CN110409181A - A kind of water-proof aagent and its preparation method and application method - Google Patents

A kind of water-proof aagent and its preparation method and application method Download PDF

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Publication number
CN110409181A
CN110409181A CN201910819963.7A CN201910819963A CN110409181A CN 110409181 A CN110409181 A CN 110409181A CN 201910819963 A CN201910819963 A CN 201910819963A CN 110409181 A CN110409181 A CN 110409181A
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parts
water
weight
proof
added
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戴大亮
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Sanyeng Household Products (heyuan) Co Ltd
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Sanyeng Household Products (heyuan) Co Ltd
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Priority to CN201910819963.7A priority Critical patent/CN110409181A/en
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
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    • D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
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    • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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Abstract

The invention discloses a kind of water-proof aagent and preparation method and application methods.Water-proof aagent comprises the following components in parts by weight: 45-55 parts of acrylic acid esters co-polymers, 2.5-3.5 parts of acrylamide/ammonium acrylate copolymers, 1.8-2.2 parts of formaldehyde, 45-55 parts of water.Water-proof aagent of the invention can make bathroom waterproof window shade surface, and elasticity is good, more soft, and has good waterproof performance, ventilation and the advantage that penetrability is lower, anti-microbial property is excellent.

Description

A kind of water-proof aagent and its preparation method and application method
Technical field
The present invention relates to technical field of textile auxiliary agent, more specifically, it relates to a kind of water-proof aagent and its preparation side Method and methods for using them.
Background technique
Bathroom is suspended from outside the bathtub with shower nozzle with anti-Water curtain or the curtain shape article of shower area, Anti- Water curtain is mainly used for the spray of water for preventing from drenching with rain and plays the role of blocking to the outer place of shower, and for the people of shower, In When room temperature is lower, anti-Water curtain, which also has, gathers hot steam, maintains the effect of shower area local temperature.
Traditional bathroom is made with anti-Water curtain of materials such as plastics or cloth, and the anti-Water curtain of cloth type is by cloth by anti- Water arrangement is made, and there are mainly three types of the methods that water-proof finish is carried out to fabric, water repellent finish method, and top finish method and lamination are whole Logos.Wherein water repellent finish method is that high-density fabric is woven by using superfine fibre, and the gap very little between yarn can hinder Sealing drop passes through, but vapor can be made to penetrate, to have waterproof and moisture permeability.Top finish method is using dry or wet Top finish, so that fabric be made to have waterproofness, applies so that the gap coated of fabric surface is completely enclosed or is reduced to very little The micropore that hydrophilic radical or coating in layer agent are formed can make fabric have penetrability.Lamination method for sorting refers to using lamination Technology, so that fabric is combined with each other with micropore or the hydrophilic film lamination with waterproof and moisture permeability, so that it is saturating that waterproof is made Wet fabric.In these three methods, the applicable fabric type of top finish method is wider, and housekeeping operation is relatively simple, therefore applies Also relatively broad.
In the prior art, application No. is disclose one kind in the Chinese invention patent application file of CN201410249590.1 Water-proof aagent is grouped as by the group of following weight: 10~20 parts by weight of methanol, 40~60 weight of fluorine-containing boronic acid derivatives Measure part, 4~8 parts by weight of sodium soap, 5~10 parts by weight of polythene wax emulsion, 4~8 parts by weight of organosilicon, surfactant 1 200 parts by weight of~3 parts by weight and water, wherein fluorine-containing boronic acid derivatives be 2- trifluoromethylbenzene boronic acid, 3- trifluoromethylbenzene boronic acid, 4- trifluoromethylbenzene boronic acid, 4- trifluomethoxybenzene boron, 3,5- bis- (trifluoromethyl) and 3, one of 4,5- trifluoro phenyl boric acids.
Existing this water-proof aagent uses fluorine-containing boronic acid derivatives to be made of primary raw material, using common two leaching two It rolls production technology and is acted on by ligand complex, by water-proof aagent arrangement to textile, obtained textile not only has Good waterproof performance, and do not influence its intrinsic fastness to washing, whiteness again, but the fabric after finishing agent arrangement is soft Soft and elasticity is poor, and when pleated, folding line easily occurs in surface.
Therefore research and develop it is a kind of can make waterproof window shade surface that there is elasticity, and soft water-repellent paint is to need what is solved to ask Topic.
Summary of the invention
In view of the deficienciess of the prior art, the first purpose of this invention is to provide a kind of water-proof aagent, tool Having makes waterproof window shade surface have elasticity, and more soft advantage.
Second object of the present invention is to provide a kind of preparation method of water-proof aagent, with preparation method letter Single, easily operated advantage.
Third object of the present invention is to provide a kind of application method of water-proof aagent, with easy to operate excellent Point.
To realize above-mentioned first purpose, the present invention provides the following technical scheme that a kind of water-proof aagent, including it is following The component of parts by weight: 45-55 parts of acrylic acid esters co-polymers, 2.5-3.5 parts of acrylamide/ammonium acrylate copolymers, 1.8-2.2 Part formaldehyde, 45-55 parts of water.
By using above-mentioned technical proposal, the good fluidity of acrylic acid esters co-polymer forms a film in anti-Water curtain base fabric It is more soft, make scrim surfaces high resilience, acrylamide/ammonium acrylate copolymer be in water soluble polymer polyelectrolyte most Important kind, application is relatively broad, cooperates with acrylic acid esters co-polymer, can make water-proof aagent in anti-Water curtain base fabric Adherency securely, and makes water-proof finish form more soft and flexible film in base fabric, when anti-Water curtain folds, no It will appear fold.
Further, it comprises the following components in parts by weight: 50 parts of acrylic acid esters co-polymers, 3 parts of acrylamide/acrylic acid Ammonium copolymer, 2 parts of formaldehyde, 50 parts of water.
By using above-mentioned technical proposal, the proportion of each component is more accurate rationally, makes the water-proof aagent coating of preparation Effect is more preferable.
Further, component further includes 3.3-3.8 parts of synergist, and the synergist comprises the following components in parts by weight: 10- 15 parts of modified polyurethane emulsions, 12-18 parts of modified polyvinylalcohols, 0.1-0.5 parts of dispersing agents, 1.8-3.4 parts of amino resins, 0.1- 0.5 part of catalyst, 0.5-1 parts of defoaming agents, 80-90 parts of deionized waters, 10-15 parts of polyamide, 1.5-2.5 parts of three-proof finishing agents.
By using above-mentioned technical proposal, due to using modified polyurethane emulsion, modified polyvinylalcohol, polyamide and three proofings Finishing agent etc. prepares water-proof aagent, and after modified, barrier property is improved polyaminoester emulsion, and water resistance is improved, and resists Tearing strength is high, and resilience and wear-resisting property are good, and polyvinyl alcohol after modified, obtains the barrier property of vapor and oxygen Promoted, and Adhesion enhancement, polyamide is in molecule include amide structure high polymer, have that flexibility is good, intensity is high and resistance to The excellent feature of corrosive nature mutually cooperates with use with the pure and mild modified polyurethane emulsion of modified poly ethylene, has preferable water-fast Performance, three-proof finishing agent then further improve the Water-proof and oil-proof and anti-fouling effect of water-proof aagent, and each substance cooperates, Make water-proof aagent obtained that there is good water-proof effect, vapor transfer rate is low, and it is good to the barrier property of vapor, make bathroom waterproof window Curtain has preferable vapor gather effect.
Further, the modified polyurethane emulsion is made of following methods: (1) by 1-3 parts by weight organo montmorillonite, 1.5-2.5 parts by weight of graphite is mixed with 4-10 parts by weight polyether polyol, is heated under 85-90 DEG C of water-bath, and 2.5-3h is stirred, It is cooled to room temperature, and 5-15 parts by weight of deionized water is added, stirring filters, vacuum drying, grinding, crosses 200 meshes, is made and inserts Strata ethoxylated polyhydric alcohol；
(2) by 3.5-4.5 parts by weight polyether polyol, the resulting intercalation polyether polyol of 0.05-0.1 parts of steps (1), 1.2- 2.4 parts by weight N, N- dimethyl cyclohexyl amines, are stirred at 75-85 DEG C, react 5-8h, and three ethyl alcohol of 0.15-0.25 parts by weight is added Amine stirs 30-45min, and 5-8 parts by weight of deionized water is added and disperses that lotion is made, it is more that 5.5-8.5 parts by weight polymethine is added Polyphenyl polyisocyanate continues to stir 4-5h, modified polyurethane emulsion is made.
By using above-mentioned technical proposal, intercalation processing is carried out using montmorillonite and polyether polyol, so that organic illiteracy is de- Soil is uniformly dispersed in polyether polyol, then polyurethane is made in intercalation polyether polyol, thus promoted the heat resistance of polyurethane, Tensile strength, adhesion strength etc., the montmorillonite with more structures can make polyurethane specifically higher elasticity modulus, toughness and barrier Performance, and montmorillonite can play humidification in two-dimensional directional, silicate is orientated at slice plane in montmorillonite, so that poly- ammonia Ester is to vapor barrier property with higher, so that curtain be made to have preferable vapor gather effect.
Further, the modified polyvinylalcohol is made of following methods: by the pure and mild 3-9 weight of 1-3 weight account polyethylene Part water mixing, heating stirring, water-bath is kept the temperature at 95-100 DEG C, and polyvinyl alcohol after completely dissolution, is cooled to room temperature, addition 1.2- 1.8 parts by weight dehydrated alcohols, are sufficiently stirred, and it is even that 0.8-1.6 parts by weight nano silica, 0.1-0.3 parts by weight silane is added Join agent and 1.5-2.5 parts by weight of urea, stir evenly, modified polyvinylalcohol is made.
By using above-mentioned technical proposal, modification of the polyvinyl alcohol through nano silica, silane coupling agent and urea makes The hydrophobic performance and barrier property for obtaining polyvinyl alcohol get a promotion, and viscosity increases, so that water-proof aagent is solidificated in waterproof window After on curtain cloth, there is water-tolerant, the advantages of to the good barrier property of vapor.
Further, the polyvinyl alcohol degree of polymerization is 1700-1900, alcoholysis degree 99%；Amino resins is methyl-etherified One or more of melamine resin and methyl-etherified Lauxite；Catalyst be maleic acid, citric acid, p-methyl benzenesulfonic acid, It is one or more of in phosphoric acid, alkyl phosphoric acid；Defoaming agent is organic silicon defoamer, and dispersing agent is lauryl sodium sulfate.
Further, the synergist the preparation method is as follows:
S1, modified polyurethane emulsion is added in deionized water, stirs 1-2h at 85-95 DEG C；
S2, it is cooled to 65-70 DEG C, the amino resins of modified polyvinylalcohol, defoaming agent, catalyst and 2/3 dosage is added, stirring is anti- Answer 2-4h；
S3, it is cooled to 35-40 DEG C, amino resins, polyamide, long-acting antibiotic agent, dispersing agent and the three-prevention finishing of 1/3 dosage is added Agent is stirred to react 0.5-1h, stands, cooling, and water-proof aagent is made in discharging.
By using above-mentioned technical proposal, modified polyurethane emulsion is adequately dispersed in water, then by with other objects The cooperation of matter, water-proof aagent obtained have waterproof performance good, the advantage that vapor transfer rate is few, antibacterial effect is excellent.
Further, component further includes ingredient long-acting antibiotic agent, and the dosage of the long-acting antibiotic agent is 5-10 parts, the length Effect antibacterial agent is made of following methods: (1) 1.2-1.8 parts by weight of carbon nanotubes, 2.2-2.6 parts by weight of titanium dioxide being carried silver and resisted Microbial inoculum, 1.1-1.5 parts by weight Irgacare MP, 3-5 parts by weight epoxy resin mix in a high speed mixer It closes, then through melting extrusion, master batch is made；
(2) by master batch and 2.2-2.8 parts by weight propylene acid resin, 0.8-1.6 parts by weight chitosan, 0.6-1.2 parts by weight carbonic acid Calcium and 0.4-0.8 parts by weight styrax, mixing, melting extrusion crush, and long-acting antibiotic agent is made.
By using above-mentioned technical proposal, because being easy to grow in toilet of the bathroom with anti-Water curtain long-term disposal humidity Endophytic bacteria adds long-acting antibiotic agent in water-proof aagent, can make anti-Water curtain bacteria can be prevented from growing, mould etc.；By carbon nanometer Pipe, titanium dioxide carrying silver antimicrobials and Irgacare MP mixing, and with chitosan, calcium carbonate and rest in peace The mixing such as perfume (or spice) squeeze out, and silver ion is easier to penetrating cell wall in the antibacterial agent of preparation, to Escherichia coli, staphylococcus aureus and Gram- bacteria all has preferable antibacterial effect and longer Durability of antimicrobial effect.
To realize above-mentioned second purpose, the present invention provides the following technical scheme that a kind of preparation side of water-proof aagent Method, comprising the following steps: water is passed through formaldehyde while stirring, acrylic acid esters co-polymer and acrylamide/ammonium acrylate is added Copolymer is uniformly mixed, adds synergist and long-acting antibiotic agent, is uniformly mixed, and water-proof aagent is made.
It is first that formaldehyde is soluble in water by using above-mentioned technical proposal, it is acrylic acid esters co-polymer, acryloyl Amine/ammonium acrylate copolymer mixing, it is easy to operate.
To realize above-mentioned third purpose, the present invention provides the following technical scheme that a kind of application side of water-proof aagent Method, comprising the following steps: water-proof aagent is mixed with water, the water-proof finish liquid that concentration is 2-4% is configured to, by anti-Water curtain It is put into three-prevention finishing liquid with cloth, normal temperature dipping, dries 30-90s at 160-180 DEG C.
By using above-mentioned technical proposal, water-proof aagent is mixed with water, water-proof finish liquid, waterproof fabric for curtains is made Material is immersed in water-proof finish liquid, and uniformly, after drying, water-proof finish liquid is solidificated in cloth to the adherency of water-proof finish liquid on cloth On, being formed has waterproof performance good, and the anti-Water curtain that vapor transfer rate is few.
By using above-mentioned technical proposal, the waterproof Curtain cloth comfortable feel of the blended and comprehensive material of terylene, polyester-cotton blend.
In conclusion the invention has the following advantages:
The first, the present invention is due to using acrylic acid esters co-polymer, acrylamide/ammonium acrylate copolymer, formaldehyde and water preparation Water-proof aagent, the good film-forming property of acrylic acid esters co-polymer can be under the action of acrylamide/ammonium acrylate copolymer One layer is formed in anti-Water curtain base fabric with elastic and more soft waterproof membrane, making anti-Water curtain not only has preferable waterproof Performance is not in folding line when folding.
The second, increased due to the present invention using the preparation of the substances such as modified polyurethane emulsion, modified polyvinylalcohol and polyamide Agent is imitated, since tensile property raising, water resistance, barrier property and the resilience of modified polyurethane and polyvinyl alcohol are changed Kind, the high mechanical strength of polyamide, good toughness, corrosion resistance is strong, cooperates with modified polyurethane emulsion and modified polyvinylalcohol, energy Make water-proof aagent that there is preferable waterproof performance and higher vapor water barriers performance, to enhance the vapor of anti-Water curtain Gather effect.
Intercalation processing is preferably carried out to polyether polyol using organo montmorillonite in third, the present invention, then with intercalation polyethers Polyalcohol and isocyanates prepare polyaminoester emulsion, and humidification is played in montmorillonite in the two-dimensional direction, and silicate is in lamella Planar orientation, so that modified polyurethane has stronger vapor water barriers performance and waterproof performance.
4th, have in the present invention since long-acting antibiotic agent is made using carbon nanotube, titanium dioxide carrying silver antimicrobials etc. Stronger antibacterial effect and Durability of antimicrobial effect, make the anti-Water curtain in bathroom have in wet condition preferable antibacterial effect and compared with Strong Durability of antimicrobial effect.
Specific embodiment
Invention is further described in detail with reference to embodiments.
The preparation example 1-3 of modified polyurethane emulsion
In preparation example 1-3 organo montmorillonite be selected from Weifang Sheng Shi montmorillonite Science and Technology Ltd. sell article No. be 689 it is organic Montmorillonite, graphite are selected from the graphite that the article No. that Shijiazhuang Li Shang mineral products Co., Ltd sells is 612, and polyether polyol is selected from river The article No. that the Hai'an Su Sheng petrochemical plant is sold is the polyether polyol of P123.
Preparation example 1:(1) 1kg organo montmorillonite, 1.5kg graphite are mixed with 4kg polyether polyol, in 85 DEG C of water-bath Lower heating is stirred 2.5h, is cooled to room temperature, and 5kg deionized water is added, and stirring filters, vacuum drying, grinding, crosses 200 mesh Intercalation polyether polyol is made in sieve；
(2) by 3.5kg polyether polyol, the resulting intercalation polyether polyol of 0.05kg step (1), 1.2kg N, N- diformazan basic ring Hexylamine stirs at 75 DEG C, reacts 5h, and 0.15kg triethanolamine is added, and stirs 30min, and the dispersion of 5kg deionized water is added and is made 5.5kg polymethine polyphenyl polyisocyanate is added in lotion, continues to stir 4h, modified polyurethane emulsion is made.
Preparation example 2:(1) 2kg organo montmorillonite, 2kg graphite are mixed with 7kg polyether polyol, under 88 DEG C of water-bath Heating is stirred 2.8h, is cooled to room temperature, and 10kg deionized water is added, and stirring filters, vacuum drying, grinding, crosses 200 mesh Intercalation polyether polyol is made in sieve；
(2) by 4kg polyether polyol, the resulting intercalation polyether polyol of 0.08kg step (1), 1.8kg N, N- dimethyleyelohexane Amine stirs at 75 DEG C, reacts 6h, and 0.2kg triethanolamine is added, and stirs 40min, the dispersion of 6kg deionized water is added, cream is made 7kg polymethine polyphenyl polyisocyanate is added in liquid, continues to stir 4.5h, modified polyurethane emulsion is made.
Preparation example 3:(1) 3kg organo montmorillonite, 2.5kg graphite are mixed with 10kg polyether polyol, in 90 DEG C of water-bath Lower heating is stirred 3h, is cooled to room temperature, and 15kg deionized water is added, and stirring filters, vacuum drying, grinding, crosses 200 mesh Intercalation polyether polyol is made in sieve；
(2) by 4.5kg polyether polyol, the resulting intercalation polyether polyol of 0.1kg step (1), 2.4kg N, N- diformazan basic ring Hexylamine stirs at 85 DEG C, reacts 8h, and 0.25kg triethanolamine is added, and stirs 45min, and the dispersion of 8kg deionized water is added and is made 8.5kg polymethine polyphenyl polyisocyanate is added in lotion, continues to stir 5h, modified polyurethane emulsion is made.
The preparation example 4-6 of modified polyvinylalcohol
Nano silica is selected from the nanometer two that the article No. that Lingshou County Shuo Long mineral products processing factory sells is A300 in preparation example 4-6 Silica, silane coupling agent are selected from the silane coupling agent for the model 550 that Zhengzhou City Jinshui District Fu Jia chemical industry firm sells, urea The urea that the article No. sold selected from Beijing Kang Puhui dimension Science and Technology Ltd. is 003.
Preparation example 4: 1kg polyvinyl alcohol and 3kg water are mixed, and heating stirring, water-bath is kept the temperature at 95 DEG C, and polyvinyl alcohol fills After dividing dissolution, it is cooled to room temperature, 1.2kg dehydrated alcohol is added, is sufficiently stirred, 0.8kg nano silica, 0.1kg silicon is added Alkane coupling agent and 1.5kg urea, stir evenly, and modified polyvinylalcohol are made, the degree of polymerization of polyvinyl alcohol is 1700, and alcoholysis degree is 99%.
Preparation example 5: 2kg polyvinyl alcohol and 6kg water are mixed, and heating stirring, water-bath is kept the temperature at 98 DEG C, and polyvinyl alcohol fills After dividing dissolution, it is cooled to room temperature, 1.5kg dehydrated alcohol is added, is sufficiently stirred, 1.2kg nano silica, 0.2kg silicon is added Alkane coupling agent and 2kg urea, stir evenly, and modified polyvinylalcohol are made, the degree of polymerization of polyvinyl alcohol is 1800, and alcoholysis degree is 99%.
Preparation example 6: 3kg polyvinyl alcohol and 9kg water are mixed, and heating stirring, water-bath is kept the temperature at 100 DEG C, polyvinyl alcohol After completely dissolution, it is cooled to room temperature, 1.8kg dehydrated alcohol is added, is sufficiently stirred, 1.6kg nano silica, 0.3kg is added Silane coupling agent and 2.5kg urea, stir evenly, and modified polyvinylalcohol is made, and the degree of polymerization of polyvinyl alcohol is 1900, alcoholysis degree It is 99%.
The preparation example 7-9 of long-acting antibiotic agent
Carbon nanotube is selected from the carbon nanometer that the article No. that gloomy navigator Science and Technology Ltd., state, Shenzhen sells is 008 in preparation example 7-9 Pipe, titanium dioxide carrying silver antimicrobials are selected from the dioxy that the model TBD-TY01 of boda titanium white Products Co., Ltd sale is opened up in Wuxi Change titanium carrying silver antimicrobials, epoxy resin is selected from the epoxy resin that the article No. that the multifarious Chemical Co., Ltd. in Jiangyin sells is 001, propylene Acid resin is selected from the acrylic resin that the trade mark that Guangzhou Lian Shu commerce and trade Co., Ltd sells is C-735, and chitosan is selected from Shandong The chitosan that the article No. that great Xu bioengineering Co., Ltd sells is 101, styrax are selected from Anguo City tawny daylily commerce and trade Co., Ltd The styrax that the article No. of sale is 01.
Preparation example 7:(1) by 1.2kg carbon nanotube, 2.2kg titanium dioxide carrying silver antimicrobials, 1.1kg 2,4,4 '-three is chloro- 2 '-dihydroxy diphenyl ethers, 3kg epoxy resin mix in a high speed mixer, then through melting extrusion, master batch is made；
(2) it by master batch and 2.2kg acrylic resin, 0.8kg chitosan, 0.6kg calcium carbonate and 0.4kg styrax, mixes, melting It squeezes out, crushes, long-acting antibiotic agent is made.
Preparation example 8:(1) by 1.5kg carbon nanotube, 2.4kg titanium dioxide carrying silver antimicrobials, 1.3kg 2,4,4 '-three is chloro- 2 '-dihydroxy diphenyl ethers, 4kg epoxy resin mix in a high speed mixer, then through melting extrusion, master batch is made；
(2) it by master batch and 2.5kg acrylic resin, 1.2kg chitosan, 0.9kg calcium carbonate and 0.6kg styrax, mixes, melting It squeezes out, crushes, long-acting antibiotic agent is made.
Preparation example 9:(1) by 1.8kg carbon nanotube, 2.6kg titanium dioxide carrying silver antimicrobials, 1.5kg 2,4,4 '-three is chloro- 2 '-dihydroxy diphenyl ethers, 5kg epoxy resin mix in a high speed mixer, then through melting extrusion, master batch is made；
(2) it by master batch and 2.8kg acrylic resin, 1.6kg chitosan, 1.2kg calcium carbonate and 0.8kg styrax, mixes, melting It squeezes out, crushes, long-acting antibiotic agent is made.
Embodiment
In embodiment 1-9, acrylic acid esters co-polymer is selected from Liaoning Sunichem Co., Ltd., model HU- 212, acrylamide/ammonium acrylate copolymer is selected from Liaoning Sunichem Co., Ltd., model FS-80F, and formaldehyde is selected from Liaoning Sunichem Co., Ltd., model FS-850A, organic silicon defoamer are selected from Guangzhou Nan Hui new material Co., Ltd The organic silicon defoamer of the model CI-1104 of sale, methyl-etherified melamine resin are selected from Shandong Mo Bei Chemical Co., Ltd. The methyl-etherified melamine resin that the article No. of sale is 11, polyamide are selected from the model that Ao Hua plastic cement trade Co., Ltd sells 0330 polyamide, methyl-etherified Lauxite are selected from the methyl-etherified for the model M-03 that Ai Kema Chemical Co., Ltd. in Xiamen sells Lauxite, three-proof finishing agent are selected from the three-prevention finishing for the model SLR-01 that Shanghai Sai Chao auxiliary chemicals Co., Ltd sells Agent.
Embodiment 1: a kind of water-proof aagent, raw material proportioning is as shown in table 1, the water-proof aagent the preparation method comprises the following steps: 45kg water is passed through 1.8kg formaldehyde while stirring, 45kg acrylic acid esters co-polymer and 2.5kg acrylamide/acrylic acid is added Ammonium copolymer is uniformly mixed, and water-proof aagent is made.
The following steps are included: water-proof aagent is mixed with water, be configured to concentration is the application method of the three-proof finishing agent 2% water-proof finish liquid, waterproof fabric for curtains material is put into three-prevention finishing liquid, and normal temperature dipping dries 90s at 160 DEG C.
The raw material proportioning of water-proof aagent in 1 embodiment 1-9 of table
The raw material proportioning of synergist in 2 embodiment 4-6 of table
Embodiment 2-3: a kind of water-proof aagent, the difference from embodiment 1 is that, the raw material proportioning of water-proof aagent such as 1 institute of table Show.
Embodiment 4: a kind of water-proof aagent, the difference from embodiment 1 is that, it further include that 3.3kg increases in water-proof aagent Imitate agent, preparation method are as follows: 45kg water is passed through 1.8kg formaldehyde while stirring, be added 45kg acrylic acid esters co-polymer and 2.5kg acrylamide/ammonium acrylate copolymer is uniformly mixed, adds 3.3kg synergist, is uniformly mixed, and water-proof finish is made Agent；
Wherein the raw material proportioning of synergist is as shown in table 2, the preparation method of synergist the following steps are included:
S1,10kg modified polyurethane emulsion is added in 80kg deionized water, stirs 1h at 85 DEG C, modified polyurethane emulsion by Preparation example 1 is made；
S2,65 DEG C are cooled to, 12kg modified polyvinylalcohol, 0.5kg defoaming agent, 0.1kg catalyst and 1.2kg amino tree is added Rouge is stirred to react 2h, and modified polyvinylalcohol is made of preparation example 4, and defoaming agent is organic silicon defoamer, and catalyst is maleic acid, Amino resins is methyl-etherified melamine resin；
S3,35 DEG C are cooled to, 0.6kg amino resins, 10kg polyamide, 0.1kg dispersing agent and 1.5kg three-proof finishing agent are added, It is stirred to react 0.5h, is stood, water-proof aagent is made in cooling, discharging, and amino resins is methyl-etherified melamine resin, dispersion Agent is lauryl sodium sulfate.
The following steps are included: water-proof aagent is mixed with water, be configured to concentration is the application method of the three-proof finishing agent 3% water-proof finish liquid, waterproof fabric for curtains material is put into three-prevention finishing liquid, and normal temperature dipping dries 60s at 170 DEG C.
Embodiment 5: a kind of water-proof aagent, the difference with embodiment 4 be, the dosage of synergist is such as in water-proof aagent Shown in table 1, the raw material proportioning of synergist is as shown in table 2, and the preparation method of synergist is the following steps are included: S1, modified by 13kg Polyaminoester emulsion is added in 85kg deionized water, 1.5h is stirred at 90 DEG C, modified polyurethane emulsion is made of preparation example 2；
S2,68 DEG C are cooled to, 16kg modified polyvinylalcohol, 0.7kg defoaming agent, 0.3kg catalyst and 1.7kg amino tree is added Rouge is stirred to react 4h, and modified polyvinylalcohol is made of preparation example 6, and defoaming agent is organic silicon defoamer, and catalyst is that mass ratio is The citric acid and p-methyl benzenesulfonic acid of 1:1, amino resins are methyl-etherified Lauxite；
S3,38 DEG C are cooled to, 0.9kg amino resins, 13kg polyamide, 0.3kg dispersing agent and 2kg three-proof finishing agent is added, stirs Reaction 0.8h is mixed, is stood, water-proof aagent is made in cooling, discharging, and amino resins is methyl-etherified Lauxite, dispersing agent ten Sodium dialkyl sulfate.
Embodiment 6: a kind of water-proof aagent, the difference with embodiment 4 be, the dosage of synergist is such as in water-proof aagent Shown in table 1, the raw material proportioning of synergist is as shown in table 2, and the preparation method of synergist is the following steps are included: S1, modified by 15kg Polyaminoester emulsion is added in 90kg deionized water, 2h is stirred at 95 DEG C, modified polyurethane emulsion is made of preparation example 3；
S2,70 DEG C are cooled to, 18kg modified polyvinylalcohol, 1kg defoaming agent, 0.5kg catalyst and 2.7kg amino resins are added, It is stirred to react 3h, modified polyvinylalcohol is made of preparation example 5, and defoaming agent is organic silicon defoamer, and catalyst is that mass ratio is 1:1 Phosphoric acid and alkyl phosphoric acid, amino resins be methyl-etherified Lauxite；
S3,40 DEG C are cooled to, 0.7kg amino resins, 15kg polyamide, 0.5kg dispersing agent and 2.5kg three-proof finishing agent are added, It is stirred to react 1h, is stood, water-proof aagent is made in cooling, discharging, and amino resins is methyl-etherified Lauxite, dispersing agent ten Sodium dialkyl sulfate.
The following steps are included: water-proof aagent is mixed with water, be configured to concentration is the application method of the three-proof finishing agent 4% water-proof finish liquid, waterproof fabric for curtains material is put into three-prevention finishing liquid, and normal temperature dipping dries 30s at 180 DEG C.
Embodiment 7: a kind of water-proof aagent, the difference with embodiment 4 are, further include 5kg long-acting in water-proof aagent Antibacterial agent, preparation method are as follows: 45kg water is passed through 1.8kg formaldehyde while stirring, be added 45kg acrylic acid esters co-polymer and 2.5kg acrylamide/ammonium acrylate copolymer is uniformly mixed, and adds 3.3kg synergist and 5kg long-acting antibiotic agent, and mixing is equal It is even, water-proof aagent is made；Long-acting antibiotic agent is made of preparation example 7.
Embodiment 8: a kind of water-proof aagent, the difference from embodiment 1 is that, it further include 7.5kg long in water-proof aagent Imitate antibacterial agent, preparation method are as follows: 45kg water is passed through 1.8kg formaldehyde while stirring, 45kg acrylic acid esters co-polymer is added It with 2.5kg acrylamide/ammonium acrylate copolymer, is uniformly mixed, adds 7.5kg long-acting antibiotic agent, be uniformly mixed, be made anti- Water finishing agent；Long-acting antibiotic agent is made of preparation example 8.
Embodiment 9: a kind of water-proof aagent, the difference from embodiment 1 is that, it further include 10kg long-acting in water-proof aagent Antibacterial agent, preparation method are as follows: 45kg water is passed through 1.8kg formaldehyde while stirring, be added 45kg acrylic acid esters co-polymer and 2.5kg acrylamide/ammonium acrylate copolymer is uniformly mixed, and adds 3.3kg synergist and 5kg long-acting antibiotic agent, and mixing is equal It is even, water-proof aagent is made；Long-acting antibiotic agent is made of preparation example 9.
Comparative example comparative example 1: a kind of water-proof aagent, the difference from embodiment 1 is that, it is not added in synergist modified poly- Urethane lotion.
Comparative example 2: a kind of water-proof aagent, the difference from embodiment 1 is that, polyurethane is not added in synergist.
Comparative example 3: a kind of water-proof aagent, the difference from embodiment 1 is that, modified polyvinylalcohol is not by changing in synergist Property polyvinyl alcohol substitution.
Comparative example 4: the waterproof prepared with embodiment 1 in the Chinese invention patent file application No. is 201410249590.1 Finishing agent is as control, 3,5- bis- (trifluoromethyl), 40 parts by weight, 10 parts by weight of methanol, 5 parts by weight of sodium soap, poly- according to the ratio 8 parts by weight of ethylene wax emulsion (partial size 150nm), 5 parts by weight of organosilicon, 2 parts by weight of fatty alcohol polyoxyethylene ether, by each component 200 parts by weight of water are added in mixing, stir 150min, then ultrasound 15min, and standing obtains water-proof aagent.
Performance detection test one, waterproof performance test: waterproof is prepared according to the method in embodiment 1-9 and comparative example 1-4 Finishing agent mixes water-proof aagent with water, and the water-proof finish liquid that concentration is 3% is made, pure cotton base fabric is put into water-proof finish In liquid, 3h is impregnated, is taken out, is dried 90s at 160 DEG C, sample base fabric is made, according still further to AATCC22-2001 " draining: spraying examination Test " waterproof performance of testing water-proof finishing agent, with 10mL small syringe by water droplet in each sample base fabric, using JIC- 1 Wetness Angle Measuring Instrument measures contact angle, tests water vapour permeability using YG (B) 216X type vapor transfer rate instrument, test result is recorded in In table 3.
The performance test of each embodiment of table 3 and the water-proof aagent of each comparative example preparation
After water-proof aagent processing base fabric it can be seen from data in table 2 by embodiment 1-3 preparation, the waterproofness of base fabric Can be good, synergist, the pure cotton base fabric of water-proof aagent dipping and connecing for water of embodiment 4-7 preparation are added in embodiment 4-7 Feeler is big, and waterproof performance is good, and vapor transfer rate is small, has preferable vapor gather effect.
The water-proof aagent of comparative example 1-3 preparation is reduced with the contact angle of water, and waterproof performance is deteriorated, and permeable amount increases, Vapor gather effect is deteriorated.
Comparative example 4 is the water-proof aagent of prior art preparation, and waterproof performance is preferable, but vapor transfer rate is larger, and vapor is poly- It is poor to hold together effect.
Two, anti-folding line effect detection: water-proof aagent is prepared according to method in embodiment 1-9 and comparative example 4, and mixed with water It closes, the water-proof finish liquid that concentration is 3% is made, pure cotton base fabric is put into water-proof finish liquid and impregnates 3h, takes out and is done at 160 DEG C Dry 90s detects the feel of base fabric at -40 DEG C, and carries out 10 foldings to base fabric, and the article of 2kg is placed in base fabric, is placed 10min observes scrim surfaces folding line, will test detection and be reported in Table 4 below.
The anti-folding line effect detection result of water-proof aagent prepared by 4 embodiment 1-9 of table and comparative example 4
Project Feel (- 40 DEG C) Whether film cracks State at folding line
Embodiment 1 It is relatively soft It is no Microscratch
Embodiment 2 It is relatively soft It is no Microscratch
Embodiment 3 It is relatively soft It is no Microscratch
Embodiment 4 It is relatively soft It is no Microscratch
Embodiment 5 It is relatively soft It is no Microscratch
Embodiment 6 It is relatively soft It is no Microscratch
Embodiment 7 It is relatively soft It is no Microscratch
Embodiment 8 It is relatively soft It is no Microscratch
Embodiment 9 It is relatively soft It is no Microscratch
Comparative example 4 It is harder It is It is broken at folding line
After handling base fabric according to water-proof aagent prepared by method in embodiment 1-9 it can be seen from data in table 4, make base fabric Surface is more soft, and after folding and pressing, film be will not cracking, and have microscratch at folding line, and comparative example 4 is prior art preparation Water-proof aagent, feel is harder, and fold after folding line be broken.
Three, water-proof aagent, and and water anti-microbial property test: are prepared according to the method in embodiment 7-9 and comparative example 1-4 Mixing is made the water-proof finish liquid that concentration is 3%, pure cotton base fabric is put into water-proof finish liquid and impregnates 3h, takes out at 160 DEG C Dry 90s according to the antibiotic rate of FZ/T01021-1992 " antibacterial fabric method for testing performance " detection pure cotton base fabric, and will test As a result it is reported in Table 5 below.
The anti-microbial property testing result of water-proof aagent prepared by 5 embodiment 7-9 of table and comparative example 4
When the water-proof aagent prepared it can be seen from data in table 3 according to method in embodiment 7-9 was at three months, to large intestine The antibiotic rate of bacillus, staphylococcus aureus and gram- bacteria reaches 99% or more, at 9 months, to Escherichia coli, golden yellow The antibiotic rate of color staphylococcus and gram- bacteria still reaches 98% or more, and not only antibacterial effect is excellent, and Durability of antimicrobial effect compared with It is good.
Comparative example 4 is the water-proof aagent of prior art preparation, and antibacterial effect and Durability of antimicrobial effect are not so good as the present invention The water-proof aagent of embodiment 7-9 preparation.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this All by the protection of Patent Law in the scope of the claims of invention.

Claims (10)

1. a kind of water-proof aagent, which is characterized in that comprise the following components in parts by weight: 45-55 parts of acrylic acid esters co-polymers, 2.5-3.5 parts of acrylamide/ammonium acrylate copolymers, 1.8-2.2 parts of formaldehyde, 45-55 parts of water.
2. water-proof aagent according to claim 1, which is characterized in that comprise the following components in parts by weight: 50 parts of propylene Acid esters analog copolymer, 3 parts of acrylamide/ammonium acrylate copolymers, 2 parts of formaldehyde, 50 parts of water.
3. -2 described in any item water-proof aagents according to claim 1, which is characterized in that component further includes 3.3-3.8 parts of increasings Agent is imitated, the synergist comprises the following components in parts by weight: 10-15 parts of modified polyurethane emulsions, 12-18 parts of modified poly ethylenes Alcohol, 0.1-0.5 part dispersing agent, 1.8-3.4 parts of amino resins, 0.1-0.5 parts of catalyst, 0.5-1 parts of defoaming agents, 80-90 parts go Ionized water, 10-15 part polyamide, 1.5-2.5 parts of three-proof finishing agents.
4. water-proof aagent according to claim 3, which is characterized in that the modified polyurethane emulsion is by following methods system At: (1) 1-3 parts by weight organo montmorillonite, 1.5-2.5 parts by weight of graphite with 4-10 parts by weight polyether polyol are mixed, in 85- It is heated under 90 DEG C of water-bath, stirs 2.5-3h, be cooled to room temperature, and 5-15 parts by weight of deionized water is added, stirring filters, is true Sky is dry, grinding, crosses 200 meshes, and intercalation polyether polyol is made；
(2) by 3.5-4.5 parts by weight polyether polyol, the resulting intercalation polyether polyol of 0.05-0.1 parts of steps (1), 1.2- 2.4 parts by weight N, N- dimethyl cyclohexyl amines, are stirred at 75-85 DEG C, react 5-8h, and three ethyl alcohol of 0.15-0.25 parts by weight is added Amine stirs 30-45min, and 5-8 parts by weight of deionized water is added and disperses that lotion is made, it is more that 5.5-8.5 parts by weight polymethine is added Polyphenyl polyisocyanate continues to stir 4-5h, modified polyurethane emulsion is made.
5. water-proof aagent according to claim 3, which is characterized in that the modified polyvinylalcohol is by following methods system At: the pure and mild 3-9 parts by weight water of 1-3 weight account polyethylene is mixed, heating stirring, water-bath is kept the temperature at 95-100 DEG C, polyethylene Alcohol after completely dissolution, is cooled to room temperature, and 1.2-1.8 parts by weight dehydrated alcohol is added, is sufficiently stirred, and 0.8-1.6 parts by weight are added Nano silica, 0.1-0.3 parts by weight silane coupling agent and 1.5-2.5 parts by weight of urea, stir evenly, and modified poly- second is made Enol.
6. water-proof aagent according to claim 5, which is characterized in that the polyvinyl alcohol degree of polymerization is 1700-1900, Alcoholysis degree is 99%；Amino resins is one or more of methyl-etherified melamine resin and methyl-etherified Lauxite；Catalyst It is one or more of in maleic acid, citric acid, p-methyl benzenesulfonic acid, phosphoric acid, alkyl phosphoric acid；Defoaming agent is organic silicon defoamer, point Powder is lauryl sodium sulfate.
7. the preparation method of water-proof aagent according to claim 3, which is characterized in that the preparation method of the synergist It is as follows:
S1, modified polyurethane emulsion is added in deionized water, stirs 1-2h at 85-95 DEG C；
S2, it is cooled to 65-70 DEG C, the amino resins of modified polyvinylalcohol, defoaming agent, catalyst and 2/3 dosage is added, stirring is anti- Answer 2-4h；
S3, it is cooled to 35-40 DEG C, amino resins, polyamide, long-acting antibiotic agent, dispersing agent and the three-prevention finishing of 1/3 dosage is added Agent is stirred to react 0.5-1h, stands, cooling, and water-proof aagent is made in discharging.
8. -2 described in any item water-proof aagents according to claim 1, which is characterized in that component further includes ingredient long acting antibiotic Agent, the dosage of the long-acting antibiotic agent are 5-10 parts, and the long-acting antibiotic agent is made of following methods: (1) by 1.2-1.8 weight Part carbon nanotube, 2.2-2.6 parts by weight of titanium dioxide carrying silver antimicrobials, 1.1-1.5 parts by weight 2,4,4 '-three chloro- 2 '-hydroxyls two Phenylate, 3-5 parts by weight epoxy resin mix in a high speed mixer, then through melting extrusion, master batch is made；
(2) by master batch and 2.2-2.8 parts by weight propylene acid resin, 0.8-1.6 parts by weight chitosan, 0.6-1.2 parts by weight carbonic acid Calcium and 0.4-0.8 parts by weight styrax, mixing, melting extrusion crush, and long-acting antibiotic agent is made.
9. a kind of preparation method of water-proof aagent according to claim 1-8, which is characterized in that including following Step: being passed through formaldehyde for water while stirring, and acrylic acid esters co-polymer and acrylamide/ammonium acrylate copolymer, mixing is added Uniformly, synergist and long-acting antibiotic agent are added, is uniformly mixed, water-proof aagent is made.
10. a kind of application method of water-proof aagent according to claim 1-8, which is characterized in that including with Lower step: water-proof aagent is mixed with water, is configured to the water-proof finish liquid that concentration is 2-4%, waterproof fabric for curtains material is put into In three-prevention finishing liquid, normal temperature dipping dries 30-90s at 160-180 DEG C.
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