CN114108321A - Pure cotton fabric waterproof agent and preparation method thereof - Google Patents
Pure cotton fabric waterproof agent and preparation method thereof Download PDFInfo
- Publication number
- CN114108321A CN114108321A CN202111438385.6A CN202111438385A CN114108321A CN 114108321 A CN114108321 A CN 114108321A CN 202111438385 A CN202111438385 A CN 202111438385A CN 114108321 A CN114108321 A CN 114108321A
- Authority
- CN
- China
- Prior art keywords
- cotton fabric
- pure cotton
- polyvinyl alcohol
- emulsion
- reaction kettle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004744 fabric Substances 0.000 title claims abstract description 35
- 229920000742 Cotton Polymers 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 31
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000003999 initiator Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000000178 monomer Substances 0.000 claims abstract description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 5
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 5
- 239000000839 emulsion Substances 0.000 claims description 41
- 238000006243 chemical reaction Methods 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 claims description 6
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 5
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical group CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- ZNAOFAIBVOMLPV-UHFFFAOYSA-N hexadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)C(C)=C ZNAOFAIBVOMLPV-UHFFFAOYSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- ONJQDTZCDSESIW-UHFFFAOYSA-N polidocanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO ONJQDTZCDSESIW-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 claims description 4
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 2
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 2
- SNVLJLYUUXKWOJ-UHFFFAOYSA-N methylidenecarbene Chemical compound C=[C] SNVLJLYUUXKWOJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 claims description 2
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 claims description 2
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 2
- 230000002940 repellent Effects 0.000 claims 6
- 239000005871 repellent Substances 0.000 claims 6
- VEPKQEUBKLEPRA-UHFFFAOYSA-N VX-745 Chemical compound FC1=CC(F)=CC=C1SC1=NN2C=NC(=O)C(C=3C(=CC=CC=3Cl)Cl)=C2C=C1 VEPKQEUBKLEPRA-UHFFFAOYSA-N 0.000 claims 1
- 239000002131 composite material Substances 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 5
- 239000000835 fiber Substances 0.000 abstract description 3
- DVMSVWIURPPRBC-UHFFFAOYSA-N 2,3,3-trifluoroprop-2-enoic acid Chemical compound OC(=O)C(F)=C(F)F DVMSVWIURPPRBC-UHFFFAOYSA-N 0.000 abstract description 2
- 238000007730 finishing process Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 3
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004078 waterproofing Methods 0.000 description 2
- DEXFNLNNUZKHNO-UHFFFAOYSA-N 6-[3-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-3-oxopropyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)C(CCC1=CC2=C(NC(O2)=O)C=C1)=O DEXFNLNNUZKHNO-UHFFFAOYSA-N 0.000 description 1
- JTHZUSWLNCPZLX-UHFFFAOYSA-N 6-fluoro-3-methyl-2h-indazole Chemical compound FC1=CC=C2C(C)=NNC2=C1 JTHZUSWLNCPZLX-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- PZDUWXKXFAIFOR-UHFFFAOYSA-N hexadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)C=C PZDUWXKXFAIFOR-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
- D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/22—Esters containing halogen
- C08F220/24—Esters containing halogen containing perhaloalkyl radicals
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
- D06M15/277—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof containing fluorine
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a pure cotton fabric waterproof agent and a preparation method thereof, wherein the pure cotton fabric waterproof agent comprises the following components in percentage by mass: acrylate monomer: 5% -20%; perfluoroacrylate monomer: 3% -15%; emulsifier: 0.1 to 5 percent; initiator: 0.05 percent to 0.2 percent; chain transfer agent: 0.05 percent to 0.2 percent; polyvinyl alcohol: 0.5 to 5 percent; deionized water: 50 to 90 percent. According to the pure cotton fabric waterproof agent and the preparation method thereof, in the finishing process, the hydroxyl groups of the polyvinyl alcohol seal a large number of hydroxyl groups in the high molecular structure of the fibers of the pure cotton fabric, so that the waterproof grade of the waterproof agent is greatly improved.
Description
Technical Field
The invention relates to the technical field of waterproof agents, in particular to a pure cotton fabric waterproof agent and a preparation method thereof.
Background
In recent years, with the rapid development of social life, the living standard of people is improved, and the requirements on clothes, food, live and walk are higher and higher. For wearing, people not only need the clothes to have the functions of shielding, heat preservation and the like, but also need the clothes to have the functions of comfort, moisture permeability, perspiration, wrinkle resistance, water and oil resistance, easy decontamination, ultraviolet resistance, static resistance and the like. In the prior art, because the macromolecular structure of the pure cotton fabric fiber contains a large number of hydroxyl groups, the surface tension of the pure cotton fabric is higher than that of a chemical fiber fabric, and the waterproof grade of the pure cotton fabric is generally lower when the pure cotton fabric is subjected to waterproof finishing, so that a pure cotton fabric waterproof agent with high waterproof grade is provided.
Disclosure of Invention
The invention aims to provide a pure cotton fabric waterproof agent and a preparation method thereof.
In order to realize the aim, the invention provides a pure cotton fabric waterproof agent and a preparation method thereof, wherein the pure cotton fabric waterproof agent comprises the following components in percentage by mass:
preferably, the acrylate monomer is one or more of stearyl acrylate, stearyl methacrylate, cetyl acrylate, cetyl methacrylate, lauryl acrylate, lauryl methacrylate, acrylonitrile, styrene, vinyl acetate, glycidyl acrylate, and the like.
Preferably, the perfluoroacrylate monomer is H2C＝CH-COO-CH2-CH2-CnF2n+1、CH2＝C(CH3)-COO-CH2-CH2-CnF2n+1Wherein n is one or more of 2 to 16.
Preferably, the emulsifier is one or more of AEO-3, AEO-5, AEO-7, AEO-9, peregal O-15, peregal O-20, peregal O-25, octadecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride, etc.
Preferably, the initiator is persulfate, wherein the persulfate is one or more of ammonium persulfate, potassium persulfate and the like.
Preferably, the chain transfer agent is n-dodecyl mercaptan.
Preferably, the polyvinyl alcohol is one or a mixture of two of polyvinyl alcohol 1788, polyvinyl alcohol 1799 and the like.
A preparation method of a pure cotton fabric waterproof agent comprises the following reaction steps:
1) adding polyvinyl alcohol into a dry reaction kettle, then adding most of deionized water, heating to 70-90 ℃, and fully dissolving the polyvinyl alcohol to obtain a polyvinyl alcohol solution;
2) adding an acrylate monomer, a perfluorinated acrylate monomer, an emulsifier and a chain transfer agent into a dried reaction kettle, and dropwise adding the polyvinyl alcohol solution obtained in the step 1) into the reaction kettle while stirring at a high speed for emulsification to obtain a primary emulsion;
3) homogenizing the primary emulsion obtained in the step 2) twice in a high-pressure homogenizer, and respectively applying 20-40 kg of pressure to the homogenizer twice to obtain pre-emulsion;
4) preparing an initiator into a 5% aqueous initiator solution by using the rest deionized water;
5) adding 30-40% of the pre-emulsion obtained in the step 3) and 30-40% of the initiator aqueous solution obtained in the step 4) into a dry reaction kettle, introducing nitrogen, heating the reaction kettle to 75-90 ℃, and carrying out heat preservation reaction until the emulsion becomes semitransparent and blue-emitting to obtain seed emulsion;
6) dropwise adding the rest pre-emulsion and the initiator aqueous solution into the seed emulsion obtained in the step 5), continuously carrying out heat preservation reaction at the temperature of 75-90 ℃ for 2-4 h after dropwise adding is finished for 2-4 h, cooling, filtering, discharging and barreling to obtain the pure cotton fabric waterproof agent,
the invention has the beneficial effects that: in the synthesis process, polyvinyl alcohol is added into the traditional fluorine-containing acrylate emulsion waterproof agent, and the hydroxyl of the polyvinyl alcohol seals the hydroxyl in hydrophilic cellulose of pure cotton fabric, so that the waterproof grade of the waterproof agent is greatly improved.
The technical solution of the present invention is further described in detail by the following examples.
Detailed Description
The present invention will be further described with reference to examples, in which various chemicals and reagents are commercially available unless otherwise specified.
Example 1
1) Adding 10 g of polyvinyl alcohol 1788 into a dry reaction kettle, adding 757 g of deionized water into the reaction kettle, and heating to 80 ℃ to fully dissolve the polyvinyl alcohol 1788 to obtain a polyvinyl alcohol solution.
2) Adding 50 g of octadecyl acrylate, 10 g of vinyl acetate, 20 g of styrene, 40 g of hexadecyl methacrylate, 80 g of perfluoroalkyl hexyl ethyl acrylate, 3 g of AEO-9, 8 g of octadecyl trimethyl ammonium chloride and 1 g of n-dodecyl mercaptan into a dried reaction kettle, and dropwise adding the polyvinyl alcohol solution obtained in the step 1) into the reaction kettle while stirring at a high speed for emulsification to obtain a primary emulsion.
3) Homogenizing the primary emulsion obtained in the step 2) twice in a high-pressure homogenizer, and respectively using 25 kg and 35 kg of pressure to obtain the pre-emulsion.
4) 1 g of ammonium persulfate is prepared into a 5 percent initiator aqueous solution by using 20 g of deionized water for standby.
5) Adding 35% of the pre-emulsion obtained in the step 3) and 40% of the initiator aqueous solution obtained in the step 4) into a dry reaction kettle, introducing nitrogen, heating the reaction kettle to 80 ℃, and carrying out heat preservation reaction until the emulsion becomes semitransparent and turns blue light to obtain the seed emulsion.
6) And (3) dropwise adding the rest of pre-emulsion and initiator aqueous solution into the seed emulsion obtained in the step 5), finishing dropwise adding for 3h, and continuously carrying out heat preservation reaction for 3h at the temperature of 80 ℃. Cooling, filtering, discharging and barreling to obtain the pure cotton fabric waterproof agent.
Example 2
1) Adding 10 g of polyvinyl alcohol 1799 into a dry reaction kettle, adding 757 g of deionized water into the reaction kettle, and heating to 80 ℃ to fully dissolve the polyvinyl alcohol 1788 to obtain a polyvinyl alcohol solution.
2) Adding 50 g of octadecyl acrylate, 10 g of vinyl acetate, 20 g of styrene, 40 g of hexadecyl methacrylate, 80 g of perfluoroalkyl hexyl ethyl acrylate, 3 g of AEO-9, 8 g of octadecyl trimethyl ammonium chloride and 1 g of n-dodecyl mercaptan into a dried reaction kettle, and dropwise adding the polyvinyl alcohol solution obtained in the step 1) into the reaction kettle while stirring at a high speed for emulsification to obtain a primary emulsion.
3) Homogenizing the primary emulsion obtained in the step 2) twice in a high-pressure homogenizer, and respectively using 25 kg and 35 kg of pressure to obtain the pre-emulsion.
4) 1 g of ammonium persulfate is prepared into a 5 percent initiator aqueous solution by using 20 g of deionized water for standby.
5) Adding 35% of the pre-emulsion obtained in the step 3) and 40% of the initiator aqueous solution obtained in the step 4) into a dry reaction kettle, introducing nitrogen, heating the reaction kettle to 80 ℃, and carrying out heat preservation reaction until the emulsion becomes semitransparent and turns blue light to obtain the seed emulsion.
6) And (3) dropwise adding the remaining pre-emulsion and the initiator aqueous solution into the seed emulsion obtained in the step 5), finishing dropwise adding for 3h, and continuously carrying out heat preservation reaction for 3h at the temperature of 80 ℃. Cooling, filtering, discharging and barreling to obtain the pure cotton fabric waterproof agent.
Example 3
1) Adding 10 g of polyvinyl alcohol 1799 into a dry reaction kettle, adding 757 g of deionized water into the reaction kettle, and heating to 80 ℃ to fully dissolve the polyvinyl alcohol 1788 to obtain a polyvinyl alcohol solution.
2) Adding 50 g of octadecyl acrylate, 10 g of vinyl acetate, 20 g of styrene, 40 g of hexadecyl methacrylate, 80 g of perfluoroalkyl hexyl ethyl acrylate, 3 g of AEO-9, 8 g of octadecyl trimethyl ammonium chloride and 1 g of n-dodecyl mercaptan into a dried reaction kettle, and dropwise adding the polyvinyl alcohol solution obtained in the step 1) into the reaction kettle while stirring at a high speed for emulsification to obtain a primary emulsion.
3) Homogenizing the primary emulsion obtained in the step 2) twice in a high-pressure homogenizer, and respectively using 25 kg and 35 kg of pressure to obtain the pre-emulsion.
4) 1 g of potassium persulfate is prepared into a 5 percent aqueous initiator solution by using 20 g of deionized water for standby.
5) Adding 35% of the pre-emulsion obtained in the step 3) and 40% of the initiator aqueous solution obtained in the step 4) into a dry reaction kettle, introducing nitrogen, heating the reaction kettle to 80 ℃, and carrying out heat preservation reaction until the emulsion becomes semitransparent and turns blue light to obtain the seed emulsion.
6) And (3) dropwise adding the remaining pre-emulsion and the initiator aqueous solution into the seed emulsion obtained in the step 5), finishing dropwise adding for 3h, and continuously carrying out heat preservation reaction for 3h at the temperature of 80 ℃. Cooling, filtering, discharging and barreling to obtain the pure cotton fabric waterproof agent.
And (3) testing the waterproof performance:
the comparative example is a commercially available waterproofing agent not containing polyvinyl alcohol, and a cotton fabric is soaked in the waterproofing agent of examples 1 to 3 and the comparative example for 30 minutes, and a two-dip two-roll process (a rolling retention rate of 90% to 100%, room temperature) → pre-baking (80 ℃. times.3 minutes) → baking (160 ℃. times.2 minutes) is performed at a temperature of 25 ℃ to obtain a finished fabric.
The cotton fabric finished by the waterproof agent is subjected to open-air water spraying test according to AATCC-22, and the finished cotton fabric is detected by using a JC2000D3 type contact angle measuring instrument, and the experimental result is shown in Table 1.
TABLE 1
| Water resistance rating | Contact angle | |
| Example 1 | 5 | 158 |
| Example 2 | 5 | 155 |
| Example 3 | 5 | 156 |
| Comparative example | 4 | 149 |
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (8)
1. A pure cotton fabric waterproof agent is characterized in that: the composite material comprises the following components in percentage by mass:
2. a pure cotton fabric water repellent according to claim 1, characterized in that: the acrylate monomer is one or more of octadecyl acrylate, octadecyl methacrylate, hexadecyl acrylate, hexadecyl methacrylate, dodecyl acrylate, dodecyl methacrylate, acrylonitrile, styrene, vinyl acetate, glycidyl acrylate and the like.
3. A pure cotton fabric water repellent according to claim 1, characterized in that: the perfluoroacrylic ester monomer is H2C＝CH-COO-CH2-CH2-CnF2n+1、CH2＝C(CH3)-COO-CH2-CH2-CnF2n+1Wherein n is one or more of 2 to 16.
4. A pure cotton fabric water repellent according to claim 1, characterized in that: the emulsifier is one or more of AEO-3, AEO-5, AEO-7, AEO-9, peregal O-15, peregal O-20, peregal O-25, octadecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride, etc.
5. A pure cotton fabric water repellent according to claim 1, characterized in that: the initiator is persulfate, wherein the persulfate is one or more of ammonium persulfate, potassium persulfate and the like.
6. A pure cotton fabric water repellent according to claim 1, characterized in that: the chain transfer agent is n-dodecyl mercaptan.
7. A pure cotton fabric water repellent according to claim 1, characterized in that: the polyvinyl alcohol is one or a mixture of two of polyvinyl alcohol 1788, polyvinyl alcohol 1799 and the like.
8. A preparation method of a pure cotton fabric waterproof agent as claimed in claims 1-7, characterized by comprising the following reaction steps:
1) adding polyvinyl alcohol into a dry reaction kettle, then adding most of deionized water, heating to 70-90 ℃, and fully dissolving the polyvinyl alcohol to obtain a polyvinyl alcohol solution;
2) adding an acrylate monomer, a perfluorinated acrylate monomer, an emulsifier and a chain transfer agent into a dried reaction kettle, and dropwise adding the polyvinyl alcohol solution obtained in the step 1) into the reaction kettle while stirring at a high speed for emulsification to obtain a primary emulsion;
3) homogenizing the primary emulsion obtained in the step 2) twice in a high-pressure homogenizer, and respectively applying 20-40 kg of pressure to the homogenizer twice to obtain pre-emulsion;
4) preparing an initiator into a 5% aqueous initiator solution by using the rest deionized water;
5) adding 30-40% of the pre-emulsion obtained in the step 3) and 30-40% of the initiator aqueous solution obtained in the step 4) into a dry reaction kettle, introducing nitrogen, heating the reaction kettle to 75-90 ℃, and carrying out heat preservation reaction until the emulsion becomes semitransparent and blue-emitting to obtain seed emulsion;
6) dropwise adding the rest pre-emulsion and the initiator aqueous solution into the seed emulsion obtained in the step 5), continuously carrying out heat preservation reaction at the temperature of 75-90 ℃ for 2-4 h after dropwise adding is finished for 2-4 h, cooling, filtering, discharging and barreling to obtain the pure cotton fabric waterproof agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111438385.6A CN114108321A (en) | 2021-11-30 | 2021-11-30 | Pure cotton fabric waterproof agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111438385.6A CN114108321A (en) | 2021-11-30 | 2021-11-30 | Pure cotton fabric waterproof agent and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114108321A true CN114108321A (en) | 2022-03-01 |
Family
ID=80368161
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111438385.6A Pending CN114108321A (en) | 2021-11-30 | 2021-11-30 | Pure cotton fabric waterproof agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114108321A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111364A (en) * | 2015-08-04 | 2015-12-02 | 西安工程大学 | Fluorinated acrylate copolymer finishing agent and preparation method therefor |
| CN105777977A (en) * | 2016-03-22 | 2016-07-20 | 广州恒锦化工科技有限公司 | Fluorine-containing fabric waterproof agent and preparation method thereof |
| CN105924573A (en) * | 2016-06-13 | 2016-09-07 | 苏州大学 | Perfluoroalkyl polyene ester waterproof agent, preparation method and application |
| CN107245883A (en) * | 2017-06-20 | 2017-10-13 | 苏州联胜化学有限公司 | A kind of hard water three-proof finishing agent and preparation method thereof |
| CN108250350A (en) * | 2018-02-08 | 2018-07-06 | 江南大学 | A kind of preparation and its application of short-chain fluorine-containing copolymer water-refusing oil-refusing finishing agent |
-
2021
- 2021-11-30 CN CN202111438385.6A patent/CN114108321A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111364A (en) * | 2015-08-04 | 2015-12-02 | 西安工程大学 | Fluorinated acrylate copolymer finishing agent and preparation method therefor |
| CN105777977A (en) * | 2016-03-22 | 2016-07-20 | 广州恒锦化工科技有限公司 | Fluorine-containing fabric waterproof agent and preparation method thereof |
| CN105924573A (en) * | 2016-06-13 | 2016-09-07 | 苏州大学 | Perfluoroalkyl polyene ester waterproof agent, preparation method and application |
| CN107245883A (en) * | 2017-06-20 | 2017-10-13 | 苏州联胜化学有限公司 | A kind of hard water three-proof finishing agent and preparation method thereof |
| CN108250350A (en) * | 2018-02-08 | 2018-07-06 | 江南大学 | A kind of preparation and its application of short-chain fluorine-containing copolymer water-refusing oil-refusing finishing agent |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105504137B (en) | A kind of cold-resistant hot water soluble self-drying acrylic resin and preparation method thereof | |
| CN104892832B (en) | A kind of preparation method of micro-cross-linked polymethyl acyloxyethyl trimethyl ammonium chloride modification color fixing agent | |
| CN111410713A (en) | Plant-derived antibacterial microcapsule emulsion and preparation method thereof | |
| CN110607690A (en) | Polyacrylate-polyurethane composite emulsion with ultraviolet resistance function and preparation method and application thereof | |
| CN111286982B (en) | Water-repellent and oil-repellent finishing agent, preparation method and application thereof, and water-repellent and oil-repellent treatment method | |
| CN112853754A (en) | Water-repellent anti-ultraviolet polyester and preparation method thereof | |
| CN106758232A (en) | Bafta special-purpose water-proof oil-proofing agent, preparation method and its bafta processed through full low-temperature dyeing and finishing | |
| CN115874439A (en) | Antistatic breathable fabric and preparation method thereof | |
| CN114108321A (en) | Pure cotton fabric waterproof agent and preparation method thereof | |
| CN113308903B (en) | Water-based acrylate coating adhesive and preparation method thereof | |
| CN109056320B (en) | Flame-retardant hydrophobic finishing method based on cotton fabric | |
| CN108486899B (en) | Fabric softening finishing agent and preparation method thereof | |
| CN112175132A (en) | Composition containing acrylate compound and application | |
| CN110670359B (en) | Low-temperature type waterproof and oil-proof agent and preparation method thereof | |
| CN110306358B (en) | Processing method for dyeing real silk fabric by natural dye | |
| CN107686531B (en) | Polyacrylate emulsion for air filter paper and preparation method and application thereof | |
| CN108589284A (en) | The preparation method of fire-retardant carboxy methylation nylon fabric | |
| CN110845665B (en) | Fluorine-containing color fixing agent and preparation method thereof | |
| CN111851079B (en) | Microencapsulated wormwood essential oil-containing mosquito-repellent fabric finishing agent and mosquito-repellent fabric finishing method | |
| CN111286997B (en) | Silk floss dyeing method based on phellinus igniarius spore powder | |
| CN105401429A (en) | Low-temperature three-proofing finishing agent, preparation method and application of finishing agent to fabric | |
| CN109897139A (en) | A kind of fabric stiffening agent and preparation method thereof | |
| CN105732886B (en) | A kind of water repellent for textile and anti UV finishing agent, preparation method and applications | |
| CN105671995A (en) | Environmental-friendly dyeing antishifting agent and preparation method thereof | |
| CN107904333B (en) | Preparation process of fireproof flame-retardant garment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220301 |
|
| RJ01 | Rejection of invention patent application after publication |