CN102504091A - Method for preparing emulsion acrylic pressure-sensitive adhesive for high-speed coating machine - Google Patents
Method for preparing emulsion acrylic pressure-sensitive adhesive for high-speed coating machine Download PDFInfo
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Abstract
The invention discloses preparation of an emulsion acrylic pressure-sensitive adhesive for a high-speed coating machine, which comprises the following steps of: preparation of pre-emulsion, i.e. adding a reactive monomer, an emulsifier, a wetting agent, a cross-linking agent and deionized water into a high-level emulsification tank to prepare the pre-emulsion for later use; preparation of seed emulsion and primary nucleation, i.e. performing the primary nucleation reaction for 1 to 4 hours; secondary nucleation, i.e. adding a functional monomer and a small amount of deionized water into the residual pre-emulsion and continuously dropwise adding an initiator with stirring; and chain propagation and partial cross-linking polymerization of a polymer, i.e. after totally dropwise adding the raw materials in the emulsification tank and the initiator, carrying out chain propagation and partial cross-linking polymerization for 1 to 4 hours. The emulsion acrylic pressure-sensitive adhesive has low raw material cost, high bonding strength, good adhesive application performance on the premise of the same solid content, and high curing speed.
Description
Technical field
The present invention relates to the pressure sensitive adhesive preparing technical field, relate in particular to of the preparation of a kind of high speed coating machine with emulsion acrylate class pressure sensitive adhesive.
Background technology
Pressure sensitive adhesive is meant that only need impose certain pressure just can moisteningly cement by maxxaedium and with adherend, produces one type of tackiness agent of practical bonding strength.Pressure-sensitive acrylate is to use the widest pressure sensitive adhesive at present, and two types of water-latex type and solvent-borne types are arranged.It is big that solvent-type acrylic ester class pressure sensitive adhesive has an initial bonding strength, water-tolerant, and surface covered is fast, the production efficiency advantages of higher, the organic solvent consumption is big, environmental pollution serious, uneasy congruent fatal shortcoming but exist.Water-latex type then with water as solvent; Have cost low, safe in utilization, pollution-free, to various materials good bonding property is all arranged, characteristics such as the water white transparency of filming; Be China's emulsion-type pressure-sensitive with fastest developing speed since the eighties in 20th century, can be widely used in numerous areas such as advertisement consumptive material, gummed tape, Pressuresensitive Label, medical material, telecommunications, aerospace, disposable product.
But the greatest problem that emulsion acrylate class pressure sensitive adhesive exists is: the evaporation rate of water is slow when 1, being used for high-speed coating is difficult to mate with high speed coating machine; 2, the surface tension of water is greater than the surface energy that is applied material, and it is inhomogeneous therefore when high-speed coating, gluing to occur, and the problem that leveling characteristics is bad its essence is that emulsion is difficult to soak into solid surface.
Chinese patent CN 1438253A proposes a kind of employing seeded emulsion polymerization technology, selects emulsifier system and viscosity control agent with special construction for use, adopt can self-crosslinking the low emulsifier content of acrylate monomer preparation, highly filled, performance is excellent
Different vinylformic acid microemulsion.This emulsion is used to prepare woodwork coating, and the characteristics of this self-crosslinking woodwork coating are rapidly dry, and hardness is high, the transparency, good fluidity, and chemical-resistant is excellent, and has good low-temperature snappiness and resistance to blocking.
It is 65 % that the little equality of Feng (volume o. 11th in " chemical research and application " November the 22nd in 2010) report in " preparation of high-solid-content and low-viscosity acrylic ester emulsion pressure sensitive adhesive " adopts conventional seed emulsion polymerization to synthesize solid content; Viscosity is less than the emulsion pressure-sensitive of 400 mPa s, and investigated the influence to vinylformic acid wine copolymer emulsion viscosity and polymerization stability of comonomer, emulsifying agent, initiator, buffer reagent and seed emulsion amount.This article discusses the variation (200 ~ 400mPa s) of viscosity with each influence factor, does not provide the use properties situation, like cohesive strength, and coating situation etc.
Summary of the invention
In order to address the above problem, it is low to the invention provides a kind of raw materials cost, and cohesive strength is high, and the fast high speed coating machine of curing speed is with the preparation of emulsion acrylate class pressure sensitive adhesive.
In order to achieve the above object, technical scheme of the present invention general introduction is as follows: high speed coating machine may further comprise the steps with the preparation of emulsion acrylate class pressure sensitive adhesive:
(1) preparation of pre-emulsion: reaction monomers, emulsifying agent, wetting agent, linking agent and deionized water are added in the high-order emulsion tank, and emulsification also is preheated to 40 ~ 50 ℃, and the preparation pre-emulsion is subsequent use, and said reaction monomers comprises soft monomer and hard monomer.
(2) seed emulsion preparation and a nucleation: the part of the pre-emulsion for preparing and the part of initiator are put into retort; Be warming up to 55 ~ 75 ℃; Open water of condensation; Continue to be warming up to 75 ~ 85 ℃, after temperature is steady, begin to drip remaining pre-emulsion and initiator, once become nuclear reaction 1 ~ 4h under stirring.
(3) secondary nucleation: after the nucleation; In the remaining pre-emulsion of a part, add function monomer and small quantity of deionized water; The continued that stirs drips a part of remaining pre-emulsion 0 ~ 3h, continues to drip a part of remaining initiator, 80 ~ 90 ℃ of holding temperatures simultaneously.
(4) polymer chain increases and partial cross-linked polymerization: after the pre-emulsion of emulsion tank and initiator were all dripped, 80 ~ 90 ℃ of controlled temperature carried out chainpropagation and partial cross-linked polymerization 1 ~ 4h.
Further improvement of the present invention is: the parts by weight of each component of said pressure sensitive adhesive are following: 30 ~ 60 parts of soft monomers, 1 ~ 10 part of hard monomer, 1 ~ 10 part of function monomer; Linking agent 0.1 ~ 5,0. 5 ~ 5 parts of emulsifying agents, wetting agent 0.1 ~ 1 minute; 0. 05 ~ 1 part of initiator, 35 ~ 70 parts of deionized waters.
Further improvement of the present invention is: in the step of the preparation of pre-emulsion; Comprise soft monomer and hard monomer in the wherein said reaction monomers, said soft monomer is one or more in ethyl propenoate, Bing Xisuandingzhi, Isooctyl acrylate monomer or vinylformic acid-2 one ethylhexyls; Said hard monomer is TEB 3K or vinylbenzene; Said emulsifying agent is two or more in X 2073, sodium lauryl sulphate, octyl (or nonyl) phenol polyethenoxy (10) ether, the AEO; Said wetting agent is sodium butylnaphthalenesulfonate or polyoxyethylene alkanisation ether; Said linking agent is N,N methylene bis acrylamide or N hydroxymethyl acrylamide; Said initiator is a persulphate.In the step of a seed emulsion preparation and a nucleation, said initiator is a persulphate.In the step of said secondary nucleation, said function monomer is acrylic or methacrylic acid.
The present invention compared with prior art has following advantage: (1) the present invention adopts emulsifying agent and the wetting agent and composite through rationally with function functional group; Reduce the emulsion surface tension; Make it with close by the surface energy of sticking material; Thereby reach the purpose of fine infiltration, it is inhomogeneous gluing to occur when solving high-speed coating, the problem that leveling characteristics is bad.The surface tension of general Emulsion Adhesive is 42 ~ 48 mN/m; And the surface energy that is glued material PE, PP, PET commonly used is respectively 31 ~ 33,29 ~ 30 and 41 ~ 42 mN/m; Because the existence of dynamic surface tension; Glue the moment of high-speed coating surface tension continue to raise, the surface energy of itself and base material is differed greatly, so glue cannot carry out good wetting to base material.(2) the present invention repeatedly becomes nuclear reaction to form through in the emulsion polymerization process, adding emulsifying agent and function monomer, makes the diversification of emulsion particle size distribution, can reach that preparation highly contains admittedly, the purpose of low-viscosity stable polymer emulsion.(3) raw materials cost is low, and cohesive strength is high, and sizability is good under the prerequisite of same solid content, and curing speed is fast.
Embodiment
In order to deepen that understanding of the present invention is done further detailed description below in conjunction with embodiment to the present invention, this embodiment only is used to explain the present invention, does not constitute the qualification to protection domain of the present invention.
The present invention proposes the preparation method of a kind of high speed coating machine with emulsion acrylate class pressure sensitive adhesive, comprising: reaction monomers, emulsifying agent, wetting agent, linking agent and deionized water are added in the high-order emulsion tank, and emulsification also is preheated to 40 ~ 50 ℃; The preparation pre-emulsion is subsequent use, and reaction monomers comprises that soft monomer and hard monomer put into retort with the part of the pre-emulsion for preparing and the part of initiator, is warming up to 55 ~ 75 ℃; Open water of condensation, continue to be warming up to 75 ~ 85 ℃, after temperature is steady, begin to drip a part of remaining pre-emulsion and initiator; Once become nuclear reaction 1 ~ 4h under stirring, after the nucleation, in the remaining pre-emulsion of a part, add function monomer and small quantity of deionized water; The continued that stirs drips a part of remaining pre-emulsion 0 ~ 3h; Continue to drip remaining initiator simultaneously, 80 ~ 90 ℃ of holding temperatures are after the pre-emulsion of emulsion tank and initiator all dripped; 80 ~ 90 ℃ of controlled temperature carry out chainpropagation and partial cross-linked polymerization 1 ~ 4h.
Wherein, 30 ~ 60 parts of soft monomers, 1 ~ 10 part of hard monomer, 1 ~ 10 part of function monomer, linking agent 0.1 ~ 5,0. 5 ~ 5 parts of emulsifying agents, wetting agent 0.1 ~ 1 minute, 0. 05 ~ 1 part of initiator, 35 ~ 70 parts of deionized waters.
Comprise soft monomer and hard monomer in the said reaction monomers, soft monomer can be selected from one or more in ethyl propenoate, Bing Xisuandingzhi, Isooctyl acrylate monomer or vinylformic acid-2 one ethylhexyls;
Said hard monomer can be selected from TEB 3K or vinylbenzene;
Emulsifying agent can be selected from two or more in X 2073, sodium lauryl sulphate, octyl (or nonyl) phenol polyethenoxy (10) ether, the AEO;
Wetting agent can be selected from sodium butylnaphthalenesulfonate or polyoxyethylene alkanisation ether; Said linking agent is N,N methylene bis acrylamide or N hydroxymethyl acrylamide;
The optional persulphate of initiator;
In the step of said secondary nucleation, function monomer can be selected from acrylic or methacrylic acid.
Embodiment one:
In the header tank emulsion tank, add Bing Xisuandingzhi 160kg, ethyl propenoate 160kg, TEB 3K 11kg, polyoxyethylene alkanisation ether 0.1kg successively, it is subsequent use that N hydroxymethyl acrylamide 11kg, sodium lauryl sulphate 5kg, sim alkylphenol T 46155 (10) ether 1.76kg and water 189kg stir emulsification; In retort, add sodium lauryl sulphate 1.76kg, sim alkylphenol T 46155 (10) ether 1.32kg and water successively, 53kg stir dissolve subsequent use; Ammonium persulphate 0.85kg and the high-order jar that drips of water 55kg adding is subsequent use.
Retort is heated to 40 ℃; Put into wherein 55 ㎏ to emulsion in the emulsion tank, stir the initiator that continues to be heated to adding 1/10 about 60 ℃ down, open water of condensation; Begin reaction when continuing to be heated to 75 ~ 80 ℃, the automatic exothermic temperature of system rises to rapidly about 90 ℃;
When temperature falls after rise, beginning to drip emulsification material and the initiator 2h to 2/3 of header tank, temperature is controlled at 85 ~ 90 ℃, and 11kg vinylformic acid is added the header tank continued that stirs drip 2h; Chainpropagation and partial cross-linked polymerization 2h; Be cooled to 60 ℃ and filter discharging, the theoretical solid content 55% of emulsion.
Embodiment two:
In the header tank emulsion tank, add Isooctyl acrylate monomer 160kg, ethyl propenoate 160kg, TEB 3K 11kg, polyoxyethylene alkanisation ether 0.1kg successively, it is subsequent use that N hydroxymethyl acrylamide 11kg, sodium lauryl sulphate 5kg, sim alkylphenol T 46155 (10) ether 1.76kg and water 189kg stir emulsification; In retort, add sodium lauryl sulphate 1.76kg, sim alkylphenol T 46155 (10) ether 1.32kg and water successively, 53kg stir dissolve subsequent use; Ammonium persulphate 0.85kg and the high-order jar that drips of water 55kg adding is subsequent use.-·
Retort is heated to 40 ℃; Put into wherein 55 ㎏ to emulsion in the emulsion tank, stir the initiator that continues to be heated to adding 1/10 about 60 ℃ down, open water of condensation; Begin reaction when continuing to be heated to 75 ~ 80 ℃, the automatic exothermic temperature of system rises to rapidly about 90 ℃;
When temperature falls after rise, beginning to drip emulsification material and the initiator 2h to 2/3 of header tank, temperature is controlled at 85 ~ 90 ℃, adds 11kg vinylformic acid and adds 40kg water simultaneously, and the header tank continued that stirs drips 1h; Chainpropagation and partial cross-linked polymerization 2h; Be cooled to 60 ℃ and filter discharging, the theoretical solid content 52% of emulsion.
Embodiment three:
In the header tank emulsion tank, add Bing Xisuandingzhi 160kg, ethyl propenoate 160kg, TEB 3K 11kg, polyoxyethylene alkanisation ether 0.1kg successively, it is subsequent use that N hydroxymethyl acrylamide 11kg, sodium lauryl sulphate 5kg, sim alkylphenol T 46155 (10) ether 1.76kg and water 189kg stir emulsification; In retort, add sodium lauryl sulphate 1.76kg, sim alkylphenol T 46155 (10) ether 1.32kg and water successively, 53kg stir dissolve subsequent use; Ammonium persulphate 0.85kg and the high-order jar that drips of water 55kg adding is subsequent use.
Retort is heated to 40 ℃; Put into wherein 55 ㎏ to emulsion in the emulsion tank, stir the Sodium Persulfate that continues to be heated to adding 1/10 about 60 ℃ down, open water of condensation; Begin reaction when continuing to be heated to 75 ~ 80 ℃, the automatic exothermic temperature of system rises to rapidly about 90 ℃;
When temperature falls after rise, begin to drip the emulsification material and the Sodium Persulfate 1h of header tank, temperature is controlled at 85 ~ 90 ℃, and the 11kg methylacrylic acid is added the header tank continued that stirs drip 2h; Chainpropagation and partial cross-linked polymerization 2h; Be cooled to 60 ℃ and filter discharging, the theoretical solid content 60% of emulsion.
Embodiment four:
In the header tank emulsion tank, add Bing Xisuandingzhi 80kg, Isooctyl acrylate monomer 80kg successively; Ethyl propenoate 160kg, TEB 3K 11kg, polyoxyethylene alkanisation ether 0.1kg, it is subsequent use that N hydroxymethyl acrylamide 11kg, sodium lauryl sulphate 5kg, sim alkylphenol T 46155 (10) ether 1.76kg and water 189kg stir emulsification; In retort, add sodium lauryl sulphate 1.76kg, sim alkylphenol T 46155 (10) ether 1.32kg and water successively, 53kg stir dissolve subsequent use; Ammonium persulphate 0.6kg and the high-order jar that drips of water 55kg adding is subsequent use
Retort is heated to 40 ℃; Put into wherein 55 ㎏ to emulsion in the emulsion tank, stir the initiator that continues to be heated to adding 1/10 about 60 ℃ down, open water of condensation; Begin reaction when continuing to be heated to 75 ~ 80 ℃, the automatic exothermic temperature of system rises to rapidly about 90 ℃;
When temperature falls after rise, beginning to drip emulsification material and the initiator 2h to 2/3 of header tank, temperature is controlled at 85 ~ 90 ℃, and 11kg vinylformic acid is added the header tank continued that stirs drip 2h; Chainpropagation and partial cross-linked polymerization 2h; Be cooled to 60 ℃ and filter discharging, the theoretical solid content 55% of emulsion.
Embodiment five:
In the header tank emulsion tank, add Isooctyl acrylate monomer 160kg, ethyl propenoate 160kg, TEB 3K 11kg, polyoxyethylene alkanisation ether 0.1kg successively; It is subsequent use that N,N methylene bis acrylamide 8kg, sodium lauryl sulphate 5kg, sim alkylphenol T 46155 (10) ether 1.76kg and water 189kg stir emulsification; In retort, add sodium lauryl sulphate 1.76kg, sim alkylphenol T 46155 (10) ether 1.32kg and water successively, 53kg stir dissolve subsequent use; Ammonium persulphate 0.85kg and the high-order jar that drips of water 55kg adding is subsequent use.-·
Retort is heated to 40 ℃; Put into wherein 55 ㎏ to emulsion in the emulsion tank, stir the initiator that continues to be heated to adding 1/10 about 60 ℃ down, open water of condensation; Begin reaction when continuing to be heated to 75 ~ 80 ℃, the automatic exothermic temperature of system rises to rapidly about 90 ℃;
When temperature falls after rise, beginning to drip emulsification material and the initiator 2h to 2/3 of header tank, temperature is controlled at 85 ~ 90 ℃, adds 11kg vinylformic acid and adds 40kg water simultaneously, and the header tank continued that stirs drips 1h; Chainpropagation and partial cross-linked polymerization 2h; Be cooled to 60 ℃ and filter discharging, the theoretical solid content 51% of emulsion.
Regulate the emulsion surface tension through adding special emulsifying agent and wetting agent during the present invention is synthetic, make it with close by the surface energy of sticking material, thereby reach the purpose of fine infiltration, it is inhomogeneous gluing to occur when solving high-speed coating, the problem that leveling characteristics is bad; Adopt the special process of secondary nucleation to make height simultaneously and contain emulsion admittedly, the slow and high speed coating machine of the evaporation rate of water is difficult to matching problem when solving high-speed coating.
Claims (3)
1. high speed coating machine is characterized in that with the preparation method of emulsion acrylate class pressure sensitive adhesive: may further comprise the steps:
(1) preparation of pre-emulsion: reaction monomers, emulsifying agent, wetting agent, linking agent and deionized water are added in the high-order emulsion tank, and emulsification also is preheated to 40 ~ 50 ℃, and the preparation pre-emulsion is subsequent use, and said reaction monomers comprises soft monomer and hard monomer;
(2) seed emulsion preparation and a nucleation: the part of the pre-emulsion for preparing and the part of initiator are put into retort; Be warming up to 55 ~ 75 ℃; Open water of condensation; Continue to be warming up to 75 ~ 85 ℃, after temperature is steady, begin to drip a part of remaining pre-emulsion and initiator, once become nuclear reaction 1 ~ 4h under stirring;
(3) secondary nucleation: after the nucleation; Again with adding function monomer and small quantity of deionized water in the remaining pre-emulsion of a part; The continued that stirs drips a part of remaining pre-emulsion 0 ~ 3h, continues to drip a part of remaining initiator, 80 ~ 90 ℃ of holding temperatures simultaneously;
(4) polymer chain increases and partial cross-linked polymerization: after the remaining pre-emulsion of emulsion tank and initiator were all dripped, 80 ~ 90 ℃ of controlled temperature carried out chainpropagation and partial cross-linked polymerization 1 ~ 4h.
2. according to the preparation method of the said high speed coating machine of claim 1 with emulsion acrylate class pressure sensitive adhesive, it is characterized in that: the parts by weight of each component of said pressure sensitive adhesive are following: 30 ~ 60 parts of soft monomers, 1 ~ 10 part of hard monomer; 1 ~ 10 part of function monomer; Linking agent 0.1 ~ 5,0. 5 ~ 5 parts of emulsifying agents, wetting agent 0.1 ~ 1 minute; 0. 05 ~ 1 part of initiator, 35 ~ 70 parts of deionized waters.
According to claim 1 or 2 said high speed coating machines with the preparation method of emulsion acrylate class pressure sensitive adhesive, it is characterized in that:
In the step of the preparation of pre-emulsion, comprise soft monomer and hard monomer in the wherein said reaction monomers, said soft monomer is one or more in ethyl propenoate, Bing Xisuandingzhi, Isooctyl acrylate monomer or vinylformic acid-2 one ethylhexyls; Said hard monomer is TEB 3K or vinylbenzene; Said emulsifying agent is two or more in X 2073, sodium lauryl sulphate, octyl (or nonyl) phenol polyethenoxy (10) ether, the AEO; Said wetting agent is sodium butylnaphthalenesulfonate or polyoxyethylene alkanisation ether; Said linking agent is N,N methylene bis acrylamide or N hydroxymethyl acrylamide; Said initiator is a persulphate;
In the step of a seed emulsion preparation and a nucleation, said initiator is a persulphate;
In the step of said secondary nucleation, said function monomer is acrylic or methacrylic acid.
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| CN102863929A (en) * | 2012-09-17 | 2013-01-09 | 马千里 | Anti-yellowing emulsion polyacrylic ester pressure-sensitive adhesive and preparation method thereof |
| 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 |
| CN105255403A (en) * | 2015-11-01 | 2016-01-20 | 上海晶华胶粘新材料股份有限公司 | Water-based adhesive, preparation method, adhesive tape and preparation method thereof |
| CN105505262A (en) * | 2015-12-31 | 2016-04-20 | 宁波大榭开发区综研化学有限公司 | Adhesive, FPC (flexible printed circuit) protective film using adhesive and preparation method thereof |
| CN105504143A (en) * | 2014-09-26 | 2016-04-20 | 中国石油化工股份有限公司 | Non-polyether demulsifier and preparation method thereof |
| CN106290150A (en) * | 2016-08-18 | 2017-01-04 | 广州市金万正印刷材料有限公司 | Pressure-sensitive adhesive goods cull rank test method |
| 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 |
| CN115895526A (en) * | 2022-11-18 | 2023-04-04 | 康达新材料(集团)股份有限公司 | Low-boiling-point amine-free hot-pressing fast-curing type double-component acrylate structural adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102863929A (en) * | 2012-09-17 | 2013-01-09 | 马千里 | Anti-yellowing emulsion polyacrylic ester pressure-sensitive adhesive and preparation method thereof |
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| 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 |
| CN115895526A (en) * | 2022-11-18 | 2023-04-04 | 康达新材料(集团)股份有限公司 | Low-boiling-point amine-free hot-pressing fast-curing type double-component acrylate structural adhesive and preparation method thereof |
| CN115895526B (en) * | 2022-11-18 | 2024-04-02 | 康达新材料(集团)股份有限公司 | Quick-curing type double-component acrylate structural adhesive free of low-boiling-point amine and capable of being subjected to hot pressing and preparation method thereof |
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