CN104151526A - Novel photosensitive resin material applied to DLP3D printer - Google Patents
Novel photosensitive resin material applied to DLP3D printer Download PDFInfo
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- CN104151526A CN104151526A CN201410386203.9A CN201410386203A CN104151526A CN 104151526 A CN104151526 A CN 104151526A CN 201410386203 A CN201410386203 A CN 201410386203A CN 104151526 A CN104151526 A CN 104151526A
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Abstract
The invention discloses a novel photosensitive resin material applied to a DLP3D printer. The novel photosensitive resin material comprises the components in parts by mass: 25-70 parts of prepolymer, 30-60 parts of epoxy resin, 15-30 parts of a diluent, 1-5 parts of a photosensitizer, 0.5-13 parts of a defoaming agent, 0.5-12 parts of a flatting agent, 1-8 parts of a cationic photoinitiator, 1-8 parts of a free radical photoinitiator, 2-8 parts of a polymerization inhibitor, 0.7-1.3 parts of a catalyst, 5-15 parts of a toughening agent and 3-12 parts of a cross-linking agent. The novel photosensitive resin material can achieve the effects of shortening the curing time, improving the comprehensive performance of coatings, improving the toughness and the hardness of models, optimizing the mechanical property of photosensitive resin materials, improving the production efficiency and greatly improving the energy utilization rate.
Description
Technical field
The present invention relates to 3D printer technology field, relate in particular to a kind of novel photosensitive resin material of the DLP3D of being applied to printer.
Background technology
Along with scientific and technical development and the variation of social demand, the competition of product is more and more fierce, the cycle of upgrading is shorter and shorter, thereby require the planner not only can be according to the designing new product that requires in market, and can within the short as far as possible time, produce prototype, thereby carry out necessary performance test, make corresponding amendment simultaneously, finally form the standardized product that can put on market.Along with the appearance of rapid shaping technique has well solved the problems such as in conventional fabrication processes, cost is high, the cycle is long with development, it can the quick accurate very complicated workpiece of manufacturing without any need for machining equipment in recent years.
DLP3D printer is a kind of technology based on digital light processing, this technology is first the digital processing of signal of video signal process, and then model is printed, its principle is by condensation lens by the cold light source going out by UHP lamps emission, by Rod (optical wand), by light uniformization, light is after treatment by a colour wheel, and light is divided into RGB tri-looks (or RGBW etc. more polychrome), then by printer by image print out, greatly improved printing precision.
Photosensitive resin is UV resin, is made up of polymer monomer and performed polymer, under the UV-irradiation of certain wavelength, causes at once polyreaction, completes curing.But there are some shortcomings in photosensitive resin of the prior art: 1, the curing time longer, and then affected production efficiency, and increased the probability of substandard products; 2, the over-all properties of photosensitive resin material and mechanical property are not high, and then have affected the scope of its application; 3, photosensitive resin material energy waste of the prior art is comparatively serious.
Summary of the invention
The object of the present invention is to provide a kind of novel photosensitive resin material of the DLP3D of being applied to printer, reach and shorten set time, improve the over-all properties of coating, improve toughness and the hardness of model, optimize the mechanical property of photosensitive resin material, improve production efficiency, the object that capacity usage ratio improves greatly.
The present invention adopts following technical scheme:
A novel photosensitive resin material that is applied to DLP3D printer, is characterized in that, comprises following mass parts: prepolymer 25～70, epoxy resin 30～60, thinner 15～30, photosensitizers 1～5, defoamer 0.5～13, flow agent 0.5～12, cation light initiator 1～8, free radical photo-initiation 1～8, stopper 2～8, catalyzer 0.7～1.3, toughner 5～15, linking agent 3～12.
Further, prepolymer is acrylate, acrylate is the positive butyl ester of propylene, isobornyl acrylate, vinylformic acid-2 (ethyl hexyl) ester, vinylformic acid phenoxy group ethyl ester, propylene 2-hydroxypropyl ester, vinylformic acid cyclohexyl ester, glycidyl acrylate, vinylformic acid dimethylamino ethyl ester, Viscoat 295, polyethyleneglycol diacrylate, 1, the own diacrylate of 6-, tripropylene glycol diacrylate, PDDA, the mixture of one or more in dihydroxyphenyl propane diethylene glycol diacrylate and propoxylation Viscoat 295, can greatly strengthen the reactive behavior of single functionality acrylate, even in the situation that aerobic exists, do not have the light trigger can polymerization yet, therefore there is good sticking power, chemical resistant properties and snappiness.
Further, thinner is at least one in Viscoat 295, neopentylglycol diacrylate and tri (propylene glycol) diacrylate, resin is had be convenient to the viscosity of processing, promotes the formation of cross-linked polymer simultaneously.
Further, photosensitizers is free radical type photosensitizers, and free radical type photosensitizers is the one in methyl phenyl ketone, aromatic ketone or acylphosphine oxide.
Further, cation light initiator is at least one in the luxuriant molysite of cumyl virtue, the luxuriant molysite of tolyl virtue, the phenyl luxuriant molysite of virtue and two-[4-(hexichol sulfenyl) phenyl] sulphur-2-phosphofluoric acid, after overcoming small molecules light trigger and decomposing in cured film residual small molecules or the bad effect of fragment to cured film.
Further, free radical photo-initiation comprises that two methyl ammonia is to oxygen azo-cycle butanone, a pair of oxygen azo-cycle of thio-phenyl acetone, 2-Yang Liu Za Onion quinone and 2,2-dimethyl-2-hydroxy acetophenone, increase the transparency to UV-light, because two methyl ammonia has higher photochemical activity to oxygen azo-cycle butanone, can be directly under light action and acrylate take out H-H reaction, produce macromolecular chain free radical, cause crosslinking reaction, and there is the low and photocuring operation of price and the advantage such as can under air conditions, carry out.
Further, stopper is at least one in Resorcinol and MEHQ, can effectively prevent that the unsaturated group on vinylformic acid from the process of preparing acrylate, radical polymerization occurring, and prevents that photosensitive resin from producing gel.
Further, catalyzer is trolamine, N, and two or more mixture in N-dimethyl benzylamine, DMA, triethylamine, can improve speed of response, reduces the viscosity of synthetics.
Further, toughner is at least one in urethane acrylate and dioctyl phthalate (DOP), has improved the shock resistance of photosensitive resin material.
Further, linking agent is one or more the mixture in bisphenol A epoxy acrylate, phenolic aldehyde acrylate, glycerine epoxy acrylate and trimethylolpropane acrylates, makes linking agent system have higher laser curing velocity and cured film hardness.
The present invention, owing to having adopted technique scheme, has following beneficial effect:
1, shorten the curing time, strengthened photosensitive property;
2, improve over-all properties and the mechanical property of coating, improve toughness and the hardness of model, optimized the mechanical property of photosensitive resin material;
3, improved production efficiency, capacity usage ratio improves greatly;
4, toughner add the impact property that can improve photosensitive resin, extended the work-ing life of material.
Embodiment
A kind of novel photosensitive resin material that is applied to DLP3D printer of the present invention, comprises following mass parts: prepolymer 25～70, epoxy resin 30～60, thinner 15～30, photosensitizers 1～5, defoamer 0.5～13, flow agent 0.5～12, cation light initiator 1～8, free radical photo-initiation 1～8, stopper 2～8, catalyzer 0.7～1.3, toughner 5～15, linking agent 3～12.
A kind of preparation method of the novel photosensitive resin material that is applied to DLP3D printer, comprise the steps: agitator is being housed, in the four-hole boiling flask of reflux exchanger and empty temperature facility, drop into epoxy resin, catalyzer, stopper etc., and make it to mix, during with oil bath heating flask to 80 DEG C, drip vinylformic acid with dropping funnel, slowly heat up and strictly control temperature of reaction at 115 DEG C, in this temperature range, dropwise, after when reacting certain, start to measure the acid number of reactant, in the time that the pH value of reactant is down to below 3.5, stopped reaction, then product is carried out to purification process, add appropriate hot water, stir 5min, upper water solution is removed in stratification hypsokinesis, to remove as stopper and the catalyzer of reaction.After repetition said process 5 times, remove remaining moisture in system, obtain yellow liquid and be novel photosensitive resin material.
Data parameters of the present invention is if table 1 is to as shown in the of 2
The impact of table 1 catalyst type on reaction times and product
The comparison of table 2 cation light initiator
When determination of acid value, measure sample to be tested, dissolve with ethanol or acetone, add 3～4 phenolphthalein reagents, be titrated to the obvious variable color of indicator with the KOH solution of the 0.1mol/L having demarcated under shake ceaselessly till.Method of calculation are: A=V*N*56.1/m
In formula: A---acid number/mg*g
-1;
Volume/ml of the KOH that V---titration spends;
Accurate concentration/mol*L of N---KOH
-1;
56.1---molar mass/g*mol of KOH
-1;
M---sample quality.
When measuring, first gets oxirane value two of 125ml iodine flasks, on analytical balance, respectively take sample 1.00g, put into the Erlenmeyer flask with stopper, add 20ml hydrochloric acid acetone soln with transfer pipet, then the vibration of jumping a queue, after resin is dissolved completely, places 1h in the cool, 3 of the red indicator of methylate, when the NaOH standardized solution that is 0.1mol/L by concentration is titrated to color and has red stain yellow till.Method of calculation:
In formula: E---oxirane value;
V
0---the volume/ml of the NaOH standardized solution that blank assay consumes;
V
1---titration sample consumes the volume/ml of NaOH standardized solution;
K---the concentration/mol*L of the amount of substance of NaOH standardized solution
-1;
Quality/the g of S---sample.
Embodiment 1:
(1) mass parts of raw material is as follows:
The positive butyl ester 25 of propylene;
Vinylformic acid-2 (ethyl hexyl) ester 25;
Propylene 2-hydroxypropyl ester 25;
Epoxy resin 30;
Viscoat 295 15;
Methyl phenyl ketone 1;
The luxuriant molysite 1 of cumyl virtue;
Two methyl ammonia is to oxygen azo-cycle butanone 2;
The a pair of oxygen azo-cycle of thio-phenyl acetone 2;
2-Yang Liu Za Onion quinone 2;
2,2-dimethyl-2-hydroxy acetophenone 2;
Defoamer 0.5;
Flow agent 0.5;
Resorcinol 4;
Trolamine 0.7;
N, N-dimethyl benzylamine 0.7;
DMA 0.7;
Triethylamine 0.7;
Urethane acrylate 5;
Bisphenol A epoxy acrylate 3.
(2) agitator is being housed, in the four-hole boiling flask of reflux exchanger and empty temperature facility, drop into epoxy resin, catalyzer, stopper etc., and make it to mix, during with oil bath heating flask to 80 DEG C, drip vinylformic acid with dropping funnel, slowly heat up and strictly control temperature of reaction at 115 DEG C, in this temperature range, dropwise, after reaction 15min, start to measure the acid number of reactant, in the time that the pH value of reactant is down to below 3.5, stopped reaction, then product is carried out to purification process, add the hot water of 25ml50 DEG C, stir 5min, upper water solution is removed in stratification hypsokinesis, to remove as stopper and the catalyzer of reaction.After repetition said process 5 times, remove remaining moisture in system, obtain yellow liquid and be the novel photosensitive resin material that is applied to DLP3D printer.
Embodiment 2:
(1) mass parts of raw material is as follows:
Isobornyl acrylate 25;
Vinylformic acid phenoxy group ethyl ester 25;
Vinylformic acid cyclohexyl ester 25;
Epoxy resin 30;
Neopentylglycol diacrylate 15;
Aromatic ketone 1;
The luxuriant molysite 1 of tolyl virtue;
Two methyl ammonia is to oxygen azo-cycle butanone 2;
The a pair of oxygen azo-cycle of thio-phenyl acetone 2;
2-Yang Liu Za Onion quinone 2;
2,2-dimethyl-2-hydroxy acetophenone 2;
Defoamer 0.5;
Flow agent 0.5;
MEHQ 4;
Trolamine 0.7;
N, N-dimethyl benzylamine 0.7;
DMA 0.7;
Triethylamine 0.7;
Dioctyl phthalate (DOP) 5;
Phenolic aldehyde acrylate 3.
(2) agitator is being housed, in the four-hole boiling flask of reflux exchanger and empty temperature facility, drop into epoxy resin, catalyzer, stopper etc., and make it to mix, during with oil bath heating flask to 80 DEG C, drip vinylformic acid with dropping funnel, slowly heat up and strictly control temperature of reaction at 115 DEG C, in this temperature range, dropwise, after reaction 15min, start to measure the acid number of reactant, in the time that the pH value of reactant is down to below 3.5, stopped reaction, then product is carried out to purification process, add the hot water of 25ml50 DEG C, stir 5min, upper water solution is removed in stratification hypsokinesis, to remove as stopper and the catalyzer of reaction.After repetition said process 5 times, remove remaining moisture in system, obtain yellow liquid and be the novel photosensitive resin material that is applied to DLP3D printer.
Embodiment 3:
(1) mass parts of raw material is as follows:
Glycidyl acrylate 25;
Viscoat 295 25;
The own diacrylate 25 of 1,6-;
Epoxy resin 30;
Tri (propylene glycol) diacrylate 15;
Acylphosphine oxide 1;
The luxuriant molysite 1 of phenyl virtue;
Two methyl ammonia is to oxygen azo-cycle butanone 2;
The a pair of oxygen azo-cycle of thio-phenyl acetone 2;
2-Yang Liu Za Onion quinone 2;
2,2-dimethyl-2-hydroxy acetophenone 2;
Defoamer 0.5;
Flow agent 0.5;
Resorcinol 4;
MEHQ 4;
Trolamine 0.7;
N, N-dimethyl benzylamine 0.7;
DMA 0.7;
Triethylamine 0.7;
Urethane acrylate 5;
Glycerine epoxy acrylate 3.
(2) agitator is being housed, in the four-hole boiling flask of reflux exchanger and empty temperature facility, drop into epoxy resin, catalyzer, stopper etc., and make it to mix, during with oil bath heating flask to 80 DEG C, drip vinylformic acid with dropping funnel, slowly heat up and strictly control temperature of reaction at 115 DEG C, in this temperature range, dropwise, after reaction 15min, start to measure the acid number of reactant, in the time that the pH value of reactant is down to below 3.5, stopped reaction, then product is carried out to purification process, add the hot water of 25ml50 DEG C, stir 5min, upper water solution is removed in stratification hypsokinesis, to remove as stopper and the catalyzer of reaction.After repetition said process 5 times, remove remaining moisture in system, obtain yellow liquid and be the novel photosensitive resin material that is applied to DLP3D printer.
Embodiment 4:
(1) mass parts of raw material is as follows:
Vinylformic acid dimethylamino ethyl ester 25;
Polyethyleneglycol diacrylate 25;
Tripropylene glycol diacrylate 25;
Epoxy resin 30;
Viscoat 295 15;
Methyl phenyl ketone 1;
Aromatic ketone 1;
Two-[4-(hexichol sulfenyl) phenyl] sulphur-2-phosphofluoric acid 1;
Two methyl ammonia is to oxygen azo-cycle butanone 2;
The a pair of oxygen azo-cycle of thio-phenyl acetone 2;
2-Yang Liu Za Onion quinone 2;
2,2-dimethyl-2-hydroxy acetophenone 2;
Defoamer 0.5;
Flow agent 0.5;
Resorcinol 4;
MEHQ 4;
Trolamine 0.7;
N, N-dimethyl benzylamine 0.7;
DMA 0.7;
Triethylamine 0.7;
Urethane acrylate 5;
Dioctyl phthalate (DOP) 5;
Trimethylolpropane acrylates 3.
(2) agitator is being housed, in the four-hole boiling flask of reflux exchanger and empty temperature facility, drop into epoxy resin, catalyzer, stopper etc., and make it to mix, during with oil bath heating flask to 80 DEG C, drip vinylformic acid with dropping funnel, slowly heat up and strictly control temperature of reaction at 115 DEG C, in this temperature range, dropwise, after reaction 15min, start to measure the acid number of reactant, in the time that the pH value of reactant is down to below 3.5, stopped reaction, then product is carried out to purification process, add the hot water of 25ml50 DEG C, stir 5min, upper water solution is removed in stratification hypsokinesis, to remove as stopper and the catalyzer of reaction.After repetition said process 5 times, remove remaining moisture in system, obtain yellow liquid and be the novel photosensitive resin material that is applied to DLP3D printer.
Embodiment 5:
(1) mass parts of raw material is as follows:
PDDA 25;
Dihydroxyphenyl propane diethylene glycol diacrylate 25;
Propoxylation Viscoat 295 25;
Epoxy resin 30;
Viscoat 295 15;
Neopentylglycol diacrylate 15;
Methyl phenyl ketone 1;
Aromatic ketone 1;
The luxuriant molysite 1 of tolyl virtue;
Two methyl ammonia is to oxygen azo-cycle butanone 2;
The a pair of oxygen azo-cycle of thio-phenyl acetone 2;
2-Yang Liu Za Onion quinone 2;
2,2-dimethyl-2-hydroxy acetophenone 2;
Defoamer 0.5;
Flow agent 0.5;
Resorcinol 4;
MEHQ 4;
Trolamine 0.7;
N, N-dimethyl benzylamine 0.7;
DMA 0.7;
Triethylamine 0.7;
Urethane acrylate 5;
Dioctyl phthalate (DOP) 5;
Trimethylolpropane acrylates 3.
(2) agitator is being housed, in the four-hole boiling flask of reflux exchanger and empty temperature facility, drop into epoxy resin, catalyzer, stopper etc., and make it to mix, during with oil bath heating flask to 80 DEG C, drip vinylformic acid with dropping funnel, slowly heat up and strictly control temperature of reaction at 115 DEG C, in this temperature range, dropwise, after reaction 15min, start to measure the acid number of reactant, in the time that the pH value of reactant is down to below 3.5, stopped reaction, then product is carried out to purification process, add the hot water of 25ml50 DEG C, stir 5min, upper water solution is removed in stratification hypsokinesis, to remove as stopper and the catalyzer of reaction.After repetition said process 5 times, remove remaining moisture in system, obtain yellow liquid and be the novel photosensitive resin material that is applied to DLP3D printer.
Gained is applied to the performance perameter of novel photosensitive resin material of DLP3D printer if table 3 is to as shown in table 5
| E ηCritical exposure | ～12.5mJ/cm 2 |
| D pCuring depth | 0.23mm |
| E 10Exposure | ～65mJ/cm 2 |
Table 3 optical property (300nm)
| Viscosity | ～250cps(25℃) |
| Density | ～1.25g/cm 3(25℃) |
| Outward appearance | Opaque white color, translucent |
Table 4 physicals
Table 5 mechanical property
These are only specific embodiments of the invention, but technical characterictic of the present invention is not limited to this.Any taking the present invention as basis, for realizing essentially identical technique effect, do ground simple change, be equal to replacement or modification etc., be all covered by among protection scope of the present invention.
Claims (10)
1. a novel photosensitive resin material that is applied to DLP3D printer, is characterized in that, comprises following mass parts: prepolymer 25～70, epoxy resin 30～60, thinner 15～30, photosensitizers 1～5, defoamer 0.5～13, flow agent 0.5～12, cation light initiator 1～8, free radical photo-initiation 1～8, stopper 2～8, catalyzer 0.7～1.3, toughner 5～15, linking agent 3～12.
2. a kind of novel photosensitive resin material that is applied to DLP3D printer according to claim 1, it is characterized in that: described prepolymer is acrylate, described acrylate is the positive butyl ester of propylene, isobornyl acrylate, vinylformic acid-2 (ethyl hexyl) ester, vinylformic acid phenoxy group ethyl ester, propylene 2-hydroxypropyl ester, vinylformic acid cyclohexyl ester, glycidyl acrylate, vinylformic acid dimethylamino ethyl ester, Viscoat 295, polyethyleneglycol diacrylate, 1, the own diacrylate of 6-, tripropylene glycol diacrylate, PDDA, the mixture of one or more in dihydroxyphenyl propane diethylene glycol diacrylate and propoxylation Viscoat 295.
3. a kind of novel photosensitive resin material that is applied to DLP3D printer according to claim 1, is characterized in that: described thinner is at least one in Viscoat 295, neopentylglycol diacrylate and tri (propylene glycol) diacrylate.
4. a kind of novel photosensitive resin material that is applied to DLP3D printer according to claim 1, is characterized in that: described photosensitizers is free radical type photosensitizers, and described free radical type photosensitizers is the one in methyl phenyl ketone, aromatic ketone or acylphosphine oxide.
5. a kind of novel photosensitive resin material that is applied to DLP3D printer according to claim 1, is characterized in that: described cation light initiator is at least one in the luxuriant molysite of cumyl virtue, the luxuriant molysite of tolyl virtue, the phenyl luxuriant molysite of virtue and two-[4-(hexichol sulfenyl) phenyl] sulphur-2-phosphofluoric acid.
6. a kind of novel photosensitive resin material that is applied to DLP3D printer according to claim 1, it is characterized in that: described free radical photo-initiation comprises that two methyl ammonia is to oxygen azo-cycle butanone, a pair of oxygen azo-cycle of thio-phenyl acetone, 2-Yang Liu Za Onion quinone and 2,2-dimethyl-2-hydroxy acetophenone.
7. a kind of novel photosensitive resin material that is applied to DLP3D printer according to claim 1, is characterized in that: described stopper is at least one in Resorcinol and MEHQ.
8. a kind of novel photosensitive resin material that is applied to DLP3D printer according to claim 1, is characterized in that: described catalyzer is trolamine, N, two or more mixture in N-dimethyl benzylamine, DMA, triethylamine.
9. a kind of novel photosensitive resin material that is applied to DLP3D printer according to claim 1, is characterized in that: described toughner is at least one in urethane acrylate and dioctyl phthalate (DOP).
10. a kind of novel photosensitive resin material that is applied to DLP3D printer according to claim 1, is characterized in that: described linking agent is one or more the mixture in bisphenol A epoxy acrylate, phenolic aldehyde acrylate, glycerine epoxy acrylate and trimethylolpropane acrylates.
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