CN113880981A - Phosphorus-containing polyacrylate adhesive and preparation method and application thereof - Google Patents
Phosphorus-containing polyacrylate adhesive and preparation method and application thereof Download PDFInfo
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- CN113880981A CN113880981A CN202111306052.8A CN202111306052A CN113880981A CN 113880981 A CN113880981 A CN 113880981A CN 202111306052 A CN202111306052 A CN 202111306052A CN 113880981 A CN113880981 A CN 113880981A
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- phosphorus
- emulsifier
- polyacrylate adhesive
- containing polyacrylate
- monomer
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- 239000000853 adhesive Substances 0.000 title claims abstract description 44
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 44
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 40
- 239000011574 phosphorus Substances 0.000 title claims abstract description 40
- 229920000058 polyacrylate Polymers 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 48
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 16
- 239000003999 initiator Substances 0.000 claims abstract description 14
- 239000012875 nonionic emulsifier Substances 0.000 claims abstract description 11
- 239000004753 textile Substances 0.000 claims abstract description 11
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 9
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012874 anionic emulsifier Substances 0.000 claims abstract description 8
- 238000004043 dyeing Methods 0.000 claims abstract description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000007720 emulsion polymerization reaction Methods 0.000 claims abstract description 7
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000049 pigment Substances 0.000 claims abstract description 7
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 7
- 229910000162 sodium phosphate Inorganic materials 0.000 claims abstract description 7
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 7
- WDHYRUBXLGOLKR-UHFFFAOYSA-N phosphoric acid;prop-2-enoic acid Chemical compound OC(=O)C=C.OP(O)(O)=O WDHYRUBXLGOLKR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000839 emulsion Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 238000007599 discharging Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000003063 flame retardant Substances 0.000 abstract description 23
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 20
- 238000013329 compounding Methods 0.000 abstract description 2
- 229910052736 halogen Inorganic materials 0.000 abstract description 2
- 150000002367 halogens Chemical class 0.000 abstract description 2
- 239000004744 fabric Substances 0.000 description 8
- 238000005096 rolling process Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000002313 adhesive film Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000675 fabric finishing Substances 0.000 description 1
- 238000009962 finishing (textile) Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000009980 pad dyeing Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Images
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
- D06M15/356—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
- D06M15/3564—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms containing phosphorus
-
- 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
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/525—Polymers of unsaturated carboxylic acids or functional derivatives thereof
- D06P1/5257—(Meth)acrylic acid
-
- 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
- D06M2200/30—Flame or heat resistance, fire retardancy 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)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to the technical field of adhesive preparation, and particularly relates to a phosphorus-containing polyacrylate adhesive as well as a preparation method and application thereof. The phosphorus-containing polyacrylate adhesive is prepared by compounding anionic emulsifier sodium dodecyl sulfate and nonionic emulsifier E1309 to serve as an emulsifier, butyl acrylate to serve as a soft monomer, methyl methacrylate to serve as a hard monomer, phosphate acrylate to serve as a phosphorus-containing monomer, diacetone acrylamide and acrylic acid to serve as functional monomers, ammonium persulfate to serve as an initiator and sodium phosphate to serve as a pH regulator through emulsion polymerization. The phosphorus-containing polyacrylate adhesive prepared by the invention can be directly used for pigment dyeing and printing and functional finishing of textiles or compounded with other flame retardants, the flame retardant property of the textiles is improved, and the phosphorus-containing polyacrylate adhesive is safer to use because of no halogen.
Description
Technical Field
The invention belongs to the technical field of adhesive preparation, and particularly relates to a phosphorus-containing polyacrylate adhesive as well as a preparation method and application thereof.
Background
The acrylate adhesive has good fixation capacity on the paint, good film forming property, flexible and elastic film, and has the advantages of light resistance, aging resistance, low cost and the like of the coating, so the acrylate adhesive is commonly used for fabric finishing, paint dyeing and printing; however, with the widespread application of polyacrylate adhesives in textiles, the disadvantage of being flammable organic matters is gradually exposed, and the development of polyacrylate adhesives with flame retardant properties is becoming one of the research directions of the public.
Polyacrylate adhesives can currently be rendered flame retardant by two methods: firstly, a flame retardant (namely an additive type flame retardant adhesive) is directly added, such as CN101407717B, an organic phosphorus-nitrogen flame retardant is added into a polyacrylate adhesive; CN102604568A is added into the polyacrylate emulsion with the expansion type flame retardant composed of acid source, carbon source and gas source; secondly, a flame-retardant monomer is selected to participate in copolymerization and is introduced into a high molecular chain segment (namely, a reactive flame-retardant adhesive), such as: CN102964514B introduces fluorine, silicon and phosphoric acid groups into the macromolecular structure of polyacrylate emulsion. The former is decomposed at high temperature by added flame retardant, absorbs heat and reduces temperature, and simultaneously, water vapor generated by decomposition can absorb toxic gas and inhibit smoke, but the addition of the flame retardant is large, so that the emulsion stability, the mechanical strength and the appearance of an adhesive film are affected, the comprehensive performance is reduced, and the adhesive film has certain limitation. The latter introduces flame-retardant elements into the molecular structure of the adhesive to improve the flame-retardant effect of the polymer, and has the advantages of low toxicity and low smoke, so that the latter becomes the key point of the current research.
Disclosure of Invention
The invention aims to solve the defects in the prior art and simultaneously meet the requirements of pigment dyeing, printing and functional finishing of textiles, and provides the phosphorus-containing polyacrylate adhesive which can be directly used for pigment dyeing, printing and functional finishing of textiles or compounded with other flame retardants to improve the flame retardant property of the textiles.
In order to achieve the purpose, the invention adopts the following technical scheme:
the phosphorus-containing polyacrylate adhesive comprises the following raw materials in percentage by mass: 0.6-1.0% of compound emulsifier, 18-28% of soft monomer butyl acrylate, 4.5-7.0% of hard monomer methyl methacrylate, 5-8% of phosphorus-containing monomer acrylic acid phosphate, 0.6-1.2% of functional monomer diacetone acrylamide, 0.3-0.4% of functional monomer acrylic acid, 0.2-0.3% of initiator ammonium persulfate, 1.5-2.0% of pH regulator sodium phosphate and the balance of deionized water, wherein the sum of the mass percentages of all the raw materials is 100%;
the compound emulsifier consists of an anionic emulsifier sodium dodecyl sulfate and a nonionic emulsifier E1309.
Further, in the compound emulsifier, the mass ratio of the anionic emulsifier sodium dodecyl sulfate to the nonionic emulsifier E1309 is 2: 1.
further, the mass ratio of the soft monomer butyl acrylate to the hard monomer methyl methacrylate is 4: 1.
further, the phosphorus-containing monomer phosphoric acrylate is phosphoric acrylate FM-20.
The preparation method of the phosphorus-containing polyacrylate adhesive comprises the following steps:
step 1, preparation of pre-emulsion: adding an anionic emulsifier and a nonionic emulsifier into deionized water, stirring and dissolving; uniformly mixing soft monomers and hard monomers to obtain soft and hard mixed monomers, quickly dropwise adding all the soft and hard monomers into an emulsifier aqueous solution, stirring at the stirring speed of 1000-;
step 2, emulsion polymerization: placing the reaction container containing the base solution obtained in the step 1 in a water bath to heat, starting to dropwise add an aqueous solution of initiator ammonium persulfate when the temperature in the reaction container rises to 82 ℃, controlling the stirring speed at 300-350 r/min, dropwise adding the remaining 2/3 pre-emulsion and a mixed solution consisting of phosphorus-containing monomers, functional monomers, a pH regulator and deionized water when the emulsion in the reaction container gradually turns blue, controlling the dropwise adding time at 1-2 h, and controlling the reaction temperature at 85 ℃;
step 3, a heat preservation stage: after all monomers and initiators are dripped in the step 2, heating to 90 ℃, and preserving heat for 0.5-1 h;
step 4, discharging: cooling to below 40 ℃, filtering and discharging with a 200-mesh sieve, and adjusting the pH value to 6-7 with ammonia water to obtain the phosphorus-containing polyacrylate adhesive.
The use of the above-mentioned phosphorus-containing polyacrylate binders in textile processing.
Further, the application comprises pigment dyeing, printing and functional finishing.
The invention has the following beneficial effects: the invention endows the adhesive with flame retardant property by directly introducing functional group phosphate with flame retardant property into polymer macromolecules. The polyacrylate adhesive with flame retardant property is prepared by emulsion polymerization by using anionic emulsifier sodium dodecyl sulfate and nonionic emulsifier E1309 as a compounded emulsifier, butyl acrylate as a soft monomer, methyl methacrylate as a hard monomer, acrylic phosphate FM-20 as a phosphorus-containing monomer, diacetone acrylamide and acrylic acid as functional monomers, ammonium persulfate as an initiator and sodium phosphate as a pH regulator. The phosphorus-containing polyacrylate adhesive prepared by the invention can be directly used for pigment dyeing and printing and functional finishing of textiles or compounded with other flame retardants, the flame retardant property of the textiles is improved, and the phosphorus-containing polyacrylate adhesive is safer to use because of no halogen.
Drawings
FIG. 1 is a thermogravimetric analysis of the fabric of example 1 before and after finishing.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
A preparation method of a phosphorus-containing polyacrylate adhesive comprises the following steps:
(1) preparation of pre-emulsion: dissolving 0.2% of sodium dodecyl sulfate and 0.4% of nonionic emulsifier E1309 in 28.8% of deionized water, and uniformly stirring to obtain an emulsifier aqueous solution; uniformly mixing 24% of butyl acrylate soft monomer and 6% of methyl methacrylate hard monomer, quickly dripping into an emulsifier aqueous solution, stirring at a stirring speed of 1000 r/min for 30 min to prepare a pre-emulsion, taking out 2/3 pre-emulsion for dripping, and using 1/3 as a base solution;
(2) emulsion polymerization: placing the reaction container filled with the primer solution obtained in the step (1) in a water bath kettle, heating, starting to dropwise add an initiator aqueous solution consisting of 0.2% of ammonium persulfate and 15% of deionized water when the temperature in the reaction container rises to 82 ℃, controlling the stirring speed at 300 r/min, simultaneously dropwise adding the remaining 2/3 pre-emulsion and a mixed solution consisting of 5% of acrylic acid phosphate FM-20, 0.6% of diacetone acrylamide, 0.3% of acrylic acid, 1.5% of sodium phosphate and 18% of deionized water when the emulsion in the reaction container gradually turns blue, controlling the dropwise adding time for 1.5 h, and controlling the reaction temperature to be 85 ℃;
(3) in the heat preservation stage, after all the monomers and the initiator are dripped, the temperature is raised to 90 ℃, and the heat preservation is carried out for 0.5 h;
(4) discharging, cooling to below 40 ℃, filtering and discharging by using a 200-mesh sieve, and adjusting the pH value to 7 by using ammonia water to obtain the phosphorus-containing polyacrylate adhesive.
The prepared phosphorus-containing polyacrylate adhesive is used for finishing cotton fabrics by adopting a rolling and baking process, and the process conditions are as follows: soaking and rolling twice (with liquid rate of 100%), pre-baking at 100 deg.C for 3 min, and baking at 130 deg.C for 3 min.
The thermogravimetric analysis of the fabric before and after finishing is shown in figure 1. The figure shows that the char forming performance of the fabric finished by the phosphorus-containing polyacrylate adhesive is obviously improved.
Example 2
A preparation method of a phosphorus-containing polyacrylate adhesive comprises the following steps:
(1) preparation of pre-emulsion: dissolving 0.3% of sodium dodecyl sulfate and 0.6% of nonionic emulsifier E1309 in 21.4% of deionized water, and uniformly stirring to obtain an emulsifier aqueous solution; uniformly mixing 28% of butyl acrylate soft monomer and 7% of methyl methacrylate hard monomer, quickly dripping into an emulsifier aqueous solution, stirring at a stirring speed of 1100 r/min for 30 min to prepare a pre-emulsion, taking out 2/3 pre-emulsion for dripping, and using 1/3 as a base solution;
(2) emulsion polymerization: placing the reaction container filled with the base solution obtained in the step (1) in a water bath kettle, heating, starting to dropwise add an initiator aqueous solution consisting of 0.3% of ammonium persulfate and 15% of deionized water when the temperature in the reaction container rises to 82 ℃, controlling the stirring speed at 300 r/min, simultaneously dropwise adding the remaining 2/3 pre-emulsion and a mixed solution consisting of 6% of acrylic acid phosphate FM-20, 1% of diacetone acrylamide, 0.4% of acrylic acid, 2% of sodium phosphate and 18% of deionized water when the emulsion in the reaction container gradually turns blue, controlling the dropwise adding time for 2 h, and controlling the reaction temperature to be 85 ℃;
(3) and (3) a heat preservation stage: after all the monomers and the initiator are dripped, heating to 90 ℃, and preserving heat for 1 h;
(4) discharging: cooling to below 40 ℃, filtering and discharging with a 200-mesh sieve, and adjusting the pH value to 7 with ammonia water to obtain the phosphorus-containing polyacrylate adhesive.
The prepared phosphorus-containing polyacrylate adhesive is used for pigment dyeing of wool fabrics by adopting a pad dyeing process, and the process conditions are as follows: 20g/L of coating, 50 g/L of adhesive, two-dipping and two-rolling (the liquid carrying rate is 100%), pre-baking at 100 ℃ for 3 min, and baking at 130 ℃ for 3 min.
The after-flame time of the dyed fabric was 1.1s, the smoldering time was 0s, and the damaged length was 1.2cm, as measured by the vertical burning test method.
Example 3
A preparation method of a phosphorus-containing polyacrylate adhesive comprises the following steps:
(1) preparation of pre-emulsion: dissolving 0.25% of sodium dodecyl sulfate and 0.5% of nonionic emulsifier E1309 in 29.4% of deionized water, and uniformly stirring to obtain an emulsifier aqueous solution; uniformly mixing 20% of butyl acrylate soft monomer and 5% of methyl methacrylate hard monomer, quickly dripping into an emulsifier aqueous solution, stirring at a stirring speed of 1100 r/min for 30 min to prepare a pre-emulsion, taking out 2/3 pre-emulsion for dripping, and using 1/3 as a base solution;
(2) emulsion polymerization: placing the reaction container filled with 1/3 base solution in the step (1) in a water bath kettle, heating, starting to dropwise add initiator aqueous solution consisting of 0.25% of ammonium persulfate and 15% of deionized water when the temperature in the reaction container rises to 82 ℃, controlling the stirring speed at 350 r/min, simultaneously dropwise adding the rest 2/3 pre-emulsion and mixed solution consisting of 8% of acrylic acid phosphate FM-20, 1.2% of diacetone acrylamide, 0.4% of acrylic acid, 2% of sodium phosphate and 18% of deionized water when the emulsion in the reaction container gradually turns blue, controlling the dropwise adding time for 2 h, and controlling the reaction temperature to be 85 ℃;
(3) and (3) a heat preservation stage: after all the monomers and the initiator are dripped, heating to 90 ℃, and preserving heat for 1 h;
(4) discharging: cooling to below 40 ℃, filtering and discharging with a 200-mesh sieve, and adjusting the pH value to 7 with ammonia water to obtain the phosphorus-containing polyacrylate adhesive.
Compounding the prepared phosphorus-containing polyacrylate adhesive with a flame retardant RFR, and finishing cotton fabrics by adopting a rolling and baking process, wherein the process conditions are as follows: two-dipping and two-rolling (200 g/L of phosphorus-containing polyacrylate adhesive, 100 g/L of flame retardant RFR and 100 percent of liquid carrying rate), pre-baking at 100 ℃ for 3 min, and baking at 130 ℃ for 3 min.
The after-flame time of the finished fabric was measured to be 0s, the smoldering time was measured to be 2.1s, and the damaged length was measured to be 4.6cm by the vertical burn test method.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A phosphorus-containing polyacrylate adhesive characterized by: the raw materials comprise the following components in percentage by mass: 0.6-1.0% of compound emulsifier, 18-28% of soft monomer butyl acrylate, 4.5-7.0% of hard monomer methyl methacrylate, 5-8% of phosphorus-containing monomer acrylic acid phosphate, 0.6-1.2% of functional monomer diacetone acrylamide, 0.3-0.4% of functional monomer acrylic acid, 0.2-0.3% of initiator ammonium persulfate, 1.5-2.0% of pH regulator sodium phosphate and the balance of deionized water, wherein the sum of the mass percentages of all the raw materials is 100%;
the compound emulsifier consists of an anionic emulsifier sodium dodecyl sulfate and a nonionic emulsifier E1309.
2. The phosphorus-containing polyacrylate adhesive of claim 1, wherein: in the compound emulsifier, the mass ratio of the anionic emulsifier sodium dodecyl sulfate to the nonionic emulsifier E1309 is 2: 1.
3. the phosphorus-containing polyacrylate adhesive of claim 1, wherein: the mass ratio of the soft monomer butyl acrylate to the hard monomer methyl methacrylate is 4: 1.
4. the phosphorus-containing polyacrylate adhesive of claim 1, wherein: the phosphorus-containing monomer phosphoric acrylate is phosphoric acrylate FM-20.
5. The process for preparing a phosphorus-containing polyacrylate adhesive according to claim 1, wherein: the method comprises the following steps:
step 1, preparation of pre-emulsion: adding an anionic emulsifier and a nonionic emulsifier into deionized water, stirring and dissolving; uniformly mixing soft monomers and hard monomers to obtain soft and hard mixed monomers, quickly dropwise adding all the soft and hard monomers into an emulsifier aqueous solution, stirring at the stirring speed of 1000-;
step 2, emulsion polymerization: placing the reaction container containing the base solution obtained in the step 1 in a water bath to heat, starting to dropwise add an aqueous solution of initiator ammonium persulfate when the temperature in the reaction container rises to 82 ℃, controlling the stirring speed at 300-350 r/min, dropwise adding the remaining 2/3 pre-emulsion and a mixed solution consisting of phosphorus-containing monomers, functional monomers, a pH regulator and deionized water when the emulsion in the reaction container gradually turns blue, controlling the dropwise adding time at 1-2 h, and controlling the reaction temperature at 85 ℃;
step 3, a heat preservation stage: after all monomers and initiators are dripped in the step 2, heating to 90 ℃, and preserving heat for 0.5-1 h;
step 4, discharging: cooling to below 40 ℃, filtering and discharging with a 200-mesh sieve, and adjusting the pH value to 6-7 with ammonia water to obtain the phosphorus-containing polyacrylate adhesive.
6. Use of a phosphorus-containing polyacrylate binder according to claim 1 in textile processing.
7. Use according to claim 6, characterized in that: the textile processing comprises pigment dyeing, printing or functional finishing.
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