CN110093126A - A kind of preparation method of medical aqueous multiple emulsion paper-plastic lamination adhesive - Google Patents
A kind of preparation method of medical aqueous multiple emulsion paper-plastic lamination adhesive Download PDFInfo
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- CN110093126A CN110093126A CN201910236015.0A CN201910236015A CN110093126A CN 110093126 A CN110093126 A CN 110093126A CN 201910236015 A CN201910236015 A CN 201910236015A CN 110093126 A CN110093126 A CN 110093126A
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- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- 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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/02—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to polysaccharides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention relates to a kind of preparation methods of medical aqueous multiple emulsion paper-plastic lamination adhesive, belong to Laminating adhesive technical field.The present invention passes through addition carboxymethyl cellulose and polyacrylamide, prepare a kind of medical aqueous multiple emulsion paper-plastic lamination adhesive, carboxymethyl cellulose is powder white or yellowish, it is to be acted under alkaline condition with monoxone by cellulose, carboxyl in carboxymethyl cellulose can be crosslinked with the several functions monomer in lotion, the polymer emulsion of self-crosslinking is obtained, the stability, heat resistance and water resistance of crosslinked emulsions film can be improved in the presence of carboxyl；Polyacrylamide is polymerized by acrylamide monomer, polyacrylamide belongs to organic polymer coargulator, bigger wadding body can be formed between the particle of lotion, resulting huge adsorption effect, there is very big viscosity, and it does not dissociate in water, can effectively improve the water resistance of paper-plastic lamination adhesive.
Description
Technical field
The present invention relates to a kind of preparation methods of medical aqueous multiple emulsion paper-plastic lamination adhesive, belong to Laminating adhesive technology neck
Domain.
Background technique
Paper-plastic lamination technique is that commonly a kind of technique, so-called paper-plastic lamination were exactly using specific to packaging industry in recent years
Polypropylene film (BOPP film) or polyester film etc. are adhered to the process on paper by adhesive, and the adhesive used in the process of this
Thus referred to as paper-plastic lamination adhesive.Paper printed matter is pasted together with polyacrylic film, both can effectively have been improved made of paper
The appearance of product, at the same it is again durable.
Laminating adhesive currently on the market can substantially be divided into three classes: organic solvent type Laminating adhesive, hot melt glue type Laminating adhesive, water
Property emulsion paper-plastic composite adhesive.Organic solvent adhesive is homogeneous system using organic solvent as decentralized medium；Water-based emulsion type gluing
Agent is heterogeneous system using water as decentralized medium；Hot melt glue type adhesive generally in blocks of solid, is heated to certain temperature at room temperature
Become fluid when spending, becomes solid glued membrane again when being cooled to room temperature after coating.
Water-based emulsion type adhesive is more at low cost than organic solvent adhesive, because even being generally the least expensive organic solvent
It is more expensive than water therefore all relatively early to the exploratory development of emulsion-type paper-plastic lamination adhesive work.Common emulsion type water-base paper-plastic lamination
Glue generally has VAE type, polyacrylate, polyurethanes etc..But there are some problems, such as small-molecular emulsifier for these lotions
Presence meeting so that the water resistance of adhesive is deteriorated.In order to solve existing these problems, researcher has done a large amount of exploration and has ground
Study carefully experimental work.First is that being carried out by development of new emulsifier or using the method for emulsifier-free emulsion polymerization to the emulsification system of lotion
It is modified；Followed by become by introducing functional monomer to change certain properties of lotion or make it have certain specific function
Functional adhesive；Third is that improve the performance of lotion and then the adjustment to lotion synthesizing formula is to change emulsion particle,
It such as can change minimum film formation temperature, the chemical corrosion resistance of lotion；Fourth is that the novel tackifier resin emulsion of research and probe or
Crosslinking agent improves the performance of gluing agent emulsion；Fifth is that improving certain performances of lotion by the solid content for improving lotion.
Aqueous paper/plastic laminating emulsion adhesive has biggish market prospects, each row is each due to its series of advantages such as environmentally friendly, at low cost
Industry has extensive use.Such as can be used for packaging industry, the gift box of some finenesses, packaging bag, which can all use, arrives this kind of glue,
Wherein have and can be used for Medical instrument packaging bag once important purposes.
Although medical package material Laminating adhesive in the market is varied, if any VAE type, polyacrylate, poly- ammonia
Esters etc., but discovery is compared, the excessively complicated not easy to control, polyurethanes of equipment is due in synthesis process in the synthesis of VAE lotion
It commonly uses isocyanates etc. and is more toxic substance, and the synthesis device of polyacrylate emulsion is relatively easy and is easy to control
System, raw material belong to hypotoxicity substance, these advantages make polyacrylic emulsion adhesive receive the favor of manufacturer greatly, also make
Obtaining polyacrylie-type emulsion adhesive has biggish market.
In addition, used in the process of paper-plastic lamination to BOPP film can be divided into the sum by sided corona treatment without sided corona treatment
Two kinds crossed.BOPP film by sided corona treatment due to that can introduce some polar groups during the treatment, so that the pole of film
Property increase；And then polarity is lower for the BOPP film crossed without sided corona treatment.For without in the processed BOPP film of surface corona
Paper-plastic lamination adhesive preferably clings the lower film of polarity, therefore such as since it should preferably cling the higher paper of polarity again
The method that fruit uses highly polar lotion and low polar latex composite compounding, for example, can be matched using the higher styrene-acrylic emulsion of polarity
With the lower wax emulsion of polarity, then obtained Laminating adhesive peel strength is higher.Simultaneously as wax emulsion is since it is without any
Organic solvent, nontoxic and pollution-free, the feature of environmental protection is high, and wax emulsion belongs to low polar substances, is a kind of good Laminating adhesive therefore
Preparation lotion.
Summary of the invention
The technical problems to be solved by the invention: resistance to for the aqueous paper/plastic laminating emulsion adhesive being currently used on medical package material
Aqueous poor, heat-resisting quantity difference problem provides a kind of preparation method of medical aqueous multiple emulsion paper-plastic lamination adhesive.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) by aqueous C 5 petroleum resin lotion be added starch graft acrylic acid ester lotion in, be placed in dispersion machine, under room temperature with
300~360r/min revolving speed stirs 10~20min, obtains mixed emulsion；
(2) acrylate and vinyl acetate emulsion, Heveatex are added in mixed emulsion, are placed in dispersion machine, turned under room temperature with 400~500r/min
Speed 20~30min of stirring, obtains compound emulsion；
(3) carboxymethyl cellulose, polyacrylamide are added in deionized water, under 30~40 DEG C of water bath condition with 200~
220r/min revolving speed stirs 10~20min, obtains thickening fluid；
(4) thickening fluid, nano-zinc oxide powder are added in compound emulsion, are placed in high shear dispersion machine, with 1500 under room temperature
~2000r/min revolving speed stirs 30~40min, then is placed in 20~30min of ultrasonic disperse in ultrasonic dispersing machine, obtains medical aqueous
Multiple emulsion paper-plastic lamination adhesive.
The starch graft acrylic acid ester lotion, acrylate and vinyl acetate emulsion, Heveatex, carboxymethyl cellulose, polyacrylamide,
Aqueous C 5 petroleum resin lotion, nano-zinc oxide powder, the parts by weight of deionized water are 60~80 parts of starch graft acrylic acids
Ester lotion, 30~40 parts of acrylate and vinyl acetate emulsions, 15~20 parts of Heveatexes, 6~8 parts of carboxymethyl celluloses, 3~4 parts of polyacrylamides,
12~16 parts of aqueous C 5 petroleum resin lotions, 6~8 parts of nano-zinc oxide powders, 15~20 parts of deionized waters.
The power of ultrasonic disperse described in step (4) is 400~500W.
The specific preparation step of starch graft acrylic acid ester lotion described in step (1) are as follows:
(1) cornstarch, neopelex, nonylphenol polyoxyethylene ether, sodium bicarbonate are added in deionized water,
5~10min is stirred with 200~240r/min revolving speed under 75~85 DEG C of water bath condition, it is molten to obtain blended emulsifier starch for heat preservation
Liquid；
(2) 1/10 acrylic acid, 1/10 Butyl acrylate, 1/10 methyl methacrylate, 1/10 ammonium persulfate are slowly added to mix
In co-emulsifier starch solution, 15~20min is stirred with 200~240r/min revolving speed under 75~85 DEG C of water bath condition, is obtained
Starch graft acrylic acid ester seed emulsion；
(3) residual acrylic acid, residual acrylic acid fourth vinegar, remaining methyl methacrylate, remaining ammonium persulfate are slowly added to form sediment
In powder grafted acrylate seed emulsion, under 80~90 DEG C of water bath condition with 300~320r/min revolving speed stirring 10~
15min, heat preservation stand 30~40min of reaction, are cooled to room temperature, adjust pH to 7~8, obtain starch graft acrylic acid ester lotion.
The cornstarch, acrylic acid, Butyl acrylate, methyl methacrylate, ammonium persulfate, detergent alkylate sulphur
Sour sodium, nonylphenol polyoxyethylene ether, sodium bicarbonate, deionized water parts by weight be 20~30 parts of cornstarch, 20~30 part third
Olefin(e) acid, 40~60 parts of Butyl acrylates, 10~15 parts of methyl methacrylates, 0.1~0.3 part of ammonium persulfate, 1~3 part 12
Sodium alkyl benzene sulfonate, 1~3 part of nonylphenol polyoxyethylene ether, 2~3 parts of sodium bicarbonates, 120~180 parts of deionized waters.
1/10 acrylic acid described in step (2), 1/10 Butyl acrylate, 1/10 methyl methacrylate, 1/10 persulfuric acid
10~15min of addition time of ammonium.
Residual acrylic acid described in step (3), residual acrylic acid fourth vinegar, remaining methyl methacrylate, remaining persulfuric acid
1~2hpH of time adjusting is added using the sodium hydroxide solution of mass concentration 1% in ammonium.
The specific preparation step of acrylate and vinyl acetate emulsion described in step (2) are as follows:
(1) by polyvinyl alcohol, hydroxyethyl cellulose, lauryl sodium sulfate, octyl phenol polyoxyethylene ether, sodium carbonate addition go from
In sub- water, 15~20min is stirred with 180~200r/min revolving speed under 80~90 DEG C of water bath condition, it is molten to obtain emulsifier mixing
Liquid；
(2) emulsifier mixed solution is added in 1/3 acrylic acid, 1/3 vinylacetate, 1/3 butyl acrylate, 1/3 sodium peroxydisulfate
In, 30~40min is stirred to react with 200~240r/min revolving speed under 60~70 DEG C of water bath condition, obtains the third seed emulsion of vinegar；
(3) residual acrylic acid, remaining vinylacetate, residual acrylic acid butyl ester, remaining sodium peroxydisulfate are slowly added to third kind of vinegar
In sub- lotion, 1~2h is stirred to react with 300~340r/min revolving speed under 70~80 DEG C of water bath condition, is cooled to room temperature, adjusted
PH to 7~8 is saved, acrylate and vinyl acetate emulsion is obtained.
The polyvinyl alcohol, hydroxyethyl cellulose, acrylic acid, vinylacetate, butyl acrylate, dodecyl sulphate
Sodium, octyl phenol polyoxyethylene ether, sodium peroxydisulfate, sodium carbonate, deionized water parts by weight be 4~6 parts of polyvinyl alcohol, 2~3 parts of hydroxyls
Ethyl cellulose, 20~30 parts of acrylic acid, 40~60 parts of vinylacetates, 20~30 parts of butyl acrylates, 1~3 part of dodecane
Base sodium sulphate, 1~3 part of octyl phenol polyoxyethylene ether, 0.1~0.3 part of sodium peroxydisulfate, 2~3 parts of sodium carbonate, 120~180 parts go
Ionized water.
Residual acrylic acid described in step (3), remaining vinylacetate, residual acrylic acid butyl ester, remaining sodium peroxydisulfate
The addition time is 3~4h, and pH adjusts the ammonium hydroxide using mass concentration 1%.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention, by compounding with acrylate and vinyl acetate emulsion, Heveatex, makes using starch graft acrylic acid ester lotion as matrix lotion
A kind of standby medical aqueous multiple emulsion paper-plastic lamination adhesive, acrylic acid ester emulsion is by esters of acrylic acid and methyl acrylic ester list
Body is copolymerized, and product has many excellent characteristics, and environmental pollution is small, and raw material sources are extensive, is easy preparation, has bonding
The features such as wide, acrylic acid ester emulsion are good to the bonding force of paper, safe and non-toxic, and starch is a kind of biodegradable natural height
Molecule, starch has many advantages, such as nontoxic, from a wealth of sources, biodegradability, low in cost, by starch-grafted to acrylic acid
On molecule, primary group of free radicals can be generated on the molecule of starch, so that acrylic monomers is grafted to shallow lake with certain degree of polymerization
The high-polymer molecule chain is formed on powder molecule, to assign the good stability of lotion and adhesivity；Acrylate and vinyl acetate emulsion has excellent
Application property, lesser smell, the advantages that unique rheological property, cheap, cementability is strong, film forming stability is good, prepare vinegar
It,, can be hydrophobic by functionalization while protecting emulsion polymerization using hydroxyethyl cellulose as protecting colloid when acrylic emulsion
Group is successfully introduced into emulsion particle surface, and while color development and the rheological property for guaranteeing vinegar third itself, lotion can be improved
Water resistance and alkali resistance, and that the copolymer in acrylate and vinyl acetate emulsion can be made to generate is slight for the hydroxyl group in hydroxyethyl cellulose
Crosslinking, and form a degree of cross-linked structure, improve the mechanical property of glue film, introducing in copolymer segment a small amount of has
Polar functional group can increase emulsion intercalation method since it is imbued with reactive feature, improve the mechanical property of glue film, especially
It has been that the introducing of the function monomer of emulsifier effect will be greatly improved to emulsion intercalation method；Heveatex is a kind of glutinous
Thick milky white liquid, it is milky aqueous dispersion of the rubber particles in Nearly neutral medium, and Heveatex belongs to rubber
Thermoplastic synthetic resin has good its main feature is that filming performance is good when high resiliency, bonding, glue film is imbued with flexibility after film forming
Good water resistance and stability, can effectively improve the comprehensive performance of paper-plastic lamination adhesive；
(2) it is multiple to prepare a kind of medical aqueous multiple emulsion paper by addition carboxymethyl cellulose and polyacrylamide by the present invention
Film glue, carboxymethyl cellulose are powder white or yellowish, are acted under alkaline condition with monoxone by cellulose,
Carboxyl in carboxymethyl cellulose can be crosslinked with the several functions monomer in lotion, obtain the polymer cream of self-crosslinking
The stability, heat resistance and water resistance of crosslinked emulsions film can be improved in liquid, the presence of carboxyl；Polyacrylamide is by acrylamide
Monomer polymerization forms, and polyacrylamide belongs to organic polymer coargulator, and bigger wadding body can be formed between the particle of lotion,
Resulting huge adsorption effect, has very big viscosity, and do not dissociate in water, can effectively improve paper-plastic lamination
The water resistance of glue.
Specific embodiment
According to parts by weight, 20~30 parts of cornstarch, 20~30 parts of acrylic acid, 40~60 parts of acrylic acid fourths are weighed respectively
Vinegar, 10~15 parts of methyl methacrylates, 0.1~0.3 part of ammonium persulfate, 1~3 part of neopelex, 1~3 part of nonyl
Base phenol polyethenoxy ether, 2~3 parts of sodium bicarbonates, 120~180 parts of deionized waters, by cornstarch, neopelex,
Nonylphenol polyoxyethylene ether, sodium bicarbonate are added in deionized water, with 200~240r/min under 75~85 DEG C of water bath condition
Revolving speed stirs 5~10min, and heat preservation obtains blended emulsifier starch solution, by 1/10 acrylic acid, 1/10 Butyl acrylate, 1/10 first
Base methyl acrylate, 1/10 ammonium persulfate are slowly added in blended emulsifier starch solution, 10~15min of time are added, 75
15~20min is stirred with 200~240r/min revolving speed under~85 DEG C of water bath condition, obtains starch graft acrylic acid ester seed cream
Residual acrylic acid, residual acrylic acid fourth vinegar, remaining methyl methacrylate, remaining ammonium persulfate are slowly added to starch and connect by liquid
In branch acrylate seed emulsion, 1~2h of time is added, with 300~320r/min revolving speed under 80~90 DEG C of water bath condition
10~15min is stirred, heat preservation stands 30~40min of reaction, is cooled to room temperature, and the sodium hydroxide solution tune of mass concentration 1% is added dropwise
PH to 7~8 is saved, obtains starch graft acrylic acid ester lotion, then according to parts by weight, weighs 4~6 parts of polyvinyl alcohol, 2~3 respectively
Part hydroxyethyl cellulose, 20~30 parts of acrylic acid, 40~60 parts of vinylacetates, 20~30 parts of butyl acrylates, 1~3 part ten
Sodium dialkyl sulfate, 1~3 part of octyl phenol polyoxyethylene ether, 0.1~0.3 part of sodium peroxydisulfate, 2~3 parts of sodium carbonate, 120~180
Polyvinyl alcohol, hydroxyethyl cellulose, lauryl sodium sulfate, octyl phenol polyoxyethylene ether, sodium carbonate are added part deionized water
In deionized water, 15~20min is stirred with 180~200r/min revolving speed under 80~90 DEG C of water bath condition, it is mixed to obtain emulsifier
Solution is closed, emulsifier mixed solution is added in 1/3 acrylic acid, 1/3 vinylacetate, 1/3 butyl acrylate, 1/3 sodium peroxydisulfate
In, 30~40min is stirred to react with 200~240r/min revolving speed under 60~70 DEG C of water bath condition, obtains the third seed emulsion of vinegar,
Residual acrylic acid, remaining vinylacetate, residual acrylic acid butyl ester, remaining sodium peroxydisulfate are slowly added to the third seed emulsion of vinegar
In, 3~4h of time is added, 1~2h is stirred to react with 300~340r/min revolving speed under 70~80 DEG C of water bath condition, it is cooling
To room temperature, the ammonium hydroxide that mass concentration 1% is added dropwise adjusts pH to 7~8, obtains acrylate and vinyl acetate emulsion, then according to parts by weight, weigh 60 respectively
~80 parts of starch graft acrylic acid ester lotions, 30~40 parts of acrylate and vinyl acetate emulsions, 15~20 parts of Heveatexes, 6~8 parts of carboxymethyl celluloses
Element, 3~4 parts of polyacrylamides, 12~16 parts of aqueous C 5 petroleum resin lotions, 6~8 parts of nano-zinc oxide powders, 15~20
Part deionized water, aqueous C 5 petroleum resin lotion is added in starch graft acrylic acid ester lotion, is placed in dispersion machine, room temperature
Under with 300~360r/min revolving speed stir 10~20min, obtain mixed emulsion, by acrylate and vinyl acetate emulsion, Heveatex be added mixed emulsion
In, it is placed in dispersion machine, 20~30min is stirred with 400~500r/min revolving speed under room temperature, obtains compound emulsion, by carboxymethyl fibre
Dimension element, polyacrylamide are added in deionized water, with 200~220r/min revolving speed stirring 10 under 30~40 DEG C of water bath condition
~20min, obtains thickening fluid, and thickening fluid, nano-zinc oxide powder are added in compound emulsion, are placed in high shear dispersion machine, often
30~40min is stirred with 1500~2000r/min revolving speed under temperature, then is placed in ultrasonic dispersing machine, in the condition of 400~500W
20~30min of lower ultrasonic disperse obtains medical aqueous multiple emulsion paper-plastic lamination adhesive.
According to parts by weight, 20 parts of cornstarch, 20 parts of acrylic acid, 40 parts of Butyl acrylates, 10 parts of methyl are weighed respectively
Methyl acrylate, 0.1 part of ammonium persulfate, 1 part of neopelex, 1 part of nonylphenol polyoxyethylene ether, 2 parts of sodium bicarbonates,
Deionization is added in cornstarch, neopelex, nonylphenol polyoxyethylene ether, sodium bicarbonate by 120 parts of deionized waters
In water, 5min is stirred with 200r/min revolving speed under 75 DEG C of water bath condition, heat preservation obtains blended emulsifier starch solution, by 1/
10 acrylic acid, 1/10 Butyl acrylate, 1/10 methyl methacrylate, 1/10 ammonium persulfate are slowly added to blended emulsifier starch
In solution, time 10min is added, 15min is stirred with 200r/min revolving speed under 75 DEG C of water bath condition, obtains starch-grafted propylene
Acid esters seed emulsion is slow by residual acrylic acid, residual acrylic acid fourth vinegar, remaining methyl methacrylate, remaining ammonium persulfate
It is added in starch graft acrylic acid ester seed emulsion, time 1h is added, is stirred under 80 DEG C of water bath condition with 300r/min revolving speed
10min is mixed, heat preservation stands reaction 30min, is cooled to room temperature, and the sodium hydroxide solution that mass concentration 1% is added dropwise adjusts pH to 7, obtains
Starch graft acrylic acid ester lotion, then according to parts by weight, 4 parts of polyvinyl alcohol, 2 parts of hydroxyethyl celluloses, 20 parts are weighed respectively
Acrylic acid, 40 parts of vinylacetates, 20 parts of butyl acrylates, 1 part of lauryl sodium sulfate, 1 part of octyl phenol polyoxyethylene ether,
0.1 part of sodium peroxydisulfate, 2 parts of sodium carbonate, 120 parts of deionized waters, by polyvinyl alcohol, hydroxyethyl cellulose, lauryl sodium sulfate,
Octyl phenol polyoxyethylene ether, sodium carbonate are added in deionized water, with the stirring of 180r/min revolving speed under 80 DEG C of water bath condition
15min obtains emulsifier mixed solution, and 1/3 acrylic acid, 1/3 vinylacetate, 1/3 butyl acrylate, 1/3 sodium peroxydisulfate are added
Enter in emulsifier mixed solution, 30min is stirred to react with 200r/min revolving speed under 60 DEG C of water bath condition, obtains vinegar the third seed cream
Residual acrylic acid, remaining vinylacetate, residual acrylic acid butyl ester, remaining sodium peroxydisulfate are slowly added to vinegar the third seed cream by liquid
In liquid, time 3h is added, 1h is stirred to react with 300r/min revolving speed under 70 DEG C of water bath condition, is cooled to room temperature, matter is added dropwise
The ammonium hydroxide for measuring concentration 1% adjusts pH to 7, obtains acrylate and vinyl acetate emulsion, then according to parts by weight, weighs 60 parts of starch graft acrylic acids respectively
Ester lotion, 30 parts of acrylate and vinyl acetate emulsions, 15 parts of Heveatexes, 6 parts of carboxymethyl celluloses, 3 parts of polyacrylamides, 12 parts of aqueous light dydrocarbon stones
Oleoresin lotion, 6 parts of nano-zinc oxide powders, 15 parts of deionized waters aqueous C 5 petroleum resin lotion are added starch-grafted
It in acrylic acid ester emulsion, is placed in dispersion machine, 10min is stirred with 300r/min revolving speed under room temperature, obtains mixed emulsion, by the third cream of vinegar
Liquid, Heveatex are added in mixed emulsion, are placed in dispersion machine, stir 20min under room temperature with 400r/min revolving speed, must compound cream
Carboxymethyl cellulose, polyacrylamide are added in deionized water, are stirred under 30 DEG C of water bath condition with 200r/min revolving speed by liquid
10min is mixed, thickening fluid is obtained, thickening fluid, nano-zinc oxide powder are added in compound emulsion, are placed in high shear dispersion machine, often
30min is stirred with 1500r/min revolving speed under temperature, then is placed in ultrasonic dispersing machine, ultrasonic disperse under conditions of 400W
20min obtains medical aqueous multiple emulsion paper-plastic lamination adhesive.
According to parts by weight, 25 parts of cornstarch, 25 parts of acrylic acid, 50 parts of Butyl acrylates, 12 parts of methyl are weighed respectively
Methyl acrylate, 0.2 part of ammonium persulfate, 2 parts of neopelexes, 2 parts of nonylphenol polyoxyethylene ether, 2 parts of sodium bicarbonates,
Deionization is added in cornstarch, neopelex, nonylphenol polyoxyethylene ether, sodium bicarbonate by 150 parts of deionized waters
In water, 8min is stirred with 220r/min revolving speed under 80 DEG C of water bath condition, heat preservation obtains blended emulsifier starch solution, by 1/
10 acrylic acid, 1/10 Butyl acrylate, 1/10 methyl methacrylate, 1/10 ammonium persulfate are slowly added to blended emulsifier starch
In solution, time 12min is added, 18min is stirred with 220r/min revolving speed under 80 DEG C of water bath condition, obtains starch-grafted propylene
Acid esters seed emulsion is slow by residual acrylic acid, residual acrylic acid fourth vinegar, remaining methyl methacrylate, remaining ammonium persulfate
It is added in starch graft acrylic acid ester seed emulsion, time 1h is added, is stirred under 85 DEG C of water bath condition with 310r/min revolving speed
12min is mixed, heat preservation stands reaction 35min, is cooled to room temperature, and the sodium hydroxide solution that mass concentration 1% is added dropwise adjusts pH to 7, obtains
Starch graft acrylic acid ester lotion, then according to parts by weight, 5 parts of polyvinyl alcohol, 2 parts of hydroxyethyl celluloses, 25 parts are weighed respectively
Acrylic acid, 50 parts of vinylacetates, 25 parts of butyl acrylates, 2 parts of lauryl sodium sulfate, 2 parts of octyl phenol polyoxyethylene ether,
0.2 part of sodium peroxydisulfate, 2 parts of sodium carbonate, 150 parts of deionized waters, by polyvinyl alcohol, hydroxyethyl cellulose, lauryl sodium sulfate,
Octyl phenol polyoxyethylene ether, sodium carbonate are added in deionized water, with the stirring of 190r/min revolving speed under 85 DEG C of water bath condition
18min obtains emulsifier mixed solution, and 1/3 acrylic acid, 1/3 vinylacetate, 1/3 butyl acrylate, 1/3 sodium peroxydisulfate are added
Enter in emulsifier mixed solution, 35min is stirred to react with 220r/min revolving speed under 65 DEG C of water bath condition, obtains vinegar the third seed cream
Residual acrylic acid, remaining vinylacetate, residual acrylic acid butyl ester, remaining sodium peroxydisulfate are slowly added to vinegar the third seed cream by liquid
In liquid, time 3h is added, 1h is stirred to react with 320r/min revolving speed under 75 DEG C of water bath condition, is cooled to room temperature, matter is added dropwise
The ammonium hydroxide for measuring concentration 1% adjusts pH to 7, obtains acrylate and vinyl acetate emulsion, then according to parts by weight, weighs 70 parts of starch graft acrylic acids respectively
Ester lotion, 35 parts of acrylate and vinyl acetate emulsions, 18 parts of Heveatexes, 7 parts of carboxymethyl celluloses, 3 parts of polyacrylamides, 14 parts of aqueous light dydrocarbon stones
Oleoresin lotion, 7 parts of nano-zinc oxide powders, 18 parts of deionized waters aqueous C 5 petroleum resin lotion are added starch-grafted
It in acrylic acid ester emulsion, is placed in dispersion machine, 15min is stirred with 330r/min revolving speed under room temperature, obtains mixed emulsion, by the third cream of vinegar
Liquid, Heveatex are added in mixed emulsion, are placed in dispersion machine, stir 25min under room temperature with 450r/min revolving speed, must compound cream
Carboxymethyl cellulose, polyacrylamide are added in deionized water, are stirred under 35 DEG C of water bath condition with 210r/min revolving speed by liquid
15min is mixed, thickening fluid is obtained, thickening fluid, nano-zinc oxide powder are added in compound emulsion, are placed in high shear dispersion machine, often
35min is stirred with 1750r/min revolving speed under temperature, then is placed in ultrasonic dispersing machine, ultrasonic disperse under conditions of 450W
25min obtains medical aqueous multiple emulsion paper-plastic lamination adhesive.
According to parts by weight, 30 parts of cornstarch, 30 parts of acrylic acid, 60 parts of Butyl acrylates, 15 parts of methyl are weighed respectively
Methyl acrylate, 0.3 part of ammonium persulfate, 3 parts of neopelexes, 3 parts of nonylphenol polyoxyethylene ether, 3 parts of sodium bicarbonates,
Deionization is added in cornstarch, neopelex, nonylphenol polyoxyethylene ether, sodium bicarbonate by 180 parts of deionized waters
In water, 10min is stirred with 240r/min revolving speed under 85 DEG C of water bath condition, heat preservation obtains blended emulsifier starch solution, by 1/
10 acrylic acid, 1/10 Butyl acrylate, 1/10 methyl methacrylate, 1/10 ammonium persulfate are slowly added to blended emulsifier starch
In solution, time 15min is added, 20min is stirred with 240r/min revolving speed under 85 DEG C of water bath condition, obtains starch-grafted propylene
Acid esters seed emulsion is slow by residual acrylic acid, residual acrylic acid fourth vinegar, remaining methyl methacrylate, remaining ammonium persulfate
It is added in starch graft acrylic acid ester seed emulsion, time 2h is added, is stirred under 90 DEG C of water bath condition with 320r/min revolving speed
15min is mixed, heat preservation stands reaction 40min, is cooled to room temperature, and the sodium hydroxide solution that mass concentration 1% is added dropwise adjusts pH to 8, obtains
Starch graft acrylic acid ester lotion, then according to parts by weight, 6 parts of polyvinyl alcohol, 3 parts of hydroxyethyl celluloses, 30 parts are weighed respectively
Acrylic acid, 60 parts of vinylacetates, 30 parts of butyl acrylates, 3 parts of lauryl sodium sulfate, 3 parts of octyl phenol polyoxyethylene ether,
0.3 part of sodium peroxydisulfate, 3 parts of sodium carbonate, 180 parts of deionized waters, by polyvinyl alcohol, hydroxyethyl cellulose, lauryl sodium sulfate,
Octyl phenol polyoxyethylene ether, sodium carbonate are added in deionized water, with the stirring of 200r/min revolving speed under 90 DEG C of water bath condition
20min obtains emulsifier mixed solution, and 1/3 acrylic acid, 1/3 vinylacetate, 1/3 butyl acrylate, 1/3 sodium peroxydisulfate are added
Enter in emulsifier mixed solution, 40min is stirred to react with 240r/min revolving speed under 70 DEG C of water bath condition, obtains vinegar the third seed cream
Residual acrylic acid, remaining vinylacetate, residual acrylic acid butyl ester, remaining sodium peroxydisulfate are slowly added to vinegar the third seed cream by liquid
In liquid, time 4h is added, 2h is stirred to react with 340r/min revolving speed under 80 DEG C of water bath condition, is cooled to room temperature, matter is added dropwise
The ammonium hydroxide for measuring concentration 1% adjusts pH to 8, obtains acrylate and vinyl acetate emulsion, then according to parts by weight, weighs 80 parts of starch graft acrylic acids respectively
Ester lotion, 40 parts of acrylate and vinyl acetate emulsions, 20 parts of Heveatexes, 8 parts of carboxymethyl celluloses, 4 parts of polyacrylamides, 16 parts of aqueous light dydrocarbon stones
Oleoresin lotion, 8 parts of nano-zinc oxide powders, 20 parts of deionized waters aqueous C 5 petroleum resin lotion are added starch-grafted
It in acrylic acid ester emulsion, is placed in dispersion machine, 20min is stirred with 360r/min revolving speed under room temperature, obtains mixed emulsion, by the third cream of vinegar
Liquid, Heveatex are added in mixed emulsion, are placed in dispersion machine, stir 30min under room temperature with 500r/min revolving speed, must compound cream
Carboxymethyl cellulose, polyacrylamide are added in deionized water, are stirred under 40 DEG C of water bath condition with 220r/min revolving speed by liquid
20min is mixed, thickening fluid is obtained, thickening fluid, nano-zinc oxide powder are added in compound emulsion, are placed in high shear dispersion machine, often
40min is stirred with 2000r/min revolving speed under temperature, then is placed in ultrasonic dispersing machine, ultrasonic disperse under conditions of 500W
30min obtains medical aqueous multiple emulsion paper-plastic lamination adhesive.
Reference examples: the paper-plastic lamination adhesive of Dongguan Co., Ltd production.
The paper-plastic lamination adhesive that embodiment and reference examples are prepared is detected, specific detection is as follows:
180 ° of peel strengths: it is tested by GB/T2792-1998 " 180 ° of peeling strength test methods of pressure-sensitive tape ".
Heat drying stability test: the situation of change of glue-line is observed for 24 hours under 60 °C.
Moisture-resistant thermal performance test: in 110 °C of water vapor atmosphere 10min, the situation of change of peel strength is observed.
The damaged ratio of paper: breakage area accounts for the ratio of the gross area when separating for paper.
Specific test result such as table 1.
1 performance characterization contrast table of table
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples |
| 180 ° of peel strength/N/cm | 4.0 | 4.1 | 4.5 | 7.0 |
| Heat drying stability | It is not blistering, not delamination | It is not blistering, not delamination | It is not blistering, not delamination | Obvious blistering, delamination |
| Moisture-resistant hot property | Peel strength is without significant change | Peel strength is without significant change | Peel strength is without significant change | Peel strength obviously becomes larger |
| Paper sheet break rate/% | 0 | 0 | 0 | 60 |
As shown in Table 1, film adhesive surface when paper-plastic lamination adhesive glue prepared by the present invention has 180 ° of peel strength height, paper separation
Paper-tear picture, paper not will receive the smooth tack-free feature of adhesive surface after destruction, paper separation, can satisfy wanting for paper-plastic package
It asks.
Claims (10)
1. a kind of preparation method of medical aqueous multiple emulsion paper-plastic lamination adhesive, which is characterized in that specific preparation step are as follows:
(1) by aqueous C 5 petroleum resin lotion be added starch graft acrylic acid ester lotion in, be placed in dispersion machine, under room temperature with
300~360r/min revolving speed stirs 10~20min, obtains mixed emulsion；
(2) acrylate and vinyl acetate emulsion, Heveatex are added in mixed emulsion, are placed in dispersion machine, turned under room temperature with 400~500r/min
Speed 20~30min of stirring, obtains compound emulsion；
(3) carboxymethyl cellulose, polyacrylamide are added in deionized water, under 30~40 DEG C of water bath condition with 200~
220r/min revolving speed stirs 10~20min, obtains thickening fluid；
(4) thickening fluid, nano-zinc oxide powder are added in compound emulsion, are placed in high shear dispersion machine, with 1500 under room temperature
~2000r/min revolving speed stirs 30~40min, then is placed in 20~30min of ultrasonic disperse in ultrasonic dispersing machine, obtains medical aqueous
Multiple emulsion paper-plastic lamination adhesive.
2. the preparation method of the medical aqueous multiple emulsion paper-plastic lamination adhesive of one kind according to claim 1, which is characterized in that
The starch graft acrylic acid ester lotion, acrylate and vinyl acetate emulsion, Heveatex, carboxymethyl cellulose, polyacrylamide, aqueous light dydrocarbon
Petroleum resin emulsion, nano-zinc oxide powder, the parts by weight of deionized water are 60~80 parts of starch graft acrylic acid ester lotions, 30
~40 parts of acrylate and vinyl acetate emulsions, 15~20 parts of Heveatexes, 6~8 parts of carboxymethyl celluloses, 3~4 parts of polyacrylamides, 12~16 parts
Aqueous C 5 petroleum resin lotion, 6~8 parts of nano-zinc oxide powders, 15~20 parts of deionized waters.
3. the preparation method of the medical aqueous multiple emulsion paper-plastic lamination adhesive of one kind according to claim 1, which is characterized in that
The power of ultrasonic disperse described in step (4) is 400~500W.
4. the preparation method of the medical aqueous multiple emulsion paper-plastic lamination adhesive of one kind according to claim 1, which is characterized in that
The specific preparation step of starch graft acrylic acid ester lotion described in step (1) are as follows:
(1) cornstarch, neopelex, nonylphenol polyoxyethylene ether, sodium bicarbonate are added in deionized water,
5~10min is stirred with 200~240r/min revolving speed under 75~85 DEG C of water bath condition, it is molten to obtain blended emulsifier starch for heat preservation
Liquid；
(2) 1/10 acrylic acid, 1/10 Butyl acrylate, 1/10 methyl methacrylate, 1/10 ammonium persulfate are slowly added to mix
In co-emulsifier starch solution, 15~20min is stirred with 200~240r/min revolving speed under 75~85 DEG C of water bath condition, is obtained
Starch graft acrylic acid ester seed emulsion；
(3) residual acrylic acid, residual acrylic acid fourth vinegar, remaining methyl methacrylate, remaining ammonium persulfate are slowly added to form sediment
In powder grafted acrylate seed emulsion, under 80~90 DEG C of water bath condition with 300~320r/min revolving speed stirring 10~
15min, heat preservation stand 30~40min of reaction, are cooled to room temperature, adjust pH to 7~8, obtain starch graft acrylic acid ester lotion.
5. the preparation method of the medical aqueous multiple emulsion paper-plastic lamination adhesive of one kind according to claim 4, which is characterized in that
The cornstarch, acrylic acid, Butyl acrylate, methyl methacrylate, ammonium persulfate, neopelex, nonyl
Base phenol polyethenoxy ether, sodium bicarbonate, deionized water parts by weight be 20~30 parts of cornstarch, 20~30 parts of acrylic acid, 40
~60 parts of Butyl acrylates, 10~15 parts of methyl methacrylates, 0.1~0.3 part of ammonium persulfate, 1~3 part of detergent alkylate sulphur
Sour sodium, 1~3 part of nonylphenol polyoxyethylene ether, 2~3 parts of sodium bicarbonates, 120~180 parts of deionized waters.
6. the preparation method of the medical aqueous multiple emulsion paper-plastic lamination adhesive of one kind according to claim 4, which is characterized in that
The addition of 1/10 acrylic acid, 1/10 Butyl acrylate, 1/10 methyl methacrylate, 1/10 ammonium persulfate described in step (2)
10~15min of time.
7. the preparation method of the medical aqueous multiple emulsion paper-plastic lamination adhesive of one kind according to claim 4, which is characterized in that
The addition of residual acrylic acid described in step (3), residual acrylic acid fourth vinegar, remaining methyl methacrylate, remaining ammonium persulfate
1~2hpH of the time adjusts the sodium hydroxide solution using mass concentration 1%.
8. the preparation method of the medical aqueous multiple emulsion paper-plastic lamination adhesive of one kind according to claim 1, which is characterized in that
The specific preparation step of acrylate and vinyl acetate emulsion described in step (2) are as follows:
(1) by polyvinyl alcohol, hydroxyethyl cellulose, lauryl sodium sulfate, octyl phenol polyoxyethylene ether, sodium carbonate addition go from
In sub- water, 15~20min is stirred with 180~200r/min revolving speed under 80~90 DEG C of water bath condition, it is molten to obtain emulsifier mixing
Liquid；
(2) emulsifier mixed solution is added in 1/3 acrylic acid, 1/3 vinylacetate, 1/3 butyl acrylate, 1/3 sodium peroxydisulfate
In, 30~40min is stirred to react with 200~240r/min revolving speed under 60~70 DEG C of water bath condition, obtains the third seed emulsion of vinegar；
(3) residual acrylic acid, remaining vinylacetate, residual acrylic acid butyl ester, remaining sodium peroxydisulfate are slowly added to third kind of vinegar
In sub- lotion, 1~2h is stirred to react with 300~340r/min revolving speed under 70~80 DEG C of water bath condition, is cooled to room temperature, adjusted
PH to 7~8 is saved, acrylate and vinyl acetate emulsion is obtained.
9. the preparation method of the medical aqueous multiple emulsion paper-plastic lamination adhesive of one kind according to claim 8, which is characterized in that
The polyvinyl alcohol, hydroxyethyl cellulose, acrylic acid, vinylacetate, butyl acrylate, lauryl sodium sulfate, octyl
Phenol polyethenoxy ether, sodium peroxydisulfate, sodium carbonate, deionized water parts by weight be 4~6 parts of polyvinyl alcohol, 2~3 parts of ethoxy fibres
Tie up element, 20~30 parts of acrylic acid, 40~60 parts of vinylacetates, 20~30 parts of butyl acrylates, 1~3 part of dodecyl sulphate
Sodium, 1~3 part of octyl phenol polyoxyethylene ether, 0.1~0.3 part of sodium peroxydisulfate, 2~3 parts of sodium carbonate, 120~180 parts of deionized waters.
10. the preparation method of the medical aqueous multiple emulsion paper-plastic lamination adhesive of one kind according to claim 8, feature exist
In, residual acrylic acid described in step (3), remaining vinylacetate, residual acrylic acid butyl ester, remaining sodium peroxydisulfate addition when
Between be 3~4h, pH adjust using mass concentration 1% ammonium hydroxide.
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