CN114345273A - Preparation method of photocuring composition - Google Patents
Preparation method of photocuring composition Download PDFInfo
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- CN114345273A CN114345273A CN202111642382.4A CN202111642382A CN114345273A CN 114345273 A CN114345273 A CN 114345273A CN 202111642382 A CN202111642382 A CN 202111642382A CN 114345273 A CN114345273 A CN 114345273A
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- photoinitiator
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
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- 150000001875 compounds Chemical class 0.000 claims abstract description 37
- 238000003860 storage Methods 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 238000001125 extrusion Methods 0.000 claims description 27
- 239000003999 initiator Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 238000007789 sealing Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 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
- 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
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- 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
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical class CCOC(C)=O XEKOWRVHYACXOJ-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
- 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
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- 239000012948 isocyanate Substances 0.000 claims description 3
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a preparation method of a photocuring composition, which comprises the following steps: s1: preparing a photoinitiator; s2: mixing a photoinitiator with a first compound to obtain a primary composition, and putting the primary composition into a first cavity of a storage container; s3: and adding the second compound into a second cavity of the storage container, and injecting the second compound in the second cavity into the first cavity for mixing according to requirements during use. According to the invention, 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 multifunctional storage container is used, a proper amount of the second compound is added into the first compound according to actual conditions for mixing and practical use, so that waste is avoided.
Description
Technical Field
The invention relates to the field of photocuring compositions, in particular to a preparation method of a photocuring composition.
Background
Epoxy resin or silicone resin has been widely used as a packaging material for light emitting diodes to protect internal components of the light emitting diodes due to its light transmittance and heat dissipation. The conventional encapsulation materials can be classified into thermosetting type, photo-curing type, or two-liquid type (i.e., a combination of photo-curing type and thermosetting type) according to their different curing methods. The photo-curing type packaging material can generate free radical reaction or ion reaction after being irradiated by light, so that the resin generates cross-linking reaction.
In the practical process of the existing light-curing composition, the problem that the surface of the composition generates oxygen inhibition phenomenon when the light-curing process is exposed to the air is caused, in order to solve the problem, mercaptan is usually added into the composition, but the addition of the mercaptan compound is not necessary or can be reduced properly aiming at different use scenes such as under a sealed environment, and the existing light-curing composition usually directly adds the mercaptan compound into the composition, so that the environment is not high.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above-mentioned problems occurring in the conventional photocurable compositions.
Therefore, the technical problem solved by the invention is as follows: solves the problem that the prior light-cured composition can not be flexibly adjusted due to different requirements of scene change on the content of thiol compounds in the composition when in use.
In order to solve the technical problems, the invention provides a preparation method of a photocuring composition, which comprises the following steps:
s1: preparing a photoinitiator;
s2: mixing a photoinitiator with a first compound to obtain a primary composition, and putting the primary composition into a first cavity of a storage container;
s3: and adding the second compound into a second cavity of the storage container, and injecting the second compound in the second cavity into the first cavity for mixing according to requirements during use.
As a preferable aspect of the present invention, the storage container includes: the storage tank comprises a storage tank body and a tank cover, wherein a first cavity is arranged in the storage tank body, a plurality of second cavities are installed in the tank cover, the second cavities are cylinders with downward openings, and second compounds are injected into the cylinders and are packaged through heat-seal pasters.
In a preferred embodiment of the present invention, a sealing rubber sheet is installed in the can cover, the sealing rubber sheet is disposed under the heat-seal sticker, the can cover is rotatably covered on the storage tank, and the sealing rubber sheet is pressed and sealed with the top of the sidewall of the storage tank in the process of rotating the can cover.
As a preferred embodiment of the present invention, the first compound includes at least one of: dodecyl norbornyl-2-ene-5-carboxylate, 1,6 hexanediol di- (norbornyl-2-ene-5-carboxylate), trimethylolpropane tri- (norbornyl-2-ene-5-carboxylate).
As a preferable aspect of the present invention, 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.
As a preferred embodiment of the present invention, the photoinitiator is prepared according to the following steps: under the condition of keeping out of the sun, a silane coupling agent containing isocyanate and 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone react in dehydrated ethyl acetate according to the molar ratio of 2:1-4:1, dibutyltin dilaurate DBTDL is used as a catalyst, the addition of the catalyst accounts for 0.05-0.3% of the mass fraction of reactants, and the reaction is carried out for 4-8 hours at the temperature of 60-80 ℃ to obtain the silicon-containing photoinitiator.
As a preferred embodiment of the present invention, the amount of the initiator is 0.1 wt% to 20 wt%, and the amount of the first compound is 25wt% to 70 wt%, based on the total amount of the entire curing composition; the dosage of the second compound is 25wt% -70 wt%.
As a preferable aspect of the present invention, the photoinitiator is produced by using an initiator preparation apparatus, the initiator preparation apparatus including: reation kettle, agitating unit, the last feed inlet of having seted up of reation kettle, reation kettle's bottom has been seted up and has been arranged the material pipe, arrange and install the valve on the material pipe, agitating unit includes: agitator motor, bull stick, stirring fan blade, the vertical downwardly inserting of bull stick in the reation kettle, agitator motor installs reation kettle's top, agitator motor's pivot with the bull stick butt joint, stirring fan blade installs the bottom of bull stick.
As a preferable scheme of the present invention, a thermostatic control device is further disposed on the initiator preparation device, and the thermostatic control device includes: heat conduction presss from both sides chamber, constant temperature water tank, heat conduction presss from both sides the chamber setting and is in reation kettle's the lateral wall, inlet tube, outlet pipe are installed respectively to the upper and lower both ends of reation kettle lateral wall, inlet tube, outlet pipe all with heat conduction presss from both sides the chamber intercommunication, inlet tube, outlet pipe are connected to respectively on the constant temperature water tank.
As a preferable scheme of the present invention, the initiator preparation apparatus further comprises an auxiliary mixing apparatus, and the auxiliary mixing apparatus comprises: a plurality of sets of circulation pipes disposed around the outside of the reaction vessel, the circulation pipes comprising: the extrusion circulating device comprises an upper circulating pipe, a lower circulating pipe and a connecting hose, wherein 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 installed outside the reaction kettle, two ends of the connecting hose are respectively connected with the upper circulating pipe and the lower circulating pipe, and the connecting hose is provided with an extrusion circulating device.
As a preferable aspect of the present invention, the press cycle apparatus includes: the pressing seat comprises a pressing seat, a pressing plate, a rotary table, extrusion rods and an extrusion motor, wherein a semicircular groove is 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 mounted on the pressing seat, the extrusion rods are three and perpendicularly mounted on the rotary table, three extrusion rod annular arrays are mounted on the rotary table, the three extrusion rods are inserted into the pressing grooves, the rotary table is driven by the extrusion motor to rotate, and the three extrusion rods roll along the surface contour of the pressing grooves in sequence in the rotating process of the rotary table.
As a preferable mode of the present invention, the pressing rod is movably mounted to the turntable through a bearing.
Compared with the prior art, the invention provides a preparation method of the photocuring composition, which has the following beneficial effects:
1. according to the invention, 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 multifunctional storage container is used, a proper amount of the second compound is added into the first compound according to actual conditions for mixing and practical use, so that waste is avoided.
2. According to the invention, the constant temperature control device is arranged on the initiator preparation device, and 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. The extrusion circulating device is composed of the pressing seat, the pressing plate, the rotary disc, the extrusion rod and the extrusion motor, so that the pump body is prevented from being used, and the interior of the pump body is convenient to clean.
Drawings
Fig. 1 is a perspective view of a storage device.
Fig. 2 is a cross-sectional view of the storage device.
FIG. 3 is a perspective view of an initiator preparing apparatus.
FIG. 4 is a sectional view of a reaction vessel.
Fig. 5 is a schematic perspective view of the extrusion cycle apparatus.
Wherein: 1-a storage tank; 2-can cover; 3-cylinder; 4-heat sealing the paster; 5-sealing rubber sheets; 6-a reaction kettle; 601-feed inlet; 602-a discharge pipe; 701-a stirring motor; 702-a turning bar; 703-stirring fan blades; 801-heat conducting nip; 802-a water inlet pipe; 803-outlet pipe; 804-constant temperature water tank; 9-extrusion cycle equipment; 901-pressing seat; 902-a platen; 903-an extrusion rod; 904-rotating disc; 905-extrusion motor; 10-upper circulation pipe; 11-lower circulation pipe; 12-connecting hose.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
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 than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is 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 photocuring 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: 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 in the second cavity into the first cavity for mixing according to requirements during use, wherein the second compound comprises at least one of the following compounds: free trimethylolpropane tris (3-mercaptobutyrate), trimethylolethane tris (3-mercaptobutyrate), 1, 4-butanediol bis (3-mercaptobutyrate), and tris [2- (3-mercaptobutyrate) ethyl ] isocyanurate, said initiator being present in an amount of from 0.1 wt% to 20 wt%, said first compound being present in an amount of from 25wt% to 70 wt%, based on the total amount of the overall cured composition; the total amount of the second compound is 25wt% -70 wt%.
As shown in fig. 1-2, the storage container of the present invention specifically includes: holding vessel 1, cover 2, be equipped with first cavity in the holding vessel 1, install a plurality of second cavitys in the cover 2, the second cavity specifically is opening decurrent drum 3, and the second compound pours into a plurality of drums 3 and encapsulates through heat-seal sticker 4 into, install sealing rubber piece 5 in the cover 2, sealing rubber piece 5 sets up the downside of heat-seal sticker 4, 2 swivel caps of cover close on the holding vessel 1, 2 swivel caps of cover and in-process will sealing rubber piece 5 compresses tightly sealedly with the lateral wall top of holding vessel 1. When the hot air paste is used, a certain amount of hot air paste 4 is torn off according to the requirement, the sealing rubber sheet is removed, the second compound is added into the storage tank 1, then the sealing rubber sheet is put again, the tank cover 2 is covered, and the inner composition is uniformly mixed by shaking.
The preparation method of the photoinitiator according to the present invention is specifically described below, and the photoinitiator according to the present invention is prepared according to the following steps: under the condition of keeping out of the sun, a silane coupling agent containing isocyanate and 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone react in dehydrated ethyl acetate according to the molar ratio of 2:1-4:1, dibutyltin dilaurate DBTDL is used as a catalyst, the addition of the catalyst accounts for 0.05-0.3% of the mass fraction of reactants, and the reaction is carried out for 4-8 hours at the temperature of 60-80 ℃ to obtain the silicon-containing photoinitiator.
In order to specifically limit the initiator preparation method of the present invention, the photoinitiator of the present invention is produced by using an initiator preparation apparatus, as shown in fig. 3 to 4, the initiator preparation apparatus of the present invention specifically includes: reation kettle 6, agitating unit, feed inlet 601 has been seted up on reation kettle 6, row's material pipe 602 has been seted up to reation kettle 6's bottom, arrange and install the valve on the material pipe 602, agitating unit includes: stirring motor 701, bull stick 702, stirring fan blade 703, bull stick 702 is vertical downwards inserted in reation kettle 6, stirring motor 701 is installed at reation kettle 6's top, stirring motor 701's pivot with bull stick 702 butt joint, stirring fan blade 703 is installed the bottom of bull stick 702.
Because the temperature needs to be controlled at 60-80 ℃ during the preparation of the initiator, the initiator preparation device is also provided with a constant temperature control device, and the constant temperature control device comprises: heat conduction presss from both sides chamber 801, constant temperature water tank 804, heat conduction presss from both sides the chamber 801 setting and is in reation kettle 6's the lateral wall, inlet tube 802, outlet pipe 803 are installed respectively to the upper and lower both ends of reation kettle 6 lateral wall, inlet tube 802, outlet pipe 803 all with heat conduction presss from both sides chamber 801 intercommunication, inlet tube 802, outlet pipe 803 are connected to respectively on the constant temperature water tank 804.
In order to further improve the stirring effect during the preparation of the initiator, the initiator preparation device also comprises an auxiliary mixing device, and the auxiliary mixing device comprises: a circulation pipe having a plurality of groups and disposed around the outside of the reaction vessel 6, the circulation pipe comprising: the device comprises an upper circulating pipe 10, a lower circulating pipe 11 and a connecting hose 12, wherein 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 an extrusion circulating device 9 is installed on the connecting hose 12.
The following describes the extrusion cycle apparatus 9 of the present invention in detail, and as shown in fig. 5, the extrusion cycle apparatus 9 of the present invention includes: the pressing device comprises a pressing seat 901, a pressing plate 902, a rotating disc 904, three extrusion rods 903 and an extrusion motor 905, wherein the side wall of the pressing seat 901 is provided with a semicircular groove, the pressing plate 902 is provided with a pressing groove symmetrical to the groove, the pressing plate 902 is detachably mounted on the pressing seat 901, the three extrusion rods 903 are vertically mounted on the rotating disc 904, the three extrusion rods 903 are mounted on the rotating disc 904 in an annular array mode, the three extrusion rods are all inserted into the pressing groove, the rotating disc 904 is driven by the extrusion motor 905 to rotate, and the three extrusion rods 903 sequentially roll along the surface contour of the pressing groove in the rotating process of the rotating disc 904.
To reduce the wear of the squeeze rod 903 on the connection hose 12, the squeeze rod 903 of the present invention is movably mounted to the turntable 904 by a bearing.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, 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 modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A process for producing a photocurable composition, characterized by comprising the steps of:
s1: preparing a photoinitiator;
s2: mixing a photoinitiator with a first compound to obtain a primary composition, and putting the primary composition into a first cavity of a storage container;
s3: and adding the second compound into a second cavity of the storage container, and injecting the second compound in the second cavity into the first cavity for mixing according to requirements during use.
2. The method of claim 1, wherein the storage container comprises: holding vessel (1), cover (2), be equipped with first cavity in holding vessel (1), install a plurality of second cavities in cover (2), the second cavity specifically is opening decurrent drum (3), and the second compound is poured into in a plurality of drums (3) and is capsulated through heat-seal sticker (4).
3. A storage device of photo-curable composition according to claim 2, wherein a sealing rubber sheet (5) is installed in the can lid (2), the sealing rubber sheet (5) is disposed on the lower side of the heat seal sticker (4), the can lid (2) is rotatably closed on the storage can (1), and the sealing rubber sheet (5) is press-sealed with the top of the sidewall of the storage can (1) in the process of rotating the can lid (2).
4. The method of claim 3, wherein the first compound comprises at least one of: dodecyl norbornyl-2-ene-5-carboxylate, 1,6 hexanediol di- (norbornyl-2-ene-5-carboxylate), trimethylolpropane tri- (norbornyl-2-ene-5-carboxylate).
5. The method of claim 4, wherein the second compound comprises 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.
6. The method of claim 5, wherein the photoinitiator is prepared by the steps of: under the condition of keeping out of the sun, a silane coupling agent containing isocyanate and 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone react in dehydrated ethyl acetate according to the molar ratio of 2:1-4:1, dibutyltin dilaurate DBTDL is used as a catalyst, the addition of the catalyst accounts for 0.05-0.3% of the mass fraction of reactants, and the reaction is carried out for 4-8 hours at the temperature of 60-80 ℃ to obtain the silicon-containing photoinitiator.
7. The method of claim 6, 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 25wt% to 70 wt%, based on the total amount of the entire cured composition; the dosage of the second compound is 25wt% -70 wt%.
8. The method of claim 7, wherein the photoinitiator is produced using an initiator preparation apparatus, the initiator preparation apparatus comprising: reation kettle (6), agitating unit, feed inlet (601) have been seted up on reation kettle (6), row material pipe (602) have been seted up to the bottom of reation kettle (6), arrange and install the valve on material pipe (602), agitating unit includes: agitator motor (701), bull stick (702), stirring fan blade (703), bull stick (702) is vertical to be inserted downwards in reation kettle (6), agitator motor (701) is installed the top of reation kettle (6), agitator motor (701) the pivot with bull stick (702) butt joint, stirring fan blade (703) are installed the bottom of bull stick (702).
9. The method for preparing a photocurable composition according to claim 8, wherein a thermostat control device is further disposed on the initiator preparation device, the thermostat control device comprising: heat conduction presss from both sides chamber (801), constant temperature water tank (804), heat conduction presss from both sides chamber (801) and sets up in the lateral wall of reation kettle (6), inlet tube (802), outlet pipe (803) are installed respectively to the upper and lower both ends of reation kettle (6) lateral wall, inlet tube (802), outlet pipe (803) all with heat conduction presss from both sides chamber (801) intercommunication, inlet tube (802), outlet pipe (803) are connected to respectively on constant temperature water tank (804).
10. The method of claim 9, further comprising an auxiliary mixing device on the initiator preparation device, wherein the auxiliary mixing device comprises: a circulation pipe having a plurality of groups and disposed around the outside of the reaction tank (6), the circulation pipe comprising: the device comprises an upper circulation pipe (10), a lower circulation pipe (11) and a connecting hose (12), wherein the upper circulation 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 circulation 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) and the two ends of the connecting hose (12) are respectively connected with the upper circulation pipe (10) and the lower circulation pipe (11), and an extrusion circulation device (9) is installed on the connecting 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 |
Applications Claiming Priority (1)
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