CN109137497B - Application of environment-friendly fluorine-free waterproof agent to umbrella surface cloth - Google Patents

Application of environment-friendly fluorine-free waterproof agent to umbrella surface cloth Download PDF

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CN109137497B
CN109137497B CN201810620587.4A CN201810620587A CN109137497B CN 109137497 B CN109137497 B CN 109137497B CN 201810620587 A CN201810620587 A CN 201810620587A CN 109137497 B CN109137497 B CN 109137497B
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refining
liquid
base cloth
fluorine
waterproof agent
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CN109137497A (en
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许尔明
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Zhejiang Shengshan Technology Textile Co ltd
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Zhejiang Shengshan Technology Textile Co ltd
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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
    • 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
    • D06M13/188Monocarboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06LDRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
    • D06L1/00Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
    • D06L1/12Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using aqueous solvents
    • D06L1/16Multi-step processes
    • 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
    • D06M11/68Treating 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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70Treating 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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
    • D06M11/71Salts of phosphoric acids
    • 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
    • D06M13/02Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
    • 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
    • D06M13/207Substituted carboxylic acids, e.g. by hydroxy or keto groups; 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
    • D06M13/244Treating 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 sulfur or phosphorus
    • D06M13/282Treating 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 sulfur or phosphorus with compounds containing phosphorus
    • D06M13/288Phosphonic or phosphonous acids or derivatives 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
    • D06M13/325Amines
    • D06M13/342Amino-carboxylic acids; Betaines; Aminosulfonic acids; Sulfo-betaines
    • 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
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/6436Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
    • 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
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/12Hydrophobic properties

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

Abstract

The invention provides an application of an environment-friendly fluorine-free waterproof agent to umbrella surface cloth, which comprises the following steps of 1) refining: adding water and desizing agent into a liquid cylinder of a refining machine to prepare refining liquid; heating to 50-70 deg.C, putting the base cloth into a liquid cylinder, and circulating the refining liquid and the base cloth in the liquid cylinder; heating to 80-100 deg.C, refining for 30-60min, removing refined solution, washing with cold water, and taking out the base cloth; 2) finishing: adding water and 0.6-0.8g/L of fluorine-free waterproofing agent into a liquid tank of a finishing machine to prepare processing liquid, and adjusting the pH value to 5.6-6.0 by using an acidic solution; soaking the base cloth in a rolling processing liquid; and drying and shaping the base cloth in a drying and shaping machine. The acidic solution is added to maintain the pH value of the processing liquid to be 5.6-6.0, so that the continuous processing stability of the waterproof agent is greatly improved.

Description

Application of environment-friendly fluorine-free waterproof agent to umbrella surface cloth
Technical Field
The invention relates to the field of textile production, in particular to application of an environment-friendly fluorine-free waterproof agent to umbrella surface cloth.
Background
The fluoride PFOA (perfluorooctane sulfonyl compound) and PFOS (perfluorooctanoic acid ammonium) in the common waterproof agent at present belong to environment, human and animal unfriendly compounds, and have the advantages of bioaccumulation, genetic toxicity, stable performance and difficult degradation. With the improvement of environmental protection requirements, the environmental protection requirements on the waterproof agent are higher and higher, and the application of the waterproof agent is from 8-carbon waterproof agent to 6-carbon waterproof agent to fluorine-free waterproof agent. Especially, the products exported in Europe and America are always required to be free of fluorine. The existing fluorine-free waterproof agent usually contains active hydrogen or amino, and the fluorine-free waterproof agent is easily oxidized due to high processing temperature in the processing process, so that the waterproof agent is difficult to attach to umbrella cloth, and the waterproof performance of the product is finally reduced.
The prior patent document with the application number of CN201510645951.9 discloses a preparation method of environment-friendly waterproof all-cotton colored polishing coating grid cloth, wherein a C6 waterproof agent or a fluorine-free waterproof agent and a penetrating agent are prepared and poured into a water tank; heating the oven to 150-180 ℃, then guiding the grid cloth into the water tank, passing through a clamping rod and then entering the oven; the temperature is high during processing, the fluoride-free waterproof agent is easy to oxidize, so that the waterproof agent is difficult to attach to the umbrella surface cloth, and the waterproof performance of the product is finally reduced.
Disclosure of Invention
Technical problem to be solved
The invention aims to provide an application of an environment-friendly fluorine-free waterproof agent to umbrella cloth, and overcomes the defects that the existing fabric finishing process using the environment-friendly fluorine-free waterproof agent has high temperature and is easy to oxidize, so that the waterproof agent is difficult to attach to the umbrella cloth, and finally the waterproof performance of a product is reduced.
The invention also aims to provide the application of the environment-friendly fluorine-free waterproof agent to the umbrella surface cloth, which solves the problem that the existing environment-friendly fluorine-free waterproof agent is used
(II) technical scheme
In order to solve the technical problems, the invention provides an application of an environment-friendly fluorine-free waterproof agent on umbrella surface cloth, which comprises the following steps:
1) refining: adding water and desizing agent into a liquid cylinder of a refining machine to prepare refining liquid; heating to 50-70 deg.C, putting the base cloth into a liquid cylinder, and circulating the refining liquid and the base cloth in the liquid cylinder; heating to 80-100 deg.C, refining for 30-60min, removing refined solution, washing with cold water, and taking out the base cloth;
2) finishing: adding water and 0.6-0.8g/L of fluorine-free waterproofing agent into a liquid tank of a finishing machine to prepare processing liquid, and adjusting the pH value to 5.6-6.0 by using an acidic solution; soaking the base cloth in a rolling processing liquid; and drying and shaping the base cloth in a drying and shaping machine.
The acidic solution is added to maintain the pH value of the processing liquid to be 5.6-6.0, so that the continuous processing stability of the waterproof agent is greatly improved.
Preferably, the refining liquid and the base cloth rotate circularly for 15-20min in the refining process.
Preferably, in the refining process, the refining time is 46-50 min.
Preferably, in the finishing process, the drying and setting temperature of the dryer is 160-.
Preferably, in the finishing process, the speed of the dryer is 60-70 m/min.
Preferably, the acidic solution comprises acetic acid, monopotassium phosphate, citric acid and a stabilizer, wherein the concentrations of the acetic acid, the monopotassium phosphate and the citric acid in the acidic solution are respectively (2.2% -2.4%), (0.6% -1.0%) and (0.3% -0.5%), and the concentration of the stabilizer is 0.5-0.7 g/L. According to the acidic buffer solution consisting of acetic acid, monopotassium phosphate, citric acid and the stabilizer, the pH of the blended processing solution is more stable, 0.5-0.7g/L of the stabilizer is added under an acidic condition, so that the fluorine-free waterproof agent is not easily oxidized, the probability of sticking the waterproof cloth to a roller is reduced on the premise of ensuring that the waterproof effect meets the requirement, and the application performance of the waterproof agent is greatly improved; the demand for fluorine-free waterproofing agents is reduced.
Preferably, the fluorine-free waterproof agent is prepared by compounding polydimethylsiloxane containing amino, active hydrogen and long-chain fatty alkyl and paraffin; the stabilizer comprises, by weight, 5-7 parts of sodium ethylene diamine tetra methylene phosphonate, 1-3 parts of triammonium citrate and 1-3 parts of cationic surfactant. The stabilizer provided by the invention adopts the sodium ethylene diamine tetra (methylene phosphonic acid) to settle heavy metals in water, so that the effect of the adsorption of the heavy metals on the base cloth on the subsequent pigment adsorption is reduced; the triammonium citrate, acetic acid, potassium dihydrogen phosphate and citric acid can form a stable solution system, and the more active reducing group of the triammonium citrate can protect polydimethylsiloxane containing amino, active hydrogen and long-chain fatty alkyl from being oxidized easily; the stability of the fluorine-free waterproof agent is enhanced, and the ethylene diamine tetraacetic acid disodium salt and the potassium dihydrogen phosphate are further compounded into a stable ionic solution which is not easy to decompose.
Preferably, the cationic surfactant comprises, by weight, 2-3 parts of dodecyl dimethyl tertiary amine acetate, 0.5-0.7 part of octadecyl organosilicon copper quaternary ammonium salt and 1-2 parts of sodium citrate. The fluorine-free water-proofing agent is easy to attach to the base cloth by adopting the cationic surfactant matched with the stabilizing agent, and the flexibility of the base cloth is improved.
Preferably, in the finishing process, the rolling allowance of the base cloth in the primary soaking and rolling processing liquid is 74-76%.
Preferably, in the refining process, the cold water washing frequency is two times, and the water temperature is 10-12 ℃ during the first cold water washing, and the washing time is 10-14 min; and during the second cold water washing, the water temperature is 20-25 ℃, and the washing time is 20-30 min. The water washing is carried out twice, the temperature of the first water washing is lower, the fibers of the base cloth are quickly shrunk through the temperature difference, the fiber intervals are smaller, the flexibility of the fibers is enhanced, and the adhesion of the waterproof agent is facilitated.
(III) advantageous effects
The invention provides an application of an environment-friendly fluorine-free waterproof agent to umbrella surface cloth, which has the following advantages:
1. the acidic solution is added to maintain the pH value of the processing liquid to be 5.6-6.0, so that the continuous processing stability of the waterproof agent is greatly improved.
2. According to the acidic buffer solution consisting of acetic acid, monopotassium phosphate, citric acid and the stabilizer, the pH of the blended processing solution is more stable, 0.5-0.7g/L of the stabilizer is added under an acidic condition, so that the fluorine-free waterproof agent is not easily oxidized, the probability of sticking the waterproof cloth to a roller is reduced on the premise of ensuring that the waterproof effect meets the requirement, and the application performance of the waterproof agent is greatly improved; the demand for fluorine-free waterproofing agents is reduced.
3. The stabilizer provided by the invention adopts the sodium ethylene diamine tetra (methylene phosphonic acid) to settle heavy metals in water, so that the effect of the adsorption of the heavy metals on the base cloth on the subsequent pigment adsorption is reduced; the triammonium citrate, acetic acid, potassium dihydrogen phosphate and citric acid can form a stable solution system, and the more active reducing group of the triammonium citrate can protect polydimethylsiloxane containing amino, active hydrogen and long-chain fatty alkyl from being oxidized easily; the stability of the fluorine-free waterproof agent is enhanced, and the ethylene diamine tetraacetic acid disodium salt and the potassium dihydrogen phosphate are further compounded into a stable ionic solution which is not easy to decompose.
4. The fluorine-free water-proofing agent is easy to attach to the base cloth by adopting the cationic surfactant matched with the stabilizing agent, and the flexibility of the base cloth is improved.
5. The water washing is carried out twice, the temperature of the first water washing is lower, the fibers of the base cloth are quickly shrunk through the temperature difference, the fiber intervals are smaller, the flexibility of the fibers is enhanced, and the adhesion of the waterproof agent is facilitated.
Drawings
FIG. 1 is a schematic flow chart of the application of the environment-friendly fluorine-free waterproof agent of the invention to umbrella cloth.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The cloth in the following examples is umbrella-surface cloth.
Example 1: as shown in the attached figure 1, the application of the environment-friendly fluorine-free waterproof agent on the umbrella surface cloth provided by the invention comprises the following steps:
1) refining: adding water and desizing agent into a liquid cylinder of a refining machine to prepare refining liquid; heating to 50 deg.C, adding the base cloth into the liquid cylinder, and circulating the refining liquid and the base cloth in the liquid cylinder for 15 min. (ii) a Then heating to 80 ℃, refining for 30min, discharging the refining liquid, adding cold water for washing, and taking out the base fabric; the number of cold water washing times is two, and when the water is washed for the first time, the water temperature is 10 ℃, and the washing time is 10 min; and during the second cold water washing, the water temperature is 20-25 ℃, and the washing time is 20 min.
2) Finishing: adding water and 0.6g/L of fluorine-free waterproofing agent into a liquid tank of a finishing machine to prepare processing liquid, and adjusting the pH value to 5.6 by using an acidic solution; soaking the base cloth in a rolling processing liquid; the percent rolling of the base cloth in the processing liquid of soaking and rolling is 74 percent. And drying and shaping the base fabric in a drying and shaping machine, wherein the drying and shaping temperature of the drying machine is 160 ℃, and the vehicle speed is 60 m/min. The acid solution comprises acetic acid, monopotassium phosphate, citric acid and a stabilizer, wherein the concentrations of the acetic acid, the monopotassium phosphate and the citric acid in the acid solution are respectively 2.2%, 0.6% and 0.3%, and the concentration of the stabilizer is 0.5 g/L. The fluorine-free waterproof agent is prepared by compounding polydimethylsiloxane containing amino, active hydrogen and long-chain fatty alkyl and paraffin; the stabilizer comprises, by weight, 5 parts of sodium ethylene diamine tetra methylene phosphonate, 1 part of triammonium citrate and 1 part of cationic surfactant. The cationic surfactant comprises, by weight, 2 parts of dodecyl dimethyl tertiary amine acetate, 0.5 part of octadecyl organosilicon copper quaternary ammonium salt and 1 part of sodium citrate.
Example 2: the invention provides an application of an environment-friendly fluorine-free waterproof agent to umbrella surface cloth, which comprises the following steps:
1) refining: adding water and desizing agent into a liquid cylinder of a refining machine to prepare refining liquid; heating to 70 deg.C, adding the base cloth into the liquid cylinder, and circulating the refining liquid and the base cloth in the liquid cylinder for 20 min. (ii) a Then heating to 100 ℃, refining for 60min, discharging the refining liquid, adding cold water, washing and taking out the base fabric; the number of cold water washing times is two, and when the water is washed for the first time, the water temperature is 12 ℃, and the washing time is 14 min; and in the second cold water washing, the water temperature is 25 ℃, and the washing time is 30 min.
2) Finishing: adding water and 0.8g/L of fluorine-free waterproofing agent into a liquid tank of a finishing machine to prepare processing liquid, and adjusting the pH value to 6.0 by using an acidic solution; soaking the base cloth in a rolling processing liquid; the percent rolling in the base cloth soaking and rolling processing liquid is 76 percent. And drying and shaping the base fabric in a drying and shaping machine, wherein the drying and shaping temperature of the drying machine is 170 ℃, and the vehicle speed is 70 m/min. The acid solution comprises acetic acid, monopotassium phosphate, citric acid and a stabilizer, wherein the concentrations of the acetic acid, the monopotassium phosphate and the citric acid in the acid solution are respectively 2.4%, 1.0% and 0.5%, and the concentration of the stabilizer is 0.7 g/L. The fluorine-free waterproof agent is prepared by compounding polydimethylsiloxane containing amino, active hydrogen and long-chain fatty alkyl and paraffin; the stabilizer comprises, by weight, 5-7 parts of sodium ethylene diamine tetra methylene phosphonate, 3 parts of triammonium citrate and 3 parts of cationic surfactant. The cationic surfactant comprises, by weight, 3 parts of dodecyl dimethyl tertiary amine acetate, 0.7 part of octadecyl organosilicon copper quaternary ammonium salt and 2 parts of sodium citrate.
Example 3: the invention provides an application of an environment-friendly fluorine-free waterproof agent to umbrella surface cloth, which comprises the following steps:
1) refining: adding water and desizing agent into a liquid cylinder of a refining machine to prepare refining liquid; after the temperature is raised to 60 ℃, the base cloth is put into a liquid cylinder, and the scouring liquid and the base cloth rotate in the liquid cylinder for 17.5min in a circulating way. (ii) a Then heating to 90 ℃, refining for 46min, discharging the refining liquid, adding cold water, washing and taking out the base fabric; the number of cold water washing times is two, and when the water is washed for the first time, the water temperature is 11 ℃, and the washing time is 12 min; the second cold water washing is carried out at 22.5 deg.C for 25 min.
2) Finishing: adding water and 0.7g/L of fluorine-free waterproofing agent into a liquid tank of a finishing machine to prepare processing liquid, and adjusting the pH value to 5.8 by using an acidic solution; soaking the base cloth in a rolling processing liquid; the percent rolling in the base cloth one-dipping-one-rolling processing liquid is 75 percent. And drying and shaping the base fabric in a drying and shaping machine, wherein the drying and shaping temperature of the drying machine is 165 ℃, and the vehicle speed is 65 m/min. The acid solution comprises acetic acid, monopotassium phosphate, citric acid and a stabilizer, wherein the concentrations of the acetic acid, the monopotassium phosphate and the citric acid in the acid solution are respectively 2.3%, 0.8% and 0.4%, and the concentration of the stabilizer is 0.6 g/L. The fluorine-free waterproof agent is prepared by compounding polydimethylsiloxane containing amino, active hydrogen and long-chain fatty alkyl and paraffin; the stabilizer comprises 6 parts of ethylene diamine tetramethylene phosphonic acid sodium, 2 parts of triammonium citrate and 2 parts of cationic surfactant according to weight percentage. The cationic surfactant comprises, by weight, 2.5 parts of dodecyl dimethyl tertiary amine acetate, 0.6 part of octadecyl organosilicon copper quaternary ammonium salt and 1.5 parts of sodium citrate.
Example 4: the invention provides an application of an environment-friendly fluorine-free waterproof agent to umbrella surface cloth, which comprises the following steps:
1) refining: adding water and desizing agent into a liquid cylinder of a refining machine to prepare refining liquid; heating to 60 deg.C, and placing the base cloth into the liquid cylinder to make the refining liquid and the base cloth rotate together in the liquid cylinder for 18 min. (ii) a Then heating to 90 ℃, refining for 50min, discharging the refining liquid, adding cold water, washing and taking out the base fabric; the number of cold water washing times is two, and when the water is washed for the first time, the water temperature is 11 ℃, and the washing time is 12 min; and in the second cold water washing, the water temperature is 23 ℃, and the washing time is 25 min.
2) Finishing: adding water and 0.7g/L of fluorine-free waterproofing agent into a liquid tank of a finishing machine to prepare processing liquid, and adjusting the pH value to 5.8 by using an acidic solution; soaking the base cloth in a rolling processing liquid; the percent rolling in the base cloth one-dipping-one-rolling processing liquid is 75 percent. And drying and shaping the base fabric in a drying and shaping machine, wherein the drying and shaping temperature of the drying machine is 165 ℃, and the vehicle speed is 65 m/min. The acid solution comprises acetic acid, monopotassium phosphate, citric acid and a stabilizer, wherein the concentrations of the acetic acid, the monopotassium phosphate and the citric acid in the acid solution are respectively 2.3%, 0.8% and 0.4%, and the concentration of the stabilizer is 0.6 g/L. The fluorine-free waterproof agent is prepared by compounding polydimethylsiloxane containing amino, active hydrogen and long-chain fatty alkyl and paraffin; the stabilizer comprises 6 parts of ethylene diamine tetramethylene phosphonic acid sodium, 2 parts of triammonium citrate and 2 parts of cationic surfactant according to weight percentage. The cationic surfactant comprises, by weight, 2.5 parts of dodecyl dimethyl tertiary amine acetate, 0.6 part of octadecyl organosilicon copper quaternary ammonium salt and 1.5 parts of sodium citrate.
Comparative example 1: the invention provides an application of an environment-friendly fluorine-free waterproof agent to umbrella surface cloth, which comprises the following steps:
1) refining: adding water and desizing agent into a liquid cylinder of a refining machine to prepare refining liquid; heating to 49 deg.C, adding the base cloth into the liquid cylinder, and circulating the refining liquid and the base cloth in the liquid cylinder for 14 min. (ii) a Then heating to 79 ℃, refining for 29min, discharging the refining liquid, adding cold water, washing and taking out the base fabric; the number of cold water washing times is two, and when the water is washed for the first time, the water temperature is 9 ℃, and the washing time is 9 min; the second cold water washing is carried out at the water temperature of 19 ℃ for 19 min.
2) Finishing: adding water and 0.5g/L of fluorine-free waterproofing agent into a liquid tank of a finishing machine to prepare processing liquid, and adjusting the pH value to 5.0 by using an acidic solution; soaking the base cloth in a rolling processing liquid; the percent rolling in the base cloth soaking and rolling processing liquid is 73 percent. And drying and shaping the base fabric in a drying and shaping machine at 159 ℃ and 59 m/min. The acid solution comprises acetic acid, monopotassium phosphate, citric acid and a stabilizer, wherein the concentrations of the acetic acid, the monopotassium phosphate and the citric acid in the acid solution are respectively 2.1%, 0.5% and 0.2%, and the concentration of the stabilizer is 0.4 g/L. The fluorine-free waterproof agent is prepared by compounding polydimethylsiloxane containing amino, active hydrogen and long-chain fatty alkyl and paraffin; the stabilizer comprises 8 parts by weight of sodium ethylene diamine tetra methylene phosphonate, 0.9 part by weight of ammonium citrate tribasic and 0.9 part by weight of cationic surfactant. The cationic surfactant comprises, by weight, 1 part of dodecyl dimethyl tertiary amine acetate, 0.4 part of octadecyl organosilicon copper quaternary ammonium salt and 0.9 part of sodium citrate.
Comparative example 2: the invention provides an application of an environment-friendly fluorine-free waterproof agent to umbrella surface cloth, which comprises the following steps:
1) refining: adding water and desizing agent into a liquid cylinder of a refining machine to prepare refining liquid; heating to 71 deg.C, adding the base cloth into the liquid cylinder, and circulating the refining liquid and the base cloth in the liquid cylinder for 21 min. (ii) a Then heating to 101 ℃, refining for 61min, discharging the refining liquid, adding cold water, washing and taking out the base fabric; the number of cold water washing times is two, and when the water is washed for the first time, the water temperature is 13 ℃, and the washing time is 15 min; and in the second cold water washing, the water temperature is 26 ℃, and the washing time is 31 min.
2) Finishing: adding water and 0.9g/L of fluorine-free waterproofing agent into a liquid tank of a finishing machine to prepare processing liquid, and adjusting the pH value to 6.5 by using an acidic solution; soaking the base cloth in a rolling processing liquid; the rolling residual rate of the base cloth in the processing liquid of soaking and rolling is 74-76 percent. And drying and shaping the base fabric in a drying and shaping machine, wherein the drying and shaping temperature of the drying machine is 171 ℃, and the vehicle speed is 71 m/min. The acid solution comprises acetic acid, monopotassium phosphate, citric acid and a stabilizer, wherein the concentrations of the acetic acid, the monopotassium phosphate and the citric acid in the acid solution are respectively 2.5%, 1.1% and 0.6%, and the concentration of the stabilizer is 0.8 g/L. The fluorine-free waterproof agent is prepared by compounding polydimethylsiloxane containing amino, active hydrogen and long-chain fatty alkyl and paraffin; the stabilizer comprises 4 parts of ethylene diamine tetramethylene phosphonic acid sodium, 4 parts of citric acid triammonium and 4 parts of cationic surfactant according to weight percentage. The cationic surfactant comprises, by weight, 4 parts of dodecyl dimethyl tertiary amine acetate, 0.8 part of octadecyl organosilicon copper quaternary ammonium salt and 3 parts of sodium citrate.
The performance parameters of the textiles (umbrella fabrics) prepared in examples 1, 2, 3 and 4 above compared with those of comparative examples 1 and 2 are as follows:
wherein the color fastness is detected by GB/T5713-2013 (color fastness to water of textile color fastness test). Hydrostatic pressure test the hydrostatic pressure test for the water impermeability of textile fabrics is adopted according to the national standard GB/T4744-1997. The fastness of the adhesive film adopts the enterprise standard. Wherein, the waterproof performance is tested according to the test standard of AATCC 22-2014.
Product index item Color fastness Hydrostatic pressure test Water resistance
Example 1 4.5 stage 9100 MM/H2O 91 is divided into
Example 2 4.5 stage 9000 MM/H2O 92 point is
Example 3 Grade 5.0 9700 MM/H2O 96 minutes
Example 4 Grade 5.0 9600 MM/H2O 95 minutes
Comparative example 1 Grade 3.5 7800 MM/H2O 85 minutes
Comparative example 2 Grade 3.5 8000 MM/H2O 84 minutes
Dye printed and pigment printed articles on the market Grade 3.5 8200 MM/H2O 72 points of
In conclusion, the products prepared by the processes of example 1, example 2, example 3 and example 4 have better color fastness, hydrostatic pressure and waterproof performance than the products of comparative example 1 and comparative example 2 and the products printed by the dyes and the paints on the market, which are out of the process range. Particularly, the color fastness of the embodiment 3 and the embodiment 4 adopting the optimized process is 0.5 grade higher than that of the embodiment 1 and the embodiment 2, and the hydrostatic pressure is higher; the waterproof performance is also better.
The above embodiments are only used for illustrating the present invention, and the structure, connection mode and the like of each component can be changed, and all equivalent changes and improvements made on the basis of the technical scheme of the present invention should not be excluded from the protection scope of the present invention.

Claims (7)

1. The application of the environment-friendly fluorine-free waterproof agent to the umbrella surface cloth is characterized by comprising the following steps:
1) refining: adding water and desizing agent into a liquid cylinder of a refining machine to prepare refining liquid; heating to 50-70 deg.C, putting the base cloth into a liquid cylinder, and circulating the refining liquid and the base cloth in the liquid cylinder; heating to 80-100 deg.C, refining for 30-60min, removing the refining solution, washing with cold water, and taking out the base cloth;
2) finishing: adding water and 0.6-0.8g/L of fluorine-free waterproofing agent into a liquid tank of a finishing machine to prepare processing liquid, and adjusting the pH value to 5.6-6.0 by using an acidic solution;
soaking the base cloth in a rolling processing liquid; drying and shaping the base cloth in a drying and shaping machine; the acid solution comprises acetic acid, monopotassium phosphate, citric acid and a stabilizer, wherein the concentrations of the acetic acid, the monopotassium phosphate and the citric acid in the acid solution are respectively (2.2% -2.4%), (0.6% -1.0%) and (0.3% -0.5%), and the concentration of the stabilizer is 0.5-0.7 g/L;
the fluorine-free waterproof agent is prepared by compounding polydimethylsiloxane containing amino, active hydrogen and long-chain fatty alkyl and paraffin; according to the weight percentage, the stabilizer comprises 5-7 parts of ethylene diamine tetramethylene phosphonic acid sodium, 1-3 parts of citric acid triammonium and 1-3 parts of cationic surfactant;
the cationic surfactant comprises, by weight, 2-3 parts of dodecyl dimethyl tertiary amine acetate, 0.5-0.7 part of octadecyl organosilicon copper quaternary ammonium salt and 1-2 parts of sodium citrate.
2. The application of the environment-friendly fluorine-free waterproof agent on the umbrella surface cloth as claimed in claim 1, wherein the scouring solution and the base cloth circularly rotate for 15-20min in the scouring process.
3. The application of the environment-friendly fluorine-free waterproof agent to the umbrella surface cloth according to claim 1, wherein in the scouring process, the scouring time is 46-50 min.
4. The application of the environmentally friendly fluorine-free waterproof agent on the umbrella cloth as claimed in claim 1, 2 or 3, wherein in the finishing process, the drying and setting temperature of the dryer is 160-170 ℃.
5. The application of the environment-friendly fluorine-free waterproof agent on the umbrella surface cloth as claimed in claim 4, wherein in the finishing process, the running speed of a dryer is 60-70 m/min.
6. The application of the environment-friendly fluorine-free waterproof agent on the umbrella surface cloth according to claim 1, 2 or 3, wherein in the finishing process, the percent rolling of the base cloth in the one-time soaking and one-time rolling processing liquid is 74-76%.
7. The application of the environment-friendly fluorine-free waterproof agent on the umbrella surface cloth according to claim 1, 2 or 3, wherein in the refining process, the cold water washing frequency is two times, and the water temperature is 10-12 ℃ in the first cold water washing, and the washing time is 10-14 min; and during the second cold water washing, the water temperature is 20-25 ℃, and the washing time is 20-30 min.
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CN110904686A (en) * 2019-11-28 2020-03-24 浙江圣山科纺有限公司 Application of environment-friendly fluorine-free waterproof agent to umbrella surface cloth

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