CN114345273B - Preparation method of photo-curing composition - Google Patents
Preparation method of photo-curing composition Download PDFInfo
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- CN114345273B CN114345273B CN202111642382.4A CN202111642382A CN114345273B CN 114345273 B CN114345273 B CN 114345273B CN 202111642382 A CN202111642382 A CN 202111642382A CN 114345273 B CN114345273 B CN 114345273B
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- 239000000203 mixture Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 40
- 238000003860 storage Methods 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000001125 extrusion Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- 239000003999 initiator Substances 0.000 claims description 18
- 238000007789 sealing Methods 0.000 claims description 14
- 244000309464 bull Species 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 241000883990 Flabellum Species 0.000 claims description 6
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- QSOFJLDXOMMNNK-UHFFFAOYSA-N 2-(hydroxymethyl)-2-methylpropane-1,3-diol 3-sulfanylbutanoic acid Chemical compound CC(S)CC(O)=O.CC(S)CC(O)=O.CC(S)CC(O)=O.OCC(C)(CO)CO QSOFJLDXOMMNNK-UHFFFAOYSA-N 0.000 claims description 3
- GJKGAPPUXSSCFI-UHFFFAOYSA-N 2-Hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone Chemical compound CC(C)(O)C(=O)C1=CC=C(OCCO)C=C1 GJKGAPPUXSSCFI-UHFFFAOYSA-N 0.000 claims description 3
- WBEKRAXYEBAHQF-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;3-sulfanylbutanoic acid Chemical compound CC(S)CC(O)=O.CC(S)CC(O)=O.CC(S)CC(O)=O.CCC(CO)(CO)CO WBEKRAXYEBAHQF-UHFFFAOYSA-N 0.000 claims description 3
- RQPNXPWEGVCPCX-UHFFFAOYSA-N 3-sulfanylbutanoic acid Chemical compound CC(S)CC(O)=O RQPNXPWEGVCPCX-UHFFFAOYSA-N 0.000 claims description 3
- LABQKWYHWCYABU-UHFFFAOYSA-N 4-(3-sulfanylbutanoyloxy)butyl 3-sulfanylbutanoate Chemical compound CC(S)CC(=O)OCCCCOC(=O)CC(C)S LABQKWYHWCYABU-UHFFFAOYSA-N 0.000 claims description 3
- KEKXPPLELQNJEO-UHFFFAOYSA-N 6-(bicyclo[2.2.1]hept-2-ene-5-carbonyloxy)hexyl bicyclo[2.2.1]hept-2-ene-5-carboxylate Chemical compound C1C(C=C2)CC2C1C(=O)OCCCCCCOC(=O)C1C(C=C2)CC2C1 KEKXPPLELQNJEO-UHFFFAOYSA-N 0.000 claims description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007983 Tris buffer Substances 0.000 claims description 3
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 claims description 3
- HFCWPHDGLPTTAP-UHFFFAOYSA-N bicyclo[2.2.1]hept-2-ene-5-carboxylic acid;2-ethyl-2-(hydroxymethyl)propane-1,3-diol Chemical compound CCC(CO)(CO)CO.C1C2C(C(=O)O)CC1C=C2.C1C2C(C(=O)O)CC1C=C2.C1C2C(C(=O)O)CC1C=C2 HFCWPHDGLPTTAP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 230000008878 coupling Effects 0.000 claims 4
- 238000010168 coupling process Methods 0.000 claims 4
- 238000005859 coupling reaction Methods 0.000 claims 4
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 description 31
- 239000005022 packaging material Substances 0.000 description 5
- -1 thiol compound Chemical class 0.000 description 5
- 239000000243 solution Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 238000003491 array Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- Mixers Of The Rotary Stirring Type (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention provides a preparation method of a photo-curing composition, which comprises the following steps: s1: preparing a photoinitiator; s2: mixing a photoinitiator with a first compound to obtain a primary composition, and placing the primary composition into a first cavity of a storage container; s3: and adding the second compound into the second cavity of the storage container, and injecting the second compound into the first cavity according to the requirement for mixing when in use. The photoinitiator and the first compound are uniformly mixed and then are filled into the first cavity of the storage container, the second compound containing mercaptan is stored into the second cavity of the storage container, and when the photoinitiator and the first compound are used, a proper amount of the second compound is added into the first compound for mixing according to actual conditions, so that the photoinitiator and the first compound are practical, and waste is avoided.
Description
Technical Field
The invention relates to the field of photo-curing compositions, in particular to a preparation method of a photo-curing composition.
Background
Epoxy resins or silicone resins have been used in large amounts as packaging materials for light emitting diodes to protect the internal components of the light emitting diodes because of their light transmittance and heat dissipation properties. The conventional packaging materials can be classified into thermosetting type, photo-curing type or two-liquid type packaging materials (i.e., a combination of photo-curing type and thermosetting type packaging materials) according to different curing modes. Wherein, the photo-curing packaging material can generate free radical reaction or ion reaction after being irradiated by light, so that the resin generates cross-linking reaction.
In practical use, the conventional photocurable composition has a problem that oxygen inhibition occurs on the surface of the composition when the photocuring process is exposed to air, and in order to solve the problem, thiol is usually added into the composition, but for different use situations, for example, under a sealed environment, the thiol compound is not necessarily added or can be added with a proper reduction, and the conventional photocuring composition generally directly adds the thiol compound into the composition, so that the environment is not high.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above-described problems occurring in the conventional photocurable compositions.
Therefore, the technical problems solved by the invention are as follows: solves the problem that the existing photo-curing composition cannot be flexibly adjusted due to different requirements of scene change on the content of thiol compounds in the composition.
In order to solve the technical problems, the invention provides a preparation method of a photo-curing composition, which comprises the following steps:
s1: preparing a photoinitiator;
s2: mixing a photoinitiator with a first compound to obtain a primary composition, and placing the primary composition into a first cavity of a storage container;
s3: and adding the second compound into the second cavity of the storage container, and injecting the second compound into the first cavity according to the requirement for mixing when in use.
As a preferred embodiment of the present invention, the storage container includes: the storage tank is internally provided with a first cavity, a plurality of second cavities are arranged in the tank cover, the second cavities are specifically cylinders with downward openings, and second compounds are injected into the cylinders and packaged through heat seal stickers.
As a preferable scheme of the invention, a sealing rubber sheet is arranged in the tank cover, the sealing rubber sheet is arranged on the lower side of the heat-seal sticker, the tank cover is rotationally covered on the storage tank, and the sealing rubber sheet and the top of the side wall of the storage tank are tightly pressed and sealed in the process of rotating the tank cover.
As a preferred embodiment of the present invention, the first compound includes at least one of the following: dodecyl norborn-2-ene-5-carboxylate, 1, 6-hexanediol di- (norborn-2-ene-5-carboxylate), trimethylolpropane tri- (norborn-2-ene-5-carboxylate).
As a preferred embodiment of the present invention, the second compound includes at least one of the following: free trimethylol propane tris (3-mercaptobutyrate), trimethylol ethane tris (3-mercaptobutyrate), 1, 4-butanediol bis (3-mercaptobutyrate) and tris [2- (3-mercaptobutyrate) ethyl ] isocyanurate.
As a preferred embodiment of the present invention, the photoinitiator is prepared according to the following steps: under the condition of avoiding light, the silane coupling agent containing isocyanic acid radical and 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone react in ethyl acetate with water in a molar ratio of 2:1-4:1, dibutyl tin dilaurate DBTDL is used as a catalyst, the adding amount of the catalyst accounts for 0.05-0.3 percent of the mass fraction of the reactant, and the silicon-containing photoinitiator is obtained after the reaction for 4-8 hours at 60-80 ℃.
As a preferred embodiment of the present invention, the initiator is used in an amount of 0.1% wt to 20% wt% and the first compound is used in an amount of 25% wt to 70% wt% based on the total amount of the entire cured composition; the second compound is used in an amount of 25wt% to 70 wt%.
As a preferred embodiment of the present invention, the photoinitiator is produced by an initiator preparation apparatus comprising: reaction kettle, agitating unit, the feed inlet has been seted up on the reaction kettle, row's material pipe has been seted up to the bottom of reaction kettle, install the valve on the row's material pipe, agitating unit includes: stirring motor, bull stick, stirring flabellum, the bull stick is vertical to insert downwards in the reation kettle, stirring motor installs reation kettle's top, stirring motor's pivot with the bull stick butt joint, stirring flabellum is installed the bottom of bull stick.
As a preferable mode of the present invention, the initiator preparation device is further provided with a thermostatic control device, and the thermostatic control device includes: the heat conduction clamp cavity and the constant temperature water tank, the heat conduction clamp cavity is arranged in the side wall of the reaction kettle, the upper end and the lower end of the side wall of the reaction kettle are respectively provided with a water inlet pipe and a water outlet pipe, the water inlet pipe and the water outlet pipe are communicated with the heat conduction clamp cavity, and the water inlet pipe and the water outlet pipe are respectively connected to the constant temperature water tank.
As a preferred embodiment of the present invention, the initiator preparation apparatus further includes an auxiliary mixing apparatus, the auxiliary mixing apparatus including: a circulation pipe having a plurality of groups and being circumferentially disposed at an outside of the reaction vessel, the circulation pipe comprising: the upper circulating pipe penetrates through the side wall of the top of the reaction kettle and is inserted into the reaction kettle, the lower circulating pipe penetrates through the side wall of the bottom of the reaction kettle and is inserted into the reaction kettle, the connecting hose is arranged outside the reaction kettle, two ends of the connecting hose are respectively connected with the upper circulating pipe and the lower circulating pipe, and an extrusion circulating device is arranged on the connecting hose.
As a preferred embodiment of the present invention, the extrusion circulation device includes: the pressing device comprises a pressing seat, a pressing plate, a rotating disc, pressing rods and a pressing motor, wherein semicircular grooves are formed in the side wall of the pressing seat, pressing grooves symmetrical to the grooves are formed in the pressing plate, the pressing plate is detachably arranged on the pressing seat, the pressing rods are three and are vertically arranged on the rotating disc, three pressing rod annular arrays are arranged on the rotating disc, the three pressing rods are inserted into the pressing grooves, the rotating disc is driven by the pressing motor to rotate, and the three pressing rods roll along the surface profile of the pressing grooves in sequence in the rotating process of the rotating disc.
As a preferred embodiment of the present invention, the extrusion rod is movably mounted to the turntable through a bearing.
Compared with the prior art, the invention provides a preparation method of a photo-curing composition, which has the following beneficial effects:
1. the photoinitiator and the first compound are uniformly mixed and then are filled into the first cavity of the storage container, the second compound containing mercaptan is stored into the second cavity of the storage container, and when the photoinitiator and the first compound are used, a proper amount of the second compound is added into the first compound for mixing according to actual conditions, so that the photoinitiator and the first compound are practical, and waste is avoided.
2. According to the invention, the constant temperature control device is arranged on the initiator preparation device, the temperature in the reaction kettle is kept constant by using a water bath heating method, so that the temperature is uniformly conducted, and the phenomenon of local overheating is avoided.
3. According to the invention, the auxiliary mixing device is arranged on the initiator preparation device, and the raw materials at the top of the reaction kettle are pressed into the bottom of the reaction kettle by using the auxiliary mixing device, so that the stirring effect is improved.
4. According to the invention, the extrusion circulation device is formed by the pressing seat, the pressing plate, the turntable, the extrusion rod and the extrusion motor, so that the pump body is prevented from being used, and the internal cleaning is convenient.
Description of the drawings:
fig. 1 is a perspective view of a storage device.
Fig. 2 is a cross-sectional view of a storage device.
FIG. 3 is a perspective view of an initiator preparation apparatus.
FIG. 4 is a cross-sectional view of the reaction vessel.
Fig. 5 is a schematic perspective view of an extrusion circulation device.
Wherein: 1-a storage tank; 2-a tank cover; 3-cylinder; 4-heat sealing the sticker; 5-sealing rubber sheets; 6-a reaction kettle; 601-a feed inlet; 602-discharging pipe; 701-a stirring motor; 702-a rotating rod; 703-stirring fan blades; 801-a heat conducting clamping cavity; 802-water inlet pipe; 803-a water outlet pipe; 804-constant temperature water tank; 9-an extrusion circulation device; 901-pressing a seat; 902-a pressing plate; 903-squeeze bar; 904-a turntable; 905-an extrusion motor; 10-upper circulation pipe; 11-a lower circulation pipe; 12-connecting hose.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The invention provides a preparation method of a photo-curing composition, which comprises the following steps:
s1: preparing a photoinitiator;
s2: mixing a photoinitiator with a first compound to obtain a primary composition, and placing the primary composition into a first cavity of a storage container, wherein the first compound comprises at least one of the following components: dodecyl norborn-2-ene-5-carboxylate, 1,6 hexanediol di- (norborn-2-ene-5-carboxylate), trimethylolpropane tri- (norborn-2-ene-5-carboxylate);
s3: adding a second compound into a second cavity of the storage container, and injecting the second compound into the first cavity according to the requirement for mixing when in use, wherein the second compound comprises at least one of the following components: free trimethylolpropane tris (3-mercaptobutyrate), trimethylolethane tris (3-mercaptobutyrate), 1, 4-butanediol bis (3-mercaptobutyrate) and tris [2- (3-mercaptobutyrate) ethyl ] isocyanurate, the initiator being used in an amount of 0.1% wt to 20% wt% and the first compound being used in an amount of 25% wt% to 70% wt% based on the total amount of the overall cured composition; the total amount of the second compound is 25wt% to 70 wt%.
As shown in fig. 1 to 2, the storage container of the present invention specifically includes: the storage tank comprises a storage tank 1 and a tank cover 2, wherein a first cavity is arranged in the storage tank 1, a plurality of second cavities are arranged in the tank cover 2, the second cavities are specifically cylinders 3 with downward openings, second compounds are injected into the cylinders 3 and are packaged through heat seal stickers 4, sealing rubber sheets 5 are arranged in the tank cover 2, the sealing rubber sheets 5 are arranged on the lower side of the heat seal stickers 4, the tank cover 2 is rotationally covered on the storage tank 1, and the sealing rubber sheets 5 are tightly sealed with the top of the side wall of the storage tank 1 in a pressing manner in the process of rotating the tank cover 2. When in use, a certain amount of hot air stickers 4 are torn off according to the need, sealing rubber sheets are removed, a second compound is added into the storage tank 1, then the sealing rubber sheets are put on again, the tank cover 2 is covered, and the internal composition is uniformly mixed by shaking.
The following describes the preparation method of the photoinitiator according to the present invention, and the photoinitiator according to the present invention is prepared according to the following steps: under the condition of avoiding light, the silane coupling agent containing isocyanic acid radical and 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone react in ethyl acetate with water in a molar ratio of 2:1-4:1, dibutyl tin dilaurate DBTDL is used as a catalyst, the adding amount of the catalyst accounts for 0.05-0.3 percent of the mass fraction of the reactant, and the silicon-containing photoinitiator is obtained after the reaction for 4-8 hours at 60-80 ℃.
In order to specifically define the initiator preparation method of the present invention, the photoinitiator of the present invention is produced using an initiator preparation apparatus, as shown in fig. 3 to 4, which specifically includes: reaction kettle 6, agitating unit, feed inlet 601 has been seted up on the reaction kettle 6, discharge pipe 602 has been seted up to the bottom of reaction kettle 6, install the valve on the discharge pipe 602, agitating unit includes: stirring motor 701, bull stick 702, stirring flabellum 703, bull stick 702 is vertical to be inserted downwards in the reation kettle 6, stirring motor 701 installs the top of reation kettle 6, the pivot of stirring motor 701 with bull stick 702 dock, stirring flabellum 703 is installed the bottom of bull stick 702.
Because the temperature is controlled to be 60-80 ℃ during the preparation of the initiator, the invention also provides a constant temperature control device on the initiator preparation device, and the constant temperature control device comprises: the heat conduction clamp cavity 801 and the constant temperature water tank 804, the heat conduction clamp cavity 801 is arranged in the side wall of the reaction kettle 6, the upper end and the lower end of the side wall of the reaction kettle 6 are respectively provided with the water inlet pipe 802 and the water outlet pipe 803, the water inlet pipe 802 and the water outlet pipe 803 are communicated with the heat conduction clamp cavity 801, and the water inlet pipe 802 and the water outlet pipe 803 are respectively connected to the constant temperature water tank 804.
In order to further improve the stirring effect during the preparation of the initiator, the initiator preparation device of the invention further comprises an auxiliary mixing device, wherein the auxiliary mixing device comprises: a circulation pipe having a plurality of groups and being circumferentially disposed outside the reaction vessel 6, the circulation pipe comprising: the upper circulating pipe 11 penetrates through the side wall of the top of the reaction kettle 6 and is inserted into the reaction kettle 6, the lower circulating pipe 11 penetrates through the side wall of the bottom of the reaction kettle 6 and is inserted into the reaction kettle 6, the connecting hose 12 is installed outside the reaction kettle 6, two ends of the connecting hose 12 are respectively connected with the upper circulating pipe 10 and the lower circulating pipe 11, and the connecting hose 12 is provided with the extrusion circulating device 9.
The extrusion cycle apparatus 9 of the present invention will be specifically described below, and as shown in fig. 5, the extrusion cycle apparatus 9 of the present invention includes: the pressing seat 901, the pressing plate 902, the turntable 904, the extrusion rods 903 and the extrusion motor 905, wherein semicircular grooves are formed in the side wall of the pressing seat 901, pressing grooves symmetrical to the grooves are formed in the pressing plate 902, the pressing plate 902 is detachably arranged on the pressing seat 901, the extrusion rods 903 are three and vertically arranged on the turntable 904, the three extrusion rods 903 are annularly arranged on the turntable 904 in an array mode, the three extrusion rods are inserted into the pressing grooves, the turntable 904 is driven by the extrusion motor 905 to rotate, and the three extrusion rods 903 roll along the surface profile of the pressing grooves in sequence in the rotation process of the turntable 904.
In order to reduce the wear of the squeeze lever 903 on the connection hose 12, the squeeze lever 903 of the present invention is movably mounted to the turntable 904 by a bearing.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (6)
1. A method of preparing a photocurable composition comprising the steps of:
s1: preparing a photoinitiator;
s2: mixing a photoinitiator with a first compound to obtain a primary composition, and placing the primary composition into a first cavity of a storage container;
s3: adding a second compound into a second cavity of the storage container, and injecting the second compound into the first cavity according to the requirement for mixing when in use;
the storage container includes: the storage tank comprises a storage tank (1) and a tank cover (2), wherein a first cavity is arranged in the storage tank (1), a plurality of second cavities are arranged in the tank cover (2), the second cavities are specifically cylinders (3) with downward openings, and second compounds are injected into the cylinders (3) and are packaged through heat sealing stickers (4);
the first compound includes at least one of: dodecyl norborn-2-ene-5-carboxylate, 1,6 hexanediol di- (norborn-2-ene-5-carboxylate), trimethylolpropane tri- (norborn-2-ene-5-carboxylate);
the second compound includes at least one of: free trimethylolpropane tris (3-mercaptobutyrate), trimethylolethane tris (3-mercaptobutyrate), 1, 4-butanediol bis (3-mercaptobutyrate) and tris [2- (3-mercaptobutyrate) ethyl ] isocyanurate;
the photoinitiator is prepared according to the following steps: under the condition of avoiding light, the silane coupling agent containing isocyanic acid radical and 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone react in ethyl acetate with water in a molar ratio of 2:1-4:1, dibutyl tin dilaurate DBTDL is used as a catalyst, the adding amount of the catalyst accounts for 0.05-0.3 percent of the mass fraction of the reactant, and the silicon-containing photoinitiator is obtained after the reaction for 4-8 hours at 60-80 ℃.
2. The preparation method of the photo-curing composition according to claim 1, wherein a sealing rubber sheet (5) is installed in the can cover (2), the sealing rubber sheet (5) is arranged on the lower side of the heat-seal sticker (4), the can cover (2) is rotationally covered on the storage can (1), and the sealing rubber sheet (5) is tightly sealed with the top of the side wall of the storage can (1) in the process of rotating the can cover (2).
3. The method of claim 1, wherein the initiator is used in an amount of 0.1% wt to 20% wt% and the first compound is used in an amount of 25% wt to 70% wt% based on the total amount of the entire cured composition; the second compound is used in an amount of 25wt% to 70 wt%.
4. The method of preparing a photocurable composition according to claim 1, wherein said photoinitiator is produced using an initiator preparation apparatus comprising: reaction kettle (6), agitating unit, feed inlet (601) have been seted up on reaction kettle (6), discharge pipe (602) have been seted up to the bottom of reaction kettle (6), install the valve on discharge pipe (602), agitating unit includes: stirring motor (701), bull stick (702), stirring flabellum (703), bull stick (702) are vertical to be inserted downwards in reation kettle (6), stirring motor (701) are installed the top of reation kettle (6), the pivot of stirring motor (701) with bull stick (702) dock, stirring flabellum (703) are installed the bottom of bull stick (702).
5. The method of producing a photocurable composition according to claim 4, wherein said initiator producing means is further provided with a thermostatic control means comprising: the heat conduction clamp cavity (801) and the constant temperature water tank (804), the heat conduction clamp cavity (801) is arranged in the side wall of the reaction kettle (6), the upper end and the lower end of the side wall of the reaction kettle (6) are respectively provided with the water inlet pipe (802) and the water outlet pipe (803), the water inlet pipe (802) and the water outlet pipe (803) are respectively communicated with the heat conduction clamp cavity (801), and the water inlet pipe (802) and the water outlet pipe (803) are respectively connected to the constant temperature water tank (804).
6. The method of preparing a photocurable composition according to claim 5, wherein said initiator preparing means further comprises auxiliary mixing means, said auxiliary mixing means comprising: circulation pipe, the said circulation pipe has multiunit and surrounds setting up in the outside of the reaction kettle (6), the said circulation pipe includes: go up circulating pipe (10), circulating pipe (11), coupling hose (12) down, go up circulating pipe (10) run through the lateral wall at reation kettle (6) top and insert in reation kettle (6), circulating pipe (11) down run through the lateral wall at reation kettle (6) bottom and insert in reation kettle (6), coupling hose (12) are installed the outside of reation kettle (6) and coupling hose (12) both ends are connected with last circulating pipe (10), circulating pipe (11) down respectively, install extrusion circulating device (9) on coupling hose (12).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111642382.4A CN114345273B (en) | 2021-12-30 | 2021-12-30 | Preparation method of photo-curing composition |
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| KR20130059287A (en) * | 2011-11-28 | 2013-06-05 | 주식회사 엘지화학 | Photo-curable composition, optical anistropic film and its preparation method |
| CN103221458A (en) * | 2010-10-01 | 2013-07-24 | 莫赛纳实验室公司 | Method for the manufacture of articles of thiol-ene polymers |
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| EP1477511A1 (en) * | 2003-05-15 | 2004-11-17 | DSM IP Assets B.V. | Radiation curable thiol-ene composition |
| US8283095B2 (en) * | 2006-08-23 | 2012-10-09 | Showa Denko K.K. | Thiourethane compound and photosensitive resin composition |
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| CN103221458A (en) * | 2010-10-01 | 2013-07-24 | 莫赛纳实验室公司 | Method for the manufacture of articles of thiol-ene polymers |
| KR20130059287A (en) * | 2011-11-28 | 2013-06-05 | 주식회사 엘지화학 | Photo-curable composition, optical anistropic film and its preparation method |
| CN208642661U (en) * | 2018-07-16 | 2019-03-26 | 武汉铌欧能源材料有限公司 | A kind of recombination reaction kettle |
| CN110218323A (en) * | 2019-06-06 | 2019-09-10 | 南京恒桥化学技术材料有限公司 | One kind light-cured type composition of structures alone containing norbornene and light-cured type encapsulating material |
| CN214416343U (en) * | 2021-03-19 | 2021-10-19 | 湖北铭泉科技有限公司 | Raw material quantitative feeder for production of passivator |
| CN113667094A (en) * | 2021-08-31 | 2021-11-19 | 万华化学（宁波）有限公司 | Exposure-resistant isocyanate composition, preparation method and application thereof in preparation of high-strength polyurethane optical resin |
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