CN211586951U - Polyether ketone dry-type crushing system - Google Patents
Polyether ketone dry-type crushing system Download PDFInfo
- Publication number
- CN211586951U CN211586951U CN201922434219.3U CN201922434219U CN211586951U CN 211586951 U CN211586951 U CN 211586951U CN 201922434219 U CN201922434219 U CN 201922434219U CN 211586951 U CN211586951 U CN 211586951U
- Authority
- CN
- China
- Prior art keywords
- dichloromethane
- polyether ketone
- double
- crushing
- screw extruder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Polyethers (AREA)
Abstract
The invention relates to the technical field of polyether ketone production, in particular to a polyether ketone dry type crushing system and a crushing process. The polyether ketone dry type crushing system comprises a reaction kettle, a double-screw extruder, a recovery kettle and a centrifugal machine which are sequentially connected; a plurality of dichloromethane air outlets are formed in a discharge pipe of the double-screw extruder; the polyether ketone dry type crushing process adopts a double-screw extruder to replace an emulsifying machine, no water phase is introduced during crushing, the double-screw extruder is heated during crushing by using the double-screw extruder, polyether ketone is crushed, and dichloromethane is recovered. The polyether ketone dry type crushing system solves the problems of slow crushing and incomplete dichloromethane recovery in the wet type crushing process, realizes dry type crushing, improves the crushing speed, and thoroughly recovers the dichloromethane; the invention also provides a crushing process thereof.
Description
Technical Field
The utility model relates to a polyether ketone production technical field, concretely relates to polyether ketone dry-type crushing system.
Background
Polyether ketone (PEKK) resin is a special engineering plastic with excellent performance, belongs to one kind of polyaryletherketone, has a chemical structure that benzene ring ether bond ketone groups are arranged in order in a molecular structure, and endows molecules with a highly stable chemical bond characteristic, so that the polyether ketone has excellent mechanical performance, radiation resistance, high temperature resistance, chemical corrosion resistance and good electrical insulation and flame retardant performance, can be processed and formed by processing methods such as extrusion, injection molding, mould pressing and the like, and has extremely high application requirements in the aspects of aerospace, electronic and electrical, automobiles and petroleum.
The structural formula of PEKK is shown below:
at present, the synthesis methods of polyether ketone are more reported in the literature, but two methods are really commercialized, one is a two-step method of DuPont, and the other is a Lewis acid-Lewis base synchronous catalysis method developed by Raychem (WO 8403891). For example, in patent CN101812170, a lewis acid-lewis base synchronous catalysis method is adopted, which uses dichloromethane as a solvent, and adds diphenyl ether, acyl chloride and lewis acid at low temperature, and prepares polyether ketone at room temperature under the co-catalysis of lewis base/lewis acid. After the reaction is finished, a complex formed by the polyether ketone, Lewis base/Lewis acid and dichloromethane is wrapped in the complex to form a gel substance. To obtain the coarse powder of polyether ketone, the gel-like material can be decomplexed in water or hydrochloric acid solution and pulverized to obtain the coarse powder of polyether ketone. On one hand, the polymer is wrapped by a complex formed by Lewis base/Lewis acid and dichloromethane, so that the complex needs to be crushed and decomplexed at the same time, and the industrial production can be realized by adopting equipment such as an emulsifying machine, but the gel-like material is difficult to crush, so that the crushing time is longer, on the other hand, the boiling point of dichloromethane is lower, so that the volatilization of dichloromethane is easy to cause in the crushing and decomplexing process, on the other hand, after the decomplexing, the dichloromethane solution and water are mixed together, and because dichloromethane has certain solubility in water, the dichloromethane in the crushed water is difficult to completely remove, and the cost of subsequent water treatment is increased.
SUMMERY OF THE UTILITY MODEL
Not enough to prior art, the utility model aims at providing a polyetherketoneketone dry-type crushing system has solved that conventional crushing in-process time is slow, the dichloromethane volatilizes, and the higher problem of aquatic dichloromethane content, has improved crushing speed, has avoided volatilizing of dichloromethane, has reduced the content of aquatic dichloromethane.
The utility model discloses a polyetherketoneketone dry-type crushing system, including consecutive reation kettle, twin-screw extruder, recovery kettle and centrifuge; and a plurality of dichloromethane air outlets are formed in a discharge pipe of the double-screw extruder.
The discharge port of the reaction kettle is connected with the feed port of the double-screw extruder through a blanking pipeline.
The discharge pipe of the double-screw extruder is connected with the feed inlet of the recovery kettle through a transfer pipeline.
The discharge hole of the recovery kettle is connected with a centrifuge.
The outlet at the lower end of the centrifuge is connected with an aluminum-containing water pipeline, and the polyether ketone product is discharged from the upper end.
The working process of the polyether ketone dry type crushing system comprises the following steps:
adding the gel-like material in the reaction kettle into a double-screw extruder through a blanking pipeline, discharging dichloromethane in the gel-like material through a dichloromethane gas outlet, and recovering the dichloromethane, wherein the gel-like material is crushed into mixed powder of polyether ketone and aluminum trichloride; and putting the mixed powder into a recovery kettle through a transfer pipeline, adding water into the recovery kettle, dissolving aluminum trichloride powder to obtain a polyetherketoneketone product and aluminum-containing water, carrying out subsequent treatment on the polyetherketoneketone product, and allowing the aluminum-containing water to enter an aluminum-containing water collecting pool along an aluminum-containing water pipeline.
The gel-like material in the reaction kettle is formed by polyether ketone, dichloromethane and aluminum trichloride.
The temperature of the double-screw extruder is set to be 35-60 ℃.
Compared with the prior art, the utility model discloses there is following beneficial effect:
(1) the utility model adopts the double screw extruder to replace the emulsifying machine, the water phase is not introduced during the crushing, the original wet type crushing process is changed, the dry type crushing is realized, because the water phase is not existed, the aluminum trichloride does not participate in the reaction in the process, the heat can not be emitted, and the complex state of the polyether ketone in the system of dichloromethane, Lewis acid and Lewis base is directly removed by reducing the content of the dichloromethane;
(2) the utility model discloses heating twin-screw extruder at the kibbling in-process of use twin-screw extruder, directly retrieving dichloromethane through the dichloromethane gas outlet, do not have the participation in aqueous phase, just avoided dichloromethane to dissolve in aqueous, solved dichloromethane's waste and dichloromethane to the influence problem that contains aluminium water.
Drawings
FIG. 1 is a schematic diagram of the dry pulverizing system for polyetherketoneketone of the present invention;
FIG. 2 is a schematic diagram of a conventional wet polyetherketoneketone comminution system;
in the figure: 1. the device comprises a reaction kettle, 2 parts of a blanking pipeline, 3 parts of a double-screw extruder, 4 parts of a dichloromethane exhaust port, 5 parts of a transfer pipeline, 6 parts of a recovery kettle, 7 parts of a polyether ketone product, 8 parts of a centrifugal machine, 9 parts of an aluminum-containing water pipeline, 10 parts of an emulsifying machine, 11 parts of a water inlet pipeline, 12 parts of a discharging pipeline, 13 parts of a dichloromethane recovery pipeline.
Detailed Description
The following embodiments are combined to further explain the present invention, but the protection scope of the present invention is not limited thereto, and the professional in this field should be right the technical solution of the present invention should all belong to the protection scope of the present invention.
Example 1
As shown in fig. 1, the utility model discloses a polyetherketoneketone dry-type pulverizing system, which comprises a reaction kettle 1, a twin-screw extruder 3, a recovery kettle 6 and a centrifuge 8 which are connected in sequence; and a plurality of dichloromethane air outlets 4 are formed in a discharge pipe of the double-screw extruder 3.
The discharge port of the reaction kettle 1 is connected with the feed port of the double-screw extruder 3 through a discharge pipeline 2.
The discharge pipe of the double-screw extruder 3 is connected with the feed inlet of the recovery kettle 6 through a transfer pipeline 5.
The discharge hole of the recovery kettle 6 is connected with a centrifuge 8.
The outlet at the lower end of the centrifuge 8 is connected with an aluminum-containing water pipeline 9, and the polyether ketone product 7 is discharged at the upper end.
The polyether ketone dry grinding system is used for carrying out polyether ketone dry grinding, and the steps are as follows:
(1) adding 270L of dichloromethane solution into a reaction kettle, cooling to below-5 ℃, keeping the temperature in the reaction kettle not to exceed-5 ℃, respectively adding 38.98Kg of terephthaloyl chloride, 9.74Kg of isophthaloyl chloride, 41.25Kg of diphenyl ether and 0.67Kg of benzoyl chloride into the reaction kettle, mixing, then adding 35.43Kg of N, N-dimethylformamide, adding 160Kg of aluminum trichloride in batches, stirring for 2 hours after the addition is finished, slowly raising the temperature in the reaction kettle to room temperature, stirring continuously until the viscosity is not changed any more, stopping stirring and curing for 8 hours to obtain a gel-like material;
(2) the gel-like material in the reaction kettle 1 is connected into a double-screw extruder 3 through a blanking pipeline 2, a double screw (the diameter of the adopted screw is 120mm, the length-diameter ratio is 42) is started, the rotating speed is set to be 400rmp/min, the temperature is set to be 35 ℃, vacuum pumping is carried out at a dichloromethane outlet 4, dichloromethane in the gel-like material is discharged, and the discharge port is recovered after three-stage condensation and secondary activated carbon absorption. At this time, the colloidal material in the twin screw was pulverized into a mixed powder of polyetherketoneketone and aluminum trichloride. And (3) putting the mixed powder into a recovery kettle 6 which is provided with stirring and contains hydrochloric acid water through a transfer pipeline 5, and filtering to obtain polyether ketone coarse powder and aluminum-containing water respectively. The total time of the crushing process is 4 hours. The recovery rate of the dichloromethane is 99.3 percent
And taking a sample of the aluminum-containing water to detect the content of the dichloromethane.
Example 2
Polyetherketoneketone dry milling was performed using the polyetherketoneketone dry milling system of example 1, with the following steps:
(1) adding 270L of dichloromethane solution into a reaction kettle, cooling to below-5 ℃, keeping the temperature in the reaction kettle not to exceed-5 ℃, respectively adding 34.11Kg of terephthaloyl chloride, 14.62Kg of isophthaloyl chloride, 41.25Kg of diphenyl ether and 0.67Kg of benzoyl chloride into the reaction kettle, mixing, then adding 35.43Kg of N, N-dimethylformamide, adding 160Kg of aluminum trichloride in batches, stirring for 2 hours after the addition is finished, slowly raising the temperature in the reaction kettle to room temperature, stirring continuously until the viscosity is not changed any more, stopping stirring and curing for 8 hours to obtain a gel material;
(2) the gel-like material in the reaction kettle 1 is connected into a double-screw extruder 3 through a blanking pipeline 2, double screws (the diameter of the adopted screw is 120mm, the length-diameter ratio is 42) are started, the rotating speed is set to be 600rmp/min, the temperature is set to be 50 ℃, vacuum pumping is carried out at a dichloromethane outlet 4, dichloromethane in the gel-like material is discharged, and the discharge port is recovered after three-stage condensation and two-stage activated carbon absorption. At this time, the colloidal material in the twin screw was pulverized into a mixed powder of polyetherketoneketone and aluminum trichloride. And (3) putting the mixed powder into a recovery kettle 6 which is provided with stirring and contains hydrochloric acid water through a transfer pipeline 5, and filtering to obtain polyether ketone coarse powder and aluminum-containing water respectively. The total time of the crushing process is 2 hours. The recovery rate of the dichloromethane is 98.5 percent
And taking a sample of the aluminum-containing water to detect the content of the dichloromethane.
Example 3
Polyetherketoneketone dry milling was performed using the polyetherketoneketone dry milling system of example 1, with the following steps:
(1) adding 270L of dichloromethane solution into a reaction kettle, cooling to below-5 ℃, keeping the temperature in the reaction kettle not to exceed-5 ℃, respectively adding 29.23Kg of terephthaloyl chloride, 19.48Kg of isophthaloyl chloride, 41.25Kg of diphenyl ether and 0.67Kg of benzoyl chloride into the reaction kettle, mixing, then adding 35.43Kg of N, N-dimethylformamide, adding 160Kg of aluminum trichloride in batches, stirring for 2 hours after the addition is finished, slowly raising the temperature in the reaction kettle to room temperature, stirring continuously until the viscosity is not changed any more, stopping stirring and curing for 8 hours to obtain a gel material;
(2) the gel-like material in the reaction kettle 1 is connected into a double-screw extruder 3 through a blanking pipeline 2, a double screw (the diameter of the adopted screw is 120mm, the length-diameter ratio is 42) is started, the rotating speed of the double screw is set to be 300rmp/min, the temperature of the double screw is set to be 60 ℃, vacuum pumping is carried out at a dichloromethane outlet 4, dichloromethane in the gel-like material is discharged, and the discharge outlet is recovered after three-stage condensation and two-stage activated carbon absorption. At this time, the colloidal material in the twin screw was pulverized into a mixed powder of polyetherketoneketone and aluminum trichloride. And (3) putting the mixed powder into a recovery kettle 6 which is provided with stirring and contains hydrochloric acid water through a transfer pipeline 5, and filtering to obtain polyether ketone coarse powder and aluminum-containing water respectively. The total time of the crushing process is 2.5 h. The recovery rate of the dichloromethane is 98.2 percent
And taking a sample of the aluminum-containing water to detect the content of the dichloromethane.
Comparative example 1
As shown in fig. 2, a conventional wet pulverizing system for polyetherketoneketone comprises a reaction kettle 1, an emulsifying machine 10, a recovery kettle 6 and a centrifuge 8 which are connected in sequence; the discharge hole of the recovery kettle 6 is also connected with the water inlet of the emulsifying machine 10 through a water inlet pipeline 11.
The discharge port of the reaction kettle 1 is connected with the feed port of the emulsifying machine 10 through a discharge pipeline 2.
The discharge port of the emulsifying machine 10 is connected with the feed port of the recovery kettle 6 through a transfer pipeline 5.
The discharge port of the recovery kettle 6 is respectively connected with the water inlet of the emulsifying machine 10 and the feed inlet of the centrifugal machine 8 through a water outlet pipeline 11 and a discharge pipeline 12.
The upper end of the recovery kettle 6 is connected with a dichloromethane recovery pipeline 13.
The outlet at the lower end of the centrifuge 8 is connected with an aluminum-containing water pipeline 9, and the polyether ketone product 7 is discharged at the upper end.
The wet polyether ketone crushing system is used for carrying out dry polyether ketone crushing, and the steps are as follows:
(1) adding 270L of dichloromethane solution into a reaction kettle, cooling to below-5 ℃, keeping the temperature in the reaction kettle not to exceed-5 ℃, respectively adding 38.98Kg of terephthaloyl chloride, 9.74Kg of isophthaloyl chloride, 41.25Kg of diphenyl ether and 0.67Kg of benzoyl chloride into the reaction kettle, mixing, then adding 35.43Kg of N, N-dimethylformamide, adding 160Kg of aluminum trichloride in batches, stirring for 2 hours after the addition is finished, slowly raising the temperature in the reaction kettle to room temperature, stirring continuously until the viscosity is not changed any more, stopping stirring and curing for 8 hours to obtain a gel-like material;
(2) adding water into a recovery kettle 6, enabling the water to enter an emulsifying machine 10 along a water outlet pipeline 11, enabling a gelatinous material in a reaction kettle 1 to enter the emulsifying machine 10 along a blanking pipeline 2, grinding and crushing the gelatinous material in the emulsifying machine 10, enabling the ground material to enter the recovery kettle 6 along a transfer pipeline 5, opening steam to heat the recovery kettle 6, distilling and recovering dichloromethane with a low boiling point along a dichloromethane recovery pipeline 13, enabling the residual polyetherketoneketone powder, the water and aluminum trichloride dissolved in the water to enter a centrifugal machine 8 through a discharge pipeline 12, enabling the aluminum-containing water to enter an aluminum-containing water collecting tank along an aluminum-containing water pipeline 9 after centrifugation, and carrying out subsequent treatment on a polyetherketoneketone product 7. The total time of the grinding process and the distillation is 16 h. The recovery rate of the dichloromethane is 76.5 percent
And taking a sample of the aluminum-containing water to detect the content of the dichloromethane.
Comparative example 2
Polyetherketoneketone dry milling was performed using the polyetherketoneketone wet milling system of comparative example 1, with the following steps:
(1) adding 270L of dichloromethane solution into a reaction kettle, cooling to below-5 ℃, keeping the temperature in the reaction kettle not to exceed-5 ℃, respectively adding 34.11Kg of terephthaloyl chloride, 14.62Kg of isophthaloyl chloride, 41.25Kg of diphenyl ether and 0.67Kg of benzoyl chloride into the reaction kettle, mixing, then adding 35.43Kg of N, N-dimethylformamide, adding 160Kg of aluminum trichloride in batches, stirring for 2 hours after the addition is finished, slowly raising the temperature in the reaction kettle to room temperature, stirring continuously until the viscosity is not changed any more, stopping stirring and curing for 8 hours to obtain a gel material;
(2) adding water into a recovery kettle 6, enabling the water to enter an emulsifying machine 10 along a water outlet pipeline 11, enabling a gelatinous material in a reaction kettle 1 to enter the emulsifying machine 10 along a blanking pipeline 2, grinding and crushing the gelatinous material in the emulsifying machine 10, enabling the ground material to enter the recovery kettle 6 along a transfer pipeline 5, opening steam to heat the recovery kettle 6, distilling and recovering dichloromethane with a low boiling point along a dichloromethane recovery pipeline 13, enabling the residual polyetherketoneketone powder, the water and aluminum trichloride dissolved in the water to enter a centrifugal machine 8 through a discharge pipeline 12, enabling the aluminum-containing water to enter an aluminum-containing water collecting tank along an aluminum-containing water pipeline 9 after centrifugation, and carrying out subsequent treatment on a polyetherketoneketone product 7. The total time consumption of the grinding process and the distillation is 14.5 h. The recovery rate of the dichloromethane is 78 percent
And taking a sample of the aluminum-containing water to detect the content of the dichloromethane.
Comparative example 3
Polyetherketoneketone dry milling was performed using the polyetherketoneketone wet milling system of comparative example 1, with the following steps:
(1) adding 270L of dichloromethane solution into a reaction kettle, cooling to below-5 ℃, keeping the temperature in the reaction kettle not to exceed-5 ℃, respectively adding 29.23Kg of terephthaloyl chloride, 19.48Kg of isophthaloyl chloride, 41.25Kg of diphenyl ether and 0.67Kg of benzoyl chloride into the reaction kettle, mixing, then adding 35.43Kg of N, N-dimethylformamide, adding 160Kg of aluminum trichloride in batches, stirring for 2 hours after the addition is finished, slowly raising the temperature in the reaction kettle to room temperature, stirring continuously until the viscosity is not changed any more, stopping stirring and curing for 8 hours to obtain a gel material;
(2) adding water into a recovery kettle 6, enabling the water to enter an emulsifying machine 10 along a water outlet pipeline 11, enabling a gelatinous material in a reaction kettle 1 to enter the emulsifying machine 10 along a blanking pipeline 2, grinding and crushing the gelatinous material in the emulsifying machine 10, enabling the ground material to enter the recovery kettle 6 along a transfer pipeline 5, opening steam to heat the recovery kettle 6, distilling and recovering dichloromethane with a low boiling point along a dichloromethane recovery pipeline 13, enabling the residual polyetherketoneketone powder, the water and aluminum trichloride dissolved in the water to enter a centrifugal machine 8 through a discharge pipeline 12, enabling the aluminum-containing water to enter an aluminum-containing water collecting tank along an aluminum-containing water pipeline 9 after centrifugation, and carrying out subsequent treatment on a polyetherketoneketone product 7. The total time of the grinding process and the distillation is 18 hours. The recovery rate of the dichloromethane is 73.2 percent
And taking a sample of the aluminum-containing water to detect the content of the dichloromethane.
The results of measuring the methylene chloride content in the aluminum-containing water samples of examples 2 to 4 and comparative examples 2 to 4 are shown in Table 1.
TABLE 1 results of measuring the methylene chloride content in the aluminum-containing water samples of examples 2 to 4 and comparative examples 2 to 4
Claims (5)
1. A polyetherketoneketone dry pulverization system is characterized in that: comprises a reaction kettle (1), a double-screw extruder (3), a recovery kettle (6) and a centrifuge (8) which are connected in sequence; a plurality of dichloromethane air outlets (4) are arranged on a discharge pipe of the double-screw extruder (3).
2. The polyetherketoneketone dry milling system of claim 1, wherein: the discharge hole of the reaction kettle (1) is connected with the feed inlet of the double-screw extruder (3) through a blanking pipeline (2).
3. The polyetherketoneketone dry milling system of claim 1, wherein: the discharge pipe of the double-screw extruder (3) is connected with the feed inlet of the recovery kettle (6) through a transfer pipeline (5).
4. The polyetherketoneketone dry milling system of claim 1, wherein: the discharge hole of the recovery kettle (6) is connected with a centrifuge (8).
5. The polyetherketoneketone dry milling system of claim 1, wherein: the outlet at the lower end of the centrifuge (8) is connected with an aluminum-containing water pipeline (9), and the polyether ketone product (7) is discharged from the upper end.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922434219.3U CN211586951U (en) | 2019-12-30 | 2019-12-30 | Polyether ketone dry-type crushing system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922434219.3U CN211586951U (en) | 2019-12-30 | 2019-12-30 | Polyether ketone dry-type crushing system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN211586951U true CN211586951U (en) | 2020-09-29 |
Family
ID=72597625
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201922434219.3U Active CN211586951U (en) | 2019-12-30 | 2019-12-30 | Polyether ketone dry-type crushing system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN211586951U (en) |
-
2019
- 2019-12-30 CN CN201922434219.3U patent/CN211586951U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105417523B (en) | Low cost, large-scale production process and its equipment used of graphene nano powder | |
| CN102888003B (en) | High polymer material precipitation method and industrial production method of polysulfone resin | |
| CN106832397B (en) | The method of online reuse PET Polymerization Waste | |
| CN108659876A (en) | The method for preparing bio oil is combined in pretreatment of raw material with hydrothermal liquefaction | |
| CN211586951U (en) | Polyether ketone dry-type crushing system | |
| CN112552528B (en) | Method for removing solvent in high-temperature-resistant polymer solution | |
| CN111013787A (en) | Polyether ketone dry type crushing system and crushing process | |
| CN114773587B (en) | Epoxy propane removal process for PPC production process | |
| CN112045964A (en) | Polycarbonate additive adding device and adding process | |
| CN104163914B (en) | Utilize maleic anhydride and butanediol to prepare the equipment of voluminous thing | |
| CN216998325U (en) | Extraction device for extracting wax | |
| CN101492330B (en) | Modified ammonium nitrate fuel mixture serial production line | |
| CN203938627U (en) | Utilize MALEIC ANHYDRIDE and butyleneglycol to prepare the system of voluminous thing | |
| CN202909718U (en) | Special polymer flash vaporization and precipitation kettle | |
| CN111054289A (en) | Production process and device of polyether ketone | |
| CN112897523B (en) | Graphite purification equipment | |
| CN211514526U (en) | Production device of polyether ketone | |
| CN211566551U (en) | Epoxy apparatus for producing | |
| CN203938628U (en) | Utilize MALEIC ANHYDRIDE and butyleneglycol to prepare the equipment of voluminous thing | |
| CN113968782A (en) | Method for removing impurities in recycled acetic acid | |
| CN113120867A (en) | Insoluble sulfur processing method and system | |
| CN204079854U (en) | A kind of green serialization can prepare the system of high-purity thermoplastic phenolic resin | |
| CN221310648U (en) | Efficient carbonization reaction integrated device | |
| CN219169610U (en) | Slurry bed system for preparing graphene aluminum alloy powder | |
| CN213803578U (en) | Separator for processing and producing epoxy resin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |