Sulfonated mother liquor recovery system

Abstract

The utility model discloses a sulfonation mother liquor recovery system which comprises a vacuum concentration tower, a mother liquor inlet pipeline and a concentrated liquor output pipeline are arranged on the vacuum concentration tower, one end, far away from the vacuum concentration tower, of the mother liquor inlet pipeline is connected with a primary centrifugal separator and a dilution tank, and a mother liquor pipeline and a diluent pipeline are arranged on the dilution tank. The output end of the concentrated solution output pipeline is connected with the cooling tank and the secondary centrifugal separator, an intermediate solution output by the secondary centrifugal separator is communicated with the evaporation purification tower through a splitting pipeline, and the secondary centrifugal separator is provided with a product pipeline. According to the sulfonation mother liquor recovery system, useful materials in mother liquor can be efficiently recovered through deep crystallization and step-by-step reduced pressure concentration, the resource utilization rate is increased, the sewage discharge amount is reduced, a water adding dilution method and an extraction separation method are combined, acetic acid is recovered through centrifugal separation and reduced pressure concentration, and the recovery rate is increased.

Description

TECHNICAL FIELD

[0001] The utility model relates to a kind of sulfonated mother liquor processing equipment, specifically a kind of sulfonated mother liquor recovery system. BACKGROUND

[0002] Camphor sulfonic acid is the derivative of camphor, with chiral corresponding body structure, and can be divided into left and right isomers according to its optical properties, and is widely used in pharmaceutical, light industry and daily chemical industry, etc. The company carries out camphor sulfonic acid synthesis and resolution process technology research, and uses camphor powder, acetic anhydride and fuming sulfuric acid as raw materials to prepare left and right camphor sulfonic acid with optical activity through sulfonation and chiral resolution. The production process is optimized, the product quality is improved, the material utilization rate is increased, and the industrial application value of camphor sulfonic acid is improved.

[0003] Sulfonation refers to the chemical reaction process of introducing sulfonic acid group or corresponding salt or sulfonyl halide group in the molecule of organic compound. The existing sulfonation methods include sulfuric acid sulfonation method, azeotropic dehydration sulfonation method, sulfur trioxide sulfonation method and baking sulfonation method. At present, aiming at the synthesis and resolution process technology of camphor sulfonic acid, there are problems such as complex operation, low yield and insufficient purity in the preparation process of D-camphor sulfonic acid and L-camphor sulfonic acid. The production process is optimized, the product quality is improved, and the material utilization rate is increased. In order to optimize the existing process, the present application is proposed. UTILITY MODEL CONTENT

[0004] The utility model aims at providing a kind of sulfonated mother liquor recovery system to solve the problems raised in the above background art.

[0005] To achieve the above-mentioned purpose, the utility model provides the following technical scheme:

[0006] A sulfonated mother liquor recovery system includes a vacuum concentration tower, a mother liquor inlet pipeline and a concentrated liquid output pipeline are arranged on the vacuum concentration tower, one end of the mother liquor inlet pipeline away from the vacuum concentration tower is connected with a primary centrifugal separator and a dilution tank, and a mother liquor pipeline and a dilution liquid pipeline are arranged on the dilution tank.

[0007] As a further scheme of the utility model: the output end of the concentrated liquid output pipeline is connected with a cooling tank and a secondary centrifugal separator, the intermediate liquid output by the secondary centrifugal separator is communicated with an evaporation purification tower through a split section pipeline, and the secondary centrifugal separator is provided with a product pipeline.

[0008] As a further scheme of the utility model: the crystallization separated by the primary centrifugal separator and the secondary centrifugal separator is output through a crystallization pipeline.

[0009] As a further scheme of the utility model: the top of the vacuum concentration tower and the evaporation purification tower is connected with a gas-liquid separation tank through a steam pipeline, and the gas-liquid separation tank is connected with a vacuum extractor through a vacuum pipeline.

[0010] As a further scheme of the utility model: the steam pipeline is provided with a pre-wetting air cooler, and the steam is cooled by the pre-wetting air cooler and then enters the gas-liquid separation tank.

[0011] As a further scheme of the utility model: the condensate in the gas-liquid separation tank is sent into the cooling tank and the dilution tank through condensate pipelines respectively, and the condensate pipelines are provided with flow control valves at the ends close to the cooling tank and the dilution tank respectively.

[0012] As a further scheme of the utility model: the cooling tank is further provided with an additive pipeline.

[0013] As a further scheme of the utility model: the output end of the cooling tank is connected with a sampling pipeline.

[0014] Compared with the prior art, the utility model has the beneficial effects that:

[0015] The sulfonated mother liquor recovery system can efficiently recover useful materials in the mother liquor through deep crystallization and stepwise vacuum concentration, improves resource utilization rate, reduces sewage discharge amount, and improves recovery rate through mutual combination of water dilution method and extraction separation method, setting centrifugal separation and vacuum concentration recovery of acetic acid. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 It is a structural schematic view of a sulfonated mother liquor recovery system.

[0017] In the figure: 1, vacuum concentration tower; 2, pre-wetting air cooler; 3, gas-liquid separation tank; 4, vacuum extractor; 5, vacuum pipeline; 6, mother liquor pipeline; 7, dilution liquid pipeline; 8, cooling tank; 9, dilution tank; 10, primary centrifugal separator; 11, crystallization pipeline; 12, mother liquor liquid inlet pipeline; 13, split section pipeline; 14, concentrated liquid output pipeline; 15, condensate pipeline; 16, secondary centrifugal separator; 17, steam pipeline; 18, additive pipeline; 19, sampling pipeline; 20, evaporation purification tower; 21, product pipeline. DETAILED DESCRIPTION

[0018] Please refer to Figure 1The utility model discloses an embodiment of a kind of sulfonated mother liquor recovery system, including vacuum concentration tower 1, vacuum concentration tower 1 is provided with mother liquor liquid inlet pipeline 12 and concentrated liquid output pipeline 14, the one end of mother liquor liquid inlet pipeline 12 away from vacuum concentration tower 1 is connected with primary centrifugal separator 10 and dilution tank 9, dilution tank 9 is provided with mother liquor pipeline 6 and dilution liquid pipeline 7, sulfonic acid compound solubility is very small in medium concentration sulfuric acid, higher or lower than this concentration then solubility increases dramatically, so it can be after sulfonation, sulfonation liquid is added to water and appropriately diluted, sulfuric acid can be precipitated, and separated by primary centrifugal separator 10, under the action of primary centrifugal separator 10, the crystallization of precipitation is separated, and mother liquor is sent into vacuum concentration tower 1 by primary centrifugal separator 10.

[0019] In a preferred embodiment, the output end of the concentrated liquid output pipeline 14 is connected to a cooling tank 8 and a secondary centrifugal separator 16, the intermediate liquid output by the secondary centrifugal separator 16 is communicated with an evaporation purification tower 20 through a split section pipeline 13, the secondary centrifugal separator 16 is provided with a product pipeline 21, the mother liquor is vacuum concentrated after entering the inside of the vacuum concentration tower 1, and is sent into the cooling tank 8 through the concentrated liquid output pipeline 14, the cooling tank 8 is also provided with an additive pipeline 18, the split solvent is added through the additive pipeline 18, the selection of the split solvent directly affects the yield and purity of the final product, a certain amount of DL-camphor sulfonic acid and L-phenylglycine are respectively dissolved in organic acid, alcohol solution and deionized water, and then refluxed and reacted, and then cooled and rested, and the purity of the generated L-phenylglycine-L-camphor sulfate is measured, and the split solvent with high product yield and purity, low price and easy availability is selected.

[0020] In a preferred embodiment, the crystallization separated by the primary centrifugal separator 10 and the secondary centrifugal separator 16 is output through a crystallization pipeline 11.

[0021] In a preferred embodiment, the top of the vacuum concentration tower 1 and the evaporation purification tower 20 is connected to a gas-liquid separation tank 3 through a steam pipeline 17, the gas-liquid separation tank 3 is connected to a vacuum extractor 4 through a vacuum pipeline 5, the vacuum concentration is to reduce the boiling temperature of water by using vacuum extraction to make water evaporate and dry, and the vacuum extractor 4 provides vacuum pressure to generate a vacuum environment.

[0022] In a preferred embodiment, a pre-wetting air cooler 2 is installed on the steam pipeline 17, the steam enters the gas-liquid separation tank 3 by cooling through the pre-wetting air cooler 2, the pre-wetting air cooler 2 cools the steam to make the steam condense, and after the condensed water enters the inside of the gas-liquid separation tank 3, the liquid phase sinks to the bottom and the gas phase rises to generate a vacuum environment.

[0023] In a preferred embodiment, the condensed liquid in the gas-liquid separation tank 3 is sent into the cooling tank 8 and the dilution tank 9 respectively through condensed liquid pipelines 15, and the condensed liquid pipelines 15 are provided with flow control valves at the ends close to the cooling tank 8 and the dilution tank 9 respectively, and the condensed water in the gas-liquid separation tank 3 is sent into the cooling tank 8 and the dilution tank 9 through the condensed liquid pipelines 15 for further cooling or dilution to release sulfuric acid.

[0024] In a preferred embodiment, the output end of the cooling tank 8 is connected with a sampling pipeline 19, and the sampling pipeline 19 is used to extract the mother liquor in the cooling tank 8 for detection.

[0025] It should be noted that the above embodiments all belong to the same utility model concept, and the description of each embodiment has its own emphasis, and the description of the individual embodiments is not exhaustive, and the description of the other embodiments can be referred to.

[0026] The above embodiments only express the embodiments of the utility model, and the description is more specific and detailed, but it should not be understood as the limitation of the utility model patent range. It should be pointed out that for ordinary skilled in the art, without departing from the concept of the utility model, a number of modifications and improvements can be made, which all belong to the protection range of the utility model. Therefore, the protection range of the utility model patent should be subject to the appended claims.

Claims

1. A sulfonation mother liquor recovery system comprising a vacuum concentration column (1) provided with a mother liquor inlet line (12) and a concentrated liquor outlet line (14), characterized in that, The mother liquor inlet pipeline (12) is connected with the primary centrifugal separator (10) and the dilution tank (9) away from one end of the vacuum concentration tower (1), and the dilution tank (9) is provided with a mother liquor pipeline (6) and a dilution liquid pipeline (7).

2. A system for recovering a sulfonation mother liquor according to claim 1, wherein The output end of the concentrated liquid output pipeline (14) is connected with the cooling tank (8) and the secondary centrifugal separator (16), the intermediate liquid output by the secondary centrifugal separator (16) is communicated with the evaporation purification tower (20) through the split section pipeline (13), and the secondary centrifugal separator (16) is provided with a product pipeline (21).

3. A system for recovering a sulfonation mother liquor according to claim 2, wherein The crystallization separated by the primary centrifugal separator (10) and the secondary centrifugal separator (16) is output through a crystallization pipeline (11).

4. A system for recovering a sulfonation mother liquor according to claim 2, wherein The top of the vacuum concentration tower (1) and the evaporation purification tower (20) is connected with the gas-liquid separation tank (3) through a steam pipeline (17), and the gas-liquid separation tank (3) is connected with the vacuum pump (4) through a vacuum pipeline (5).

5. A system for recovering a sulfonation mother liquor according to claim 4, wherein A pre-wetting air cooler (2) is installed on the steam pipeline (17), and the steam is cooled by the pre-wetting air cooler (2) and then enters the gas-liquid separation tank (3).

6. A system for recovering a sulfonation mother liquor according to claim 4, wherein The condensate in the gas-liquid separation tank (3) is sent into the cooling tank (8) and the dilution tank (9) through a condensate pipeline (15), and the condensate pipeline (15) is provided with a flow control valve near the cooling tank (8) and the dilution tank (9).

7. A system for recovering a sulfonation mother liquor according to claim 3, wherein The cooling tank (8) is also provided with an additive pipeline (18).

8. A system for recovering a sulfonation mother liquor according to claim 2, wherein The output end of the cooling tank (8) is connected with a sampling pipeline (19).

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