CN104496853B - A kind of UV solidifies peelable gum resin and preparation method thereof - Google Patents
A kind of UV solidifies peelable gum resin and preparation method thereof Download PDFInfo
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- CN104496853B CN104496853B CN201510011918.0A CN201510011918A CN104496853B CN 104496853 B CN104496853 B CN 104496853B CN 201510011918 A CN201510011918 A CN 201510011918A CN 104496853 B CN104496853 B CN 104496853B
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Abstract
The invention discloses a kind of UV solidifies peelable gum resin and preparation method thereof, the component comprising following weight proportion：2-(Acryloyloxy)ethanol 23.0～27.5%, methyl hexahydrophthalic anhydride 30.0～35.0%, epoxychloropropane 25.0～29.5%, hexamethylene diisocyanate 13.0～15.0%, catalyst 0.1～0.2%, polymerization inhibitor 0.1～0.2%.The present invention provides a kind of peelable gum resin of UV solidifications and sees, mixed using raw material that is the more commonly used, being easy to get, by the temperature for controlling reaction, the open loop between compound and chain extending reaction are realized, generate the larger straight chain compound of molecular weight, one end is the acrylic acid structure group that can carry out photocuring, cost is relatively low, and synthesis temperature is low, saves energy consumption, non-volatility organic compound (VOC) pollutes, and curing rate is fast.
Description
【Technical field】
The invention belongs to cold coating technical field, and in particular to a kind of UV solidifies peelable gum resin and preparation method thereof.
【Background technology】
In recent years, as global environmental pollution crisis is increasingly serious, people are trying to find new coating replacement biography
System coating, and UV photocureable coating is one of optimum selection.UV is exactly the English abbreviation of ultraviolet (Ultra-Violet Ray).
Industrial UV wavelength is with 200nm to 450nm as its range of application." UV irradiates hardenable material " is irradiated with UV and it is made
The processing procedure of hardening, we term it " UV Curing Process ".UV coating can be applied by dip-coating, showering, paint, spin coating, or even
After the method coating such as vacuum painting, then Jing UV photons irradiate and film-forming.This technology originates from the international painting of the seventies
Material market, is a kind of brand-new green technology.In 20 end of the centurys, UV is coating material solidified to come into vogue in west, Japan and other places, is a kind of
Represent the coating variety of fashion.It is applied to mobile phone, DVD, the external coating of walkman shell earliest to process, existing its application is entered
One step expands to the household appliance technical fields such as cosmetics, television set and computer.
UV photocureable coating has without VOC (VOC), and environmental pollution is little, and curing rate is fast, section
The energy is saved, cured product performance is good, the advantages of be suitable for high-speed automated production.And traditional coating is volatile, curing rate slow,
It is unfavorable for environmental conservation.Therefore, UV coating is the main succedaneum of traditional coating.
Traditional peelable glue coating is a kind of mixture with compared with high solvent content, wherein solvent about 40% with
On, its curing mode is generally divided into heat curing-type and thermoplastics type, and heat curing-type film forming mechanism is the volatilization by solvent, and with molecule
Between chemical crosslinking, so as to film-forming, and thermoplastics type's film forming mechanism is the volatilization only by solvent, between no molecule
Chemical crosslinking and film-forming.Either heat curing-type or thermoplastics type's coating, its condition of cure must possess infrared heat source,
Under the heating of infrared heat source, by the volatilization of solvent, paint solidification film forming is made, so as to following problem can be caused：
1. heat cure, high energy consumption are unfavorable for energy-conservation；
2. curing rate is slow, reduces production efficiency, is unfavorable for the automatization of producing line；
3., to a large amount of VOCs of environmental emission, workers ' health is affected, while causing air pollution.
UV solidifies the main composition that peelable gum resin is UV photocureable coating, and traditional peelable gum has been broken in his generation
Fat curing mode, it is mainly several into packet by resin, monomer, light trigger, auxiliary agent and filler etc. that UV solidifies peelable gum resin
Into, therefore in UV Light Curings, no VOC is produced, environmentally safe, and solidification rate is fast,
Improve production efficiency.
【The content of the invention】
The purpose of the present invention is the defect for overcoming prior art, there is provided a kind of synthesis temperature is low, and curing rate is quick, is saved
Energy consumption, the UV of reduces cost solidify peelable gum resin.
It is a further object of the present invention to provide a kind of above-mentioned UV solidifies the preparation method of peelable gum resin.
In order to realize the purpose of the present invention, employ the following technical solutions：
A kind of UV solidifies peelable gum resin, it is characterised in that the component comprising following weight proportion：
Catalyst used in the present invention is benzyltriethylammoinium chloride and dibutyl tin laurate.
Polymerization inhibitor used in the present invention is MEHQ.
A kind of UV in the present invention solidifies peelable gum resin, the component comprising following weight proportion：
UV of the present invention solidifies the preparation method of peelable gum resin, it is characterised in that comprise the following steps：
1) by 2-(Acryloyloxy)ethanol, methyl hexahydrophthalic anhydride, epoxychloropropane, catalyst and polymerization inhibitor are mixed in container；
2) reflux condensing tube and mercurial thermometer are arranged on container, stirring；
3), after heating makes mixture be warming up to 70～80 DEG C, 50～70min is incubated, and is stirred；
4), after being warming up to 80～90 DEG C, 50～70min is incubated, and is stirred；
5), after being warming up to 100 DEG C, 20～40min is incubated, and is stirred；
6) after being warming up to 118 DEG C, 180～240min is incubated, and is stirred, survey the acid number≤3mgKOH/g of reaction system；
7) stop heating up, and after being cooled to room temperature, add hexamethylene diisocyanate and polymerization inhibitor, and stir；
8) polymerization inhibitor is added, is warming up to 70 DEG C, be incubated 20～40min, and stir；
9) 75 DEG C are warming up to, 240min is incubated, after be cooled to room temperature, survey-NCO% values after≤2, to obtain UV solidifications peelable
Gum resin.
It is 2500 ± 500cps/60 DEG C that UV of the present invention solidifies the viscosity of peelable gum resin.
UV of the present invention solidifies the synthetic route of peelable gum resin：
Advantages of the present invention：
The present invention provides a kind of UV and solidifies peelable gum resin, using 2-(Acryloyloxy)ethanol, epoxychloropropane, methyl hexahydrobenzene
Acid anhydride, catalyst and polymerization inhibitor are mixed, and by the temperature for controlling reaction, realize that open loop between compound and chain extension are anti-
Should, the larger straight chain compound of molecular weight is generated, one end is the acrylic acid structure group that can carry out photocuring, peelable with traditional
Gum resin is compared, and cost is relatively low, and synthesis temperature is low, saves energy consumption, non-volatility organic compound (VOC) pollution, curing rate
Hurry up.
By raw material that is the more commonly used, being easy to get, through two step synthesis paths, synthesize the relatively low polyurethane third of viscosity
Olefin(e) acid resin, under the irradiation of UV lamp, into free radical, acrylic acid unsaturated double-bond gains freedom base light trigger heterolytic fission, and then
There is the cross-linking reaction between molecule, form the cured film that can be completely stripped.
1st, the synthetic route that the present invention is adopted is more brief, the repeatability that operating process tool will be higher；
2nd, the raw material of production is simple, cheap, and VOC (VOC) is not used, and reduces into
This；
3rd, synthesize heating-up temperature in production process and be less than 118 DEG C, safe operation saves the energy；
4th, product adopts UV fast setting, significantly foreshortens to 3-5S, improves production efficiency hardening time.
5th, the boiling point of the raw material and final products of production is higher, low volatilization, low stain.
【Specific embodiment】
With reference to specific embodiment, the invention will be further described：
Embodiment 1:
A kind of UV solidifies peelable gum resin, the component comprising following weight proportion：
This kind of UV solidifies the preparation method of peelable gum resin：
1) by 2-(Acryloyloxy)ethanol, methyl hexahydrophthalic anhydride, epoxychloropropane, benzyltriethylammoinium chloride and para hydroxybenzene first
Ether is mixed in container；
2) reflux condensing tube and mercurial thermometer are arranged on container, stirring；
3), after heating makes mixture be warming up to 70 DEG C, 50min is incubated, and is stirred；
4), after being warming up to 80 DEG C, 50min is incubated, and is stirred；
5), after being warming up to 100 DEG C, 40min is incubated, and is stirred；
6) after being warming up to 118 DEG C, 240min is incubated, and is stirred, survey the acid number≤3mgKOH/g of reaction system；
7) stop heating up, and after being cooled to room temperature, add hexamethylene diisocyanate and MEHQ, and stir
Mix；
8) dibutyl tin laurate is added, is warming up to 70 DEG C, be incubated 20min, and stir；
9) 75 DEG C are warming up to, 240min is incubated, and it is room temperature to be cooled to after≤2 to survey-NCO% values, obtains UV and solidifies peelable glue
Resin, viscosity are 2600cps/60 DEG C.
Embodiment 2:
A kind of UV solidifies peelable gum resin, the component comprising following weight proportion：
This kind of UV solidifies the preparation method of peelable gum resin：
1) by 2-(Acryloyloxy)ethanol, methyl hexahydrophthalic anhydride, epoxychloropropane, benzyltriethylammoinium chloride and para hydroxybenzene first
Ether is mixed in container；
2) reflux condensing tube and mercurial thermometer are arranged on container, stirring；
3), after heating makes mixture be warming up to 80 DEG C, 60min is incubated, and is stirred；
4), after being warming up to 90 DEG C, 60min is incubated, and is stirred；
5), after being warming up to 100 DEG C, 30min is incubated, and is stirred；
6) after being warming up to 118 DEG C, 210min is incubated, and is stirred, survey the acid number≤3mgKOH/g of reaction system；
7) stop heating up, and after being cooled to room temperature, add hexamethylene diisocyanate and MEHQ, and stir
Mix；
8) dibutyl tin laurate is added, is warming up to 70 DEG C, be incubated 30min, and stir；
9) 75 DEG C are warming up to, 240min is incubated, and it is room temperature to be cooled to after≤2 to survey-NCO% values, obtains UV and solidifies peelable glue
Resin, viscosity are 2500cps/60 DEG C.
Embodiment 3:
A kind of UV solidifies peelable gum resin, the component comprising following weight proportion：
This kind of UV solidifies the preparation method of peelable gum resin：
1) by 2-(Acryloyloxy)ethanol, methyl hexahydrophthalic anhydride, epoxychloropropane, benzyltriethylammoinium chloride and para hydroxybenzene first
Ether is mixed in container；
2) reflux condensing tube and mercurial thermometer are arranged on container, stirring；
3), after heating makes mixture be warming up to 75 DEG C, 60min is incubated, and is stirred；
4), after being warming up to 85 DEG C, 60min is incubated, and is stirred；
5), after being warming up to 100 DEG C, 20min is incubated, and is stirred；
6) after being warming up to 118 DEG C, 180min is incubated, and is stirred, survey the acid number≤3mgKOH/g of reaction system；
7) stop heating up, and after being cooled to room temperature, add hexamethylene diisocyanate and MEHQ, and stir
Mix；
8) dibutyl tin laurate is added, is warming up to 70 DEG C, be incubated 30min, and stir；
9) 75 DEG C are warming up to, 240min is incubated, and it is room temperature to be cooled to after≤2 to survey-NCO% values, obtains UV and solidifies peelable glue
Resin, viscosity are 2000cps/60 DEG C.
Embodiment 4:
A kind of UV solidifies peelable gum resin, the component comprising following weight proportion：
This kind of UV solidifies the preparation method of peelable gum resin：
1) by 2-(Acryloyloxy)ethanol, methyl hexahydrophthalic anhydride, epoxychloropropane, benzyltriethylammoinium chloride and para hydroxybenzene first
Ether is mixed in container；
2) reflux condensing tube and mercurial thermometer are arranged on container, stirring；
3), after heating makes mixture be warming up to 80 DEG C, 60min is incubated, and is stirred；
4), after being warming up to 88 DEG C, 60min is incubated, and is stirred；
5), after being warming up to 100 DEG C, 35min is incubated, and is stirred；
6) after being warming up to 118 DEG C, 220min is incubated, and is stirred, survey the acid number≤3mgKOH/g of reaction system；
7) stop heating up, and after being cooled to room temperature, add hexamethylene diisocyanate and MEHQ, and stir
Mix；
8) dibutyl tin laurate is added, is warming up to 70 DEG C, be incubated 0min, and stir；
9) 75 DEG C are warming up to, 240min is incubated, and survey-NCO% values room temperature to be cooled to after≤2,
Obtain UV and solidify peelable gum resin, viscosity is 3000cps/60 DEG C.
Embodiment 5:
A kind of UV solidifies peelable gum resin, the component comprising following weight proportion：
This kind of UV solidifies the preparation method of peelable gum resin：
1) by 2-(Acryloyloxy)ethanol, methyl hexahydrophthalic anhydride, epoxychloropropane, benzyltriethylammoinium chloride and para hydroxybenzene first
Ether is mixed in container；
2) reflux condensing tube and mercurial thermometer are arranged on container, stirring；
3), after heating makes mixture be warming up to 82 DEG C, 65min is incubated, and is stirred；
4), after being warming up to 90 DEG C, 55min is incubated, and is stirred；
5), after being warming up to 100 DEG C, 30min is incubated, and is stirred；
6) after being warming up to 118 DEG C, 230min is incubated, and is stirred, survey the acid number≤3mgKOH/g of reaction system；
7) stop heating up, and after being cooled to room temperature, add hexamethylene diisocyanate and MEHQ, and stir
Mix；
8) dibutyl tin laurate is added, is warming up to 70 DEG C, be incubated 25min, and stir；
9) 75 DEG C are warming up to, 240min is incubated, and it is room temperature to be cooled to after≤2 to survey-NCO% values, obtains UV and solidifies peelable glue
Resin, viscosity are 2800cps/60 DEG C.
The hardening time test such as table 1 of embodiment 1-5：
Table 1：
| Sequence number | UV energy of light source | Transfer rate | Hardening time | Remarks |
| Embodiment 1 | 400mJ/cm2 | 60m/min | 5S | Drive 1 mercury lamp |
| Embodiment 2 | 800mJ/cm2 | 60m/min | 4S | Drive 2 mercury lamps |
| Embodiment 3 | 1200mJ/cm2 | 60m/min | 3S | Drive 3 mercury lamps |
| Embodiment 4 | 1600mJ/cm2 | 60m/min | 3S | Drive 4 mercury lamps |
| Embodiment 5 | 2000mJ/cm2 | 60m/min | 3S | Drive 5 mercury lamps |
1st, solidify liquid manufacturing process：Take UV and solidify peelable 71 parts of gum resin (weight), volume is added for the plastic cup of 150ml
In, then add 21 parts of tripropylene glycol diacrylate, add 2 parts of benzophenone, 2 parts of 2- hydroxy-2-methyls-
1- phenyl -1- acetone, is stirred with Glass rod, until solid dissolving is completely, system is transparent.With the screen printing plate of 250 mesh, will mix
Liquid is printed on ito glass plate, the solidification of Jing UV lamps, is positioned under room temperature condition, is clung one foot of cured film with adhesive tape, gently
Pull, monolithic cured film is thoroughly split away off from ito glass plate, remain without fragment.
2nd, test process hardening time：With the screen printing plate of 250 mesh, solidify liquid is respectively printed at into 5 ito glass plates
On, numbering is 1,2,3,4,5, and transfer rate is set as 60m/min, gradually increases and opens UV mercury lamp quantity, from 1～5,
The ito glass plate that solidify liquid is scribbled by 1,2,3,4, No. 5 respectively under the conditions of 1～5 UV lamps solidify (UV hardening times and energy
Relation between amount such as table 1), through cured film surface viscosity judging whether drying and forming-film, the ITO glass of film forming will be solidified into
Glass plate is positioned under room temperature condition, is clung one foot of cured film with adhesive tape, is gently pulled, and monolithic cured film will thoroughly from ITO
Split away off on glass plate, remain without fragment.
Claims (5)
1. a kind of UV solidifies the preparation method of peelable gum resin, it is characterised in that comprise the following steps：
1) by the 2-(Acryloyloxy)ethanol that mass percent is 23.0～27.5%, 30.0～35.0% methyl hexahydrophthalic anhydride,
25.0～29.5% epoxychloropropane, the catalyst that benzyltriethylammoinium chloride is constituted, is mixed in container；
2) reflux condensing tube and mercurial thermometer are arranged on container, stirring；
3), after heating makes mixture be warming up to 70～80 DEG C, 50～70min is incubated, and is stirred；
4), after being warming up to 80～90 DEG C, 50～70min is incubated, and is stirred；
5), after being warming up to 100 DEG C, 20～40min is incubated, and is stirred；
6), after being warming up to 118 DEG C, 180～240min is incubated, and is stirred；
7) stop heating up, and after being cooled to room temperature, add 13.0～15.0% hexamethylene diisocyanate, and to hydroxyl
The polymerization inhibitor that methyl phenyl ethers anisole is constituted, and stir；
8) catalyst for adding dibutyl tin laurate to constitute, is warming up to 70 DEG C, is incubated 20～40min, and stirs；
9) 75 DEG C are warming up to, be incubated 240min, after be cooled to room temperature, obtain UV solidification use peelable gum resin.
2. a kind of UV according to claim 1 solidifies the preparation method of peelable gum resin, it is characterised in that the step 6)
Temperature-rise period stops heating to 118 DEG C and insulated and stirred to reactant liquor acid number≤3mgKOH/g.
3. a kind of UV according to claim 1 solidifies the preparation method of peelable gum resin, it is characterised in that the step 9)
To 75 DEG C and insulated and stirred ,-NCO% the values to reactant liquor are≤2 to temperature-rise period, stopped reaction.
4. a kind of UV according to claim 1 solidifies the preparation method of peelable gum resin, it is characterised in that the UV solidifications
The viscosity of peelable gum resin is 2500 ± 500cps/60 DEG C.
5. a kind of UV according to claim 1 solidifies the preparation method of peelable gum resin, it is characterised in that the reaction
Synthetic route is：
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| CN201510011918.0A CN104496853B (en) | 2015-01-10 | 2015-01-10 | A kind of UV solidifies peelable gum resin and preparation method thereof |
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| CN109130442B (en) * | 2018-08-15 | 2021-03-05 | 广东尚联新材料科技有限公司 | Integrated forming processing technology for pressing and pasting wood veneer by using film spraying and rolling technology |
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|---|---|---|---|---|
| US3907574A (en) * | 1973-02-07 | 1975-09-23 | Fuji Photo Film Co Ltd | Photopolymerizable composition |
| US4108666A (en) * | 1975-04-11 | 1978-08-22 | Hitachi Chemical Co., Ltd. | Monofunctional monomer-containing photosensitive composition for photoresist |
| JPH06236031A (en) * | 1993-02-12 | 1994-08-23 | Asahi Denka Kogyo Kk | Photosensitive resin composition and photosensitive element using the same |
| CN101024683A (en) * | 2006-02-20 | 2007-08-29 | 四川大学 | Reactable resin and optical-imaging composition |
| CN102977335A (en) * | 2012-11-30 | 2013-03-20 | 深圳职业技术学院 | Method for preparing resin containing light-heat dual cured groups from epoxy chloropropane as raw material |
| CN103492446A (en) * | 2011-05-16 | 2014-01-01 | 三井化学株式会社 | Novel compound, composition containing said compound, and cured product |
-
2015
- 2015-01-10 CN CN201510011918.0A patent/CN104496853B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3907574A (en) * | 1973-02-07 | 1975-09-23 | Fuji Photo Film Co Ltd | Photopolymerizable composition |
| US4108666A (en) * | 1975-04-11 | 1978-08-22 | Hitachi Chemical Co., Ltd. | Monofunctional monomer-containing photosensitive composition for photoresist |
| JPH06236031A (en) * | 1993-02-12 | 1994-08-23 | Asahi Denka Kogyo Kk | Photosensitive resin composition and photosensitive element using the same |
| CN101024683A (en) * | 2006-02-20 | 2007-08-29 | 四川大学 | Reactable resin and optical-imaging composition |
| CN103492446A (en) * | 2011-05-16 | 2014-01-01 | 三井化学株式会社 | Novel compound, composition containing said compound, and cured product |
| CN102977335A (en) * | 2012-11-30 | 2013-03-20 | 深圳职业技术学院 | Method for preparing resin containing light-heat dual cured groups from epoxy chloropropane as raw material |
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