CN107459605A - A kind of high-speed coating paper-plastic stick high solid content and low viscosity acrylic pressure sensitive adhesives preparation method - Google Patents
A kind of high-speed coating paper-plastic stick high solid content and low viscosity acrylic pressure sensitive adhesives preparation method Download PDFInfo
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- CN107459605A CN107459605A CN201710684952.3A CN201710684952A CN107459605A CN 107459605 A CN107459605 A CN 107459605A CN 201710684952 A CN201710684952 A CN 201710684952A CN 107459605 A CN107459605 A CN 107459605A
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 21
- 239000011248 coating agent Substances 0.000 title claims abstract description 21
- 238000000576 coating method Methods 0.000 title claims abstract description 21
- 239000004033 plastic Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 239000007787 solid Substances 0.000 title abstract description 18
- 239000003999 initiator Substances 0.000 claims abstract description 43
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 32
- 239000000178 monomer Substances 0.000 claims abstract description 29
- 230000006911 nucleation Effects 0.000 claims abstract description 15
- 238000010899 nucleation Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004816 latex Substances 0.000 claims abstract description 10
- 229920000126 latex Polymers 0.000 claims abstract description 10
- 239000003792 electrolyte Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000004945 emulsification Methods 0.000 claims abstract description 4
- 239000000839 emulsion Substances 0.000 claims description 80
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 22
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000010792 warming Methods 0.000 claims description 12
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical group [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 11
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 11
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 239000003755 preservative agent Substances 0.000 claims description 6
- 230000002335 preservative effect Effects 0.000 claims description 6
- 230000001360 synchronised effect Effects 0.000 claims description 6
- 125000004205 trifluoroethyl group Chemical group [H]C([H])(*)C(F)(F)F 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 210000000481 breast Anatomy 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- JFATZQWHTPPTEJ-UHFFFAOYSA-N 6-methylheptan-3-yl 2-sulfanylpropanoate Chemical group SC(C(=O)OC(CC)CCC(C)C)C JFATZQWHTPPTEJ-UHFFFAOYSA-N 0.000 claims description 2
- 230000000844 anti-bacterial effect Effects 0.000 claims description 2
- 239000003899 bactericide agent Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 10
- 230000001070 adhesive effect Effects 0.000 abstract description 10
- 238000009826 distribution Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 9
- 238000001035 drying Methods 0.000 abstract description 7
- 238000006116 polymerization reaction Methods 0.000 abstract description 6
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 abstract description 5
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 abstract description 5
- 230000002902 bimodal effect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000012528 membrane Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract 1
- 239000003643 water by type Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 15
- 239000003292 glue Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 230000001804 emulsifying effect Effects 0.000 description 4
- 125000005395 methacrylic acid group Chemical class 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- -1 persulfuric acid Ammonium salt Chemical class 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical group OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000009331 sowing Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
Classifications
-
- 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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
-
- 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
-
- 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
- C09J151/08—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 macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
Abstract
The invention discloses a kind of high-speed coating paper-plastic stick high solid content and low viscosity acrylic pressure sensitive adhesives preparation method, secondary Micellar nucleation in polymerization process is realized by secondary addition emulsifying agent, latex particle size and its distribution is realized bimodal distribution, reach high solid content and low viscosity purpose.Formed including electrolyte, initiator, emulsifying agent, butyl acrylate, Isooctyl acrylate monomer, function monomer etc..The present invention passes through pre-emulsification, it is secondary to add emulsifying agent technique, prepare milky white liquid of the outward appearance with blue-fluorescence, for viscosity in 300 600mPa.s, solid content is 64% 70%, film forming matter is water white transparency, pH between 46, have initial bonding strength is fast, rate of drying is fast, the high feature of adhesive strength, adapt to high-speed coating automatic machine construction process requirement, surface tension is adjusted by function monomer, realized using specific function monomer to the preferable bonding of membrane material.Volatile matter will not damage to human body and environment, production environment safety.
Description
Technical field
The present invention relates to adhesive technology of preparing, more particularly to a kind of low viscous propylene of high-speed coating paper-plastic stick large arch dam
Acid fracturing sensitive adhesive.
Background technology
The extensive stock housing materials such as paper material is bonded and is used for box of mobile telephone, milk box.With various advanced technologies,
The appearance of sophisticated equipment, automatic coating production efficiency of equipment is high, can produce individual paper boxes up to ten thousand per hour, therefore to bonding
Requirements at the higher level are proposed with glue performance：1st, just gluing will soon, and paper is combined and wants rapid link after coating at high speed, quick fixed
Position；2nd, glue dries speed is fast, because high-speed coating is automation, pile line operation entirely, product has been descended after streamline directly
Vanning, it is desirable to which glue will realize drying and forming-film on streamline.Polyacrylate dispersion type pressure sensitive adhesive have cost it is low, use
It is safe and pollution-free, polymerization time is short, has the advantages that good cementability, film water white transparency to various materials, be pressure sensitive adhesive
Middle yield highest, most widely used kind.Emulsion pressure-sensitive to some due to using water as medium, slow drying speed, particularly applying
The big pressure sensitive adhesive product of glue amount, drying is particularly problematic, therefore, it is necessary to improve solid content in emulsion pressure-sensitive application
Solves the problems, such as its drying.High solid content emulsion pressure sensitive adhesive can improve the utilization rate of production equipment, reduce transport, the expense of storage,
Accelerate the rate of drying of latex, glue process can reach the thickness required by product in reduction.But the solid content of polymer emulsion
During more than 50%, viscosity increases and steeply risen with solid content, and viscosity increases the mixing for making polymerization system, heat transfer turns into problem,
Therefore, while synthesis of high solid content, viscosity can not be too high, and synthesis difficulty is larger.
For above-mentioned phenomenon, patent CN104371607A discloses a kind of high-solid-content and low-viscosity acrylic emulsion pressure sensitive adhesive
Stick and preparation method thereof.But the influence fluctuation that polymerization stability and viscosity be present is larger, and then causes the viscosity of pressure sensitive adhesive not
It is enough low, and then the tack of pressure sensitive adhesive and holding power are reduced.It is pressure-sensitive that patent CN101676347A discloses 60% large arch dam
Glue and preparation method thereof, but pressure sensitive adhesive is solid when containing more than 50%, and viscosity starts to steeply rise with solid content increase, makes condensate
Mixing, the heat transfer of system turn into problem.Compared with prior art, the adhesive solid content for preparing of the present invention is close to 70%, initial bonding strength
It is fast with rate of drying；Surface energy is low, can carry out quick humidification to material under certain condition and sprawl so as to realize effective bonding；System
Simply and stably, only certain time pause need to be added dropwise in pre-emulsion in standby technique, and emulsifying agent is disposably added into reactor,
Continue that remaining monomer and initiator is added dropwise after 5 minutes.
The content of the invention
Present invention aims at for high-speed coating Adhesive for Paper-Plastic Lamination deficiency, there is provided one kind meets high-speed coating
The preparation method of paper-plastic stick high solid content and low viscosity adhesive.
The purpose of the present invention is achieved through the following technical solutions：A kind of high-speed coating paper-plastic stick large arch dam is low viscous
The preparation method of acrylic pressure sensitive adhesives, it is characterised in that comprise the following steps：
A, 0.06-0.1 parts by weight initiators are dissolved in 1 parts by weight of deionized water, obtain 1.06-1.1 parts by weight systems
Make preparations for sowing son initiator solution；The initiator of 0.14-0.2 parts by weight is dissolved in the deionized water of 4 parts by weight, obtains 4.14-
The dropwise addition initiator solution of 4.2 parts by weight；0.6-0.8 parts by weight Emulsifier is dissolved in 2 parts by weight water, obtains 2.6-2.8 weights
Measure the secondary Micellar nucleation emulsifying agent of part.
B, 11-8.3 parts by weight of deionized water, 0.1 parts by weight electrolyte, 0.05 parts by weight molecular weight are added into pre-emulsification cylinder
Conditioning agent, 0.9-1.2 parts by weight Emulsifier, scattered stirring sequentially add 30-32 parts by weight propylene acid butyl ester, 1-1.5 after 5 minutes
Parts by weight function monomer, the different monooctyl ester of 16-16.5 parts by weight of acrylic acid, 13-14 parts by weight of methylmethacrylate, 2-3 parts by weight
Methacrylic acid, the pre-emulsion of 74.05-76.65 parts by weight is made after high-speed stirred is scattered 50 minutes；
C, into reactor, the deionized water of addition 18-15 parts by weight, 0.05 parts by weight electrolyte are well mixed, and are warming up to
81 DEG C, the pre-emulsion that 4 parts by weight step b are prepared is added, the 1.06-1.1 parts by weight seed initiators that step a is prepared are molten
Liquid, react 30 minutes；
D, the pre-emulsion of 70.05-72.65 parts by weight is added dropwise, the synchronous 4.14-4.2 parts by weight that step a preparations are added dropwise are drawn
Agent solution is sent out, time for adding 4.0 hours, pre-emulsion drips off simultaneously with initiator；When half is added dropwise in pre-emulsion, pause drop
Pre-emulsion and initiator, the disposable secondary Micellar nucleation emulsifying agent of 2.6-2.8 parts by weight for adding step a and preparing, stirring point
Continue that pre-emulsion and initiator is added dropwise after dissipating 5 minutes, form latex, wherein emulsion particle is not of uniform size, increase emulsion particle accumulation
Density, so as to carry large arch dam, reduce viscosity；
E, after pre-emulsion and initiator continue reaction 20 minutes after dripping off, 85 degree are warming up to, insulation reaction is after 90 minutes
Less than 50 DEG C are cooled to, adds the preservative of 0.1-0.2 parts by weight, stirring is vacuumized after 20 minutes, and filtered through gauze, which discharges, to be produced
The low viscous acrylic pressure sensitive adhesives of high-speed coating large arch dam.
Further, the function monomer is the trifluoro ethyl ester of methacrylic acid 2,2,2- or Sartomer chemistry CN704.
Further, the initiator is ammonium persulfate, emulsifying agent be one or both of COPS-1 and Co436 according to
Any mixture than composition, electrolyte is sodium pyrosulfite, and molecular weight regulator is 3- isooctyl mercaptopropionates (IOMP), work(
Energy monomer is the mixture of the trifluoro ethyl ester of methacrylic acid 2,2,2- and Sartomer chemistry CN704 according to any ratio composition, is sterilized
Agent is Clariant NIPACIDE CI 15HS.
The beneficial effects of the present invention are：
1st, when remaining half is added dropwise in pre-emulsion, pause drop monomer and initiator, the emulsification prepared is disposably added
Agent solution, the emulsifying agent of addition form micella, make the secondary Micellar nucleation of emulsion particle, the emulsion particle ultimately formed is not of uniform size, makes
Bimodal or multi-modal is presented in latex particle size, and bead is inserted between big ball space, increases emulsion particle bulk density, so as to improve
Admittedly containing, viscosity is reduced；
2nd, first to stop that pre-emulsion and monomer, and second is added dropwise before adding emulsifying agent in production process again
After secondary addition emulsifier for mixing is scattered 5 minutes it is further continued for that pre-emulsion and initiator is added dropwise.Swelling can so be made in emulsion particle
Middle monomer stabilization reaction is complete, if not stopping that pre-emulsion and initiator is added dropwise, avoids system glue after secondary addition emulsifying agent
Beam increases, and polymerisation place is increased, system reaction liberated heat increase, cause temperature to rise, polymerisation it is uncontrollable from
And influence quality；
3rd, function monomer is the trifluoro ethyl ester of methacrylic acid 2,2,2- and Sartomer chemistry CN704, methacrylic acid 2,2,
Fluorine element surface energy is very low in 2- trifluoro ethyl esters, contributes to reduce product surface energy after introducing, so as to improve in plastic film material
Expect the wetting on surface and sprawl, realize effectively bonding；Sartomer CN704 belongs to urethane acrylate monomer, as to membrane material
Expect adhesion promoter, while chain is more flexible, has to spread in membrane material.
Embodiment
The preparation method of the present invention is described in detail below in conjunction with specific embodiment.In following examples, initiator
For ammonium persulfate, emulsifying agent is COPS-1 and Co436, and electrolyte is sodium pyrosulfite, and molecular weight regulator is 3- mercaptopropionic acids
Different monooctyl ester (IOMP), function monomer are that the trifluoro ethyl ester of methacrylic acid 2,2,2- and Sartomer chemistry CN704 are mixed, and bactericide is
Clariant NIPACIDE CI 15HS, when mentioned component not limited to this.
One total amount of embodiment=1000kg
A, 0.6 kilogram of ammonium persulfate is dissolved in 10 kilograms of deionized waters, obtains 10.6 kilograms and prepare seed persulfuric acid
Ammonium salt solution；1.4 kilograms of ammonium persulfates are dissolved in 40 kilograms of deionized waters, obtain 41.4 kilograms of dropwise addition ammonium persulfate solutions；By 3
Kilogram COPS-1,3 kilograms of Co436 emulsifying agents are dissolved in 20 kilograms of deionized waters, obtain 26 kilograms of secondary Micellar nucleation emulsifying agents.
B, 110 kilograms of deionized waters are added in emulsifying kettle, is dispersed with stirring and adds 1 kilogram of sodium pyrosulfite, 0.5 kilogram
IOMP, 6 kilograms of COPS-1,3 kilograms of Co436 emulsifying agents, scattered stirring sequentially add 300 kilograms of butyl acrylates, 2 after 5 minutes
Kilogram trifluoro ethyl ester of function monomer methacrylic acid 2,2,2-, 8 kilograms of function monomer CN704,160 kilograms of Isooctyl acrylate monomers,
130 kilograms of methyl methacrylates, 20 kilograms of methacrylic acids, 740.5 kilograms of pre- breasts are made after high-speed stirred is scattered 50 minutes
Change liquid；
C, 180 kilograms of deionized waters, 0.5 kilogram of sodium pyrosulfite are added into reactor, is warming up to 81 DEG C, it is public to add 40
Jin step b pre-emulsion, step a 10.6 kilograms of seed ammonium persulfate solutions, reacts 30 minutes.
D, step b 700.5 kilograms of pre-emulsion, synchronous 41.4 kilograms of ammonium persulfates that step a is added dropwise and prepares are added dropwise
Solution, time for adding 4.0 hours, pre-emulsion drips off simultaneously with initiator；When remaining half is added dropwise in pre-emulsion, pause drop
Pre-emulsion and initiator, disposable 26 kilograms of secondary Micellar nucleation emulsifying agents for adding step a, be dispersed with stirring 5 minutes it is follow-up
Continuous that pre-emulsion and initiator is added dropwise, the emulsion particle of formation is not of uniform size, increases emulsion particle bulk density, so as to carry large arch dam,
Reduce viscosity；
E, after pre-emulsion and initiator continue reaction 20 minutes after dripping off, 85 degree are warming up to, insulation reaction is after 90 minutes
Less than 50 DEG C are cooled to, adds 1 kilogram of preservative, stirring vacuumizes after 20 minutes, and filtered through gauze, which discharges, produces high-speed coating use
The low viscous pressure-sensitive adhesive of large arch dam.
Two total amounts of embodiment=1000kg
A, 1 kilogram of ammonium persulfate is dissolved in 10 kilograms of deionized waters, obtaining 11 kilograms, to prepare seed ammonium persulfate molten
Liquid；2 kilograms of ammonium persulfates are dissolved in 40 kilograms of deionized waters, obtain 42 kilograms of dropwise addition ammonium persulfate solutions；By 5 kilograms
COPS-1,2 kilograms of Co436 emulsifying agents are dissolved in 20 kilograms of deionized waters, obtain 27 kilograms of secondary Micellar nucleation emulsifying agents.
B, 10 kilograms of deionized waters are added in emulsifying kettle, is dispersed with stirring and adds 1 kilogram of sodium pyrosulfite, 0.5 kilogram of IOMP,
4 kilograms of COPS-1,6 kilograms of Co436 emulsifying agents, scattered stirring sequentially add 310 kilograms of butyl acrylates, 3 kilograms of work(after 5 minutes
Can monomer methacrylic acid 2,2,2- trifluoro ethyl ester, 9 kilograms of function monomer CN704,160 kilograms of Isooctyl acrylate monomers, 135 kilograms
Methyl methacrylate, 20 kilograms of methacrylic acids, 748.5 kilograms of pre-emulsions are made after high-speed stirred is scattered 50 minutes；
C, 170 kilograms of deionized waters, 0.5 kilogram of sodium pyrosulfite are added into reactor, is warming up to 81 DEG C, it is public to add 40
Jin step b pre-emulsion, step a 11 kilograms of seed ammonium persulfate solutions, reacts 30 minutes；
D, step b 708.5 kilograms of pre-emulsion is added dropwise, 42 kilograms of ammonium persulfates that synchronous dropwise addition step a is prepared are molten
Liquid, time for adding 4.0 hours, pre-emulsion drips off simultaneously with initiator；When remaining half is added dropwise in pre-emulsion, pause drop is pre-
Emulsion and initiator, disposable 27 kilograms of secondary Micellar nucleation emulsifying agents for adding step a, continue after being dispersed with stirring 5 minutes
Pre-emulsion and initiator is added dropwise, the emulsion particle of formation is not of uniform size, increases emulsion particle bulk density, so as to carry large arch dam, drop
Low viscosity；
E, after pre-emulsion and initiator continue reaction 20 minutes after dripping off, 85 degree are warming up to, insulation reaction is after 90 minutes
Less than 50 DEG C are cooled to, adds 1 kilogram of preservative, stirring vacuumizes after 20 minutes, and filtered through gauze, which discharges, produces high-speed coating use
The low viscous pressure-sensitive adhesive of large arch dam.
Three total amounts of embodiment=1000kg
A, 0.8 kilogram of ammonium persulfate is dissolved in 10 kilograms of deionized waters, obtains 10.8 kilograms and prepare seed persulfuric acid
Ammonium salt solution；1.7 kilograms of ammonium persulfates are dissolved in 40 kilograms of deionized waters, obtain 41.7 kilograms of dropwise addition ammonium persulfate solutions；By 3
Kilogram COPS-1,4.5 kilograms of Co436 emulsifying agents are dissolved in 20 kilograms of deionized waters, obtain 27.5 kilograms of secondary Micellar nucleations breasts
Agent.
B, 90 kilograms of deionized waters are added in emulsifying kettle, is dispersed with stirring and adds 1 kilogram of sodium pyrosulfite, 0.5 kilogram of IOMP,
3 kilograms of COPS-1,8 kilograms of Co436 emulsifying agents, scattered stirring sequentially add 320 kilograms of butyl acrylates, 2 kilograms of work(after 5 minutes
Energy monomer methacrylic acid 2,2,2- trifluoro ethyl ester, 11 kilograms of function monomer CN704,163 kilograms of Isooctyl acrylate monomers, 130 public affairs
Jin methyl methacrylate, 30 kilograms of methacrylic acids, 758.5 kilograms of pre-emulsions are made after high-speed stirred is scattered 50 minutes；
C, 160 kilograms of deionized waters, 0.5 kilogram of sodium pyrosulfite are added into reactor, is warming up to 81 DEG C, it is public to add 40
Jin step b pre-emulsion, step a 10.8 kilograms of seed ammonium persulfate solutions, reacts 30 minutes；
D, step b 718.5 kilograms of pre-emulsion, synchronous 41.7 kilograms of dropwise addition over cures that step a is added dropwise and prepares are added dropwise
Acid ammonium solution, time for adding 4.0 hours, pre-emulsion drips off simultaneously with initiator；When remaining half is added dropwise in pre-emulsion, temporarily
Stop dripping pre-emulsion and initiator, disposable 27.5 kilograms of secondary Micellar nucleation emulsifying agents for adding step a, be dispersed with stirring 5 points
Continue that pre-emulsion and initiator is added dropwise after clock, the emulsion particle of formation is not of uniform size, increases emulsion particle bulk density, so as to improve
Admittedly containing, viscosity is reduced；
E, after pre-emulsion and initiator continue reaction 20 minutes after dripping off, 85 degree are warming up to, insulation reaction is after 90 minutes
Less than 50 DEG C are cooled to, adds 1 kilogram of preservative, stirring vacuumizes after 20 minutes, and filtered through gauze, which discharges, produces high-speed coating use
The low viscous pressure-sensitive adhesive of large arch dam.
Example IV total amount=1000kg
A, 1 kilogram of ammonium persulfate is dissolved in 10 kilograms of deionized waters, obtaining 11 kilograms, to prepare seed ammonium persulfate molten
Liquid；2 kilograms of ammonium persulfates are dissolved in 40 kilograms of deionized waters, obtain 42 kilograms of dropwise addition ammonium persulfate solutions；By 5 kilograms
COPS-1,3 kilograms of Co436 emulsifying agents are dissolved in 20 kilograms of deionized waters, obtain 28 kilograms of secondary Micellar nucleation emulsifying agents.
B, 83 kilograms of deionized waters are added in emulsifying kettle, is dispersed with stirring and adds 1 kilogram of sodium pyrosulfite, 0.5 kilogram of IOMP,
6 kilograms of COPS-1,6 kilograms of Co436 emulsifying agents, scattered stirring sequentially add 320 kilograms of butyl acrylates, 3 kilograms of work(after 5 minutes
Can monomer methacrylic acid 2,2,2- trifluoro ethyl ester, 12 kilograms of function monomer CN704, it is 165 kilograms of Isooctyl acrylate monomers, 140 public
Jin methyl methacrylate, 30 kilograms of methacrylic acids, 766.5 kilograms of pre-emulsions are made after high-speed stirred is scattered 50 minutes；
C, 150 kilograms of deionized waters, 0.5 kilogram of sodium pyrosulfite are added into reactor, is warming up to 81 DEG C, it is public to add 40
Jin step b pre-emulsion, step a 11 kilograms of seed ammonium persulfate solutions, reacts 30 minutes；
D, step b 726.5 kilograms of pre-emulsion is added dropwise, 42 kilograms of ammonium persulfates that synchronous dropwise addition step a is prepared are molten
Liquid, time for adding 4.0 hours, pre-emulsion drips off simultaneously with initiator；When remaining half is added dropwise in pre-emulsion, pause drop is pre-
Emulsion and initiator, disposable 28 kilograms of secondary Micellar nucleation emulsifying agents for adding step a, continue after being dispersed with stirring 5 minutes
Pre-emulsion and initiator is added dropwise, the emulsion particle of formation is not of uniform size, increases emulsion particle bulk density, so as to carry large arch dam, drop
Low viscosity；
E, after pre-emulsion and initiator continue reaction 20 minutes after dripping off, 85 degree are warming up to, insulation reaction is after 90 minutes
Less than 50 DEG C are cooled to, adds 1 kilogram of preservative, stirring vacuumizes after 20 minutes, and filtered through gauze, which discharges, produces high-speed coating use
The low viscous pressure-sensitive adhesive of large arch dam.
In order to which four embodiments obtain to more than high-speed coating paper-plastic stick is carried out pair with high solid content and low viscosity adhesive
Than evaluation, following contrast experiment is carried out：Formula is (wherein by 3 kilograms of COPS-1,3 kilograms of Co436 emulsifying agents as described in embodiment one
It is dissolved in 20 kilograms of deionized waters, the secondary Micellar nucleation emulsifying agent of 26 kilograms obtained, is not after half is added dropwise in pre-emulsion
Add, and be changed to it is disposable before polymerization add C step by step in rapid reactor, obtain comparative example 1) prepares it is corresponding identical solid containing producing
Product.
Embodiment 1 is to implementation 4, the product physics of comparative example 1 and performance indications, according to GB/T 11175-2002 synthetic resin
Emulsion Test Method detects；Determined using GB/T 4852-2002 pressure-sensitive tape tacks experimental test procedures and adhesive is made
It is just viscous；It is viscous that holding for the obtained glue of test method test of viscosity is held using GB/T 4851-2014 adhesive tapes；GB/T 2792-
The peeling force of glue is made in the test method measure of 2014 adhesive tape peel strengths；Latex particle size and particle diameter distribution using water as point
Dispersion media, determined by DelsaTM Nano.If detection is as shown in the table：
Table embodiment 1-3 high-speed coating paper-plastic stick high-solid lower-viscosity pressure-sensitive adhesives, the test result of comparative example 1.
| Embodiment 1 | Comparative example 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Admittedly contain | 63.5% | 63.5% | 68% | 66% | 69.2% |
| Viscosity | 420mPa.S | 12300mPa.S | 470mPa.S | 410mPa.S | 530mPa.S |
| pH | 5 | 5 | 6 | 5 | 6 |
| Peel off N/25um | 7.6 | 5.3 | 8.2 | 8.1 | 8.6 |
| It is just viscous | 23Pa.S | 21Pa.S | 24Pa.S | 22Pa.S | 24Pa.S |
| Hold viscous | 110Pa.S | 90Pa.S | 115Pa.S | 116Pa.S | 125Pa.S |
As can be seen from the above table, high-speed coating paper-plastic stick high-solid lower-viscosity degree pressure-sensitive adhesive of the invention is by adding breast
Agent technique, is copolymerized that to prepare viscosity low with function monomer, there is preferable wetting and spreading performance to membrane material, so as to just glue it is fast, hold
Glue, and peel strength is high.
Micelle grain grain is tested in the adhesive prepared by the adhesive and comparative example 1 that are prepared to embodiment 1-4, real
Test result to find, in embodiment 1-4 product, product latex particle size is more to be distributed between 800nm and 100nm, particle diameter distribution
Width, bimodal or multi-modal is presented；Emulsion particle is not of uniform size, and particle diameter distribution index is about 0.83.This be due to latex repeatedly into
Core, emulsion particle is not of uniform size, and particle diameter distribution is wide, and bead is inserted between big ball space, makes latex particle size that bimodal or multimodal be presented
Distribution, increase emulsion particle bulk density, so as to carry large arch dam, reduce viscosity.And the particle size analysis size about 800nm of comparative example 1
It is more uniform, Unimodal Distribution is only presented, this is due to that the emulsifying agent of comparative example 1 is to add before polymerization in reactor, and latex seed is same
One time grew up into emulsion particle, but because emulsion particle is to increase simultaneously, terminated simultaneously, therefore particle diameter distribution is narrower, i.e. emulsion particle
Size is than more uniform, therefore obtained viscosity is larger.
Claims (3)
- A kind of 1. preparation method of the low viscous acrylic pressure sensitive adhesives of high-speed coating paper-plastic stick large arch dam, it is characterised in that Comprise the following steps：A, 0.06-0.1 parts by weight initiators are dissolved in 1 parts by weight of deionized water, obtain 1.06-1.1 parts by weight and prepare kind Son initiator solution；The initiator of 0.14-0.2 parts by weight is dissolved in the deionized water of 4 parts by weight, obtains 4.14-4.2 weights Measure the dropwise addition initiator solution of part；0.6-0.8 parts by weight Emulsifier is dissolved in 2 parts by weight water, obtains 2.6-2.8 parts by weight two Secondary Micellar nucleation emulsifying agent.B, 11-8.3 parts by weight of deionized water, 0.1 parts by weight electrolyte, 0.05 parts by weight molecular-weight adjusting are added into pre-emulsification cylinder Agent, 0.9-1.2 parts by weight Emulsifier, scattered stirring sequentially add 30-32 parts by weight propylene acid butyl ester, 1-1.5 weight after 5 minutes Part function monomer, the different monooctyl ester of 16-16.5 parts by weight of acrylic acid, 13-14 parts by weight of methylmethacrylate, 2-3 parts by weight methyl Acrylic acid, the pre-emulsion of 74.05-76.65 parts by weight is made after high-speed stirred is scattered 50 minutes；C, into reactor, the deionized water of addition 18-15 parts by weight, 0.05 parts by weight electrolyte are well mixed, and are warming up to 81 DEG C, the pre-emulsion that 4 parts by weight step b of addition are prepared, the 1.06-1.1 parts by weight seed initiator solutions that step a is prepared, Reaction 30 minutes；D, the pre-emulsion of 70.05-72.65 parts by weight, the synchronous 4.14-4.2 parts by weight initiators that step a is added dropwise and prepares is added dropwise Solution, time for adding 4.0 hours, pre-emulsion drips off simultaneously with initiator；When half is added dropwise in pre-emulsion, pre- breast is dripped in pause Change liquid and initiator, the disposable secondary Micellar nucleation emulsifying agent of 2.6-2.8 parts by weight for adding step a and preparing, be dispersed with stirring 5 points Continuing that pre-emulsion and initiator is added dropwise after clock, form latex, wherein emulsion particle is not of uniform size, increases emulsion particle bulk density, So as to carry large arch dam, viscosity is reduced；E, after pre-emulsion and initiator continue reaction 20 minutes after dripping off, 85 degree are warming up to, insulation reaction cools after 90 minutes To less than 50 DEG C, the preservative of 0.1-0.2 parts by weight is added, stirring is vacuumized after 20 minutes, and filtered through gauze, which discharges, to be produced at a high speed The low viscous acrylic pressure sensitive adhesives of coating large arch dam.
- 2. according to the method for claim 1, it is characterised in that the function monomer is the trifluoro second of methacrylic acid 2,2,2- Ester or Sartomer chemistry CN704.
- 3. according to the method for claim 1, it is characterised in that the initiator is ammonium persulfate, emulsifying agent COPS-1 With one or both of Co436 according to any mixture than composition, electrolyte is sodium pyrosulfite, and molecular weight regulator is 3- isooctyl mercaptopropionates (IOMP), function monomer are that the trifluoro ethyl ester of methacrylic acid 2,2,2- and Sartomer chemistry CN704 are pressed According to any mixture than composition, bactericide is Clariant NIPACIDE CI 15HS.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109134743A (en) * | 2018-08-14 | 2019-01-04 | 顶立新材料科技有限公司 | A kind of high solid content and low viscosity acrylic pressure sensitive adhesives preparation method |
| CN109837046A (en) * | 2019-02-28 | 2019-06-04 | 广东星宇耐力新材料股份有限公司 | A kind of compound aqueous adhesive and preparation method thereof of plastic film dry type |
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| CN104178065A (en) * | 2014-08-14 | 2014-12-03 | 汕头市龙湖昌丰化工有限公司 | Preparation method of high-speed coating/connecting line peeling transfer adhesive |
| CN106349982A (en) * | 2016-08-26 | 2017-01-25 | 江苏国胶化学科技有限公司 | Preparation method of high-solid-content low-viscosity pressure-sensitive adhesive |
| CN106519106A (en) * | 2016-10-18 | 2017-03-22 | 无锡海特新材料研究院有限公司 | Super-transparent acrylate pressure-sensitive adhesive emulsion capable of being coated at high speed as well as preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104178065A (en) * | 2014-08-14 | 2014-12-03 | 汕头市龙湖昌丰化工有限公司 | Preparation method of high-speed coating/connecting line peeling transfer adhesive |
| CN106349982A (en) * | 2016-08-26 | 2017-01-25 | 江苏国胶化学科技有限公司 | Preparation method of high-solid-content low-viscosity pressure-sensitive adhesive |
| CN106519106A (en) * | 2016-10-18 | 2017-03-22 | 无锡海特新材料研究院有限公司 | Super-transparent acrylate pressure-sensitive adhesive emulsion capable of being coated at high speed as well as preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109134743A (en) * | 2018-08-14 | 2019-01-04 | 顶立新材料科技有限公司 | A kind of high solid content and low viscosity acrylic pressure sensitive adhesives preparation method |
| CN109837046A (en) * | 2019-02-28 | 2019-06-04 | 广东星宇耐力新材料股份有限公司 | A kind of compound aqueous adhesive and preparation method thereof of plastic film dry type |
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