-neck flask in a constant-temperature water bath kettle at 65 ℃, and fully reacting for 1h under continuous stirring;
and step two, slowly dripping NaOH into the solution by using a separating funnel to neutralize acrylic acid, controlling the neutralization degree to be about 70%, fully stirring 3g of epsilon-polylysine until the solution has proper viscosity, and obtaining the product of the moisture-proof and mildew-proof resin prepolymer.
The application of the moisture-proof and mildew-proof resin and the moisture-proof and mildew-proof resin prepared by the preparation method are used for padding the polyester fabric to prepare the fabric with water absorption and mildew-proof characteristics; the specific finishing process is as follows: padding → drying → baking → rolling; wherein:
the padding is one padding and one rolling, and the mangle ratio is 100 percent;
the drying temperature is 105 ℃, and the time is 2 min;
the baking temperature is 190-200 ℃, and the time is 90 s;
the formula of the padding treating fluid is as follows:
300g/L of moistureproof and mildewproof prepolymer;
30-40g/L of polyethylene glycol;
as an optimization: the molecular weight of the polyethylene glycol is 1000.
Has the advantages that: the invention adopts the composite finishing of the water-absorbing resin and the bacteriostatic component, so that the fabric has the effects of moisture absorption and mildew prevention, and the water-absorbing resin on the surface can quickly absorb the water in the wall surface, keep the wall body dry and slowly release the water to the indoor. Meanwhile, even if the fabric has a certain water content, the fabric can effectively avoid the mildew phenomenon caused by the fabric due to the antibacterial and mildewproof component epsilon-polylysine. Can be applied to the fields of wall cloth in humid and dark environment and the like.
The invention uses polyethylene glycol and polyacrylic acid prepolymer for crosslinking, which has great influence on the viscosity increasing and moisture absorbing capacity of the product. The neutralization degree is controlled to be about 70 percent, if the neutralization degree is too low, the viscosity of the obtained prepolymer is too high, the prepolymer cannot be finished on the fabric, and if the neutralization degree is too high, redundant carboxyl is difficult to react with hydroxyl in polyethylene glycol, a product with certain strength cannot be obtained, and the moisture-proof capability is reduced.
The epsilon-polylysine (epsilon-PL) in the invention is a natural lysine homopolymer generated by microbial metabolism, has inhibition effect on gram-positive bacteria, gram-negative bacteria, fungi, certain mycoplasma and chlamydia, and has extremely high broad-spectrum antibacterial activity. Coli, the diameter of the zone of inhibition of staphylococcus aureus SAU reaches 14.9mm, and the diameter of the zone of inhibition of staphylococcus aureus SAU reaches 15.2 mm. The antibacterial rate is more than 95%.
The finishing process adopted by the invention is used for finishing the water-absorbent resin for the fabric, and the effect of uniform application is achieved. And is matched with the heat setting process of the polyester fabric.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below so that those skilled in the art can better understand the advantages and features of the present invention, and thus the scope of the present invention will be more clearly defined. The embodiments described herein are only a few embodiments of the present invention, rather than all embodiments, and all other embodiments that can be derived by one of ordinary skill in the art without inventive faculty based on the embodiments described herein are intended to fall within the scope of the present invention.
Examples
The invention takes acrylic acid, NaOH and epsilon-polylysine as raw materials to synthesize the moisture-proof and mildew-proof prepolymer, and the fabric with the water-absorbing and mildew-proof characteristics is prepared by padding the polyester fabric. The water absorption rate of the distilled water is controlled between 40 and 50 times. After being treated in an environment with room temperature and relative humidity of 90% for 28d, no mold growth is found on the surface of the mildew-proof cloth sample. Especially, when the fabric is applied to rainy and humid areas, the fabric has good water absorption performance, can play a better role in preventing moisture and mildew, and effectively prevents wall cloth and walls from being damaged by mildew. The preparation method is simple, low in cost and high in safety, and can be applied to the fields of basement water absorption, moisture prevention and mildew prevention wall cloth and the like.
The preparation method of the moisture-proof and mildew-proof resin takes acrylic acid, NaOH and epsilon-polylysine as raw materials to synthesize the prepolymer of the moisture-proof and mildew-proof resin, and comprises the following specific operation steps:
step one, adopting a polymerization building device of prepolymer, and matching and stably building a stirrer, a thermometer and a constant-pressure separating funnel with a three-necked flask; adding 300mL of deionized water, 200mL of acrylic acid and 1g of initiator potassium persulfate into a three-neck flask, placing the three-neck flask in a constant-temperature water bath kettle at 65 ℃, and fully reacting for 1h under continuous stirring;
and step two, slowly dripping NaOH into the solution by using a separating funnel to neutralize acrylic acid, controlling the neutralization degree to be about 70%, fully stirring 3g of epsilon-polylysine until the solution has proper viscosity, and obtaining the product of the moisture-proof and mildew-proof resin prepolymer.
The synthesis of the prepolymer of the invention is as follows:
Figure BDA0003351427410000041
the grafted antibacterial groups in the invention are as follows:
Figure BDA0003351427410000042
according to the application of the moisture-proof and mildew-proof resin, the moisture-proof and mildew-proof resin prepared by the preparation method is used for padding the polyester fabric to prepare the fabric with water absorption and mildew-proof characteristics; the specific finishing process is as follows: padding → drying → baking → rolling; wherein:
the padding is one padding and one rolling, and the mangle ratio is 100 percent;
the drying temperature is 105 ℃, and the time is 2 min;
the baking temperature is 190-200 ℃, and the time is 90 s;
the formula of the padding treating fluid is as follows:
300g/L of moistureproof and mildewproof prepolymer;
30-40g/L of polyethylene glycol;
the molecular weight of the polyethylene glycol is 1000.
The mechanism of the invention is as follows:
Figure BDA0003351427410000051
wherein R is an antibacterial group.
The invention uses polyethylene glycol and polyacrylic acid prepolymer for crosslinking, which has great influence on the viscosity increasing and moisture absorbing capacity of the product. The neutralization degree is controlled to be about 70 percent, if the neutralization degree is too low, the viscosity of the obtained prepolymer is too high, the prepolymer cannot be finished on the fabric, and if the neutralization degree is too high, redundant carboxyl is difficult to react with hydroxyl in polyethylene glycol, a product with certain strength cannot be obtained, and the moisture-proof capability is reduced.
The epsilon-polylysine (epsilon-PL) in the invention is a natural lysine homopolymer generated by microbial metabolism, has inhibition effect on gram-positive bacteria, gram-negative bacteria, fungi, certain mycoplasma and chlamydia, and has extremely high broad-spectrum antibacterial activity. Coli, the diameter of the zone of inhibition of staphylococcus aureus SAU reaches 14.9mm, and the diameter of the zone of inhibition of staphylococcus aureus SAU reaches 15.2 mm. The antibacterial rate is more than 95%.
The finishing process adopted by the invention is used for finishing the water-absorbent resin for the fabric, and the effect of uniform application is achieved. And is matched with the heat setting process of the polyester fabric.

Claims (3)

1. A preparation method of moisture-proof and mildew-proof resin is characterized by comprising the following steps: acrylic acid, NaOH and epsilon-polylysine are used as raw materials to synthesize the moisture-proof and mildew-proof resin prepolymer, and the specific operation steps are as follows:
step one, adopting a polymerization building device of prepolymer, and matching and stably building a stirrer, a thermometer and a constant-pressure separating funnel with a three-necked flask; adding 300mL of deionized water, 200mL of acrylic acid and 1g of initiator potassium persulfate into a three-neck flask, placing the three-neck flask in a constant-temperature water bath kettle at 65 ℃, and fully reacting for 1h under continuous stirring;
and step two, slowly dripping NaOH into the solution by using a separating funnel to neutralize acrylic acid, controlling the neutralization degree to be about 70%, fully stirring 3g of epsilon-polylysine until the solution has proper viscosity, and obtaining the product of the moisture-proof and mildew-proof resin prepolymer.
2. Use of the moisture and mold resistant resin according to claim 1, wherein: the moisture-proof and mildew-proof resin prepared by the preparation method of the moisture-proof and mildew-proof resin according to claim 1 is used for padding a polyester fabric to prepare a fabric with water absorption and mildew-proof properties; the specific finishing process is as follows: padding → drying → baking → rolling; wherein:
the padding is one padding and one rolling, and the mangle ratio is 100 percent;
the drying temperature is 105 ℃, and the time is 2 min;
the baking temperature is 190-200 ℃, and the time is 90 s;
the formula of the padding treating fluid is as follows:
300g/L of moistureproof and mildewproof prepolymer;
30-40g/L of polyethylene glycol;
3. the use of the moisture and mold resistant resin as defined in claim 2, wherein: the molecular weight of the polyethylene glycol is 1000.
CN202111339713.7A 2021-11-12 2021-11-12 Preparation method and application of moisture-proof and mildew-proof resin Pending CN114032687A (en)

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Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10237320A (en) * 1997-02-26 1998-09-08 Chisso Corp Antimicrobial resin composition and antimicrobial resin molded product using the same
JP2005002264A (en) * 2003-06-13 2005-01-06 Chisso Corp Silicone-containing antibacterial resin
CN102229689A (en) * 2011-05-11 2011-11-02 华侨大学 Preparation method of absorbent resin with bacteriostasis function
CN102408510A (en) * 2011-09-09 2012-04-11 宜兴丹森科技有限公司 Preparation method for super absorbent resin
CN105884959A (en) * 2016-05-10 2016-08-24 中山大学 Preparation method of polyacrylic acid super absorbent resin through room-temperature solution polymerization
CN105906413A (en) * 2016-04-15 2016-08-31 陕西科技大学 Water-retaining chitosan bacteriostatic antibiotic fertilizer and preparation method thereof
CN106977756A (en) * 2017-05-24 2017-07-25 常德金德镭射科技股份有限公司 A kind of antimildew and antibacterial coated film and preparation method thereof
CN107823696A (en) * 2017-09-22 2018-03-23 北京大清生物技术股份有限公司 A kind of water suction biocidal property material for personal-care supplies and preparation method thereof
CN110497635A (en) * 2019-08-21 2019-11-26 无锡腾华电缆材料科技有限公司 Sea water resistance waterstop production technology
CN111962305A (en) * 2020-08-27 2020-11-20 青岛阳光动力生物医药技术有限公司 Preparation method of light-energy antiviral self-disinfecting mask
CN112876694A (en) * 2020-06-30 2021-06-01 南京工业大学 Preparation method and application of acrylic acid/epsilon-polylysine adhesive antibacterial hydrogel

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10237320A (en) * 1997-02-26 1998-09-08 Chisso Corp Antimicrobial resin composition and antimicrobial resin molded product using the same
JP2005002264A (en) * 2003-06-13 2005-01-06 Chisso Corp Silicone-containing antibacterial resin
CN102229689A (en) * 2011-05-11 2011-11-02 华侨大学 Preparation method of absorbent resin with bacteriostasis function
CN102408510A (en) * 2011-09-09 2012-04-11 宜兴丹森科技有限公司 Preparation method for super absorbent resin
CN105906413A (en) * 2016-04-15 2016-08-31 陕西科技大学 Water-retaining chitosan bacteriostatic antibiotic fertilizer and preparation method thereof
CN105884959A (en) * 2016-05-10 2016-08-24 中山大学 Preparation method of polyacrylic acid super absorbent resin through room-temperature solution polymerization
CN106977756A (en) * 2017-05-24 2017-07-25 常德金德镭射科技股份有限公司 A kind of antimildew and antibacterial coated film and preparation method thereof
CN107823696A (en) * 2017-09-22 2018-03-23 北京大清生物技术股份有限公司 A kind of water suction biocidal property material for personal-care supplies and preparation method thereof
CN110497635A (en) * 2019-08-21 2019-11-26 无锡腾华电缆材料科技有限公司 Sea water resistance waterstop production technology
CN112876694A (en) * 2020-06-30 2021-06-01 南京工业大学 Preparation method and application of acrylic acid/epsilon-polylysine adhesive antibacterial hydrogel
CN111962305A (en) * 2020-08-27 2020-11-20 青岛阳光动力生物医药技术有限公司 Preparation method of light-energy antiviral self-disinfecting mask

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