CN104927744B - A kind of water resistance corrugated board adhesive and preparation method thereof - Google Patents
A kind of water resistance corrugated board adhesive and preparation method thereof Download PDFInfo
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- CN104927744B CN104927744B CN201510351715.6A CN201510351715A CN104927744B CN 104927744 B CN104927744 B CN 104927744B CN 201510351715 A CN201510351715 A CN 201510351715A CN 104927744 B CN104927744 B CN 104927744B
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- corrugated board
- water
- temperature
- water resistance
- diisocyanate
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Abstract
A kind of water resistance corrugated board adhesive and preparation method thereof.The present invention provides a kind of single-component water-based polyurethane adhesive and preparation method thereof, and the mass ratio of its constitutive material is：PEPA：Emulsifying agent：Diisocyanate：Tin catalyst：Dihydric alcohol：Acetone：Sulfonate：Deionized water：2,2-two beautiful jade Anaesthetie Ether=100：7.5~8.5：65~72：0.3~0.5：21~23：100~160：2.0~3.5：200~260：0.25~0.5.The present invention uses self-emulsification, it is the single-component water-based polyurethane adhesive that main Material synthesis is glued dedicated for water-resistant type corrugated board using PEPA, emulsifying agent, diisocyanate, dibutyl tin laurate, dihydric alcohol, volatile substance generation is not had when in use, to strong by viscous adaptability for materials, it is curable at ambient temperature and need not uses other crosslinking agents, easy construction, the gluing and secondary operation for corrugated board that can be wide.
Description
Technical field
The invention belongs to technical field of adhesive preparation, and in particular to a kind of water resistance corrugated board adhesive and its system
Preparation Method.
Background technology
With the development of packaging industry, the consumption figure of adhesive remains higher level, global packaging industry glue consumption
The 35% of the total consumption of adhesive is accounted for, packaging industry turns into the maximum industry of adhesive applications, and it is gluing that current packaging industry is used
Agent, is largely dual-component polyurethane adhesive, needs to carry out live allotment when using, can be made troubles to production process,
Influence production efficiency；A large amount of volatile matters are had and one-component polyurethane adhesive is all then solvent-based adhesive, in production process
Produce, production and application is not environmentally friendly enough；And it is used for the water-based polyurethane adhesive of packaging field, with packaging facilities automaticity
With the continuous lifting of running speed, the curing rate of adhesive in itself can not meet the technological requirement of existing production line；When
The preceding water-based polyurethane adhesive for packaging material is not good due to the wetability to glued substrate surface, causes cohesive force not
Height, equally also limit its application in terms of water resistance bond for corrugated board.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of curing rate is fast, nothing
Strong single-component water-based polyurethane adhesive of volatile matter, caking property and preparation method thereof.
The technical scheme that the present invention takes：A kind of water resistance corrugated board adhesive, the mass ratio of its constitutive material is：
PEPA：Emulsifying agent：Diisocyanate：Tin catalyst：Dihydric alcohol：Acetone：Sulfonate：Deionized water：2,2-two
Beautiful jade Anaesthetie Ether=100：7.5~8.5：65~72：0.3~0.5：21~23：100~160：2.0~3.5：200~260：
0.25~0.5.
The molecular weight of the PEPA is controlled 1000-3500.
The emulsifying agent includes dihydromethyl propionic acid, dimethylolpropionic acid, dodecyl sodium sulfate, dioctyl succinic acid sulphur
At least one of sour sodium.
The diisocyanate includes toluene di-isocyanate(TDI)（TDI）, IPDI（IPDI）, 4,4- bis-
Methylenebis phenyl isocyanate（MDI）, hexamethylene diisocyanate（HDI）At least one of.
The tin catalyst is dibutyl tin laurate.
The dihydric alcohol is included in ethylene glycol, propane diols, diglycol, BDO, terephthalic acid (TPA) extremely
Few one kind.
The sulfonate includes dialkyl benzene sulfonic acids sodium, sodium alklyarylsulfonate, neopelex, dibutyl naphthalene sulphur
At least one of sour sodium, nekal.
A kind of preparation method of water resistance corrugated board adhesive, comprises the following steps：
（1）Reactor is heated to 50-80 DEG C, is evacuated to negative pressure 0.05-0.18Pa, PEPA is dissolved into water
Concentration 45%-60% solution, and be pumped into reactor；
（2）Charging aperture is opened, makes, into normal pressure in kettle, to add emulsifying agent, reaction time 10-20min；
（3）Temperature of reaction kettle is raised to 80-95 DEG C, diisocyanate and tin catalyst, diisocyanate are added dropwise successively
Time for adding control is in 5-15 minutes, and the control of tin catalyst time for adding is in 15-25 minutes, and motor speed control exists
50-120 revs/min, react 3-5.5 hours；
（4）Temperature of reaction kettle is reduced to 60 DEG C, dihydric alcohol is added, reacted 1-2 hours；
（5）Acetone is added, reaction adds sulfonate after 30 minutes, control temperature of reaction kettle is in 50-60 DEG C, insulation reaction
30-40min；
（6）Progressively add deionized water into reactor（Amount of water per minute is no more than 12g）, control reactor temperature to exist
40-55 DEG C, adjustment of rotational speed reacts 1-2 hours to 300-400 revs/min；
（7）Temperature of reaction kettle is raised to 65-85 DEG C, acetone is evacuated to and all exhausts；
（8）Temperature of reaction kettle is reduced to normal temperature, is required to add 2,2-two beautiful jade Anaesthetie Ethers, stirring according to solidification rate
Filtering blowing, obtains final water-based polyurethane adhesive after uniform.
The present invention uses self-emulsification, using PEPA, emulsifying agent, diisocyanate, dibutyl tin laurate,
Dihydric alcohol is the single-component water-based polyurethane adhesive that main Material synthesis is glued dedicated for water-resistant type corrugated board, wherein two
The addition of first alcohol not only acts as the effect of chain extender and can improve the water resistance of adhesive；Also by controlling to emulsify in reaction
The amount of agent improves initial bonding strength and initial adhesion strength, and adds catalyst 2, and 2-two beautiful jade Anaesthetie Ethers (DM-DEE) can
To significantly improve the curing rate and stability of adhesive；Acetone is added in late phase reaction as cosolvent, that is, facilitates heat transfer same
When advantageously reduce reactant viscosity, and step（7）It is middle to pump acetone so that adhesive does not have volatile matter when in use
Matter is produced, to strong by viscous adaptability for materials, i.e. curable at ambient temperature and need not use other crosslinking agents, construction party
Just, the gluing and secondary operation for corrugated board that can be wide.
Embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1：
（1）Reactor is heated to 50 DEG C, is evacuated to negative pressure 0.05Pa, by PEPA（Molecular weight is 1000）Use water
The solution of concentration 45% is dissolved into, and is pumped into reactor, because PEPA has certain toxicity, and generally sealed storage,
So being fed using sealed negative-pressure, it is ensured that the security of operating personnel；
（2）Charging aperture is opened, is made into normal pressure in kettle, dihydromethyl propionic acid is added and is emulsified, react 10min；
（3）Temperature of reaction kettle is raised to 80 DEG C, toluene di-isocyanate(TDI) is added dropwise successively（TDI）And di lauric dibutyl
Tin, toluene di-isocyanate(TDI)（TDI）Time for adding is 5 minutes, and dibutyl tin laurate time for adding is 15 minutes, and motor turns
Speed control is reacted 3 hours at 50 revs/min, prepares the base polyurethane prepolymer for use as of the terminal isocyanate groups containing hydrophilic group；
（4）Temperature of reaction kettle is reduced to 60 DEG C, ethylene glycol is added, reacted 1 hour, addition ethylene glycol is chain extender, increase
Molecular weight；
（5）Acetone is added, acetone is in the reaction cosolvent, facilitates reactant internal heat transfer, the addition in later stage is conducive to
Reduce the viscosity of adhesive；Reaction adds dialkyl benzene sulfonic acids sodium after 30 minutes and carries out neutralization ionization, that is, causes adhesive tool
There is water solubility, control temperature of reaction kettle is in 50 DEG C, insulation reaction 30min.
（6）Progressively add deionized water into reactor（Amount of water per minute is no more than 12g）, control in reactor 40
DEG C, adjustment of rotational speed reacts 1 hour, for the addition of deionized water is compared with light water, obtained adhesive is steady to 300 revs/min
It is qualitative higher；
（7）Temperature of reaction kettle is raised to 65 DEG C, acetone is evacuated to and all exhausts so that adhesive does not have when in use
Volatile substance is produced；
（8）Temperature of reaction kettle is reduced to normal temperature, catalyst 2 is added, 2-two beautiful jade Anaesthetie Ethers can significantly improve gluing
The curing rate and stability of agent, blowing is filtered after stirring, and obtains final water-based polyurethane adhesive.
The mass ratio of all raw materials is：PEPA：Dihydromethyl propionic acid：Toluene di-isocyanate(TDI)（TDI）：Two bays
Sour dibutyl tin：Ethylene glycol：Acetone：Dialkyl benzene sulfonic acids sodium：Deionized water：2,2-two beautiful jade Anaesthetie Ether=100：7.5：
65：0.3：21：100：2.0：200：0.25.
The water-based polyurethane adhesive finally given, viscosity（Apply -4 glasss/30 DEG C）19 seconds, with solvent borne polyurethane adhesive
Compared to bonding force increase by 12%, solid content reaches 52%, 18 minutes hardening times.
Embodiment 2：
（1）Reactor is heated to 80 DEG C, is evacuated to negative pressure 0.18Pa, by PEPA（Molecular weight is 3500）Use water
The solution of concentration 60% is dissolved into, and is pumped into reactor, there is certain toxicity, and generally sealed storage, institute in PEPA
With using sealed negative-pressure charging, it is ensured that the security of operating personnel；
（2）Charging aperture is opened, is made into normal pressure in kettle, dimethylolpropionic acid is added and is emulsified, react 20min；
（3）Temperature of reaction kettle is raised to 80 DEG C, 4,4- methyl diphenylene diisocyanates are added dropwise successively（MDI）With two bays
Sour dibutyl tin, 4,4- methyl diphenylene diisocyanates（MDI）Time for adding is 15 minutes, and dibutyl tin laurate is added dropwise
Time is 25 minutes, motor speed is controlled at 120 revs/min, is reacted 5.5 hours, prepares the isocyanates end containing hydrophilic group
The base polyurethane prepolymer for use as of base；
（4）Temperature of reaction kettle is reduced to 60 DEG C, propane diols is added, reacted 2 hours, addition propane diols is chain extender, increase
Molecular weight；
（5）Acetone is added, acetone is in the reaction cosolvent, facilitates reactant internal heat transfer, the addition in later stage is conducive to
Reduce the viscosity of adhesive；Reaction adds neopelex after 30 minutes and carries out neutralization ionization, that is, causes adhesive
With water solubility, control temperature of reaction kettle is in 60 DEG C, insulation reaction 40min.
（6）Progressively add deionized water into reactor（Amount of water per minute is no more than 12g）, control in reactor 55
DEG C, adjustment of rotational speed reacts 2 hours, for the addition of deionized water is compared with light water, obtained adhesive is steady to 400 revs/min
It is qualitative higher；
（7）Temperature of reaction kettle is raised to 85 DEG C, acetone is evacuated to and all exhausts so that adhesive does not have when in use
Volatile substance is produced；
（8）Temperature of reaction kettle is reduced to normal temperature, catalyst 2,2-two beautiful jade Anaesthetie Ethers can significantly improve adhesive
Curing rate and stability, blowing is filtered after stirring, and obtains final water-based polyurethane adhesive.
The mass ratio of all raw materials is：PEPA：Dimethylolpropionic acid：4,4- methyl diphenylene diisocyanates
（MDI）：Dibutyl tin laurate：Terephthalic acid (TPA)：Acetone：Neopelex：Deionized water：2,2-two beautiful jades
Anaesthetie Ether=100：8.5：72：0.5：23：160：3.5：260：0.5.
The water-based polyurethane adhesive finally given, viscosity（Apply -4 glasss/30 DEG C）38 seconds, with solvent borne polyurethane adhesive
Compared to bonding force increase by 26%, solid content reaches 58%, 9 minutes hardening times.
Embodiment 3：
（1）Reactor is heated to 70 DEG C, is evacuated to negative pressure 0.09Pa, by PEPA（Molecular weight is 3000）Use water
The solution of concentration 55% is dissolved into, and is pumped into reactor, because PEPA has certain toxicity, and generally sealed storage,
So being fed using sealed negative-pressure, it is ensured that the security of operating personnel；
（2）Charging aperture is opened, is made into normal pressure in kettle, dioctyl succinic acid sodium sulfonate is added and is emulsified, react 15min；
（3）Temperature of reaction kettle is raised to 87 DEG C, IPDI is added dropwise successively（IPDI）With tin dilaurate two
Butyl tin, IPDI（IPDI）Time for adding is 10 minutes, and dibutyl tin laurate time for adding is 20
Minute, motor speed is controlled at 80 revs/min, is reacted 4.5 hours, prepares the polyurethane of the terminal isocyanate groups containing hydrophilic group
Performed polymer；
（4）Temperature of reaction kettle is reduced to 60 DEG C, BDO is added, reacted 1.5 hours, adds BDO to expand
Chain agent, increases molecular weight；
（5）Acetone is added, acetone is in the reaction cosolvent, facilitates reactant internal heat transfer, the addition in later stage is conducive to
Reduce the viscosity of adhesive；Reaction adds nekal after 30 minutes and carries out neutralization ionization, that is, causes adhesive tool
There is water solubility, control temperature of reaction kettle is in 55 DEG C, insulation reaction 35min.
（6）Progressively add deionized water into reactor（Amount of water per minute is no more than 12g）, control in reactor 45
DEG C, adjustment of rotational speed reacts 1.5 hours to 350 revs/min, for the addition of deionized water is compared with light water, obtained adhesive
Stability is higher；
（7）Temperature of reaction kettle is raised to 75 DEG C, acetone is evacuated to and all exhausts so that adhesive does not have when in use
Volatile substance is produced；
（8）Temperature of reaction kettle is reduced to normal temperature, catalyst 2 is added, 2-two beautiful jade Anaesthetie Ethers can significantly improve gluing
The curing rate and stability of agent, blowing is filtered after stirring, and obtains final water-based polyurethane adhesive.
The mass ratio of all raw materials is：PEPA：Dioctyl succinic acid sodium sulfonate：IPDI
（IPDI）：Dibutyl tin laurate：BDO：Acetone：Nekal：Deionized water：2,2-two beautiful jades two
Ethylether=100：8：68：0.4：22：130：2.8：230：0.3.
The water-based polyurethane adhesive finally given, viscosity（Apply -4 glasss/30 DEG C）24 seconds, with solvent borne polyurethane adhesive
Compared to bonding force increase by 20%, solid content reaches 55%, 12 minutes hardening times.
Claims (7)
1. a kind of water resistance corrugated board adhesive, it is characterised in that the mass ratio of its constitutive material is：PEPA：Breast
Agent：Diisocyanate：Tin catalyst：Dihydric alcohol：Acetone：Sulfonate：Deionized water：2,2-two beautiful jade Anaesthetie Ethers=
100：7.5~8.5：65~72：0.3~0.5：21~23：100~160：2.0~3.5：200~260：0.25~0.5；
The preparation method of the adhesive comprises the following steps：
（1）Reactor is heated to 50-80 DEG C, is evacuated to negative pressure 0.05-0.18Pa, and PEPA is dissolved into concentration with water
45%-60% solution, and be pumped into reactor；
（2）Charging aperture is opened, makes, into normal pressure in kettle, to add emulsifying agent, reaction time 10-20min；
（3）Temperature of reaction kettle is raised to 80-95 DEG C, diisocyanate and tin catalyst are added dropwise successively, diisocyanate is added dropwise
Time control is in 5-15 minutes, and the control of tin catalyst time for adding is in 15-25 minutes, and motor speed is controlled in 50-120
Rev/min, react 3-5.5 hours；
（4）Temperature of reaction kettle is reduced to 60 DEG C, dihydric alcohol is added, reacted 1-2 hours；
（5）Acetone is added, reaction adds sulfonate after 30 minutes, control temperature of reaction kettle is in 50-60 DEG C, insulation reaction 30-
40min；
（6）Progressively add deionized water into reactor, amount of water per minute is no more than 12g, and control reactor temperature is in 40-55
DEG C, adjustment of rotational speed reacts 1-2 hours to 300-400 revs/min；
（7）Temperature of reaction kettle is raised to 65-85 DEG C, acetone is evacuated to and all exhausts；
（8）Temperature of reaction kettle is reduced to normal temperature, is required to add 2 according to solidification rate, 2-two beautiful jade Anaesthetie Ethers stir
After filter blowing, obtain final water-based polyurethane adhesive.
2. the water resistance corrugated board adhesive according to claim 1, it is characterised in that the PEPA
Molecular weight is controlled 1000-3500.
3. the water resistance corrugated board adhesive according to claim 1, it is characterised in that the emulsifying agent includes two
At least one of hydroxymethyl propionic acid, dimethylolpropionic acid, dodecyl sodium sulfate, dioctyl succinic acid sodium sulfonate.
4. the water resistance corrugated board adhesive according to claim 1, it is characterised in that the diisocyanate bag
Include toluene di-isocyanate(TDI) TDI, IPDI IPDI, 4,4- methyl diphenylene diisocyanate MDI, six methylenes
At least one of group diisocyanate HDI.
5. the water resistance corrugated board adhesive according to claim 1, it is characterised in that the tin catalyst is
Dibutyl tin laurate.
6. the water resistance corrugated board adhesive according to claim 1, it is characterised in that the dihydric alcohol includes second
At least one of glycol, propane diols, diglycol, BDO.
7. the water resistance corrugated board adhesive according to claim 1, it is characterised in that the sulfonate includes two
In sodium alkyl benzene sulfonate, sodium alklyarylsulfonate, neopelex, sodium butylnaphthalenesulfonate, nekal
It is at least one.
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| CN201510351715.6A CN104927744B (en) | 2015-06-24 | 2015-06-24 | A kind of water resistance corrugated board adhesive and preparation method thereof |
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| CN201510351715.6A CN104927744B (en) | 2015-06-24 | 2015-06-24 | A kind of water resistance corrugated board adhesive and preparation method thereof |
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| CN104927744B true CN104927744B (en) | 2017-10-27 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108300403A (en) * | 2018-01-30 | 2018-07-20 | 陈良地 | The high-strength shockproof combined corrugated board of one kind and its preparation process |
| CN111484826A (en) * | 2020-03-16 | 2020-08-04 | 徐汉昇 | Single-component water polyurethane adhesive |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1329469A1 (en) * | 2002-01-18 | 2003-07-23 | Sika Schweiz AG | Polyurethane composition |
| CN101235264A (en) * | 2007-01-30 | 2008-08-06 | 中国科学院福建物质结构研究所 | Water-based polyurethane adhesive and preparation method thereof |
| CN102618202B (en) * | 2012-04-01 | 2013-12-25 | 江阴市诺科科技有限公司 | Water-based polyurethane composite adhesive for tanning and preparation method and application of composite adhesive |
| CN102827571B (en) * | 2012-09-28 | 2014-12-10 | 广东多正化工科技有限公司 | Preparation method of water-based polyurethane adhesive |
| CN104371631B (en) * | 2014-12-05 | 2016-04-13 | 浙江多邦化工有限公司 | A kind of one-component solvent-free moisture cure urethanes glue paste and preparation method thereof |
| CN104673174B (en) * | 2015-02-13 | 2017-05-10 | 杭州传化精细化工有限公司 | Single-component waterborne polyurethane adhesive and preparation method thereof |
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