CN113372457A - Production process of high-purity hydroxypropyl methylcellulose phthalate for photoresist - Google Patents
Production process of high-purity hydroxypropyl methylcellulose phthalate for photoresist Download PDFInfo
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- CN113372457A CN113372457A CN202110576638.XA CN202110576638A CN113372457A CN 113372457 A CN113372457 A CN 113372457A CN 202110576638 A CN202110576638 A CN 202110576638A CN 113372457 A CN113372457 A CN 113372457A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B13/00—Preparation of cellulose ether-esters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B15/00—Preventing escape of dirt or fumes from the area where they are produced; Collecting or removing dirt or fumes from that area
- B08B15/02—Preventing escape of dirt or fumes from the area where they are produced; Collecting or removing dirt or fumes from that area using chambers or hoods covering the area
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B5/00—Cleaning by methods involving the use of air flow or gas flow
- B08B5/04—Cleaning by suction, with or without auxiliary action
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
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- Organic Chemistry (AREA)
- Crushing And Pulverization Processes (AREA)
Abstract
The invention discloses a production process of high-purity hypromellose phthalate for photoresist, which comprises the following steps: a. heating and homogenizing cellulose ether, acetic anhydride, glacial acetic acid, phthalic anhydride and succinic anhydride which are used as raw materials; b. adding sodium acetate as a raw material in the process of adding a proper amount of catalyst to obtain a mixture; c. after the mixture was heated to 60 to 85 ℃, the reaction was thermostatted. According to the invention, dust generated in the step of crushing can be absorbed, dust overflow is reduced, and the influence of dust on workers is reduced.
Description
Technical Field
The invention relates to the technical field of chemical preparation, in particular to a production process of high-purity hydroxypropyl methylcellulose phthalate for photoresist.
Background
Hydroxypropyl methylcellulose phthalate is white odorless and tasteless particles, is an enteric coating material with excellent performance, can ensure that a medicament which plays a role in an intestinal tract or is optimally absorbed in a small intestine is positioned and released in the intestine, and avoids stomach discomfort or nausea caused by an irritant medicament, so that the enteric coating plays an important role in fully playing a curative effect on the medicament and ensuring the stability of the medicament.
In the traditional process for preparing the hydroxypropyl methylcellulose phthalate, the hydroxypropyl methylcellulose phthalate needs to be crushed, and a large amount of dust is generated in the crushing process, so that the production environment is polluted, and the harm is caused to the bodies of workers.
Disclosure of Invention
The invention aims to: in order to solve the problems, the production process of the high-purity hypromellose phthalate for the photoresist is provided.
In order to achieve the purpose, the invention adopts the following technical scheme:
the production process of the high-purity hydroxypropyl methylcellulose phthalate for the photoresist comprises the following steps:
a. heating and homogenizing cellulose ether, acetic anhydride, glacial acetic acid, phthalic anhydride and succinic anhydride which are used as raw materials;
b. adding sodium acetate as a raw material in the process of adding a proper amount of catalyst to obtain a mixture;
c. heating the mixture to 60-85 ℃, and then carrying out a constant temperature reaction;
d. adding a proper amount of hydrochloric acid in the process of constant temperature reaction;
e. cooling to 40-66 deg.C, adding hot water for dilution, and precipitating;
f. washing for multiple times;
g. performing centrifugal dehydration;
h. drying and crushing;
the crushing equipment related in the step h comprises a crushing box, a crushing mechanism and a sieve plate, wherein the crushing mechanism and the sieve plate are arranged in the crushing box, a shell is fixed on the crushing box, a dust hood is arranged at the bottom of the shell, a turbine blade is connected into the shell through a transmission shaft, a connecting cover communicated with the shell through a communicating pipe is fixed outside the crushing box, a collecting cover is arranged at the bottom of the connecting cover through a connecting piece, and a filtering piece is fixed at the bottom of the collecting cover;
a connecting frame is fixed at the bottom of the collecting cover, a moving rod penetrates through the connecting frame, two ends of the moving rod are respectively fixed with a top block and a flange, and a first spring is arranged between the flange and the connecting frame;
a support is fixed at the bottom of the sieve plate, a top rod penetrates through the support, a rubber block and a movable frame are fixed at two ends of the top rod respectively, and a through groove is formed in the movable frame;
and the crushing box is provided with a driving piece which simultaneously drives the turbine blades to rotate and the movable rod and the ejector rod to move in the vertical direction.
As a further description of the above technical solution:
the catalyst is at least one of alkali metal carboxylate.
As a further description of the above technical solution:
the alkali metal carboxylate is at least one of lithium acetate, sodium acetate, potassium acetate, sodium propionate and potassium propionate.
As a further description of the above technical solution:
the temperature of the temperature-rising homogenization involved in the step a is 50-70 ℃.
As a further description of the above technical solution:
the driving member includes:
the output end of the motor is provided with a first transmission shaft, the first transmission shaft penetrates through the shell and is internally provided with a second bevel gear, and a fourth transmission shaft is sleeved with a first bevel gear meshed with the second bevel gear;
install transmission shaft two and transmission shaft three on broken case, the output and the transmission shaft two of motor are connected through driving belt one, connect through driving belt two between transmission shaft two and the transmission shaft three, the cam with flange matched with has been cup jointed on the transmission shaft two, install the actuating arm on the transmission shaft three, be fixed with the rotation pin that runs through logical groove on the actuating arm.
As a further description of the above technical solution:
the connecting piece is including rotating the rotor arm on the connecting cover, the last shaping of rotor arm has the stopper, collect and cover and be fixed with the lug and have the spacing groove with stopper looks adaptation on the lug, it has the locating hole to collect to cover, be equipped with on the rotor arm and act on the locating hole, carry out the setting element of location to the rotor arm.
As a further description of the above technical solution:
the positioning piece comprises a pull rod penetrating through the rotating arm, and a second spring and a positioning pin matched with the positioning hole are arranged on the pull rod.
As a further description of the above technical solution:
the filter piece comprises an annular frame, a fixed block is fixed inside the annular frame through a connecting rod, and an annular filter screen is arranged between the fixed block and the annular frame.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
according to the invention, dust generated in the step of crushing can be absorbed, dust overflow is reduced, and the influence of dust on workers is reduced.
Drawings
Fig. 1 shows a schematic structural view of a crushing plant provided according to an embodiment of the invention;
FIG. 2 is a schematic side view of a stent provided according to an embodiment of the present invention;
FIG. 3 is a schematic diagram illustrating a partially enlarged structure of the part A in FIG. 1 according to an embodiment of the present invention;
FIG. 4 is a schematic diagram illustrating a partial enlarged structure of B in FIG. 1 according to an embodiment of the present invention;
FIG. 5 is a schematic diagram of an internal structure of a collection hood provided according to an embodiment of the invention;
fig. 6 shows a schematic view of the internal structure of a filter element provided according to an embodiment of the invention.
Illustration of the drawings:
1. a crushing box; 2. a crushing mechanism; 3. a communicating pipe; 4. a first transmission shaft; 5. a motor; 6. a housing; 7. a first transmission belt; 8. a second transmission shaft; 9. a connecting cover; 10. a cam; 11. a second transmission belt; 12. a sieve plate; 13. moving the frame; 14. a support; 15. a third transmission shaft; 16. positioning pins; 17. a rubber block; 18. a top rod; 19. a rotation pin; 20. a drive arm; 21. a fourth transmission shaft; 22. a first bevel gear; 23. a second bevel gear; 24. a dust hood; 25. a turbine blade; 26. a rotating arm; 27. a pull rod; 28. a collection hood; 29. a connecting frame; 30. a bump; 31. a top block; 32. a flange; 33. a first spring; 34. a limiting groove; 35. a filter member; 36. a limiting block; 37. positioning holes; 38. a through groove; 39. a travel bar; 40. a second spring; 3501. an annular frame; 3502. a connecting rod; 3503. a fixed block; 3504. and (5) filtering by using a filter screen.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-6, the present invention provides a technical solution: the production process of the high-purity hydroxypropyl methylcellulose phthalate for the photoresist comprises the following steps:
a. heating and homogenizing cellulose ether, acetic anhydride, glacial acetic acid, phthalic anhydride and succinic anhydride which are used as raw materials at the temperature of 50-70 ℃;
b. adding a raw material of sodium acetate in the process of adding a proper amount of catalyst to obtain a mixture, wherein the catalyst is at least one of alkali metal carboxylates, and the alkali metal carboxylate is at least one of lithium acetate, sodium acetate, potassium acetate, sodium propionate and potassium propionate;
c. heating the mixture to 60-85 ℃, and then carrying out a constant temperature reaction;
d. adding a proper amount of hydrochloric acid in the process of constant temperature reaction;
e. cooling to 40-66 deg.C, adding hot water for dilution, and precipitating;
f. washing for multiple times;
g. performing centrifugal dehydration;
h. drying and crushing;
the crushing equipment related in the step h comprises a crushing box 1, a crushing mechanism 2 and a sieve plate 12, wherein the crushing mechanism 2 and the sieve plate 12 are arranged inside the crushing box 1, the sieve plate 12 is arranged in an arc shape, the sieve plate 12 is used for screening crushed materials to prevent the materials which are not crushed from being discharged outwards from the crushing box 1, a shell 6 is fixed on the crushing box 1, a dust hood 24 is installed at the bottom of the shell 6, a turbine blade 25 is connected into the shell 6 through a transmission shaft IV 21, the transmission shaft IV 21 is vertically distributed, the transmission shaft IV 21 is rotatably connected with the shell 6 through a bearing, the transmission shaft IV 21 can drive the turbine blade 25 to rotate, a connecting cover 9 communicated with the shell 6 through a communicating pipe 3 is fixed outside the crushing box 1, a collecting cover 28 is installed at the bottom of the connecting cover 9 through a connecting piece, and a filtering piece 35 is fixed at the bottom of the collecting cover 28;
a connecting frame 29 is fixed at the bottom of the collecting cover 28, a moving rod 39 penetrates through the connecting frame 29, the moving rod 39 is in sliding fit with the connecting frame 29, a top block 31 and a flange 32 are respectively fixed at two ends of the moving rod 39, the top block 31 is made of rubber, a first spring 33 is arranged between the flange 32 and the connecting frame 29, the first spring 33 is sleeved outside the moving rod 39, and the first spring 33 gives the flange 32 vertical downward elastic force;
a bracket 14 is fixed at the bottom of the sieve plate 12, the bracket 14 is arranged in a U shape, a top rod 18 penetrates through the bracket 14, the top rod 18 is in sliding fit with the bracket 14, two ends of the top rod 18 are respectively fixed with a rubber block 17 and a moving frame 13, a through groove 38 is arranged on the moving frame 13, and the through groove 38 is longitudinally distributed in a strip shape;
the crushing box 1 is provided with a driving piece which simultaneously drives the turbine blades 25 to rotate and the movable rod 39 and the ejector rod 18 to move in the vertical direction.
Specifically, as shown in fig. 1 and 3, the driving member includes:
the output end of the motor 5 is provided with a first transmission shaft 4, the first transmission shaft 4 penetrates through the shell 6 and is internally provided with a second bevel gear 23, the fourth transmission shaft 21 is sleeved with a first bevel gear 22 meshed with the second bevel gear 23, and the fourth transmission shaft 21 can drive the turbine blades 25 to rotate under the action of the first bevel gear 22 and the second bevel gear 23 in the process that the motor 5 drives the first transmission shaft 4 to rotate;
a second transmission shaft 8 and a third transmission shaft 15 which are arranged on the crushing box 1, the second transmission shaft 8 and the third transmission shaft 15 are rotatably connected through bearings, the output end of the motor 5 is connected with the second transmission shaft 8 through a first transmission belt 7, the second transmission shaft 8 and the third transmission shaft 15 are connected through a second transmission belt 11, belt pulleys are arranged on the motor 5, the second transmission shaft 8 and the third transmission shaft 15, a cam 10 matched with the flange 32 is sleeved on the second transmission shaft 8, and in the rotating process of the cam 10, the flange 32 can be extruded upwards, the driving arm 20 is arranged on the third transmission shaft 15, the driving arm 20 is fixed with a rotating pin 19 which penetrates through the through groove 38, the rotating pin 19 is in sliding fit with the through groove 38, in the process that the driving arm 20 drives the rotating pin 19 to rotate, the rotating pin 19 slides back and forth in the through groove 38, and the moving frame 13 drives the rubber block 17 to move in the vertical direction through the ejector rod 18.
Specifically, as shown in fig. 4 and 5, the connecting member includes a rotating arm 26 on the rotating connection cover 9, a limiting block 36 is formed on the rotating arm 26, a protruding block 30 is fixed on the collection cover 28, a limiting groove 34 adapted to the limiting block 36 is formed on the protruding block 30, a positioning hole 37 is formed on the collection cover 28, a positioning member acting on the positioning hole 37 and positioning the rotating arm 26 is arranged on the rotating arm 26, the positioning member includes a pull rod 27 penetrating through the rotating arm 26, a second spring 40 and a positioning pin 16 adapted to the positioning hole 37 are arranged on the pull rod 27, the pull rod 27 is in sliding fit with the rotating arm 26, the positioning pin 16 is fixed at an end of the pull rod 27, the second spring 40 is sleeved outside the pull rod 27, two ends of the second spring 40 are respectively abutted to the rotating arm 26 and the positioning pin 16, under the action of the second spring 40, the positioning pin 16 is engaged with the positioning hole 37, so that the rotating arm 26 can be limited and prevented from rotating under the action of external force.
Specifically, as shown in fig. 6, the filter 35 includes an annular frame 3501, a fixing block 3503 is fixed inside the annular frame 3501 through a connecting rod 3502, the annular frame 3501, the connecting rod 3502 and the fixing block 3503 are of an integrally formed structure, so that the generation of other stresses is avoided, the stability is higher, the connecting rod 3502 is distributed around the center of the fixing block 3503 at equal angles, an annular filter screen 3504 is arranged between the fixing block 3503 and the annular frame 3501, and the filter screen 3504 is used for filtering dust.
The working principle is as follows: in the crushing process, the motor 5 is started, the first transmission shaft 4 drives the second bevel gear 23 to rotate, the first bevel gear 22 is meshed with the second bevel gear 23, the fourth transmission shaft 21 drives the turbine blades 25 to rotate, the dust suction cover 24 and the communicating pipe 3 generated by crushing enter the collecting cover 28, and dust is filtered under the action of the filtering piece 35, so that the pollution of the dust to the working environment can be reduced;
in the filtering process, under the action of the first transmission belt 7, the second transmission shaft 8 drives the cam 10 to rotate, and under the action of the cam 10 and the first spring 33, the top block 31 reciprocates in the vertical direction to beat the filtering piece 35, so that the filtering piece 35 vibrates, and the situation that the filtering net 3504 of the filtering piece 35 is blocked by particles to influence the filtering of dust can be avoided;
under the action of the second transmission belt 11, the driving arm 20 drives the rotating pin 19 to rotate in the through groove 38, and the moving frame 13 drives the ejector rod 18 and the rubber block 17 to knock the sieve plate 12, so that the sieve plate 12 vibrates, and the crushed materials are conveniently discharged;
at the broken completion, when needing to clear up the inside dust of collecting cover 28, with pull rod 27 outside a pulling, after locating pin 16 and locating hole 37 separate, rotate swivel arm 26, after stopper 36 and spacing groove 34 separate, relieved the spacing to collecting cover 28 promptly, the staff can directly take off collecting cover 28, compare traditional connected mode, this design can be convenient for the staff to the clearance of dust, has reduced staff's the amount of labour.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The production process of the high-purity hydroxypropyl methylcellulose phthalate for the photoresist is characterized by comprising the following steps of:
a. heating and homogenizing cellulose ether, acetic anhydride, glacial acetic acid, phthalic anhydride and succinic anhydride which are used as raw materials;
b. adding sodium acetate as a raw material in the process of adding a proper amount of catalyst to obtain a mixture;
c. heating the mixture to 60-85 ℃, and then carrying out a constant temperature reaction;
d. adding a proper amount of hydrochloric acid in the process of constant temperature reaction;
e. cooling to 40-66 deg.C, adding hot water for dilution, and precipitating;
f. washing for multiple times;
g. performing centrifugal dehydration;
h. drying and crushing;
the crushing equipment related in the step h comprises a crushing box, a crushing mechanism and a sieve plate, wherein the crushing mechanism and the sieve plate are arranged in the crushing box, a shell is fixed on the crushing box, a dust hood is arranged at the bottom of the shell, a turbine blade is connected into the shell through a transmission shaft, a connecting cover communicated with the shell through a communicating pipe is fixed outside the crushing box, a collecting cover is arranged at the bottom of the connecting cover through a connecting piece, and a filtering piece is fixed at the bottom of the collecting cover;
a connecting frame is fixed at the bottom of the collecting cover, a moving rod penetrates through the connecting frame, two ends of the moving rod are respectively fixed with a top block and a flange, and a first spring is arranged between the flange and the connecting frame;
a support is fixed at the bottom of the sieve plate, a top rod penetrates through the support, a rubber block and a movable frame are fixed at two ends of the top rod respectively, and a through groove is formed in the movable frame;
and the crushing box is provided with a driving piece which simultaneously drives the turbine blades to rotate and the movable rod and the ejector rod to move in the vertical direction.
2. The process for producing a high-purity hypromellose phthalate for photoresists according to claim 1, wherein the catalyst is at least one of alkali metal carboxylates.
3. The process for producing high-purity hypromellose phthalate for photoresists according to claim 2, wherein the alkali metal carboxylate is at least one of lithium acetate, sodium acetate, potassium acetate, sodium propionate, and potassium propionate.
4. The process for producing high-purity hypromellose phthalate for photoresist according to claim 1, wherein the temperature raising and homogenizing temperature involved in the step a is 50-70 ℃.
5. The process for producing high-purity hypromellose phthalate for photoresist according to claim 1, wherein the driving member comprises:
the output end of the motor is provided with a first transmission shaft, the first transmission shaft penetrates through the shell and is internally provided with a second bevel gear, and a fourth transmission shaft is sleeved with a first bevel gear meshed with the second bevel gear;
install transmission shaft two and transmission shaft three on broken case, the output and the transmission shaft two of motor are connected through driving belt one, connect through driving belt two between transmission shaft two and the transmission shaft three, the cam with flange matched with has been cup jointed on the transmission shaft two, install the actuating arm on the transmission shaft three, be fixed with the rotation pin that runs through logical groove on the actuating arm.
6. The process for producing high-purity hypromellose phthalate for photoresist according to claim 5, wherein the connecting piece comprises a rotating arm on a rotating connecting cover, a limiting block is formed on the rotating arm, a lug is fixed on the collecting cover, a limiting groove matched with the limiting block is formed on the lug, a positioning hole is formed on the collecting cover, and a positioning piece which acts on the positioning hole and positions the rotating arm is arranged on the rotating arm.
7. The production process of high-purity hypromellose phthalate for photoresist according to claim 6, wherein the positioning piece comprises a pull rod penetrating through the rotating arm, and a second spring and a positioning pin matched with the positioning hole are arranged on the pull rod.
8. The process for producing high-purity hypromellose phthalate for photoresists according to claim 7, wherein the filter comprises an annular frame, a fixed block is fixed inside the annular frame through a connecting rod, and an annular filter screen is arranged between the fixed block and the annular frame.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110576638.XA CN113372457B (en) | 2021-05-26 | 2021-05-26 | Production process of hypromellose phthalate |
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| CN202110576638.XA CN113372457B (en) | 2021-05-26 | 2021-05-26 | Production process of hypromellose phthalate |
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| CN113372457B (en) | 2022-03-01 |
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