CN214861263U - Device for removing excessive organic amine in process of synthesizing alkyl ketene dimer - Google Patents
Device for removing excessive organic amine in process of synthesizing alkyl ketene dimer Download PDFInfo
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- CN214861263U CN214861263U CN202121079297.7U CN202121079297U CN214861263U CN 214861263 U CN214861263 U CN 214861263U CN 202121079297 U CN202121079297 U CN 202121079297U CN 214861263 U CN214861263 U CN 214861263U
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Abstract
The utility model relates to an alkyl ketene dimer production field specifically provides a remove device of excessive organic amine in synthetic alkyl ketene dimer technology. The device for removing the excessive organic amine in the process of synthesizing the alkyl ketene dimer sequentially comprises a normal-pressure evaporation device and a reduced-pressure evaporation device; the normal pressure evaporation device and the reduced pressure evaporation device both comprise a centrifugal unit for centrifuging the material to make the material attached to the inner wall of the centrifugal unit; the normal-pressure evaporation device and the reduced-pressure evaporation device comprise rollers, and the rollers are positioned in the centrifugal unit and are used for rolling materials on the inner wall of the device into uniform films. The method solves the problems that in the prior art, in order to eliminate organic amine in AKD synthesis, acid water is generally adopted for removal, but in the process of removing the organic amine by adopting the acid water, a large amount of acid water is needed, resource waste is caused, and the organic amine and the acid water generate salts which are difficult to recycle.
Description
Technical Field
The utility model relates to an alkyl ketene dimer production field specifically provides a remove device of excessive organic amine in synthetic alkyl ketene dimer technology.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Alkyl Ketene Dimer (AKD) is formed by reacting stearoyl chloride and organic amine, in order to enable the stearoyl chloride to completely react, in actual production, the organic amine is often added in an excessive amount, in order to remove the excessive organic amine, acid needs to be added into a reaction system after the reaction is finished, the organic amine is enabled to form hydrochloride, and finally the hydrochloride is dissolved in water and taken away in a layered mode.
However, AKD is a compound having a lactone ring structure, and the molecular structure thereof determines that the compound is susceptible to ring opening, and the process is more severe particularly under alkaline conditions. In actual production, because the stearoyl chloride contains a large amount of acid gas, the addition amount of the organic amine is often more than 15-25% of a theoretical value in order to completely react the stearoyl chloride in a system. Therefore, under high temperature conditions, AKD is likely to react with organic amines remaining in the system, and the quality of AKD is irreversibly affected.
In order to solve the problem that excessive addition of organic amine in the synthesis of AKD affects the effective content, in the traditional process, in order to remove the excessive organic amine, hydrogen chloride in acid water and the organic amine are combined to form organic amine hydrochloride, the hydrochloride is immediately dissolved in water, and because AKD is insoluble in water, a water phase can be separated in a layering mode. However, the inventors have found that in the process of removing the organic amine with the acid water, a large amount of acid water is required, which causes resource waste, and that the organic amine and the acid water form salts, which are difficult to recycle.
SUMMERY OF THE UTILITY MODEL
To the organic amine who exists in eliminating the AKD synthesis among the prior art, generally adopt the acid water to get rid of, nevertheless adopt the acid water to get rid of the in-process of organic amine, need use a large amount of acid water, bring the wasting of resources, and organic amine and acid water generate the salt, are difficult to the reuse problem, the utility model provides a under the condition of not adding the treating agent outward, remove excessive organic amine's in the system device.
In one or more embodiments of the present invention, an apparatus for removing excess organic amine in a process for synthesizing alkyl ketene dimer is provided, which comprises an atmospheric evaporation apparatus and a reduced pressure evaporation apparatus in sequence;
the normal pressure evaporation device and the reduced pressure evaporation device both comprise a centrifugal unit for centrifuging the material to make the material attached to the inner wall of the centrifugal unit;
the normal-pressure evaporation device and the reduced-pressure evaporation device comprise rollers, and the rollers are positioned in the centrifugal unit and are used for rolling materials on the inner wall of the device into uniform films.
One or some of the above technical solutions have the following advantages or beneficial effects:
1) the utility model discloses abandoned the mode that adopts the acid water washing among the traditional handicraft, changed into vacuum distillation system, removed organic amine under anhydrous environment, AKD dwell time is short on the evaporimeter wall, and the system temperature only 65 ~ 75 degrees centigrade, the phenomenon that the material quality descends can not appear. Because no water is introduced into the system, the problem of resource waste caused by using acid water is fundamentally avoided.
2) The device in do not have moisture to introduce, avoided the energy consumption problem because of introducing the later stage desorption moisture that moisture leads to.
3) The utility model discloses relate to the gyro wheel in evaporation plant, the material dwell time is short in deamination device, has improved the productivity of single device.
Drawings
The accompanying drawings, which form a part of the specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without unduly limiting the scope of the invention.
FIG. 1 is a schematic diagram of an apparatus for removing excess organic amine in a process for synthesizing alkyl ketene dimer according to an embodiment of the present invention.
Fig. 2 is a schematic view of the roller in the embodiment of the present invention.
Wherein: 1. a material storage tank; 2. a stirring motor; 3. a heat-preserving jacket; 4. a thermal medium inlet; 5. a thermal medium outlet; 6. a material centrifugal disc; 7. a nitrogen coil pipe; 8. a nitrogen inlet pipe; 9. nitrogen heating equipment; 10. a material transfer pipeline; 11. a freezing medium inlet; 12. a freezing medium outlet; 13. a freezing coil pipe; 14. a stirring frame; 14-1, rollers; 15. a material receiving tank; 16. an organic amine receiving tank; 17. a vacuum system.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiment of the present invention, all other embodiments obtained by the person skilled in the art without creative work belong to the protection scope of the present invention.
To the organic amine who exists in eliminating the AKD synthesis among the prior art, generally adopt the acid water to get rid of, nevertheless adopt the acid water to get rid of the in-process of organic amine, need use a large amount of acid water, bring the wasting of resources, and organic amine and acid water generate the salt, are difficult to the reuse problem, the utility model provides a under the condition of not adding the treating agent outward, remove excessive organic amine's in the system device.
In one or more embodiments of the present invention, an apparatus for removing excess organic amine in a process for synthesizing alkyl ketene dimer is provided, which comprises an atmospheric evaporation apparatus and a reduced pressure evaporation apparatus in sequence;
the normal pressure evaporation device and the reduced pressure evaporation device both comprise a centrifugal unit for centrifuging the material to make the material attached to the inner wall of the centrifugal unit;
the normal pressure evaporation device and the reduced pressure evaporation device comprise rollers 14-1, and the rollers 14-1 are positioned in the centrifugal unit and are used for rolling materials on the inner wall of the device into a uniform film.
In order to realize the purpose of removing the organic amine, the process equipment adopts two groups of evaporation devices, and the working conditions are different, namely normal pressure and reduced pressure. Most of organic amine is removed in the normal pressure evaporation device, and the other small part of organic amine is closely contacted with the alkyl ketene dimer and is removed in the reduced pressure evaporation device, and the reduced pressure evaporation device uses the negative pressure provided by the vacuum system 17 as power, thereby effectively realizing the separation of the alkyl ketene dimer and the organic amine.
Preferably, the centrifugal unit comprises a stirring frame 14, which is in a container structure and is positioned inside the atmospheric evaporation device or the reduced pressure evaporation device,
the stirring motor 2 is used for providing power required by centrifugation for the stirring frame 14;
the material centrifugal disc 6 is fixed above the stirring frame 14 and is driven to rotate by the stirring motor 2.
The roller 14-1 is tightly attached to the inner wall of the evaporator, has the same spatial shape with the inner wall, and is provided with a roller in the middle of the roller 14-1, and the roller is controlled to roll. Preferably, the roller is made of corrosion-resistant materials such as polytetrafluoroethylene and the like, is hollow inside and is sleeved on the stirring frame. Under the action of the roller 14-1, the material on the evaporation surface is rolled into a uniform film, the material flows downwards along the evaporation surface under the action of gravity, the film forming descends to maximize the contact surface of the material and a heat medium, and the heat exchange effect is optimal.
The roller can be controlled to roll up and down by a rolling shaft controlled by a traction rope of the engine, and can also be provided with a sliding rail to control the rolling.
Preferably, the outer wall of the normal pressure evaporation device or the reduced pressure evaporation device is provided with a heat preservation jacket 3, and a heat medium circulates in the heat preservation jacket 3.
Preferably, a heat medium inlet 4 is arranged below the heat-insulating jacket 3, and a heat medium outlet 3 is arranged above the heat-insulating jacket. The heat medium and the material adopt a countercurrent heat exchange mode, and the reason is that the closer the material is to the lower part of the evaporation device, the more the material is evaporated out of the adherent material, and the more the heat exchange medium is needed.
Preferably, the bottom of the atmospheric evaporation device is provided with a nitrogen coil 7, and the nitrogen coil 7 is used for blowing nitrogen upwards. Specifically, the nitrogen coil 7 is uniformly perforated, and the direction of the perforation directly faces the evaporation surface, so that nitrogen is blown from bottom to top.
Preferably, the top of the atmospheric evaporation device is provided with a nitrogen outlet. The organic amine is blown out from the nitrogen outlet, the nitrogen outlet can be connected with an organic amine receiving device, or the nitrogen outlet is connected with a filtering device, the filtered nitrogen enters the nitrogen inlet to be continuously recycled, and the filtered organic amine is connected with the organic amine receiving tank 16.
Preferably, the inlet of the nitrogen coil 7 is provided with a nitrogen heating device 9. Avoid the nitrogen gas supercooling, influence the heat transfer condition in the evaporation plant.
Preferably, the decompression evaporation device comprises a freezing coil 13 inside, and the freezing coil 13 is provided with a cold medium inlet 11 and a cold medium outlet 12 which are both positioned below the freezing coil 13.
In the descending process of the material, the organic amine descends along the freezing coil pipe 13 to realize the separation of the material and the organic amine, namely the material is heated and the organic amine is separated when being cooled.
Preferably, an outlet is led out from one end of the lower part of the decompression evaporation device close to the inner wall of the centrifugal unit, and is connected with a material receiving tank 15, and an outlet is led out from the bottom of the freezing coil 13 and is connected with an organic amine receiving tank 16.
Preferably, the organic amine receiving tank 16 is connected with a vacuum system 17, and the vacuum system 17 is used for providing negative pressure.
In one or some embodiments of the present invention, there is provided a method for removing excess organic amine in a process for synthesizing alkyl ketene dimer, the method is performed in the above-mentioned apparatus for removing excess organic amine in a process for synthesizing alkyl ketene dimer, comprising the steps of:
opening the hot medium inlet 4, starting the stirring motor 2, opening the nitrogen inlet pipe 8 and the valve of the material storage tank 1, feeding the material liquid into the material centrifugal disc 6, forming centrifugal force due to the fact that the material centrifugal disc 6 rotates along with the stirring frame 14, uniformly throwing the material onto the evaporation inner wall under the action of the centrifugal force, rolling the material on the evaporation surface into a uniform thin film under the action of the roller 14-1, and enabling the material to flow downwards along the evaporation surface under the action of gravity.
The nitrogen coil 7 is uniformly perforated, the direction of the perforation is directly opposite to the evaporation surface, the material flows from top to bottom, the nitrogen is blown from bottom to top, and after the material passes through the device, the organic amine can be reduced by 55-70%.
After that, the material was transferred to the material storage tank 1 of the decompression evaporation apparatus.
Through the nitrogen purging, most of organic amine in the AKD is taken away, but a part of organic amine still remains in the AKD, and in order to thoroughly remove the organic amine, the process equipment introduces a reduced pressure evaporation system.
Opening a heat medium inlet 4, starting a stirring motor 2 and a vacuum system 17, opening a nitrogen inlet pipe 8, opening a valve of a material storage tank 1, enabling feed liquid to enter a material centrifugal disc 6, forming centrifugal force due to the fact that the material centrifugal disc 6 rotates along with a stirring frame 14, enabling the material to be uniformly thrown onto an evaporation inner wall under the action of the centrifugal force, rolling the material on an evaporation surface into a uniform thin film under the action of a roller 14-1, and enabling the material to flow downwards along the evaporation surface under the action of gravity.
Under the action of vacuum, organic amine molecules escape from a film interface, and become liquid after encountering a condensing coil pipe, and finally enter an organic amine receiving tank, and AKD enters a material receiving tank.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, therefore, the invention is not limited thereto.
Claims (10)
1. A device for removing excessive organic amine in the process of synthesizing alkyl ketene dimer is characterized by comprising a normal pressure evaporation device and a reduced pressure evaporation device in sequence;
the normal pressure evaporation device and the reduced pressure evaporation device both comprise a centrifugal unit for centrifuging the material to make the material attached to the inner wall of the centrifugal unit;
the normal-pressure evaporation device and the reduced-pressure evaporation device comprise rollers (14-1), and the rollers (14-1) are positioned in the centrifugal unit and are used for rolling materials on the inner wall of the device into a uniform film.
2. The apparatus for removing excess organic amine in the process for synthesizing alkyl ketene dimer according to claim 1, wherein said centrifugal unit comprises a stirring frame (14) having a container structure and located inside an atmospheric evaporation apparatus or a reduced pressure evaporation apparatus,
the stirring motor (2) is used for providing power required by centrifugation for the stirring frame (14);
the material centrifugal disc (6) is fixed above the stirring frame (14) and is driven to rotate by the stirring motor (2).
3. The apparatus for removing excess organic amine in the process for synthesizing alkyl ketene dimer according to claim 1, wherein there is a heat-insulating jacket (3) on the external wall of said atmospheric pressure evaporation apparatus or said vacuum evaporation apparatus, and there is a heat medium circulating in said heat-insulating jacket (3).
4. The apparatus for removing excess organic amine in the process for synthesizing alkyl ketene dimer according to claim 3, wherein said heat-insulating jacket (3) has a heat medium inlet (4) at the lower part and a heat medium outlet (5) at the upper part.
5. The apparatus for removing excess organic amine in the process for synthesizing alkyl ketene dimer according to claim 1, wherein said atmospheric evaporation unit has a nitrogen coil (7) at the bottom, said nitrogen coil (7) being used for blowing nitrogen upward.
6. The apparatus for removing excess organic amine from a process for the synthesis of an alkyl ketene dimer according to claim 5, wherein said atmospheric evaporation unit has a nitrogen outlet at the top.
7. The apparatus for removing excess organic amine in the process for the synthesis of alkyl ketene dimer according to claim 5, characterized in that there is a nitrogen heating device (9) at the inlet of said nitrogen coil (7).
8. The apparatus for removing excess organic amine in the process of synthesizing alkyl ketene dimer according to claim 1, wherein said decompression evaporation apparatus comprises a freezing coil (13) inside, and said freezing coil (13) has a cold medium inlet (11) and a cold medium outlet (12) both located below said freezing coil (13).
9. The apparatus for removing the excess organic amine in the process of synthesizing alkyl ketene dimer according to claim 8, wherein an outlet is led out from one end of the lower part of the decompression evaporation apparatus close to the inner wall of the centrifugal unit, and is connected with a material receiving tank (15), and an outlet is led out from the bottom of the freezing coil (13) and is connected with an organic amine receiving tank (16).
10. The apparatus for removing excess organic amine in the process for synthesizing alkyl ketene dimer according to claim 9, wherein said organic amine receiving tank (16) is connected to a vacuum system (17), said vacuum system (17) being used for providing negative pressure.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114146085A (en) * | 2021-12-02 | 2022-03-08 | 江苏海洋大学 | Preparation method of silybin-polyene phosphatidylcholine compound |
| CN116730952A (en) * | 2023-08-14 | 2023-09-12 | 山东天安化工股份有限公司 | Preparation method of alkyl ketene dimer |
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2021
- 2021-05-19 CN CN202121079297.7U patent/CN214861263U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114146085A (en) * | 2021-12-02 | 2022-03-08 | 江苏海洋大学 | Preparation method of silybin-polyene phosphatidylcholine compound |
| CN114146085B (en) * | 2021-12-02 | 2023-11-10 | 江苏海洋大学 | Preparation method of silybin-polyene phosphatidylcholine compound |
| CN116730952A (en) * | 2023-08-14 | 2023-09-12 | 山东天安化工股份有限公司 | Preparation method of alkyl ketene dimer |
| CN116730952B (en) * | 2023-08-14 | 2023-11-10 | 山东天安化工股份有限公司 | Preparation method of alkyl ketene dimer |
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