CN215855853U - Production system of 4, 6-diamino resorcinol dihydrochloride - Google Patents
Production system of 4, 6-diamino resorcinol dihydrochloride Download PDFInfo
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- CN215855853U CN215855853U CN202120662771.2U CN202120662771U CN215855853U CN 215855853 U CN215855853 U CN 215855853U CN 202120662771 U CN202120662771 U CN 202120662771U CN 215855853 U CN215855853 U CN 215855853U
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Abstract
The utility model discloses a production system of 4, 6-diaminoresorcinol dihydrochloride, which comprises crude product production equipment and fine product production equipment; the crude product production equipment comprises a hydrogenation kettle, a first filter, a crystallization kettle, a concentrated hydrochloric acid metering tank and a centrifuge; the fine product production equipment comprises a decoloring kettle, a second filter and an all-in-one reaction kettle; the all-in-one reaction kettle is provided with a reaction kettle feed inlet, a fine product outlet, a reaction kettle exhaust port, a reaction kettle nitrogen inlet, a mother liquor outlet and a jacket, and the jacket is provided with a solvent inlet and a solvent outlet; be equipped with agitator, filter and shower nozzle in the reation kettle of unifying more, the filter setting is at the agitator and unify at the bottom of the reation kettle cauldron of unifying more. The production system of the utility model adopts high-purity high-pressure nitrogen as the direct driving force for material transfer and filtration, ensures that the product is not oxidized and deteriorated, and particularly adopts the all-in-one reaction kettle in the key step of refining, thereby ensuring the uniformity of product washing and finally improving the product quality.
Description
Technical Field
The utility model relates to a production system of 4, 6-diaminoresorcinol dihydrochloride.
Background
With the development of aerospace and safety protection industries, higher requirements are put forward on the strength, modulus, heat resistance, flame retardance and other properties of materials, and the development of high-performance polymer materials is greatly promoted. Polybenzoxazole (PBO), which is a far superior aromatic polyamide (also called aramid) in heat resistance and flame retardancy, is one of the best fiber products among the currently commercialized artificial organic fibers.
The tensile strength of the PBO fiber can reach more than 5.8GPa, which is about 2 times of that of aramid fiber II fiber and 1.5 times of that of carbon fiber; the tensile modulus of the PBO fiber can reach more than 280GPa, which is about 2.5 times of that of the aramid fiber II fiber. The PBO fiber with the diameter of 1mm can bear the weight of 460 kilograms and has high specific strength and specific modulus. In addition, polybenzoxazole also has good flame retardant properties and thermal stability, which is reputed as "the king of fiber". 4, 6-diamino resorcinol dihydrochloride is an important monomer raw material for synthesizing polybenzoxazole, and the quality of the polybenzoxazole directly influences the performance of the material.
The synthesis method of 4, 6-diaminoresorcinol dihydrochloride is more, and the most common method is to use 2-chloro-4, 6-dinitroresorcinol or 4, 6-diphenylazoresorcinol as a starting material, prepare 4, 6-diaminoresorcinol by catalytic hydrogenation, and then add acid to form salt to obtain 4, 6-diaminoresorcinol dihydrochloride. The product is easy to oxidize and deteriorate, and the preparation of the PBO fiber has strict requirements on the purity, foreign matters, single impurities, granularity and the like of the product, so that the process flow, equipment and the like for producing the 4, 6-diaminoresorcinol dihydrochloride are challenged.
SUMMERY OF THE UTILITY MODEL
The present invention is intended to solve the above problems and provide a production system of 4, 6-diaminoresorcinol dihydrochloride.
The technical scheme for realizing the purpose of the utility model is as follows: a production system of 4, 6-diaminoresorcinol dihydrochloride comprises crude product production equipment and fine product production equipment.
The crude product production equipment comprises a hydrogenation kettle, a first filter, a crystallization kettle, a concentrated hydrochloric acid metering tank and a centrifuge; the hydrogenation kettle is provided with a hydrogenation kettle feeding hole, a hydrogenation kettle discharging hole, a hydrogenation kettle exhaust port, a hydrogenation kettle nitrogen inlet and a hydrogenation kettle hydrogen inlet; the first filter is provided with a first filter feeding hole, a first filter discharging hole and a first filter exhaust hole; a crystallization kettle is provided with a crystallization kettle feeding port, a crystallization kettle discharging port, a crystallization kettle exhaust port, a crystallization kettle nitrogen inlet and a concentrated hydrochloric acid dropping port; the concentrated hydrochloric acid metering tank is provided with a concentrated hydrochloric acid feeding hole, a concentrated hydrochloric acid discharging hole and a concentrated hydrochloric acid metering tank exhaust hole; the centrifuge is provided with a centrifuge feed inlet, a centrifuge nitrogen inlet and a crude product outlet; the first filter feed inlet of the first filter is connected with the hydrogenation kettle discharge outlet of the hydrogenation kettle; a crystallization kettle feeding port of the crystallization kettle is connected with a first filter discharging port of the first filter; a concentrated hydrochloric acid dropping port of the crystallization kettle is connected with a concentrated hydrochloric acid discharging port of the concentrated hydrochloric acid metering tank; and a centrifuge feed inlet of the centrifuge is connected with a crystallization kettle discharge outlet of the crystallization kettle.
The fine product production equipment comprises a decoloring kettle, a second filter and an all-in-one reaction kettle; the decoloring kettle is provided with a decoloring kettle feed inlet, a decoloring kettle discharge outlet, a decoloring kettle exhaust outlet and a decoloring kettle nitrogen inlet; the second filter is provided with a second filter feeding hole, a second filter discharging hole and a second filter exhaust hole; the all-in-one reaction kettle is provided with a reaction kettle feed inlet, a fine product outlet, a reaction kettle exhaust port, a reaction kettle nitrogen inlet, a mother liquor outlet and a jacket, and the jacket is provided with a solvent inlet and a solvent outlet; a stirrer, a filter plate and a spray head are arranged in the all-in-one reaction kettle, and the filter plate is arranged between the stirrer and the bottom of the all-in-one reaction kettle; a second filter feeding hole of the second filter is connected with a decoloring kettle discharging hole of the decoloring kettle; the reaction kettle feed inlet of the all-in-one reaction kettle is connected with the discharge outlet of the second filter.
The number of the spray heads in the all-in-one reaction kettle is 1-4.
The height of the stirrer in the all-in-one reaction kettle can be adjusted.
The utility model has the following positive effects: the production system of the utility model adopts high-purity high-pressure nitrogen as the direct driving force for material transfer and filtration, ensures that the product is not oxidized and deteriorated, and particularly adopts an all-in-one reaction kettle (crystallization, filtration, washing, filtration and drying of the product can be completed in the reaction kettle) in the key step of refining, thereby ensuring the uniformity of product washing and finally improving the product quality.
Drawings
FIG. 1 is a schematic diagram of a crude product production facility of the production system of the present invention.
Fig. 2 is a schematic structural diagram of a boutique production apparatus of the production system of the present invention.
Detailed Description
(example 1)
Referring to fig. 1 and 2, the production system of 4, 6-diaminoresorcinol dihydrochloride according to the present embodiment includes a crude product production apparatus including a hydrogenation kettle 11, a first filter 12, a crystallization kettle 13, a concentrated hydrochloric acid metering tank 14, and a centrifuge 15, and a fine product production apparatus including a decoloring kettle 21, a second filter 22, and an all-in-one reaction kettle 23.
The hydrogenation kettle 11 is provided with a hydrogenation kettle feed inlet 11-1, a hydrogenation kettle discharge outlet 11-2, a hydrogenation kettle exhaust port 11-3, a hydrogenation kettle nitrogen inlet 11-4 and a hydrogenation kettle hydrogen inlet 11-5.
The first filter 12 is provided with a first filter inlet 12-1, a first filter outlet 12-2 and a first filter outlet 12-3. The first filter inlet 12-1 of the first filter 12 is connected with the hydrogenation kettle outlet 11-2 of the hydrogenation kettle 11.
The crystallization kettle 13 is provided with a crystallization kettle feed inlet 13-1, a crystallization kettle discharge outlet 13-2, a crystallization kettle exhaust outlet 13-3, a crystallization kettle nitrogen inlet 13-4 and a concentrated hydrochloric acid dropping port 13-5. The crystallization kettle feed port 13-1 of the crystallization kettle 13 is connected with the first filter discharge port 12-2 of the first filter 12.
The concentrated hydrochloric acid metering tank 14 is provided with a concentrated hydrochloric acid feeding hole 14-1, a concentrated hydrochloric acid discharging hole 14-2 and a concentrated hydrochloric acid metering tank exhaust hole 14-3. A concentrated hydrochloric acid dropping port 13-5 of the crystallization kettle 13 is connected with a concentrated hydrochloric acid discharging port 14-2 of a concentrated hydrochloric acid metering tank 14.
The centrifuge 15 is provided with a centrifuge feed inlet 15-1, a centrifuge nitrogen inlet 15-2 and a crude product outlet 15-3. A centrifuge inlet 15-1 of the centrifuge 15 is connected with a crystallization kettle outlet 13-2 of the crystallization kettle 13.
The decoloring kettle 21 is provided with a decoloring kettle feed inlet 21-1, a decoloring kettle discharge outlet 21-2, a decoloring kettle exhaust port 21-3 and a decoloring kettle nitrogen inlet 21-4.
The second filter 22 is provided with a second filter inlet 22-1, a second filter outlet 22-2 and a second filter outlet 22-3. The second filter inlet 22-1 of the second filter 22 is connected with the decoloring kettle outlet 21-2 of the decoloring kettle 21.
The all-in-one reaction kettle 23 is provided with a reaction kettle feed inlet 23-1, a fine product outlet 23-2, a reaction kettle exhaust port 23-3, a reaction kettle nitrogen inlet 23-4, a mother liquid outlet 23-5 and a jacket 23-6, wherein the jacket 23-6 is provided with a solvent inlet 23-6-1 and a solvent outlet 23-6-2. The reactor feed inlet 23-1 of the all-in-one reactor 23 is connected with the second filter discharge outlet 22-2 of the second filter 22.
The all-in-one reaction kettle 23 is internally provided with a stirrer 23-7, a filter plate 23-8 and a spray head 23-9, the height of the stirrer 23-7 is adjustable, the filter plate 23-8 is arranged between the stirrer 23-7 and the bottom of the all-in-one reaction kettle 23, and 1-4 spray heads 23-9 are arranged.
The production process of the crude product comprises the following steps: adding a starting material 2-chloro-4, 6-dinitroresorcinol or 4, 6-diphenylazoresorcinol, a solvent, a catalyst and the like into a hydrogenation kettle 11, and carrying out catalytic hydrogenation in the hydrogenation kettle 11 under the protection of nitrogen to obtain 4, 6-diaminoresorcinol; then, the mixture is filtered and pressed into a crystallization kettle 13 through a first filter 12, concentrated hydrochloric acid is added into the crystallization kettle 13 from a concentrated hydrochloric acid metering tank 14, and salification is carried out in the crystallization kettle 13 under the protection of nitrogen; finally, filtering by a centrifuge 15 to obtain a crude product of 4, 6-diaminoresorcinol dihydrochloride.
The production process of the fine product comprises the following steps: adding the crude 4, 6-diaminoresorcinol dihydrochloride, a solvent, activated carbon and the like into a decoloring kettle 21, carrying out decoloring reaction in the decoloring kettle 21 under the protection of nitrogen, then carrying out pressure filtration in a multi-in-one reaction kettle 23 through a second filter 22, and carrying out crystallization, filtration, washing, filtration, drying and other technological operations in the multi-in-one reaction kettle 23 under the protection of nitrogen to obtain a refined 4, 6-diaminoresorcinol dihydrochloride.
Claims (3)
1. A production system of 4, 6-diaminoresorcinol dihydrochloride is characterized by comprising crude product production equipment and fine product production equipment;
the crude product production equipment comprises a hydrogenation kettle (11), a first filter (12), a crystallization kettle (13), a concentrated hydrochloric acid metering tank (14) and a centrifuge (15);
the hydrogenation kettle (11) is provided with a hydrogenation kettle feed inlet (11-1), a hydrogenation kettle discharge outlet (11-2), a hydrogenation kettle exhaust outlet (11-3), a hydrogenation kettle nitrogen inlet (11-4) and a hydrogenation kettle hydrogen inlet (11-5); the first filter (12) is provided with a first filter inlet (12-1), a first filter outlet (12-2) and a first filter exhaust port (12-3); a crystallization kettle (13) is provided with a crystallization kettle feeding port (13-1), a crystallization kettle discharging port (13-2), a crystallization kettle exhaust port (13-3), a crystallization kettle nitrogen inlet (13-4) and a concentrated hydrochloric acid dropping port (13-5); a concentrated hydrochloric acid feeding hole (14-1), a concentrated hydrochloric acid discharging hole (14-2) and a concentrated hydrochloric acid metering tank exhaust hole (14-3) are formed in the concentrated hydrochloric acid metering tank (14); a centrifuge feed inlet (15-1), a centrifuge nitrogen inlet (15-2) and a crude product outlet (15-3) are formed in the centrifuge (15);
a first filter feeding hole (12-1) of the first filter (12) is connected with a hydrogenation kettle discharging hole (11-2) of the hydrogenation kettle (11); a crystallization kettle feeding port (13-1) of the crystallization kettle (13) is connected with a first filter discharging port (12-2) of the first filter (12); a concentrated hydrochloric acid dropping port (13-5) of the crystallization kettle (13) is connected with a concentrated hydrochloric acid discharging port (14-2) of the concentrated hydrochloric acid metering tank (14); a centrifuge feed inlet (15-1) of the centrifuge (15) is connected with a crystallization kettle discharge outlet (13-2) of the crystallization kettle (13);
the fine product production equipment comprises a decoloring kettle (21), a second filter (22) and an all-in-one reaction kettle (23);
a decoloring kettle feed inlet (21-1), a decoloring kettle discharge outlet (21-2), a decoloring kettle exhaust outlet (21-3) and a decoloring kettle nitrogen inlet (21-4) are formed in the decoloring kettle (21); a second filter inlet (22-1), a second filter outlet (22-2) and a second filter exhaust port (22-3) are formed in the second filter (22); the all-in-one reaction kettle (23) is provided with a reaction kettle feed inlet (23-1), a fine product outlet (23-2), a reaction kettle exhaust port (23-3), a reaction kettle nitrogen inlet (23-4), a mother liquid outlet (23-5) and a jacket (23-6), and the jacket (23-6) is provided with a solvent inlet (23-6-1) and a solvent outlet (23-6-2); a stirrer (23-7), a filter plate (23-8) and a spray head (23-9) are arranged in the all-in-one reaction kettle (23), and the filter plate (23-8) is arranged between the stirrer (23-7) and the bottom of the all-in-one reaction kettle (23);
a second filter feed inlet (22-1) of the second filter (22) is connected with a decoloring kettle discharge outlet (21-2) of the decoloring kettle (21); and a reaction kettle feed port (23-1) of the all-in-one reaction kettle (23) is connected with a second filter discharge port (22-2) of the second filter (22).
2. The production system of 4, 6-diaminoresorcinol dihydrochloride according to claim 1, wherein: 1-4 spray heads (23-9) in the all-in-one reaction kettle (23) are arranged.
3. The production system of 4, 6-diaminoresorcinol dihydrochloride according to claim 1, wherein: the height of the stirrer (23-7) in the all-in-one reaction kettle (23) can be adjusted.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120662771.2U CN215855853U (en) | 2021-03-31 | 2021-03-31 | Production system of 4, 6-diamino resorcinol dihydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120662771.2U CN215855853U (en) | 2021-03-31 | 2021-03-31 | Production system of 4, 6-diamino resorcinol dihydrochloride |
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| Publication Number | Publication Date |
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| CN215855853U true CN215855853U (en) | 2022-02-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202120662771.2U Active CN215855853U (en) | 2021-03-31 | 2021-03-31 | Production system of 4, 6-diamino resorcinol dihydrochloride |
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| CN (1) | CN215855853U (en) |
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2021
- 2021-03-31 CN CN202120662771.2U patent/CN215855853U/en active Active
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