CN112062973B - Emulsification method of ethylene-vinyl acetate copolymer - Google Patents
Emulsification method of ethylene-vinyl acetate copolymer Download PDFInfo
- Publication number
- CN112062973B CN112062973B CN202011011607.1A CN202011011607A CN112062973B CN 112062973 B CN112062973 B CN 112062973B CN 202011011607 A CN202011011607 A CN 202011011607A CN 112062973 B CN112062973 B CN 112062973B
- Authority
- CN
- China
- Prior art keywords
- eva
- water
- eva resin
- reaction kettle
- vinyl acetate
- 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.)
- Active
Links
- 239000005038 ethylene vinyl acetate Substances 0.000 title claims abstract description 102
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 title claims abstract description 102
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000004945 emulsification Methods 0.000 title claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 61
- 239000011347 resin Substances 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- 239000000839 emulsion Substances 0.000 claims abstract description 31
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 26
- 239000000155 melt Substances 0.000 claims description 19
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 239000012875 nonionic emulsifier Substances 0.000 claims description 7
- 238000010907 mechanical stirring Methods 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 229940096992 potassium oleate Drugs 0.000 claims description 4
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 claims description 4
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 3
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 13
- 239000004831 Hot glue Substances 0.000 abstract description 4
- 238000010008 shearing Methods 0.000 abstract description 2
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 230000009977 dual effect Effects 0.000 abstract 1
- 239000012847 fine chemical Substances 0.000 abstract 1
- 239000004753 textile Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000004359 castor oil Substances 0.000 description 2
- 235000019438 castor oil Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000614 phase inversion technique Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 2
- 229920000053 polysorbate 80 Polymers 0.000 description 2
- -1 potassium fatty acid Chemical class 0.000 description 2
- VAKMIIPDYZXBEV-DPMBMXLASA-M potassium;(z,12r)-12-hydroxyoctadec-9-enoate Chemical compound [K+].CCCCCC[C@@H](O)C\C=C/CCCCCCCC([O-])=O VAKMIIPDYZXBEV-DPMBMXLASA-M 0.000 description 2
- NVJCKICOBXMJIJ-UHFFFAOYSA-M potassium;1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylate Chemical compound [K+].C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C([O-])=O NVJCKICOBXMJIJ-UHFFFAOYSA-M 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 229920003180 amino resin Polymers 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses an emulsification method of an ethylene-vinyl acetate copolymer, which belongs to the field of fine chemical engineering, and utilizes the dual actions of high-speed shearing action and an emulsifier to disperse molten EVA resin into fine EVA particles, and then an emulsion conversion method is used for converting EVA with a water-in-oil structure into EVA emulsion with an oil-in-water structure, so that the aim of preparing EVA aqueous emulsion is finally fulfilled. The EVA emulsion prepared by the method can be used in the field of water-based hot melt adhesives, has important application in the fields of carpets, artificial lawns and textiles, and has higher practical application significance.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to an emulsification method of an ethylene-vinyl acetate copolymer.
Background
Ethylene-vinyl acetate copolymer resin (EVA) is a novel hot melt adhesive and can be widely applied to the fields of book wireless binding, furniture edge sealing, carpets, artificial lawns and the like. Generally, the content of vinyl acetate in the EVA resin is between 5 and 55 percent, and the crystallization property of the resin is reduced due to the introduction of vinyl acetate monomer, so that the toughness and the impact resistance of the EVA resin are improved, and the application field of the EVA resin is gradually increasing year by year.
In recent years, with the increasing environmental protection requirements, the global productivity of aqueous polymer products, such as aqueous polyurethane and aqueous acrylic resin products, has been increased to a level of megaton, and most of the currently available EVA products in the market are EVA emulsions with high vinyl acetate content (vinyl acetate content > 60%) prepared by directly polymerizing ethylene and vinyl acetate monomers, and the emulsions have poor water resistance due to the excessively high vinyl acetate content and can be only used in products with low requirements on water resistance. How to develop an aqueous EVA product with low vinyl acetate content is a technical problem which is always concerned in the industrial production and application fields. Because of the limitation of the reactivity ratio of vinyl monomers and vinyl acetate monomers, the emulsion polymerization technology is difficult to directly synthesize an aqueous emulsion product with low vinyl acetate content, so that the direct emulsification of EVA resin with low vinyl acetate content into EVA emulsion is the technical scheme with the greatest feasibility at present, and few documents are reported in the current literature. As reported in fine petrochemical engineering (2016, 33, 17-20), a method for preparing ethylene-vinyl acetate copolymer emulsion is characterized in that a solvent such as toluene is adopted to dissolve EVA resin, then a composite emulsifying system is utilized to emulsify the EVA resin to prepare oil-in-water emulsion, then a steering agent is added, the mixture is still layered, water is separated to prepare oily EVA emulsion, the dispersed phase of the emulsion is EVA resin, the continuous phase is toluene, and the emulsion can be used in the fields of crude oil pour point depressant and the like. Patent CN110452393a reports a method for preparing aqueous EVA resin dispersion by melting EVA resin and rheological polyamide wax under high pressure, then adding water and stirring at high speed, and the method is characterized in that the preparation process is simple, high pressure reaction is required, the pressure can reach 10Mpa at maximum, and the rheological agent usage amount is up to 40-60% of EVA resin. Patent CN108084370a reports a preparation method of low-temperature heat-seal EVA emulsion, which is to directly emulsify EVA resin, emulsifier, defoamer, amino resin and the like in a reaction kettle, and the heat-seal temperature of the EVA emulsion prepared by the method is lower, but the particle size of the prepared EVA emulsion is larger.
Therefore, developing a novel simple EVA emulsification method is a problem to be solved by those skilled in the art.
Disclosure of Invention
In view of this, the invention provides an emulsification method of ethylene-vinyl acetate copolymer, which adopts a phase inversion method to carry out secondary emulsification on EVA resin, and the specific process is that EVA resin is melted under the action of a small amount of solvent and temperature rise to form EVA resin in a melt state, then dispersing agent, surfactant and a small amount of water are introduced into EVA resin in the melt state, the EVA resin in the melt state and water are formed into a high-viscosity multicomponent system in a water-in-oil state by using the strong stirring action of a homogenizer, then water is added into the system to carry out steering under the action of high-speed shearing, and finally the EVA resin emulsion in an oil-in-water state is formed after cooling.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the emulsification method of the ethylene-vinyl acetate copolymer comprises the following raw materials in parts by mass:
(1) 100 parts of EVA resin, 5-100 parts of solvent, 3-15 parts of ionic emulsifier and 1-10 parts of nonionic emulsifier are placed in a reaction kettle, and under the mechanical stirring action of 50-300 rpm at 10-80 ℃, the EVA resin is completely dissolved in the solvent;
(2) Adding 5-40 parts of deionized water into a reaction kettle, stirring at 50-300 rpm to fully mix the deionized water with EVA resin dissolved in a solvent, and stirring at 800-2000 rpm until the mixture is in a water-in-oil state, namely the EVA resin in a melt state is a continuous phase, and water is a disperse phase;
(3) Adding 50-200 parts of deionized water and 1-10 parts of ionic emulsifier into the reaction kettle, stirring at 50-300 rpm until the EVA resin in a melt state in the reaction kettle is reversely converted into an oil-in-water state, continuously stirring for 10-60 min, and gradually cooling to room temperature to obtain the aqueous EVA emulsion.
Preferably, the EVA resin is EVA resin with the vinyl acetate content of 5-40%.
Preferably, the EVA resin is EVA resin with 15-35% of vinyl acetate content.
Preferably, the solvent is one or more of cyclohexane, alkyl solvent oil and cycloalkyl solvent oil.
Preferably, the nonionic emulsifier is one or more of polyoxyethylene ether, polyethylene glycol, tween 80, tween 20, OP-10 and castor oil polyoxyethylene ether.
Preferably, the ionic emulsifier is one or more of potassium abietate, potassium oleate, potassium fatty acid, potassium ricinoleate, fatty alcohol polyoxyethylene ether sulfate, alpha-sodium alkenyl sulfonate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate.
Compared with the prior art, the invention provides the emulsification method of the ethylene-vinyl acetate copolymer, which adopts the phase inversion method to carry out secondary emulsification on EVA resin, so as to prepare the EVA resin emulsion taking water as a continuous phase, has good emulsion stability, can replace hot melt adhesive for use, can be used in the fields of book wireless packaging, carpets, artificial lawns and the like, and has higher practical application significance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the particle size distribution of EVA emulsion prepared in example 1 of the present invention;
FIG. 2 is a graph showing the particle size distribution of EVA emulsion prepared in example 2 of the present invention;
FIG. 3 is a graph showing the particle size distribution of EVA emulsion prepared in example 3 of the present invention;
FIG. 4 is a graph showing the particle size distribution of EVA emulsion prepared in example 4 of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) 100g of EVA resin with the vinyl acetate content of 28%, 10g of cyclohexane, 10g of polyvinyl alcohol and 5g of nonionic emulsifier op-10 are placed in a reaction kettle, and are melted under the mechanical stirring action of 50rpm at 80 ℃ to form molten EVA resin;
(2) When the temperature of the EVA resin in the molten state of the reaction kettle is reduced to 70 ℃, 5g of potassium oleate and 20g of deionized water are slowly added into the reaction kettle, and the EVA resin in the molten state is fully mixed with water by stirring at 300 rpm. In the process of rapid stirring at 800rpm, the viscosity of the EVA melt is rapidly increased to be converted into a water-in-oil state, namely, the EVA resin in the melt state is a continuous phase, and water is a disperse phase;
(3) 150g of deionized water is continuously added into the reaction kettle, and simultaneously, the stirring is carried out at 200rpm, the EVA resin in the melt state in the reaction kettle is changed into an oil-in-water state due to the reverse addition of water, the stirring is continuously carried out for 30min, the temperature is gradually reduced, and the aqueous EVA emulsion can be obtained under the condition that the temperature in the reaction kettle is reduced to room temperature.
Example 2
(1) Placing 100g of EVA resin with 15% vinyl acetate content, 10g of alkyl solvent oil, 10g of polyvinyl alcohol and 5g of non-ionic emulsifier Tween 80 in a reaction kettle, and melting under the mechanical stirring action of 150rpm at 110 ℃ to form molten EVA resin;
(2) When the temperature of the EVA resin in the molten state of the reaction kettle is reduced to 70 ℃,10 g of disproportionated potassium abietate and 30g of deionized water are slowly added into the reaction kettle, and stirring is carried out at 200rpm so that the EVA resin in the molten state is fully mixed with water. In the process of rapid stirring at 1500rpm, the viscosity of EVA melt is rapidly increased to be converted into a water-in-oil state, namely EVA resin in the melt state is a continuous phase, and water is a disperse phase;
(3) And continuously adding 140g of deionized water into the reaction kettle, simultaneously stirring rapidly, converting the EVA resin in a melt state in the reaction kettle into an oil-in-water state due to the reverse addition of water, continuously stirring for 20min, gradually cooling, and obtaining the aqueous EVA emulsion under the condition that the temperature in the reaction kettle is reduced to room temperature.
Example 3
(1) 100g of EVA resin with 33% vinyl acetate content, 5g of alkyl solvent oil, 5g of cyclohexane, 10g of polyvinyl alcohol and 5g of nonionic emulsifier castor oil polyoxyethylene ether and 5g of polyethylene glycol are placed in a reaction kettle, and are melted under the mechanical stirring action of 200rpm at 90 ℃ to form molten EVA resin;
(2) When the temperature of the EVA resin in the molten state of the reaction kettle is reduced to 75 ℃,10 g of potassium ricinoleate and 20g of deionized water are slowly added into the reaction kettle, and the EVA resin in the molten state is fully mixed with water by stirring at a speed of 100 rpm. During stirring at 1800rpm, the viscosity of EVA melt rises rapidly and is converted into a water-in-oil state, namely EVA resin in the melt state is a continuous phase, and water is a disperse phase;
(3) 180g of deionized water is continuously added into the reaction kettle, stirring is carried out at 200rpm, EVA resin in a melt state in the reaction kettle is changed into an oil-in-water state due to the reverse addition of water, stirring is continuously carried out for 20min, and then the temperature is gradually reduced, and the aqueous EVA emulsion can be obtained under the condition that the temperature in the reaction kettle is reduced to room temperature.
Example 4
(1) 100g of EVA resin with 33% vinyl acetate content, 5g of alkyl solvent oil and 5g of cycloalkyl solvent oil, 8g of polyvinyl alcohol and 5g of nonionic emulsifier polyoxyethylene ether and 5g of Tween 20 emulsifier are placed in a reaction kettle, and are melted under the mechanical stirring action of 200rpm at 100 ℃ to form molten EVA resin;
(2) When the temperature of the EVA resin in the melt state of the reaction kettle is reduced to 70 ℃, slowly adding 5g of the ionic emulsifier fatty alcohol polyoxyethylene ether sulfate, 5g of potassium oleate, 20g of deionized water and stirring at 150rpm to fully mix the EVA resin in the melt state with water, wherein the viscosity of the EVA melt is quickly increased to be converted into a water-in-oil state in the stirring process at 1000rpm, namely the EVA resin in the melt state is a continuous phase, and the water is a disperse phase;
(3) And continuously adding 180g of deionized water into the reaction kettle while rapidly stirring, wherein the EVA resin in a melt state in the reaction kettle is changed into an oil-in-water state due to the reverse addition of water, continuously stirring for 25min, gradually cooling, and obtaining the aqueous EVA emulsion under the condition that the temperature in the reaction kettle is reduced to room temperature.
The EVA emulsion obtained in examples 1-4 was subjected to particle size and particle size distribution measurement by using dynamic light scattering laser particle sizer (ZS-90) of Markov company in UK at 25℃to obtain data shown in FIGS. 1-4, wherein the average particle size of the sample prepared in example 1 was 312nm, the average particle size of the sample prepared in example 2 was 487nm, the average particle size of the sample prepared in example 3 was 546nm, and the average particle size of the sample prepared in example 4 was 196nm. The EVA emulsion prepared by the method has good stability and can be used as a water-based hot melt adhesive as no layering phenomenon is found after the EVA emulsion is still observed for 21 days.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (1)
1. The emulsification method of the ethylene-vinyl acetate copolymer is characterized by comprising the following steps of:
(1) 100g of EVA resin with 33% of vinyl acetate content, 5g of alkyl solvent oil and 5g of cycloalkyl solvent oil, 8g of polyvinyl alcohol and 5g of nonionic emulsifier polyoxyethylene ether and 5g of tween 20 emulsifier are placed in a reaction kettle, and are melted under the mechanical stirring action of 200rpm at 100 ℃ to form molten EVA resin;
(2) When the temperature of the EVA resin in the melt state of the reaction kettle is reduced to 70 ℃, slowly adding 5g of the ionic emulsifier fatty alcohol polyoxyethylene ether sulfate, 5g of potassium oleate, 20g of deionized water and stirring at 150rpm to fully mix the EVA resin in the melt state with water, wherein the viscosity of the EVA melt is quickly increased to be converted into a water-in-oil state in the stirring process at 1000rpm, namely the EVA resin in the melt state is a continuous phase, and the water is a disperse phase;
(3) And continuously adding 180g of deionized water into the reaction kettle while rapidly stirring, wherein the EVA resin in a melt state in the reaction kettle is changed into an oil-in-water state due to the reverse addition of water, continuously stirring for 25min, gradually cooling, and obtaining the aqueous EVA emulsion under the condition that the temperature in the reaction kettle is reduced to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011011607.1A CN112062973B (en) | 2020-09-23 | 2020-09-23 | Emulsification method of ethylene-vinyl acetate copolymer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011011607.1A CN112062973B (en) | 2020-09-23 | 2020-09-23 | Emulsification method of ethylene-vinyl acetate copolymer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112062973A CN112062973A (en) | 2020-12-11 |
| CN112062973B true CN112062973B (en) | 2023-08-25 |
Family
ID=73683884
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011011607.1A Active CN112062973B (en) | 2020-09-23 | 2020-09-23 | Emulsification method of ethylene-vinyl acetate copolymer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112062973B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112795336B (en) * | 2020-12-29 | 2023-02-03 | 广东威斯达新材料有限公司 | Water-based EVA hot melt adhesive, and preparation method and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0389893A2 (en) * | 1989-03-23 | 1990-10-03 | Air Products And Chemicals, Inc. | High solids emulsions of vinyl acetate/ethylene copolymers containing a water soluble comonomer |
| US5169891A (en) * | 1988-10-21 | 1992-12-08 | Nicholas Brown | Coating compositions comprising a blend of an ethylene vinyl acetate polymer with a fatty acid and emulsions |
| JP2000302808A (en) * | 1999-04-19 | 2000-10-31 | Denki Kagaku Kogyo Kk | Ethylene-vinyl acetate copolymer emulsion and its preparation |
| CN1306015A (en) * | 2000-12-27 | 2001-08-01 | 中国科学院长春应用化学研究所 | Process for preparing high-ethylene ethylene vinylacetate latex |
| CN1400244A (en) * | 2001-07-31 | 2003-03-05 | 三井武田化学株式会社 | Water soluble emulsion composite and adhesive composite |
| JP2007002212A (en) * | 2005-05-25 | 2007-01-11 | Arakawa Chem Ind Co Ltd | Tackifying resin emulsion, method for producing the same and aqueous pressure-sensitive adhesive/adhesive composition |
| CN107793518A (en) * | 2016-09-07 | 2018-03-13 | 中国石油化工股份有限公司 | Application of the nertralizer in the emulsion particle diameter of control EVA elastomer emulsions |
| CN108084370A (en) * | 2017-12-21 | 2018-05-29 | 海南必凯水性新材料有限公司 | A kind of low-temperature heat-sealing EVA lotions and its preparation method and application |
-
2020
- 2020-09-23 CN CN202011011607.1A patent/CN112062973B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5169891A (en) * | 1988-10-21 | 1992-12-08 | Nicholas Brown | Coating compositions comprising a blend of an ethylene vinyl acetate polymer with a fatty acid and emulsions |
| EP0389893A2 (en) * | 1989-03-23 | 1990-10-03 | Air Products And Chemicals, Inc. | High solids emulsions of vinyl acetate/ethylene copolymers containing a water soluble comonomer |
| JP2000302808A (en) * | 1999-04-19 | 2000-10-31 | Denki Kagaku Kogyo Kk | Ethylene-vinyl acetate copolymer emulsion and its preparation |
| CN1306015A (en) * | 2000-12-27 | 2001-08-01 | 中国科学院长春应用化学研究所 | Process for preparing high-ethylene ethylene vinylacetate latex |
| CN1400244A (en) * | 2001-07-31 | 2003-03-05 | 三井武田化学株式会社 | Water soluble emulsion composite and adhesive composite |
| JP2007002212A (en) * | 2005-05-25 | 2007-01-11 | Arakawa Chem Ind Co Ltd | Tackifying resin emulsion, method for producing the same and aqueous pressure-sensitive adhesive/adhesive composition |
| CN107793518A (en) * | 2016-09-07 | 2018-03-13 | 中国石油化工股份有限公司 | Application of the nertralizer in the emulsion particle diameter of control EVA elastomer emulsions |
| CN108084370A (en) * | 2017-12-21 | 2018-05-29 | 海南必凯水性新材料有限公司 | A kind of low-temperature heat-sealing EVA lotions and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| Evaluation of flow ability response in EVA emulsion preparation with different vinyl acetate percentage by intrinsic viscosity measurement;Rosdi MRH et al.;《Procedia Chemistry》;第19卷;第455-461页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112062973A (en) | 2020-12-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103266534B (en) | A kind of Zinc stearate water dispersion liquid and preparation method thereof | |
| DE60217072T2 (en) | METHOD FOR THE PRODUCTION OF MICRO-CAPSULES THAT INCLUDE PHASE MUSCLE | |
| CN112062973B (en) | Emulsification method of ethylene-vinyl acetate copolymer | |
| CN108114617A (en) | Small-particle-size ultralow-concentration nano emulsion composition and preparation method thereof | |
| DE60208843T2 (en) | Coagulation of PTFE latex | |
| CN112662383B (en) | High-efficiency instant multi-component copolymer dispersion liquid and preparation method thereof | |
| US10125252B2 (en) | Ethylene-vinyl alcohol copolymer microparticles, dispersion liquid and resin composition containing same, and method of producing said microparticles | |
| US9074072B2 (en) | Large-sized vinyl chloride seed, method of preparing the seed, vinyl chloride resin prepared using the seed, and method of preparing the vinyl chloride resin | |
| CN105252679A (en) | Mold release agent special for high-rebound polyurethane product and preparation method of mold release agent | |
| CN113308020A (en) | Water-based antioxidant emulsion and preparation method and application thereof | |
| CN102796474A (en) | Water-based adhesive and preparation method thereof | |
| CN108239301B (en) | Emulsion type composite antioxidant and preparation method thereof | |
| CN104262645A (en) | Method for preparing granularity controllable narrow range polymer micro-nano spheres | |
| CN106111007B (en) | Method for preparing water-based calcium stearate dispersion liquid, product and application thereof | |
| JP2008507612A (en) | Resin dispersion with multimodal particle size distribution | |
| CN101613429A (en) | Large-sized vinyl chloride seed and preparation method thereof, use the vinyl chloride resin of this seed preparation and prepare the method for this vinyl chloride resin | |
| CN104437284A (en) | Preparation method of phase change microcapsule | |
| CN110713622B (en) | Emulsification method of butylated products of paracresol and dicyclopentadiene | |
| CN105295162A (en) | PEW (Polyethylene Wax) micro-emulsion and preparation method thereof | |
| CN112824503B (en) | Nano soap-based thickener precursor for lubricating grease and preparation method and application thereof | |
| CN111718588A (en) | Modified emulsified asphalt and its production process and use | |
| CN103374086A (en) | Method for preparing polyvinyl chloride paste resin at high temperature by adopting micro-suspension method | |
| CN110305488B (en) | Water-based ethylene bis stearamide emulsion and preparation method thereof | |
| CN107778499A (en) | A kind of method that the water-based antioxidant of high-melting-point is prepared based on Dynamic Precipitation method room temperature | |
| CN110327799B (en) | Water-based erucamide emulsion and preparation method thereof |
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 | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20230726 Address after: 750300 Bayin OBO Industrial Park, WUSITAI Town, Alxa League economic and Technological Development Zone, Inner Mongolia Autonomous Region Applicant after: Inner Mongolia Haopu Technology Co.,Ltd. Address before: No. 2055, Yan'an street, Changchun City, Jilin Province Applicant before: Changchun University of Technology |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: An emulsification method for ethylene vinyl acetate copolymer Granted publication date: 20230825 Pledgee: Bank of China Limited BAYANHOT branch Pledgor: Inner Mongolia Haopu Technology Co.,Ltd. Registration number: Y2024980019962 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Granted publication date: 20230825 Pledgee: Bank of China Limited BAYANHOT branch Pledgor: Inner Mongolia Haopu Technology Co.,Ltd. Registration number: Y2024980019962 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Emulsification method of ethylene vinyl acetate copolymer Granted publication date: 20230825 Pledgee: Bank of Communications Co.,Ltd. Wuhai Branch Pledgor: Inner Mongolia Haopu Technology Co.,Ltd. Registration number: Y2024980041806 |