CN117304387B - Polymerizable near infrared dye, preparation method and polymerization equipment - Google Patents
Polymerizable near infrared dye, preparation method and polymerization equipment Download PDFInfo
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- CN117304387B CN117304387B CN202311250173.4A CN202311250173A CN117304387B CN 117304387 B CN117304387 B CN 117304387B CN 202311250173 A CN202311250173 A CN 202311250173A CN 117304387 B CN117304387 B CN 117304387B
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- polymerization
- near infrared
- fixedly connected
- polymerizable
- infrared dye
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- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000975 dye Substances 0.000 claims abstract description 62
- 238000002156 mixing Methods 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 18
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000003505 polymerization initiator Substances 0.000 claims abstract description 14
- 239000004094 surface-active agent Substances 0.000 claims abstract description 14
- 239000000178 monomer Substances 0.000 claims abstract description 13
- 239000007850 fluorescent dye Substances 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 229940094933 n-dodecane Drugs 0.000 claims abstract description 7
- YCJYNBLLJHFIIW-MBABXGOBSA-N validoxylamine A Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)C[C@@H]1N[C@@H]1[C@H](O)[C@@H](O)[C@H](O)C(CO)=C1 YCJYNBLLJHFIIW-MBABXGOBSA-N 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 55
- 238000007599 discharging Methods 0.000 claims description 27
- 238000003860 storage Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 17
- 238000001802 infusion Methods 0.000 claims description 5
- NWJTZFZQVYJIHU-UHFFFAOYSA-N ethenyl nonanoate Chemical compound CCCCCCCCC(=O)OC=C NWJTZFZQVYJIHU-UHFFFAOYSA-N 0.000 claims description 4
- 238000005192 partition Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 3
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 239000004020 conductor Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 19
- 229920000642 polymer Polymers 0.000 description 7
- 238000000799 fluorescence microscopy Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- -1 5-bromothiophene-2-yl Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012986 chain transfer agent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012632 fluorescent imaging Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- XSCHRSMBECNVNS-UHFFFAOYSA-N quinoxaline Chemical compound N1=CC=NC2=CC=CC=C21 XSCHRSMBECNVNS-UHFFFAOYSA-N 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- YPCMISLZCVOUJB-UHFFFAOYSA-N 4-cyano-4-methyl-5-phenyl-5-sulfanylidenepentanoic acid Chemical compound OC(=O)CCC(C)(C#N)C(=S)C1=CC=CC=C1 YPCMISLZCVOUJB-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 229920001109 fluorescent polymer Polymers 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003333 near-infrared imaging Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012712 reversible addition−fragmentation chain-transfer polymerization Methods 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F218/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F218/02—Esters of monocarboxylic acids
- C08F218/04—Vinyl esters
- C08F218/10—Vinyl esters of monocarboxylic acids containing three or more carbon atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F29/00—Mixers with rotating receptacles
- B01F29/60—Mixers with rotating receptacles rotating about a horizontal or inclined axis, e.g. drum mixers
- B01F29/64—Mixers with rotating receptacles rotating about a horizontal or inclined axis, e.g. drum mixers with stirring devices moving in relation to the receptacle, e.g. rotating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/83—Mixing plants specially adapted for mixing in combination with disintegrating operations
- B01F33/831—Devices with consecutive working receptacles, e.g. with two intermeshing tools in one of the receptacles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8361—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating
- B01F33/83612—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating by crushing or breaking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B59/00—Artificial dyes of unknown constitution
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
Abstract
The invention relates to the technical field of near infrared dye preparation, and particularly discloses a polymerizable near infrared dye, a preparation method and polymerization equipment, wherein the near infrared dye comprises the following raw materials: n-dodecane, vinyl pelargonate polymerizable monomer, polymerizable near infrared fluorescent dye, polymerizable photochromic compound, polymerization initiator and surfactant, wherein the polymerization equipment comprises a polymerization rack, a rotary shell is arranged on the polymerization rack, a crushing equipment is fixedly arranged on one side of the polymerization rack, and an internal rotation piece is arranged on the polymerization rack in a sliding manner; the preparation method comprises the steps of proportioning, primary mixing, secondary mixing, stirring uniformly and crushing cells. The near infrared dye adopts fewer raw materials, has low raw material biotoxicity, automatically mixes the near infrared dye sufficiently and uniformly, and the prepared superfine near infrared dye is prepared by using polymerization equipment to carry out polymerization mixing procedures on the near infrared dye, so that the preparation process is simplified, and the production cost is reduced.
Description
Technical Field
The invention relates to the technical field of near infrared dye preparation, in particular to a polymerizable near infrared dye, a preparation method and polymerization equipment.
Background
The near infrared dye is a near infrared fluorescent dye, can absorb energy in a near infrared spectrum, release fluorescence and has good dyeing effect.
In the prior art, the application number is as follows: 2017800794012 is disclosed by the name: a polymerizable near infrared dye, wherein the polymer is a luminescent polymer, the polymer is a near infrared fluorescent polymer, and has an emission wavelength of about 600-1000nm, about 650-900 nm, or about 650-850 nm. In some embodiments, the emission and absorption maxima of the monomer are unchanged when incorporated into the polymer.
In the prior art, the application number is as follows: 201911049507.5 is disclosed by the name: a near infrared two-region fluorescent imaging polymer and a preparation method and application thereof, wherein the preparation method comprises the steps of S1, reacting 4, 9-bis (5-bromothiophene-2-yl) -6, 7-bis (4- (hexyloxy) phenyl) - [1,2,5] thiadiazolo [3, quinoxaline with an electron donor to obtain an organic small molecule capable of emitting light in the near infrared two regions;
S2, reacting the organic small molecules which emit light in the near infrared two regions and are obtained in the step S1 with 4-cyano-4- (thiobenzoyl) pentanoic acid to obtain the near infrared two region fluorescence imaging molecules modified by the RAFT chain transfer agent;
S3, forming the near infrared two-region fluorescence imaging polymer through RAFT polymerization of the near infrared two-region fluorescence imaging molecule modified by the RAFT chain transfer agent and the water-soluble monomer obtained in the step S2.
However, in the prior art, the preparation methods of the near-infrared dye and the near-infrared two-region fluorescent imaging polymer are more complex in raw materials required by the actual preparation of the near-infrared dye, and the cost of the raw materials is higher, so that the production cost of the near-infrared dye is increased.
Disclosure of Invention
The invention aims to provide a polymerizable near infrared dye, a preparation method and polymerization equipment, so as to solve the problems in the prior art.
The aim of the invention can be achieved by the following technical scheme:
A polymerizable near infrared dye, the near infrared dye starting material comprising: n-dodecane, a vinyl pelargonate polymerizable monomer, a polymerizable near infrared fluorescent dye, a polymerizable photochromic compound, a polymerization initiator and a surfactant.
The polymerization initiator is one of azodiisoheptonitrile, dimethyl azodiisobutyrate and potassium persulfate.
The surfactant is one of dodecyl dimethyl benzyl ammonium chloride and octadecyl trimethyl ammonium chloride.
Further, the near infrared dye comprises the following raw materials in proportion: 0.15-0.25 part of n-dodecane, 1-2 parts of pelargonic acid vinyl ester polymerizable monomer, 0.005-0.01 part of polymerizable near infrared fluorescent dye, 0.04-0.06 part of polymerizable photochromic compound, 0.045-0.06 part of polymerization initiator and 0.1-0.2 part of surfactant.
The polymerization equipment is used for preparing the near infrared dye and comprises a polymerization rack, a rotary shell is arranged on the polymerization rack, a crushing equipment is fixedly arranged on one side of the polymerization rack, and an internal rotation piece is arranged on the polymerization rack in a sliding mode.
The polymerization rack is rotatably provided with a rotating shaft, conical surfaces are symmetrically and fixedly connected on the rotating shaft, and the conical surfaces are connected with the rotating shell to form a mixing bin for mixing near infrared dye raw materials.
Further, the conical surface is communicated with a feeding and discharging pipe, the feeding and discharging pipe is connected with an electromagnetic valve, the end part of the feeding and discharging pipe is provided with an extension pipe, and one side of the feeding and discharging pipe is fixedly connected with an air cylinder for connecting the movable extension pipe.
Round guide grooves are formed in the conical surface, side bars are fixedly connected in an array mode in the conical surface, telescopic rods which are horizontally arranged are fixedly connected to the side bars, springs are connected to the telescopic rods in a connecting mode, and spherical blocks used for mixing raw materials are fixedly connected to one ends of the telescopic rods.
Further, a first motor is fixedly connected to the polymerization rack, a second gear is fixedly connected to the output end of the first motor, a first gear is fixedly connected to the rotating shaft, the first gear is meshed below the second gear, a discharging hopper is fixedly arranged on the polymerization rack, and a discharging pipe for guiding materials to the crushing equipment is fixedly arranged on the polymerization rack.
Further, the rotary shell comprises two conical parts, the two conical parts are fixedly connected through a connecting sleeve, an annular rail is arranged on each conical part and matched with the circular guide groove, a connecting rod is fixedly connected to one end of each conical part, an annular gear is fixedly connected to the connecting rod, and the annular gear is meshed with the second outer ring of the gear.
The connecting sleeve is characterized in that a sliding block is fixedly connected to the inner wall array of the connecting sleeve, an arc-shaped rod for overturning raw materials is fixedly arranged at the end part of the conical piece, a partition plate which is in threaded arrangement and used for conducting material layering is fixedly connected to the inner wall of the conical piece, a communicating pipe is fixedly connected between the two conical pieces in an array mode, and the communicating pipe is used for communicating the two mixing bins to input and output raw materials.
Further, the rotating shaft is fixedly connected with a connecting shaft, an annular thread groove is formed in the connecting shaft, the inner rotating piece is arranged on the connecting shaft in a sliding mode, the inner rotating piece is provided with sliding grooves which are distributed in an array mode, the sliding grooves are matched with the sliding blocks, mounting rods are fixedly arranged at two ends of the inner rotating piece, and a stirring sheet is fixedly connected at the end portion of each mounting rod.
The stirring piece is vertically connected with the mounting rod, the internal rotation piece is provided with a through hole, the through hole is sleeved on the connecting shaft, the sliding shaft is fixedly arranged in the through hole, and the sliding shaft is in sliding connection with the annular thread groove.
Further, crushing apparatus includes the base, and fixed liquid storage pot that is equipped with on the base, and the transfusion hole has been seted up to one side of liquid storage pot, transfusion hole and row material pipe intercommunication, and liquid storage pot internal fixation is equipped with the riser of symmetric distribution, rotates between two risers and is equipped with crushing storehouse, and the both ends in crushing storehouse all rotate with the liquid storage pot to be connected, just lie in the liquid storage pot and fixedly be equipped with the heating module that is used for regulating temperature in the top in crushing storehouse.
The liquid inlet is formed in the upper portion of the crushing bin, a second motor for rotating the crushing bin is fixedly arranged at one end of the liquid storage tank, a liquid outlet for discharging near infrared dye is formed in the other end of the liquid storage tank, the output end of the second motor is connected with one end of the crushing bin, the liquid outlet penetrates through the other end of the crushing bin, and a liquid guide groove is communicated with the lower portion of the liquid outlet.
Further, two connecting holes have been seted up to the one end of base, and the one end of base is provided with the movable plate, and the fixed guide arm that is equipped with in one side of movable plate, and the fixed motor III that is equipped with of opposite side of movable plate, the output fixedly connected with lead screw of motor III, lead screw and a connecting hole cooperation, guide arm and another connecting hole sliding connection.
The utility model discloses a dye-crushing device, including movable plate, hollow rod, gasbag, hollow rod, fixed ultrasonic generator that is used for smashing the dye that is equipped with in one side of movable plate, ultrasonic generator's both sides are provided with two hollow poles that are used for the air feed, and hollow rod's one end and movable plate fixed connection, the other end are connected with the gasbag, also are provided with the gasbag on the hollow rod, gasbag and hollow rod inside intercommunication.
The movable plate is fixedly provided with a guide pillar, a U-shaped pipe is fixedly arranged below the guide pillar and communicated with the hollow rod, one side of the U-shaped pipe is fixedly provided with a rectangular frame, one end of the rectangular frame is communicated with the U-shaped pipe, the other end of the rectangular frame is provided with a groove-shaped plate, and one end of the groove-shaped plate is fixedly provided with a push block for extruding air in the U-shaped pipe.
The push block is connected in a sliding manner in the rectangular frame, racks are symmetrically and fixedly connected in the groove-shaped plate, an incomplete gear is arranged between the two racks, the incomplete gear is meshed with the racks, and a motor frame is fixedly arranged on one side of the moving plate.
And a motor IV is arranged on the motor frame, the output end of the motor IV is connected with the incomplete gear, and a connecting frame is fixedly arranged on the groove-shaped plate and is in sliding connection with the guide post.
A method of preparing a polymerization apparatus for a polymerizable near infrared dye, the method comprising the steps of:
s1, batching
According to the raw material proportion of the near infrared dye, each raw material is selected for standby.
S2, mixing once
Dodecane, vinyl pelargonate polymerizable monomer, polymerizable near infrared fluorescent dye, polymerizable photochromic compound and polymerization initiator are put into a rotary shell to be fully mixed into a first solution, and the next operation is carried out after the first solution and the second solution are fully mixed.
S3, secondary mixing
And adding a surfactant and clear water into the solution I mixed in the rotary shell to prepare a solution II.
S4, stirring uniformly
And (3) mixing and stirring the solution II for 20-25 minutes under the rotation mixing operation of the rotary shell to obtain the prefabricated liquid.
S5, crushing cells
And (3) sending the prefabricated liquid into a crushing device for ultrasonic crushing, and processing for 20 minutes to obtain the superfine polymerizable near infrared dye.
The invention has the beneficial effects that:
1. The near infrared dye provided by the invention adopts fewer raw materials, has low raw material biotoxicity, simple raw material collection, low raw material cost, and is beneficial to large-scale production and use in actual production, and the dye has uniform imaging color and good application prospect in the existing near infrared imaging field;
2. according to the near infrared dye polymerization equipment, the near infrared dye is fully and uniformly mixed automatically, so that the near infrared dye raw materials are thoroughly reacted, the prepared superfine near infrared dye is uniform in imaging effect, the dye material is stable in structure and thorough in polymerization reaction, and the preparation efficiency of the dye is improved;
3. According to the preparation method of the near infrared dye, the polymerization equipment is utilized to carry out the polymerization mixing process on the near infrared dye, so that the preparation process is simplified, the manual operation process is reduced, the production cost is reduced, and the near infrared dye with reliable quality is prepared.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a schematic view of the structure of a polymerization apparatus according to the present invention;
FIG. 2 is a cross-sectional view of the polymerization apparatus of the present invention;
FIG. 3 is a schematic view of the structure of a polymeric scaffold of the present invention;
FIG. 4 is a schematic view showing a part of the construction of a polymerization apparatus according to the present invention;
FIG. 5 is a schematic view of the rotary housing structure of the present invention;
FIG. 6 is a cross-sectional view of a swivel housing of the invention;
FIG. 7 is a schematic view of the structure of the inner rotary member of the present invention;
FIG. 8 is a schematic view of the structure of the pulverizing apparatus of the present invention;
FIG. 9 is a cross-sectional view of the comminution apparatus of the present invention;
Fig. 10 is a schematic view of the structure of the pulverizing apparatus of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
A polymerizable near infrared dye, the near infrared dye starting material comprising: n-dodecane, a vinyl pelargonate polymerizable monomer, a polymerizable near infrared fluorescent dye, a polymerizable photochromic compound, a polymerization initiator and a surfactant.
The polymerization initiator is one of azodiisoheptonitrile, dimethyl azodiisobutyrate and potassium persulfate.
The surfactant is one of dodecyl dimethyl benzyl ammonium chloride and octadecyl trimethyl ammonium chloride.
The near infrared dye comprises the following raw materials in proportion: 0.15-0.25 part of n-dodecane, 1-2 parts of pelargonic acid vinyl ester polymerizable monomer, 0.005-0.01 part of polymerizable near infrared fluorescent dye, 0.04-0.06 part of polymerizable photochromic compound, 0.045-0.06 part of polymerization initiator and 0.1-0.2 part of surfactant.
The polymerization equipment is used for preparing the near infrared dye by adopting a polymerization method, and is applied to the polymerization method of the near infrared dye, so that the preparation efficiency of the near infrared dye is improved.
As shown in fig. 1, the polymerization equipment comprises a polymerization rack 1, a rotary housing 3 is arranged on the polymerization rack 1, a crushing equipment 2 is fixedly arranged on one side of the polymerization rack 1, an inner rotary member 4 is arranged in the rotary housing 3, and the inner rotary member 4 is arranged on the polymerization rack 1 in a sliding manner.
As shown in fig. 1-4, a first motor 18 is fixedly arranged on the polymerization rack 1, an output end of the first motor 18 is fixedly connected with a second gear 17, a rotating shaft 11 is rotatably arranged on the polymerization rack 1, a connecting shaft 40 is fixedly arranged on the rotating shaft 11, an annular thread groove 401 is formed in the connecting shaft 40, and the annular thread groove 401 forms an annular groove structure on the surface of the connecting shaft 40.
And the rotary shaft 11 is fixedly provided with tapered surfaces 12 which are symmetrically distributed, the inner wall of the tapered surfaces 12 is fixedly provided with side bars 13 which are distributed in an array, the side bars 13 are used for stirring and mixing raw materials between the rotary shell 3 and the tapered surfaces 12 in the process of rotating the tapered surfaces 12, the uniformity of mixing is improved, the side bars 13 are fixedly provided with telescopic rods 15 which are horizontally arranged, the telescopic rods 15 are internally provided with springs, and the springs are not shown in the figure.
The conical surface 12 is communicated with a feeding and discharging pipe 121, the feeding and discharging pipe 121 is connected with an electromagnetic valve 122, the end part of the feeding and discharging pipe 121 is sleeved with an extension pipe 124, the side wall of the feeding and discharging pipe 121 is fixedly provided with an air cylinder 123, the output end of the air cylinder 123 is fixedly connected with the extension pipe 124, the extension pipe 124 is moved through the air cylinder 123, and the conical surface 12 is provided with a circular guide groove 14.
One end of the telescopic rod 15 is fixedly provided with a spherical block 151, one end of the spring is fixedly connected with the spherical block 151, the other end of the spring is fixedly connected with the side bar 13, the spherical block 151 is contacted with materials to enable the materials to move and mix in the stirring process, the materials react with the spherical block 151 to compress the spring, and when the pressure is released by the spring, the spherical block 151 can be made to extrude and push the materials.
The rotary shaft 11 is fixedly provided with a first gear 16, the first gear 16 is positioned below a second gear 17, the first gear 16 is meshed with the second gear 17, the polymerization rack 1 is fixedly provided with a discharging hopper 19 for intensively discharging symmetrically-taken raw materials, and after the discharging hopper 19 is communicated with the extension pipe 124, raw materials in the discharging hopper 19 can be input into the extension pipe 124.
A discharge pipe 10 is fixedly arranged on the polymerization rack 1, when the port of the extension pipe 124 is downward, the extension pipe 124 is controlled to move downwards to be communicated with the discharge pipe 10 through an air cylinder 123, and the solution in the rotary shell 3 can be discharged into the discharge pipe 10.
As shown in fig. 5 and 6, the rotary housing 3 includes two conical members 31, a connecting sleeve 37 is disposed between the two conical members 31, the connecting sleeve 37 is fixedly connected with the small diameter end portions of the two conical members 31, the conical members 31 are provided with annular rails 33, and the annular rails 33 are slidably matched with the circular guide grooves 14, so that the conical members 31 are rotatably mounted on the conical surfaces 12.
And one end of one conical piece 31 is fixedly provided with a connecting rod 311, the connecting rod 311 is fixedly provided with an annular gear 34, the annular gear 34 is sleeved on the outer side of the first gear 16, the second gear 17 is meshed with the annular gear 34, and the first gear 16 and the annular gear 34 are simultaneously driven to rotate through the second gear 17.
The sliding blocks 38 distributed in an array are fixedly arranged on the inner wall of the connecting sleeve 37, the end part of the conical part 31 is located on the inner side of the annular rail 33, the arc-shaped rods 35 are fixedly arranged on the inner side of the annular rail 33 and are bent towards the axis of the conical part 31, the arc-shaped rods 35 are used for turning materials in the rotating process of the conical part 31, the partition plates 36 are fixedly arranged on the inner wall of the conical part 31 in a threaded arrangement, part of the materials can move along threads among the partition plates 36 in the rotating process of the conical part 31, and the materials are conveyed and moved, so that the material mixing is facilitated.
The side of the connecting sleeve 37 is fixedly provided with communicating pipes 32 distributed in an array, two ends of the communicating pipes 32 are fixedly connected with two conical parts 31 respectively, and when the conical parts 31 and the conical surface 12 form a mixing area, the two mixing areas are communicated through the communicating pipes 32 at the moment, and the two mixing areas are used for conveying and exchanging materials and can be used for entering and discharging the materials.
As shown in fig. 7, the inner rotary member 4 has a circular structure, the inner rotary member 4 is slidably disposed on the connecting shaft 40 and is disposed in the connecting sleeve 37, the inner rotary member 4 is provided with slide grooves 43 distributed in an array, the slide grooves 43 are slidably connected with the slide blocks 38, two ends of the inner rotary member 4 are fixedly provided with mounting rods 44, ends of the mounting rods 44 are fixedly provided with stirring sheets 45, and the stirring sheets 45 are vertically disposed with the mounting rods 44.
The inner rotary member 4 is provided with a through hole 41, the through hole 41 is sleeved on the connecting shaft 40, a sliding shaft 42 is fixedly arranged in the through hole 41, one end of the sliding shaft 42 extends into the annular thread groove 401, when the rotary shaft 11 rotates, the sliding shaft 42 is driven to slide in the horizontal direction through the annular thread groove 401 on the connecting shaft 40, and then the inner rotary member 4 can also rotate under the driving of the connecting sleeve 37, so that a stirring sheet 45 at the end part of the inner rotary member 4 rotates and moves to stir and mix materials in the inner rotary member.
As shown in fig. 8 to 10, the crushing apparatus 2 includes a base 21, the base 21 is fixed on one side of the polymerization frame 1, a liquid storage tank 22 is fixedly arranged on the base 21, an infusion hole 221 is formed on one side of the liquid storage tank 22, and the infusion hole 221 is communicated with the discharge pipe 10 and is used for discharging the mixed solution from the discharge pipe 10 into the infusion hole 221 and then into the liquid storage tank 22.
The fixed riser 222 that is equipped with symmetric distribution in liquid storage pot 22, rotation is equipped with crushing storehouse 23 between two risers 222, and crushing storehouse 23's both ends all rotate with liquid storage pot 22 and are connected, and the fixed heating module 24 that is equipped with in liquid storage pot 22 and be located crushing storehouse 23's top for regulate and control crushing storehouse 23 internal temperature, and recess 223 has been seted up to riser 222's lower extreme.
The liquid inlet 230 is formed in the upper portion of the crushing bin 23, the motor II 20 is fixedly arranged at one end of the liquid storage tank 22, the liquid outlet 231 is formed in the other end of the liquid storage tank 22, the output end of the motor II 20 is fixedly connected with one end of the crushing bin 23 to control the crushing bin 23 to rotate, the liquid outlet 231 penetrates through the other end of the crushing bin 23 and is used for discharging solution in the crushing bin 23, the liquid guide groove 232 is formed in the lower portion of the liquid outlet 231, and the solution at the liquid outlet 231 can be discharged and collected from the liquid guide groove 232 to obtain the required near infrared dye.
And two connecting holes are formed in one end of the base 21, the connecting holes are not shown in the drawing, a movable plate 24 is arranged at one end of the base 21, a guide rod 242 is fixedly arranged on one side of the movable plate 24, a motor III 240 is fixedly arranged on the other side of the movable plate 24, an output end of the motor III 240 penetrates through the movable plate 24 and is fixedly connected with a lead screw 241, the lead screw 241 is in threaded connection with one connecting hole, and the guide rod 242 is in sliding connection with the other connecting hole.
When the motor III 240 drives the screw rod 241 to rotate, the screw rod 241 can be in threaded connection with a connecting hole on the base 21 to drive the movable plate 24 to be close to or far away from the base 21, and an ultrasonic generator 25 is fixedly arranged on one side of the movable plate 24, and the ultrasonic generator 25 is connected with an ultrasonic cell breaker to control the ultrasonic generator 25 to emit ultrasonic waves.
Two sides of the ultrasonic generator 25 are provided with two hollow rods 26, one end of each hollow rod 26 is fixedly connected with the movable plate 24, the other end of each hollow rod 26 is connected with an air bag 27, the hollow rods 26 are provided with through grooves, the air bags 27 are also arranged in the through grooves, the air bags 27 are communicated with the inside of the hollow rods 26, and air is supplied to the air bags 27 through the hollow rods 26.
The guide post 244 is fixedly arranged on the moving plate 24, a U-shaped pipe 260 is fixedly arranged below the guide post 244, the U-shaped pipe 260 is communicated with the hollow rod 26 and used for controlling gas flow in the hollow rod 26, a rectangular frame 261 is fixedly arranged on one side of the U-shaped pipe 260, one end of the rectangular frame 261 is communicated with the U-shaped pipe 260, a groove-shaped plate 27 is arranged at the other end of the rectangular frame 261, and a push block 29 is fixedly arranged at one end of the groove-shaped plate 27.
The pushing block 29 is slidably connected in the rectangular frame 261, symmetrically distributed racks 272 are fixedly arranged in the groove-shaped plate 27, an incomplete gear 28 is arranged between the two racks 272, the incomplete gear 28 is meshed with the racks 272, a motor frame 243 is fixedly arranged on one side of the moving plate 24, a motor four 280 is fixedly arranged on the motor frame 243, and the output end of the motor four 280 is fixedly connected to the side face of the incomplete gear 28 so as to drive the incomplete gear 28 to rotate.
The connecting frame 271 is fixedly arranged on the groove-shaped plate 27, the connecting frame 271 is in sliding connection with the guide post 244 and is used for guiding the movement of the groove-shaped plate 27, the push block 29 moves into the U-shaped pipe 260, gas in the U-shaped pipe 260 is extruded to be discharged into the hollow rod 26, and after the air bag 27 is Zhang Qi, the solution in the crushing bin 23 can be pressurized, so that the solution moves, and the solution can be conveniently and fully crushed by the ultrasonic sounder 5.
Working principle:
through selecting raw materials according to the raw material proportion of the near infrared dye, rotating the rotating shaft 11 until the extension pipe 124 is communicated with the discharging hopper 19, then mixing dodecane, a vinyl pelargonate polymerizable monomer, a polymerizable near infrared fluorescent dye, a polymerizable photochromic compound and a polymerization initiator into a solution I, and fully mixing the solution I in an energy-saving way by utilizing a mixing space formed by the conical surface 12 and the rotating shell 3 after rotating the rotating shaft 11;
Then adding the surfactant and the clear water into a mixing space by the same method, performing secondary mixing operation, and mixing and stirring for 20-25 minutes to prepare a prefabricated liquid;
Rotating the rotating shaft 11 until the extension pipe 124 is communicated with the discharge pipe 10 downwards, discharging the prefabricated liquid into the liquid storage tank 22, then rotating the crushing bin 23 until the liquid inlet 230 is flush with the groove 223, enabling the liquid in the liquid storage tank 22 to flow into the crushing bin 23 from the liquid inlet 230, starting the ultrasonic generator 25 to generate ultrasonic waves to crush the near infrared dye, and intermittently enabling the Zhang Qi air bags 27 to mix the solution in the crushing process.
After the pulverization treatment for 20 minutes, the movable plate 24 is moved in a translation manner, the liquid outlet 231 is opened, the liquid outlet 231 is communicated with the liquid guide groove 232, and the ultra-fine polymerizable near infrared dye is discharged.
A method for preparing a polymerizable near infrared dye, comprising the steps of:
s1, batching
According to the raw material proportion of the near infrared dye, each raw material is selected for standby.
S2, mixing once
0.2 Part of dodecane, 1.5 parts of a vinyl nonanoate polymerizable monomer, 0.0075 parts of a polymerizable near infrared fluorescent dye, 0.05 parts of a polymerizable photochromic compound and 0.05 parts of a polymerization initiator are put into a rotary shell 3, and mixed thoroughly to form a first solution, and the mixture is subjected to the next operation.
S3, secondary mixing
To the solution one mixed in the rotary housing 3, 0.15 parts of a surfactant and clean water were added, followed by preparing a solution two.
S4, stirring uniformly
And mixing and stirring the solution II for 20 to 25 minutes under the rotation and mixing operation of the rotary shell 3 to prepare the prefabricated liquid.
S5, crushing cells
The prefabricated liquid is sent into a crushing device 2 for ultrasonic crushing, and after 20 minutes of treatment, the superfine polymerizable near infrared dye is obtained.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims.
Claims (5)
1. A polymerization apparatus for a polymerizable near infrared dye, wherein the near infrared dye raw material comprises: n-dodecane, vinyl pelargonate polymerizable monomer, polymerizable near infrared fluorescent dye, polymerizable photochromic compound, polymerization initiator and surfactant;
The polymerization initiator is one of azodiisoheptonitrile, dimethyl azodiisobutyrate and potassium persulfate;
the surfactant is one of dodecyl dimethyl benzyl ammonium chloride and octadecyl trimethyl ammonium chloride;
the near infrared dye comprises the following raw materials in proportion: 0.15-0.25 part of n-dodecane, 1-2 parts of pelargonic acid vinyl ester polymerizable monomer, 0.005-0.01 part of polymerizable near infrared fluorescent dye, 0.04-0.06 part of polymerizable photochromic compound, 0.045-0.06 part of polymerization initiator and 0.1-0.2 part of surfactant;
the polymerization equipment comprises a polymerization rack (1), a rotary shell (3) is arranged on the polymerization rack (1), a crushing equipment (2) is fixedly arranged on one side of the polymerization rack (1), and an internal rotation piece (4) is arranged on the polymerization rack (1) in a sliding manner;
A rotating shaft (11) is rotationally arranged on the polymerization rack (1), conical surfaces (12) are symmetrically and fixedly connected on the rotating shaft (11), and the conical surfaces (12) are connected with the rotating shell (3) to form a mixing bin for mixing near infrared dye raw materials;
A motor I (18) is fixedly connected to the polymerization rack (1), a gear II (17) is fixedly connected to the output end of the motor I (18), a gear I (16) is fixedly connected to the rotary shaft (11), the gear I (16) is meshed below the gear II (17), a discharging hopper (19) is fixedly arranged on the polymerization rack (1), and a discharging pipe (10) for guiding materials to the crushing equipment (2) is fixedly arranged on the polymerization rack (1);
The rotary shell (3) comprises two conical parts (31), the two conical parts (31) are fixedly connected through a connecting sleeve (37), an annular rail (33) is arranged on the conical part (31), the annular rail (33) is matched with the circular guide groove (14), a connecting rod (311) is fixedly connected to one end of the conical part (31), an inner gear ring (34) is fixedly connected to the connecting rod (311), and the inner gear ring (34) is meshed with the outer ring of the gear II (17);
The inner wall array of the connecting sleeve (37) is fixedly connected with a sliding block (38), the end part of the conical part (31) is fixedly provided with an arc-shaped rod (35) for turning over raw materials, the inner wall of the conical part (31) is fixedly connected with a partition board (36) which is in threaded arrangement and is used for conducting material layering and guiding, a communicating pipe (32) is fixedly connected between the two conical parts (31) in an array manner, and the communicating pipe (32) is used for communicating the two mixing bins to input and output raw materials;
A connecting shaft (40) is fixedly connected to the rotating shaft (11), an annular thread groove (401) is formed in the connecting shaft (40), an inner rotary piece (4) is arranged on the connecting shaft (40) in a sliding mode, sliding grooves (43) distributed in an array mode are formed in the inner rotary piece (4), the sliding grooves (43) are matched with the sliding blocks (38), mounting rods (44) are fixedly arranged at two ends of the inner rotary piece (4), and a stirring sheet (45) is fixedly connected to the end portions of the mounting rods (44);
The stirring piece (45) is vertically connected with the mounting rod (44), the inner rotary piece (4) is provided with a through hole (41), the through hole (41) is sleeved on the connecting shaft (40), the sliding shaft (42) is fixedly arranged in the through hole (41), and the sliding shaft (42) is in sliding connection with the annular thread groove (401).
2. The polymerization equipment of the polymerizable near infrared dye according to claim 1, wherein the conical surface (12) is communicated with a feeding and discharging pipe (121), the feeding and discharging pipe (121) is connected with an electromagnetic valve (122), the end part of the feeding and discharging pipe (121) is provided with an extension pipe (124), and one side of the feeding and discharging pipe (121) is fixedly connected with a cylinder (123) for connecting the movable extension pipe (124);
Circular guide grooves (14) are formed in the conical surface (12), side bars (13) are fixedly connected in the conical surface (12) in an array mode, telescopic rods (15) which are horizontally arranged are fixedly connected on the side bars (13), springs are connected in the telescopic rods (15), and spherical blocks (151) used for mixing raw materials are fixedly connected at one ends of the telescopic rods (15).
3. The polymerization equipment of the polymerizable near infrared dye according to claim 2, wherein the crushing equipment (2) comprises a base (21), a liquid storage tank (22) is fixedly arranged on the base (21), one side of the liquid storage tank (22) is provided with an infusion hole (221), the infusion hole (221) is communicated with the discharge pipe (10), vertical plates (222) which are symmetrically distributed are fixedly arranged in the liquid storage tank (22), a crushing bin (23) is rotatably arranged between the two vertical plates (222), two ends of the crushing bin (23) are rotatably connected with the liquid storage tank (22), and a heating module (24) for adjusting temperature is fixedly arranged in the liquid storage tank (22) and above the crushing bin (23);
The utility model discloses a liquid guide tank, including smashing storehouse (23), liquid storage tank (22), feed liquor mouth (230) has been seted up to the top of smashing storehouse (23), and the one end of liquid storage tank (22) is fixed to be equipped with motor two (20) that are used for rotating smashing storehouse (23), and liquid outlet (231) that are used for discharging near infrared dyestuff have been seted up to the other end, and the output of motor two (20) links to each other with the one end of smashing storehouse (23), and liquid outlet (231) runs through the other end of smashing storehouse (23), and the below intercommunication of liquid outlet (231) has liquid guide tank (232).
4. A polymerizable near-infrared dye polymerization apparatus according to claim 3, characterized in that two connecting holes are provided at one end of the base (21), a moving plate (24) is provided at one end of the base (21), a guide rod (242) is fixedly provided at one side of the moving plate (24), a motor III (240) is fixedly provided at the other side of the moving plate (24), a lead screw (241) is fixedly connected to the output end of the motor III (240), the lead screw (241) is matched with one connecting hole, and the guide rod (242) is slidingly connected with the other connecting hole;
An ultrasonic generator (25) for smashing dyes is fixedly arranged on one side of the movable plate (24), two hollow rods (26) for supplying air are arranged on two sides of the ultrasonic generator (25), one end of each hollow rod (26) is fixedly connected with the movable plate (24), the other end of each hollow rod is connected with an air bag (27), an air bag (27) is also arranged on each hollow rod (26), and the air bags (27) are communicated with the inside of each hollow rod (26);
The movable plate (24) is fixedly provided with a guide post (244), a U-shaped pipe (260) is fixedly arranged below the guide post (244), the U-shaped pipe (260) is communicated with the hollow rod (26), one side of the U-shaped pipe (260) is fixedly provided with a rectangular frame (261), one end of the rectangular frame (261) is communicated with the U-shaped pipe (260), the other end of the rectangular frame is provided with a groove-shaped plate (27), and one end of the groove-shaped plate (27) is fixedly provided with a push block (29) for extruding air in the U-shaped pipe (260);
The pushing block (29) is slidably connected in the rectangular frame (261), racks (272) are symmetrically and fixedly connected in the groove-shaped plate (27), an incomplete gear (28) is arranged between the two racks (272), the incomplete gear (28) is meshed with the racks (272), and a motor frame (243) is fixedly arranged on one side of the moving plate (24);
And a motor IV (280) is arranged on the motor frame (243), the output end of the motor IV (280) is connected with the incomplete gear (28), a connecting frame (271) is fixedly arranged on the groove-shaped plate (27), and the connecting frame (271) is in sliding connection with the guide post (244).
5. A method for preparing a polymerizable near infrared dye using the polymerization apparatus according to any one of claims 2 to 4, characterized in that the preparation method comprises the steps of:
s1, batching
Selecting all raw materials for standby according to the raw material proportion of the near infrared dye;
S2, mixing once
Adding dodecane, a vinyl pelargonate polymerizable monomer, a polymerizable near infrared fluorescent dye, a polymerizable photochromic compound and a polymerization initiator into a rotary shell (3), fully mixing to form a first solution, and performing the next operation after fully mixing;
S3, secondary mixing
Adding surfactant and clear water into the solution I mixed in the rotary shell (3) to prepare solution II;
S4, stirring uniformly
Under the rotation mixing operation of the rotary shell (3), mixing and stirring the solution II for 20-25 minutes to prepare a prefabricated liquid;
S5, crushing cells
And (3) conveying the prefabricated liquid into a crushing device (2) for ultrasonic crushing, and treating for 20 minutes to obtain the superfine polymerizable near infrared dye.
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|---|---|---|---|
| CN202311250173.4A CN117304387B (en) | 2023-09-25 | 2023-09-25 | Polymerizable near infrared dye, preparation method and polymerization equipment |
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| CN202311250173.4A CN117304387B (en) | 2023-09-25 | 2023-09-25 | Polymerizable near infrared dye, preparation method and polymerization equipment |
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| CN117304387B true CN117304387B (en) | 2024-04-23 |
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| CN212309501U (en) * | 2020-03-24 | 2021-01-08 | 李光明 | Chemical raw material stirring device |
| CN218138904U (en) * | 2022-05-24 | 2022-12-27 | 漯河市锦程建材有限公司 | Concrete mixing equipment |
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| GB1268625A (en) * | 1968-06-21 | 1972-03-29 | Gardners Of Gloucester Ltd | Improvements in or relating to double cone mixing machines |
| CN101626822A (en) * | 2006-12-28 | 2010-01-13 | 超声波系统有限公司 | Method and device for treating a liquid |
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| CN117304387A (en) | 2023-12-29 |
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