CN218879784U - Azo-bis-isobutyramidine hydrochloride synthesizer - Google Patents
Azo-bis-isobutyramidine hydrochloride synthesizer Download PDFInfo
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- CN218879784U CN218879784U CN202320280770.0U CN202320280770U CN218879784U CN 218879784 U CN218879784 U CN 218879784U CN 202320280770 U CN202320280770 U CN 202320280770U CN 218879784 U CN218879784 U CN 218879784U
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Abstract
The utility model relates to a chemical synthesis device, in particular to an azo-diisobutyl amidine hydrochloride synthesis device, which comprises an amidineization kettle, wherein the front end of the amidineization kettle is sequentially provided with a molecular sieve dryer, a regulation kettle, an extraction tank and an impurity removal kettle, and the impurity removal kettle, the extraction tank, the regulation kettle, the molecular sieve dryer and the amidineization kettle are sequentially connected; wherein the extraction tank is connected with the first methane dichloride storage tank, and the impurity removal kettle is respectively connected with the hydrogen peroxide storage tank and the azodiisobutyronitrile storage tank. The utility model discloses simple structure, edulcoration are effectual, product yield is high, drying effect is good.
Description
Technical Field
The utility model relates to a chemical synthesis device, concretely relates to azo-diisobutyl amidine hydrochloride synthesizer.
Background
The azodiisobutyamidine hydrochloride is white or yellowish powder or crystal, is easy to dissolve in water, is insoluble in an organic solvent, can be subjected to primary decomposition to form a cationic free radical, is decomposed under ultraviolet irradiation, and is compatible with a cationic surfactant.
The traditional preparation method of azodiisobutyronidine hydrochloride comprises the steps of removing impurities from azodiisobutyronitrile, adding toluene for extraction, heating an oil layer to 40 ℃ after extraction and layering, adjusting pH =7, cooling for crystallization, centrifuging, drying to obtain treated azodiisobutyronitrile, and carrying out amidine reaction on the treated azodiisobutyronitrile to obtain the azodiisobutyronidine hydrochloride. The process adopts toluene as an extracting agent, has low solubility, causes the subsequent steps of temperature reduction, crystallization and the like to be added, has low product yield and can only reach about 70 percent.
Chinese patent CN 201988384U discloses a high-efficient amidine ization reation kettle, including all coating enamel layer's kettle cover, the cauldron body and installing the agitator in the cauldron body, the kettle cover is equipped with and link up the socket of inboard and pegs graft complex accuse temperature pipe assembly with the socket from the table side, accuse temperature pipe assembly includes that the sleeve pipe in the cauldron body is pegged graft through the socket and pegs graft and arrives intubate in the sleeve pipe, the intubate includes inlet tube and outlet pipe, and sheathed tube both sides lateral wall is pressed close to respectively to inlet tube and outlet pipe, the inlet tube is intake the end and is located the intubate outside, and inlet tube outlet end is located the sleeve pipe bottom, is equipped with the elbow of opening towards outlet pipe one side lateral wall on the inlet tube outlet end, the outlet pipe is intake the end and is located the sleeve pipe top, and outlet pipe outlet end is located the sleeve pipe outside.
Chinese patent CN 212142632U discloses an amidinization reaction kettle with an adjustable kettle body angle, which comprises a fixed support, a first bearing seat, a second bearing seat, an angle adjusting structure assembly and a reaction kettle structure assembly, wherein the reaction kettle structure assembly is arranged on the fixed support through the first bearing seat and the second bearing seat and is connected with the angle adjusting structure assembly; the angle adjusting structure assembly comprises a rotating structure and a positioning structure, and the rotating structure and the positioning structure are arranged at two shaft ends of the reaction kettle structure assembly in parallel.
The above patents are all improvements on amidine reaction kettles, and a pretreatment device of raw materials is not mentioned, and the pretreatment device of the raw materials is also a key device, and has a great influence on the yield of final products.
SUMMERY OF THE UTILITY MODEL
According to the not enough among the above prior art, the utility model discloses the technical problem who solves is: the azo diisobutyl amidine hydrochloride synthesis device is simple in structure, good in impurity removal effect, high in product yield and good in drying effect.
The utility model provides a technical scheme that its technical problem adopted is:
the azodiisobutyl amidine hydrochloride synthesis device comprises an amidinization kettle, wherein the front end of the amidinization kettle is sequentially provided with a molecular sieve dryer, a regulation kettle, an extraction tank and an impurity removal kettle, and the impurity removal kettle, the extraction tank, the regulation kettle, the molecular sieve dryer and the amidinization kettle are sequentially connected; wherein, the extraction tank is connected with a first methane dichloride storage tank, and the impurity removal kettle is respectively connected with a hydrogen peroxide storage tank and an azodiisobutyronitrile storage tank.
The amidine reaction kettle is respectively connected with a hydrogen chloride storage tank and a second dichloromethane storage tank.
The amidination kettle is also connected with a finished product storage tank.
The molecular sieve dryer is characterized in that a first molecular sieve layer, a second molecular sieve layer and a third molecular sieve layer are sequentially arranged inside the molecular sieve dryer from top to bottom, wherein the first molecular sieve layer contains a 4A spherical molecular sieve with the diameter of 6-8mm, the second molecular sieve layer contains a 4A spherical molecular sieve with the diameter of 3-5mm, and the third molecular sieve layer contains a 4A spherical molecular sieve with the diameter of 1.6-2.5 mm.
The volume of the regulation and control kettle is 2000-4000L.
The extraction tank is also connected with a waste liquid storage tank.
The top of the impurity removing kettle is provided with a spray head.
The spray head is connected with a hydrogen peroxide storage tank.
The inside agitator that is provided with of edulcoration cauldron.
The volume of the impurity removing kettle is 3000-12000L.
The working principle and the process are as follows:
azodiisobutyronitrile is discharged from an azodiisobutyronitrile storage tank and enters an impurity removal kettle, hydrogen peroxide is discharged from a hydrogen peroxide storage tank and sprayed on the azodiisobutyronitrile in the impurity removal kettle through a spray head, a stirrer is started to stir, the azodiisobutyronitrile is subjected to oxidation impurity removal, after the oxidation impurity removal, feed liquid enters an extraction tank, dichloromethane is discharged from a first methane dichloride storage tank and enters the extraction tank to be extracted, after extraction layering, an oil layer enters a regulation and control kettle, and a water layer enters a waste liquid storage tank to be stored and subjected to centralized treatment; and heating the oil layer to 30-35 ℃ in the regulating kettle, regulating the pH =7, feeding the oil layer into a molecular sieve dryer, and drying the oil layer sequentially through a first molecular sieve layer, a second molecular sieve layer and a third molecular sieve layer in the molecular sieve dryer to obtain the treated azobisisobutyronitrile. And discharging dichloromethane from a second dichloromethane storage tank and allowing the dichloromethane to enter an amidification kettle, discharging hydrogen chloride from a hydrogen chloride storage tank and allowing the hydrogen chloride to enter the amidification kettle, allowing the treated azobisisobutyronitrile to enter the amidification kettle to perform amidification reaction to obtain azobisisobutyramidine hydrochloride, and allowing the azobisisobutyramidine hydrochloride to enter a finished product storage tank for storage.
The utility model discloses the beneficial effect who has is: the oxydol is sprayed on the azodiisobutyronitrile by a spray head, so that the azodiisobutyronitrile is oxidized and purified more fully, and the impurity removal effect is good; dichloromethane is used as an extracting agent, so that the solubility is high, a crystallization kettle is not required to be added for cooling crystallization subsequently, the product yield is high and can reach more than 95%; the oil layer is dried by three molecular sieve layers with the diameters of the molecular sieves reduced in sequence, and the drying effect is better.
Drawings
FIG. 1 is a schematic view of the present invention;
in the figure: 1. amidine reaction kettle; 2. a molecular sieve dryer; 3. regulating and controlling the kettle; 4. an extraction tank; 5. an impurity removal kettle; 6. a finished product storage tank; 7. a first methane chloride storage tank; 8. a waste liquid storage tank; 9. a hydrogen peroxide storage tank; 10. an azodiisobutyronitrile storage tank; 11. a hydrogen chloride storage tank; 12. a second methylene dichloride storage tank; 13. a first molecular sieve layer; 14. a second molecular sieve layer; 15. a third molecular sieve layer; 16. a spray head; 17. a stirrer.
Detailed Description
Embodiments of the present invention are further described below with reference to the accompanying drawings:
as shown in fig. 1, the utility model comprises an amidification kettle 1, wherein the front end of the amidification kettle 1 is sequentially provided with a molecular sieve dryer 2, a regulation and control kettle 3, an extraction tank 4 and an impurity removal kettle 5, and the impurity removal kettle 5, the extraction tank 4, the regulation and control kettle 3, the molecular sieve dryer 2 and the amidification kettle 1 are sequentially connected; wherein, the extraction tank 4 is connected with a first methane dichloride storage tank 7, and the impurity removal kettle 5 is respectively connected with a hydrogen peroxide storage tank 9 and an azodiisobutyronitrile storage tank 10.
Amidine kettle 1 is connected with hydrogen chloride storage tank 11 and second dichloromethane storage tank 12 respectively.
Amidine kettle 1 is also connected to finished product storage tank 6.
The molecular sieve dryer 2 is internally provided with a first molecular sieve layer 13, a second molecular sieve layer 14 and a third molecular sieve layer 15 from top to bottom in sequence, wherein the first molecular sieve layer 13 contains a 4A spherical molecular sieve with the diameter of 6-8mm, the second molecular sieve layer 14 contains a 4A spherical molecular sieve with the diameter of 3-5mm, and the third molecular sieve layer 15 contains a 4A spherical molecular sieve with the diameter of 1.6-2.5 mm.
The volume of the regulation and control kettle 3 is 3000L.
The extraction tank 4 is also connected with a waste liquid storage tank 8.
The top of the impurity removing kettle 5 is provided with a spray head 16.
The spray head 16 is connected with the hydrogen peroxide storage tank 9.
The inside of the impurity removing kettle 5 is provided with a stirrer 17.
The volume of the impurity removal kettle 5 is 5000L.
Azodiisobutyronitrile is discharged from an azodiisobutyronitrile storage tank 10 and enters an impurity removal kettle 5, hydrogen peroxide is discharged from a hydrogen peroxide storage tank 9 and sprayed on the azodiisobutyronitrile in the impurity removal kettle 5 through a spray nozzle 16, a stirrer 17 is started to stir, the azodiisobutyronitrile is subjected to oxidation impurity removal, after the oxidation impurity removal, feed liquid enters an extraction tank 4, dichloromethane is discharged from a first methane chloride storage tank 7 and enters the extraction tank 4 to be extracted, after extraction layering, an oil layer enters a regulating and controlling kettle 3, and a water layer enters a waste liquid storage tank 8 to be stored and subjected to centralized treatment; and heating the oil layer in the regulation kettle 3 to 30-35 ℃, adjusting the pH =7, feeding the oil layer into the molecular sieve dryer 2, and drying the oil layer sequentially through a first molecular sieve layer 13, a second molecular sieve layer 14 and a third molecular sieve layer 15 in the molecular sieve dryer 2 to obtain the treated azobisisobutyronitrile. And (3) discharging dichloromethane from a second dichloromethane storage tank 12 and entering an amidification kettle 1, discharging hydrogen chloride from a hydrogen chloride storage tank 11 and entering the amidification kettle 1, feeding the processed azobisisobutyronitrile into the amidification kettle 1 to perform amidification reaction to obtain azobisisobutyramidine hydrochloride, and feeding the azobisisobutyramidine hydrochloride into a finished product storage tank 6 for storage, wherein the yield of the azobisisobutyramidine hydrochloride is 95%.
Claims (10)
1. The azo diisobutyl amidine hydrochloride synthesis device comprises an amidine reaction kettle (1), and is characterized in that a molecular sieve dryer (2), a regulation kettle (3), an extraction tank (4) and an impurity removal kettle (5) are sequentially arranged at the front end of the amidine reaction kettle (1), and the impurity removal kettle (5), the extraction tank (4), the regulation kettle (3) and the molecular sieve dryer (2) are sequentially connected with the amidine reaction kettle (1); wherein the extraction tank (4) is connected with a first methane dichloride storage tank (7), and the impurity removal kettle (5) is respectively connected with a hydrogen peroxide storage tank (9) and an azodiisobutyronitrile storage tank (10).
2. The azo-bis-isobutyramidine hydrochloride synthesis device according to claim 1, wherein the amidination reactor (1) is connected to a hydrogen chloride storage tank (11) and a second dichloromethane storage tank (12) respectively.
3. The azodiisobutyl amidine hydrochloride synthesis apparatus according to claim 1, characterized in that said amidination tank (1) is further connected to a finished product storage tank (6).
4. The azo-bis-isobutyramidine hydrochloride synthesis device according to claim 1, wherein the molecular sieve dryer (2) is provided with a first molecular sieve layer (13), a second molecular sieve layer (14) and a third molecular sieve layer (15) from top to bottom in sequence, wherein the first molecular sieve layer (13) contains 4A spherical molecular sieves with a diameter of 6-8mm, the second molecular sieve layer (14) contains 4A spherical molecular sieves with a diameter of 3-5mm, and the third molecular sieve layer (15) contains 4A spherical molecular sieves with a diameter of 1.6-2.5 mm.
5. The azodiisobutyl amidine hydrochloride synthesis apparatus according to claim 1, characterized in that the volume of said control tank (3) is 2000-4000L.
6. The azo-bis-isobutyramidine hydrochloride synthesis device according to claim 1, wherein said extraction tank (4) is further connected to a waste liquid storage tank (8).
7. The azo-bis-isobutyramidine hydrochloride synthesis device according to claim 1, characterized in that a spray head (16) is arranged at the top of the impurity removal kettle (5).
8. The azo diisobutyl amidine hydrochloride synthesis device according to claim 7, wherein the spray head (16) is connected with a hydrogen peroxide storage tank (9).
9. The azo-bis-isobutyramidine hydrochloride synthesis apparatus according to claim 1, characterized in that the inside of the impurity removal kettle (5) is provided with a stirrer (17).
10. The azo-bis-isobutyramidine hydrochloride synthesis apparatus according to claim 1, wherein the volume of said trash vessel (5) is 3000-12000L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320280770.0U CN218879784U (en) | 2023-02-21 | 2023-02-21 | Azo-bis-isobutyramidine hydrochloride synthesizer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320280770.0U CN218879784U (en) | 2023-02-21 | 2023-02-21 | Azo-bis-isobutyramidine hydrochloride synthesizer |
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| CN218879784U true CN218879784U (en) | 2023-04-18 |
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| CN202320280770.0U Active CN218879784U (en) | 2023-02-21 | 2023-02-21 | Azo-bis-isobutyramidine hydrochloride synthesizer |
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