CN103965816A - Low-VOC (Volatile Organic Compound) high-performance emulsion adhesive for non-woven fabric material and preparation method thereof - Google Patents
Low-VOC (Volatile Organic Compound) high-performance emulsion adhesive for non-woven fabric material and preparation method thereof Download PDFInfo
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- CN103965816A CN103965816A CN201410220015.9A CN201410220015A CN103965816A CN 103965816 A CN103965816 A CN 103965816A CN 201410220015 A CN201410220015 A CN 201410220015A CN 103965816 A CN103965816 A CN 103965816A
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Abstract
The invention discloses a low-VOC (Volatile Organic Compound) high-performance emulsion adhesive for a non-woven fabric material and a preparation method thereof. The emulsion adhesive is prepared from hard monomers, soft monomers, functional monomers, an initiator, an emulsifier, a pH regulator, modified montmorillonite and deionized water. According to the preparation method, the emulsion adhesive is prepared by a semi-continuous core-shell polymerization method. According to the emulsion adhesive and the preparation method thereof, the reaction monomers and a reaction process are reasonably selected, and particularly, the cationic surfactant, namely modified montmorillonite, is used, so that the emulsion adhesive can play an excellent role in adhering, bonding and anchoring the non-woven fabric material, is low in VOC content, is pollution-free and environmentally friendly, can replace many related imported products currently on the market and has a broad and good application prospect.
Description
[technical field]
The present invention relates to a kind of emulsion adhesive and preparation method thereof, relate in particular to a kind of low VOC and high performance nonwoven cloth material emulsion adhesive and preparation method thereof, belong to adhesive technology field.
[background technology]
Non-woven fabrics (also referred to as " non-woven ") be widely used in industrial filter, construction work, medical material, etc. field, and range of application is in rapid expansion.In recent decades, China's non-woven fabrics technology is developed rapidly, and nonwoven cloth material output in 2010, up to 2,600,000 tons, accounts for global ultimate production 30%, and output occupies first of countries in the world.But China's non-woven fabrics correlation technique is relatively backward at present, especially because the technical development of chemical adhesion method non-woven fabrics is very backward, causes the output of China's high-performance nonwoven cloth material lower and greatly under one's control.Be mainly synthetic resin emulsion tackiness agent for the tackiness agent of non-woven fabrics at present, its kind generally has polyvinyl acetate, polyacrylate(s), polypropylene nitrile synthetic rubber latex etc.Emulsion adhesive is taking water as dispersion medium, less pollution, and to the less pollution of environment, and production cost is lower, and production unit is also fairly simple.At present domestic is mainly the related products that uses external import, and this need to spend a large amount of foreign exchanges, and many domestic manufacturers are also difficult to bear.
The emulsion adhesive of the bonding use of non-woven fabrics is one of technical bottleneck restricting at present China's non-woven fabrics industry development.Although many producers of China can produce corresponding product, from technology content, non-woven fabrics is with emulsion adhesive at home still in the preliminary stage at present, and the application performances such as the bonding of product are poor, can not meet the occasion of high requirement.Meanwhile, along with improving and propelling of domestic and international environmental law Laws & Regulations, safety and the environmental-protecting performance requirement of many fields to non-woven fabrics adhesive is more and more higher, strictly requires the toxicity control of emulsion adhesive in lowest range.But the domestic non-woven fabrics of producing is at present bonding larger with the toxicant such as formaldehyde, phenol in emulsion adhesive, easily the carcinogenic substance such as easy release formaldehyde in processing and use procedure does not meet current environmental protection demand very much.
Therefore, in order to promote China's non-woven fabrics relevant industries to develop rapidly, the competitive power of expansion China's non-woven fabrics industry development and raising non-woven cloth products, gap between reduction China's non-woven fabrics emulsion adhesive and external product, the non-woven fabrics special-purpose adhesive of Application and Development excellent property and environmental protection is badly in need of in China.
[summary of the invention]
The object of the invention is to overcome the defect of above-mentioned prior art and product, a kind of adhering to, bond, fixing and enhancement effect excellence nonwoven cloth material is provided, the low VOC and high performance nonwoven cloth material emulsion adhesive of its corresponding painting film strength, water tolerance, snappiness excellent property, is applicable to the nonwoven cloth materials such as non-woven fabrics fiber.
Another object of the present invention is to provide a kind of preparation method of above-mentioned emulsion tackiness agent.
The present invention to achieve these goals, by the following technical solutions: taking acrylate monomers such as vinylbenzene, methyl methacrylate, butyl acrylates as main polymerization single polymerization monomer, taking the function monomer that contains carboxyl and hydroxyl as modified monomer, prepare nonwoven cloth material emulsion adhesive by semicontinuous hud polymerization method.Concrete technical scheme is as follows:
A kind of low VOC and high performance nonwoven cloth material emulsion adhesive, is characterized in that being made up of following parts by weight of component:
In the present invention, hard monomer is a kind of or its arbitrary combination in vinylbenzene, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, Phthalic acid, diallyl ester, diallyl isophthalate and glycidyl methacrylate.
Soft monomer in the present invention is a kind of or its arbitrary combination in ethyl propenoate, butyl acrylate, ethyl acrylate and lauryl acrylate.
Functional monomer in the present invention is a kind of or its arbitrary combination in 2-Hydroxy ethyl acrylate, 2-hydroxypropyl acrylate, methacrylic acid-2-hydroxy methacrylate, methacrylic acid-2-hydroxy propyl ester, vinylformic acid and methacrylic acid.Functional monomer mainly provides enough hydroxyl or carboxyl to improve adhesion effect and the cohesive action of emulsion adhesive.
Initiator in the present invention is a kind of or its arbitrary combination in ammonium persulphate, Potassium Persulphate, Sodium Persulfate, tertbutyl peroxide and azo di-isopropyl imidazoline salt hydrochlorate.
Emulsifying agent in the present invention is a kind of or its arbitrary combination in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, AES, AEO-9, OP-10, Tween-60, Tween-80, Span-20, Span-60 and Span-80.Emulsifying agent can greatly reduce interfacial tension, make immiscible profit two-phase by the role transformation stirring for can stable existence, be the requisite component of letex polymerization.
PH adjusting agent in the present invention is a kind of or its arbitrary combination in 2-amino-2-methyl-1-propanol (AMP-95), KOH, NaOH, ammoniacal liquor, sodium bicarbonate.PH adjusting agent Main Function is that emulsion is regulated to most weakly alkaline state, and ammoniacal liquor can be adjusted to 1wt%, 5wt%, and the concentration of 10wt% is easy to use.
Modified montmorillonite used in the present invention prepared and obtained by following preparation method:
Cats product is dissolved in deionized water, obtains the solution that solid content is 10～15wt% completely; Then according to the mass ratio of m (montmorillonite): m (cats product)=10:1～10:3, montmorillonite is slowly added in gained solution, stir until after disperseing completely, be warming up to 60～80 DEG C and insulation reaction 10～25min, finally filter and be dried make modified montmorillonite used;
Cats product is wherein one or more in palmityl trimethyl ammonium chloride, cetyl trimethylammonium bromide, cetalkonium chloride.
Generally, emulsion adhesive, to spin sticking power on cloth ground poor, is being subject under the effect of environmental factors or external force, very easily from spinning cloth surface peeling.This point is this field the most scabrous problem at present.Research recently shows, adds cation surface activating can effectively fix emulsion adhesive coating and the sticking power that spins cloth.But emulsion adhesive system is mainly to use anion surfactant, the cats product adding can react with it and lose efficacy at once, makes rapidly emulsion system produce the destructive consequences such as flocculation, sedimentation, breakdown of emulsion.
For overcoming this deficiency, the present invention creatively uses cats product modified montmorillonite used.Montmorillonite is layered silicate, the Na that interlayer contains some amount
+or Li
+deng inorganic cation, when contact cats product, inorganic cation between the easy substituted layer of organic cation.Entered the organic cation between montmorillonite layer, owing to being subject to the obstruct of laminate structure and shielding effect and no longer contacting with the anion surfactant in emulsion system, therefore emulsion system is highly stable.After film forming, organic cation can infiltrate to promote coating and the bonding effect of adhering to of spinning cloth ground gradually.
A preparation method for emulsion adhesive for above-mentioned low VOC and high performance nonwoven cloth material, is characterized in that making by semicontinuous hud polymerization method.
The present invention prepares emulsion adhesive by semicontinuous hud polymerization method and comprises following concrete steps:
(1) first by emulsifying agent and modified montmorillonite used being dissolved in fully completely in deionized water, add again 1/4～1/2 hard monomer, 1/4～1/2 soft monomer, 1/5～1/3 functional monomer, stir and form pre-reaction liquid, then take out 1/3～1/2 pre-reaction liquid in conversion unit, add 1/2 initiator, and be warming up to 80～85 DEG C, insulation 20～60min reacts, meanwhile, the pre-reaction liquid of surplus still keeps whipped state;
(2) then the reaction system in conversion unit is cooled to 35～45 DEG C, adds pre-reaction liquid and the surplus initiator of surplus, then be warming up to 80～85 DEG C, insulation 1～4h;
(3) add again surplus hard monomer, surplus soft monomer and surplus functional monomer, at 80～85 DEG C, be incubated 1～3h, be finally down to room temperature and add pH adjusting agent to regulate pH to be 9～10, to leave standstill discharging after 5～20min.
The present invention, with respect to prior art, has following advantage:
(1) the present invention is by the choose reasonable to reaction monomers and reaction process, especially used cats product modified montmorillonite used, emulsion adhesive not only can be obtained on nonwoven cloth material good adhere to, bonding, grappling effect, and low VOC is pollution-free, environmental protection, can replace many relevant imported products in the market, have wide good application prospect.
(2) the present invention adopts semicontinuous hud polymerization method, and preparation technology is simple, is easy to control polymerization system, with low cost.Emulsion polymerisation process of the present invention is taking water as dispersion medium, cheap safety, and the trouble of having avoided using expensive organic solvent and having reclaimed solvent, has reduced the possibility that causes fire and contaminate environment.
[embodiment]
Below in conjunction with embodiment, the present invention will be further described, it should be noted that, embodiment does not form the restriction to the claimed scope of the present invention.
Embodiment 1:
Modified montmorillonite used preparation:
Cats product is dissolved in deionized water, obtains the solution that solid content is 12wt% completely; Then according to the mass ratio of m (montmorillonite): m (cats product)=10:2, montmorillonite is slowly added in gained solution, stir until after disperseing completely, be warming up to 75 DEG C and insulation reaction 20min, finally filter and be dried make modified montmorillonite used.
A kind of low VOC and high performance nonwoven cloth material is as follows by the weight fraction component of emulsion adhesive:
The preparation technology of embodiment 1:
(1) first by emulsifying agent AES and modified montmorillonite used being dissolved in fully completely in deionized water, add again 1/3 hard monomer vinylbenzene and diallyl isophthalate, 1/3 soft monomer butyl acrylate, 1/4 functional monomer methacrylic acid-2-hydroxy methacrylate and vinylformic acid, stir and form pre-reaction liquid, then take out 1/3～1/2 pre-reaction liquid in conversion unit, add 1/2 initiator potassium persulfate, and be warming up to 80～85 DEG C, insulation 30min reacts, meanwhile, keep the pre-reaction liquid of surplus still in whipped state;
(2) then the reaction system in conversion unit is cooled to 40 DEG C, adds the pre-reaction liquid of surplus and the initiator potassium persulfate of surplus, then be warming up to 80～85 DEG C, insulation 3h;
(3) add surplus hard monomer, surplus soft monomer and surplus functional monomer again, at 80～85 DEG C, be incubated 2h, being finally down to room temperature 1wt% weak ammonia adjusting pH value is 9～10, discharging after standing 5～20min.
Embodiment 2:
Modified montmorillonite used preparation:
Cats product is dissolved in deionized water, obtains the solution that solid content is 13wt% completely; Then according to the mass ratio of m (montmorillonite): m (cats product)=10:2, montmorillonite is slowly added in gained solution, stir until after disperseing completely, be warming up to 70 DEG C and insulation reaction 15min, finally filter and be dried make modified montmorillonite used.
A kind of low VOC and high performance nonwoven cloth material is as follows by the components by weight percent of emulsion adhesive:
The preparation technology of embodiment 2:
(1) first by emulsifier op-10 and modified montmorillonite used being dissolved in fully completely in deionized water, add again 1/3 hard monomer vinylbenzene and methyl methacrylate, 1/3 soft monomer butyl acrylate, 1/4 functional monomer methacrylic acid-2-hydroxy methacrylate, stir and form pre-reaction liquid, then take out 1/3～1/2 pre-reaction liquid in conversion unit, add 1/2 initiator ammonium persulfate, and be warming up to 80～85 DEG C, insulation 30min, meanwhile, keep surplus pre-reaction liquid still in whipped state;
(2) then reaction system is cooled to 40 DEG C, adds pre-reaction liquid and the surplus initiator ammonium persulfate of surplus, then be warming up to 80～85 DEG C, insulation 3h;
(3) add again surplus hard monomer, surplus soft monomer and surplus functional monomer, at 80～85 DEG C, be incubated 2h, be finally down to room temperature and add AMP-95 to regulate pH value to be 9～10, to leave standstill discharging after 5～20min.
Embodiment 3:
Modified montmorillonite used preparation:
Cats product is dissolved in deionized water, obtains the solution that solid content is 10wt% completely; Then according to the mass ratio of m (montmorillonite): m (cats product)=10:1, montmorillonite is slowly added in gained solution, stir until after disperseing completely, be warming up to 60 DEG C and insulation reaction 10min, finally filter and be dried make modified montmorillonite used.
A kind of low VOC and high performance nonwoven cloth material is as follows by the components by weight percent of emulsion adhesive:
The preparation technology of embodiment 3:
(1) first by emulsifier op-10 and modified montmorillonite used being dissolved in fully completely in deionized water, add again 1/3 hard monomer vinylbenzene, 1/3 soft monomer butyl acrylate, 1/4 functional monomer methacrylic acid-2-hydroxy methacrylate, stir and form pre-reaction liquid, then take out 1/3～1/2 pre-reaction liquid in conversion unit, add 1/2 initiator ammonium persulfate, and be warming up to 80～85 DEG C, insulation 30min, meanwhile, keep remaining pre-reaction liquid still in whipped state;
(2) then reaction system is cooled to 40 DEG C, adds remaining pre-reaction liquid and 1/2 initiator ammonium persulfate, then be warming up to 80～85 DEG C, insulation 3h;
(3) add again surplus hard monomer, surplus soft monomer and surplus functional monomer, at 80～85 DEG C, be incubated 2h, be finally down to room temperature and add AMP-95 to regulate pH value to be 9～10, to leave standstill discharging after 5～20min.
Embodiment 4:
Modified montmorillonite used preparation:
Cats product is dissolved in deionized water, obtains the solution that solid content is 15wt% completely; Then according to the mass ratio of m (montmorillonite): m (cats product)=10:3, montmorillonite is slowly added in gained solution, stir until after disperseing completely, be warming up to 80 DEG C and insulation reaction 25min, finally filter and be dried make modified montmorillonite used.
A kind of low VOC and high performance nonwoven cloth material is as follows by the components by weight percent of emulsion adhesive:
The preparation technology of embodiment 4:
(1) first by emulsifying agent AES and modified montmorillonite used being dissolved in fully completely in deionized water, add again 1/3 hard monomer vinylbenzene, 1/3 soft monomer butyl acrylate, 1/4 functional monomer methacrylic acid, stir and form pre-reaction liquid, then 1/3～1/2 pre-reaction liquid is placed in to conversion unit, add 1/2 initiator ammonium persulfate, and be warming up to 80～85 DEG C, insulation 40min, meanwhile, keep remaining pre-reaction liquid still in whipped state;
(2) then reaction system is cooled to 40 DEG C, adds remaining pre-reaction liquid and 1/2 initiator ammonium persulfate, then be warming up to 80～85 DEG C, insulation 3h;
(3) add surplus hard monomer, surplus soft monomer and surplus functional monomer again, be incubated 2h at 80～85 DEG C, being finally down to room temperature, to add AMP-95 to regulate pH value be 9～10, leaves standstill discharging after 5～20min.
Embodiment 5:
Modified montmorillonite used preparation:
Cats product is dissolved in deionized water, obtains the solution that solid content is 15wt% completely; Then according to the mass ratio of m (montmorillonite): m (cats product)=10:3, montmorillonite is slowly added in gained solution, stir until after disperseing completely, be warming up to 80 DEG C and insulation reaction 25min, finally filter and be dried make modified montmorillonite used.
A kind of low VOC and high performance nonwoven cloth material is as follows by the components by weight percent of emulsion adhesive:
The preparation technology of embodiment 5:
(1) first by emulsifying agent and modified montmorillonite used being dissolved in fully completely in deionized water, add again 1/2 hard monomer, 1/2 soft monomer, 1/3 functional monomer, stir and form pre-reaction liquid, then 1/3～1/2 pre-reaction liquid is placed in to conversion unit, add 1/2 initiator, and be warming up to 80～85 DEG C, insulation 60min, meanwhile, keep remaining pre-reaction liquid still in whipped state;
(2) then reaction system is cooled to 45 DEG C, adds remaining pre-reaction liquid and 1/2 initiator, then be warming up to 80～85 DEG C, insulation 4h;
(3) add again surplus hard monomer, surplus soft monomer and surplus functional monomer, at 80～85 DEG C, be incubated 3h, be finally down to room temperature and add pH adjusting agent to regulate pH value to be 9～10, to leave standstill discharging after 5～20min.
Embodiment 6:
Modified montmorillonite used preparation:
Cats product is dissolved in deionized water, obtains the solution that solid content is 10wt% completely; Then according to the mass ratio of m (montmorillonite): m (cats product)=10:1, montmorillonite is slowly added in gained solution, stir until after disperseing completely, be warming up to 60 DEG C and insulation reaction 10min, finally filter and be dried make modified montmorillonite used.
A kind of low VOC and high performance nonwoven cloth material is as follows by the components by weight percent of emulsion adhesive:
The preparation technology of embodiment 6:
(1) first by emulsifying agent and modified montmorillonite used being dissolved in fully completely in deionized water, add again 1/4 hard monomer, 1/4 soft monomer, 1/5 functional monomer, stir and form pre-reaction liquid, then 1/3～1/2 pre-reaction liquid is placed in to conversion unit, add 1/2 initiator, and be warming up to 80～85 DEG C, insulation 20min, meanwhile, keep remaining pre-reaction liquid still in whipped state;
(2) then reaction system is cooled to 35 DEG C, adds remaining pre-reaction liquid and 1/2 initiator, then be warming up to 80～85 DEG C, insulation 1h;
(3) add again surplus hard monomer, surplus soft monomer and surplus functional monomer, at 80～85 DEG C, be incubated 1h, be finally down to room temperature and add pH adjusting agent to regulate pH value to be 9～10, to leave standstill discharging after 5～20min.
Embodiment 1～6 is applied on non-woven fabrics fiber and carries out various tests, and result is as shown in table 1.
Table 1: emulsion adhesive finished product test result for non-woven fabrics
As shown in Table 1, non-woven fabrics of the present invention with emulsion adhesive quantitatively, the performance index such as thickness, air penetrability, flexural strength, pop strength are better, it is applied on nonwoven cloth material can obtain good bonding, fixing and enhancement, simultaneously the carcinogenic substance such as formaldehydeless, phenol discharges, not only substantially meet relevant service requirements and the standards such as non-woven fabrics enhancement process completely, and environmental protection, can not pollute environment.
The above-mentioned object with reference to embodiment is to describe the present invention, and is illustrative instead of determinate.For a person skilled in the art, do not deviating under the prerequisite of scope of the present invention and general plotting, it is apparent making different modifications and variations according to method of the present invention, within should belonging to protection scope of the present invention.
Claims (10)
1. a low VOC and high performance nonwoven cloth material emulsion adhesive, is characterized in that being made up of following parts by weight of component:
2. a kind of low VOC and high performance nonwoven cloth material emulsion adhesive according to claim 1, is characterized in that described hard monomer is a kind of or its arbitrary combination in vinylbenzene, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, Phthalic acid, diallyl ester, diallyl isophthalate and glycidyl methacrylate.
3. a kind of low VOC and high performance nonwoven cloth material emulsion adhesive according to claim 1, is characterized in that described soft monomer is a kind of or its arbitrary combination in ethyl propenoate, butyl acrylate, ethyl acrylate and lauryl acrylate.
4. a kind of low VOC and high performance nonwoven cloth material emulsion adhesive according to claim 1, is characterized in that described functional monomer is a kind of or its arbitrary combination in 2-Hydroxy ethyl acrylate, 2-hydroxypropyl acrylate, methacrylic acid-2-hydroxy methacrylate, methacrylic acid-2-hydroxy propyl ester, vinylformic acid and methacrylic acid.
5. a kind of low VOC and high performance nonwoven cloth material emulsion adhesive according to claim 1, is characterized in that described initiator is a kind of or its arbitrary combination in ammonium persulphate, Potassium Persulphate, Sodium Persulfate, tertbutyl peroxide and azo di-isopropyl imidazoline salt hydrochlorate.
6. a kind of low VOC and high performance nonwoven cloth material emulsion adhesive according to claim 1, is characterized in that described emulsifying agent is a kind of or its arbitrary combination in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, AES, AEO-9, OP-10, Tween-60, Tween-80, Span-20, Span-60 and Span-80.
7. a kind of low VOC and high performance nonwoven cloth material emulsion adhesive according to claim 1, is characterized in that described pH adjusting agent is a kind of or its arbitrary combination in 2-amino-2-methyl-1-propanol, KOH, NaOH, ammoniacal liquor, sodium bicarbonate.
8. a kind of low VOC and high performance nonwoven cloth material emulsion adhesive according to claim 1, is characterized in that described modified montmorillonite usedly prepare by following preparation method:
Cats product is dissolved in deionized water, obtains the solution that solid content is 10～15wt% completely; Then according to the mass ratio of m (montmorillonite): m (cats product)=10:1～10:3, montmorillonite is slowly added in gained solution, stir until after disperseing completely, be warming up to 60～80 DEG C and insulation reaction 10～25min, finally filter and be dried make modified montmorillonite used.
9. a preparation method for the use of the low VOC and high performance nonwoven cloth material described in any one emulsion adhesive in claim 1-8, is characterized in that making by semicontinuous hud polymerization method.
10. the preparation method of emulsion adhesive for a kind of low VOC and high performance nonwoven cloth material according to claim 9, is characterized in that comprising following concrete steps:
(1) first by emulsifying agent and modified montmorillonite used being dissolved in fully completely in deionized water, add again 1/4～1/2 hard monomer, 1/4～1/2 soft monomer, 1/5～1/3 functional monomer, stir and form pre-reaction liquid, then take out 1/3～1/2 pre-reaction liquid in conversion unit, add 1/2 initiator, and be warming up to 80～85 DEG C, insulation 20～60min reacts, meanwhile, the pre-reaction liquid of surplus still keeps whipped state;
(2) then the reaction system in conversion unit is cooled to 35～45 DEG C, adds pre-reaction liquid and the surplus initiator of surplus, then be warming up to 80～85 DEG C, insulation 1～4h;
(3) add again surplus hard monomer, surplus soft monomer and surplus functional monomer, at 80～85 DEG C, be incubated 1～3h, then being down to room temperature, to add pH adjusting agent to regulate pH value be 9～10, then after standing 5～20min, discharging makes nonwoven cloth material emulsion adhesive.
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| CN109103394A (en) * | 2018-07-30 | 2018-12-28 | 广东美联隔膜有限公司 | A kind of lithium battery diaphragm and the preparation method and application thereof for removing ultra micro modified filler containing height |
| CN109628028A (en) * | 2018-12-19 | 2019-04-16 | 常熟巴德富科技有限公司 | A kind of ceramic tile gum lotion and preparation method thereof |
| CN109628028B (en) * | 2018-12-19 | 2020-10-27 | 常熟巴德富科技有限公司 | Ceramic tile back glue emulsion and preparation method thereof |
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