Reactive distillation device for sucralose neutralization mother liquor

Abstract

The utility model relates to a sucralose neutralization mother liquor reaction rectification device, which comprises a dosing reaction component, an alkali dissolution tank, a continuous tubular reactor, an alkali dissolution tank, an alkali dissolution tank, an alkali dissolution tank, an alkali dissolution tank, an alkali dissolution tank, an alkali dissolution tank and a continuous tubular reactor, wherein the alkali dissolution tank is connected with the continuous tubular reactor through a booster pump; the continuous tubular reactor is also provided with a mother liquor inlet for inputting sucralose neutralization mother liquor; the first rectification assembly comprises a first rectification tower and a first condenser; the middle part of the first rectification tower is connected with the continuous tubular reactor; and the first condenser is communicated with the top of the first rectification tower. Through cooperation of the dosing reaction assembly with a specific structure and the first rectification assembly, the content of salt and ammonia nitrogen in the sucralose neutralization mother liquor can be greatly reduced, and the sewage treatment cost can be saved.

Description

Technical Field

[0001] This utility model belongs to the field of chemical equipment and relates to a reactive distillation device, specifically a reactive distillation device for sucralose neutralization mother liquor. Background Technology

[0002] The sucralose neutralization mother liquor contains high concentrations of salt, ammonia nitrogen, and COD. Currently, the treatment method for this type of wastewater typically involves pretreatment using advanced oxidation processes, followed by mixing with other low-concentration wastewater before entering a biological treatment system. This not only incurs high operating costs but also fails to utilize any useful substances, resulting in significant waste.

[0003] Chinese invention patent application number 201510259701.1 discloses a method for recovering dimethylamine from sucralose wastewater, comprising the steps of: adding a strong alkaline substance to wastewater containing 10-30% dimethylamine hydrochloride and 1-5% N,N-dimethylformamide to obtain an intermediate product with a dimethylamine concentration of 10-30%; and purifying the intermediate product by distillation to obtain a dimethylamine solution with a concentration greater than 35%. This application mainly utilizes an enamel-lined reactor for the reaction, and uses a condenser, bag filter, and distillation column to purify the dimethylamine; the structure is simple, but the denitrification and desalination effects are relatively poor. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the prior art by providing a reactive distillation apparatus for sucralose neutralization mother liquor.

[0005] To achieve the above objectives, the technical solution adopted by this utility model is: a reactive distillation apparatus for sucralose neutralization mother liquor, comprising:

[0006] A dosing reaction assembly, comprising a alkali dissolving tank and a continuous tubular reactor connected to the alkali dissolving tank via a booster pump; the continuous tubular reactor also has a mother liquor inlet for inputting sucralose neutralization mother liquor;

[0007] The first distillation assembly includes a first distillation column connected in the middle to the continuous tubular reactor and a first condenser connected to the top of the first distillation column.

[0008] Optimally, the dosing reaction assembly further includes a heat exchanger connected to the mother liquor inlet, so that the sucralose neutralization mother liquor enters the continuous tubular reactor after heat exchange in the heat exchanger.

[0009] Furthermore, the heat exchanger is also connected to the bottom of the first distillation column.

[0010] Furthermore, the heat exchanger is also connected to the bottom of the first distillation column, and the dosing reaction assembly also includes a continuous centrifuge connected to the heat exchanger.

[0011] Specifically, a first return pipe connected to the alkali dissolving tank is also connected to the pipeline between the heat exchanger and the continuous centrifuge.

[0012] Furthermore, the first distillation assembly also includes a second condenser connected between the first distillation column and the first condenser, and a first reflux tank connected between the first condenser and the second condenser and in communication with the first distillation column.

[0013] Furthermore, the first distillation assembly also includes a first reboiler installed at the bottom of the first distillation column and cooperating with the heat exchanger.

[0014] Ideally, the parameters of the first distillation column are: 20-36 trays, top temperature of 100-145°C and bottom temperature of 160-190°C, and internal pressure of 8-15 bar.

[0015] Due to the application of the above technical solutions, this utility model has the following advantages compared with the prior art: The sucralose neutralization mother liquor reaction distillation device of this utility model, through the cooperation of a specific structure dosing reaction component and a first distillation component, can greatly reduce the salt and ammonia nitrogen content in the sucralose neutralization mother liquor, which is conducive to saving wastewater treatment costs. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the reactive distillation apparatus for sucralose neutralization mother liquor according to this invention. Detailed Implementation

[0017] The present invention will be further described below with reference to the embodiments shown in the accompanying drawings.

[0018] like Figure 1 The sucralose neutralization mother liquor reaction distillation apparatus shown mainly includes a dosing reaction component 1 and a first distillation component 2.

[0019] The dosing reaction assembly 1 mainly comprises a lye tank 11, a booster pump 12 and a continuous tubular reactor 13. The lye tank 11 is used to store the lye (sodium hydroxide solution in this application); the continuous tubular reactor 13 is connected with the lye tank 11 through the booster pump 12, so that the booster pump 12 can continuously deliver the lye into the continuous tubular reactor 13 (the connection in this application is a conventional pipeline connection, i.e. the lye tank 11 and the booster pump 12, and the booster pump 12 and the continuous tubular reactor 13 are connected by pipelines, the same below). In this embodiment, the continuous tubular reactor 13 has at least a first feed inlet, a second feed inlet and a discharge outlet, and the first feed inlet is connected with the booster pump 12; the second feed inlet can be connected with a container for storing the neutralization mother liquor of chlorinated sucrose, so that the neutralization mother liquor of chlorinated sucrose can be continuously delivered into the continuous tubular reactor 13 through the second feed inlet (i.e. the second feed inlet is a mother liquor inlet).

[0020] The first rectification assembly 2 mainly comprises a first rectification tower 21 and a first condenser 24. The middle part of the first rectification tower 21 is connected with the continuous tubular reactor 13 (i.e. the middle part of the first rectification tower 21 is connected with the discharge outlet of the continuous tubular reactor 13), for receiving the discharge of the continuous tubular reactor 13 and performing rectification treatment thereon, and the rectification treatment obtains a first tower top product and a first tower bottom product. The first condenser 24 is connected with the top of the first rectification tower 21, for receiving the first tower top product and cooling it.

[0021] In this embodiment, the dosing reaction assembly 1 further comprises a heat exchanger 14 connected with the mother liquor inlet, so that the neutralization mother liquor of chlorinated sucrose enters the continuous tubular reactor 13 after being heated by the heat exchanger 14. As usual, the heat exchanger 14 has a heat exchange medium inlet, a heat exchange medium outlet, a neutralization mother liquor of chlorinated sucrose inlet and a neutralization mother liquor of chlorinated sucrose outlet, and at this time the heat exchanger 14 is also connected with the bottom of the first rectification tower 21 (i.e. the heat exchange medium inlet of the heat exchanger 14 is connected with the bottom of the first rectification tower 21, so that the first tower bottom product of the first rectification tower 21 is used to heat the neutralization mother liquor of chlorinated sucrose).

[0022] The dosing reaction assembly 1 further comprises a continuous centrifuge 15 connected with the heat exchanger 14 (i.e. the continuous centrifuge 15 is connected with the heat exchange medium outlet of the heat exchanger 14), for receiving the first tower bottom product after heat exchange; a first liquid return pipe 10 connected with the lye tank 11 is further connected on the pipeline between the heat exchanger 14 and the continuous centrifuge 15, so that part of the liquid outlet of the heat exchanger 14 (i.e. the first tower bottom product after heat exchange) is delivered into the lye tank 11 for dissolving sodium hydroxide to form lye, and the remaining part is delivered to a sewage treatment station after being desalted by the continuous centrifuge 15 (as a carbon source for sewage station treatment); here, the flow of the aforementioned liquid outlet of the heat exchanger 14 delivered to the lye tank 11 and the continuous centrifuge 15 can be adjusted according to actual conditions.

[0023] The first rectification assembly 2 further comprises a second condenser 22 connected between the first rectification tower 21 and the first condenser 24 (i.e. the overhead condenser of the first rectification tower 21) and a first reflux tank 23 connected between the first condenser 24 and the second condenser 22 and in communication with the first rectification tower 21, so as to condense and reflux the first overhead product first, so that the first condenser 24 only processes the gaseous product after gas-liquid separation, thereby facilitating improvement of the rectification effect. The first rectification assembly 2 further comprises a first reboiler 25 installed at the bottom of the first rectification tower 21 and matched with the heat exchanger 14, at this time, the first reboiler 25 receives part of the first bottom product of the first rectification tower 21 and re-delivers it into the first rectification tower 21 for recycling treatment; at this time, a flow distribution instrument can be additionally provided to control the proportion of the first bottom product entering the first reboiler 25 and the heat exchanger 14 (which can be adjusted according to actual conditions to ensure the rectification effect).

[0024] The use method of the above-mentioned reaction rectification device for neutralization mother liquor of trichlorogalactose, comprising the following steps:

[0025] (a) reacting the heated trichlorogalactose neutralization mother liquor (70-90℃) and the lye in the continuous tubular reactor 13 to obtain a reaction liquid (reaction temperature is 90-150℃, reaction time is 10-30min);

[0026] (b) introducing the reaction liquid into the first rectification tower 21 for rectification treatment to obtain a first overhead product and a first bottom product; after partial condensation of the first overhead product, a first gaseous product and a first liquid product (part of the first liquid product is refluxed into the first rectification tower 21) are obtained; after heat exchange of the first bottom product as a heat exchange medium, part of it is used as a solvent of alkali, and the rest is used as a carbon source after desalination; the parameters of the first rectification tower 21 are as follows: the number of trays is 20-36, the overhead temperature is 100-145℃, the bottom temperature is 160-190℃, and the pressure in the tower is 8-15bar; part of the first bottom product is heated and then input into the first rectification tower;

[0027] (c) re-condensing the first gaseous product into a liquid phase.

[0028] Specifically as follows: (1) the trichlorosucrose neutralization mother liquor 576 t / d (containing about 10% of ammonium chloride salt, about 8% of dimethylamine salt, about 7% of formic acid salt, about 6% of DMF, about 7% of sucrose and its derivatives, mass percentage content; COD is about 130000 mg / L, Kjeldahl nitrogen is about 49000 mg / L) is transported to the continuous tubular reactor 13 after heat exchange by the heat exchanger 14. Sodium hydroxide is put into the alkali dissolving tank 11, and the pH is controlled to be 9-12. The booster pump 12 is used to pump into the continuous tubular reactor 13, and the flow rate of the booster pump 12 is 20-30 m³ / h, and the head is 100-150 m. The continuous tubular reactor 13 keeps the temperature at 95°C, and the reaction time is 30 min; (2) the water from the continuous tubular reactor 13 is introduced into the first rectifying column 21 to obtain the first column top product and the first column bottom product; the liquid inlet flow rate of the first rectifying column 21 is 24 t / h. The first rectifying column 21 is used in cooperation with the first reboiler 25, and the number of plates of the first rectifying column 21 is 30; the parameters of the first column bottom product are 185°C, 11.5 bar, ammonia nitrogen ≤5 mg / L, and after heat exchange by the heat exchanger 14, part is used as the water source of the alkali dissolving tank 11, and the remaining part is desalted by the continuous centrifuge 15 to be used as the carbon source. The parameters of the first column top product are 140°C, 11 bar, gas phase fraction 0.65, and the column top product flow rate is 4.24 t / h; (3) the first column top product is condensed (using the second condenser 22, and the outlet liquid parameters are 118°C, 11 bar, and gas phase fraction 0.6), and refluxed (using the first reflux tank 23; in this embodiment, the condensation flow rate and the liquid inlet flow rate of the first reflux tank 23 are independently equal to the flow rate of the aforementioned first column top product, that is, 4.24 t / h) to obtain the first gas phase product (118°C, 11 bar, flow rate is 2.72 t / h) and the first liquid phase product (118°C, 11 bar, flow rate is 1.52 t / h), and the first liquid phase product is all refluxed to the first rectifying column 21; the first gas phase product is controlled to enter the first condenser 24 (outlet liquid temperature is 10°C, pressure is 10.5 bar).

[0029] The above embodiment is only for illustrating the technical concept and characteristics of the utility model, and the purpose is to enable those skilled in the art to understand the content of the utility model and implement it, and cannot limit the protection scope of the utility model. Any equivalent changes or modifications made according to the spirit and essence of the utility model should be covered within the protection scope of the utility model.

Claims

1. A reactive distillation apparatus for sucralose neutralization mother liquor, characterized in that it The application relates to a production device for producing sucralose, which comprises the following components: a dosing reaction assembly (1) comprising a caustic soda tank (11) and a continuous tubular reactor (13) connected with the caustic soda tank (11) through a booster pump (12); the continuous tubular reactor (13) is further provided with a mother liquor inlet for inputting a sucralose neutralization mother liquor; a first rectification assembly (2) comprising a first rectification tower (21) connected with the continuous tubular reactor (13) in the middle and a first condenser (24) connected with the top of the first rectification tower (21).

2. The neutralization mother liquor reaction rectification apparatus for trichlorosucrose according to claim 1, characterized by: The dosing reaction assembly (1) further comprises a heat exchanger (14) connected with the mother liquor inlet, so that the sucralose neutralization mother liquor is heated in the heat exchanger (14) and then enters the continuous tubular reactor (13).

3. The neutralization mother liquor reaction rectification apparatus for trichlorosucrose according to claim 2, characterized by: The heat exchanger (14) is further connected with the bottom of the first rectification tower (21).

4. The neutralization mother liquor reaction rectification apparatus for trichlorosucrose according to claim 2 or 3, characterized by: The dosing reaction assembly (1) further comprises a continuous centrifuge (15) connected with the heat exchanger (14).

5. The neutralization mother liquor reaction rectification apparatus for trichloro sucrose according to claim 4, characterized by: A first liquid return pipe (10) connected with the caustic soda tank (11) is further connected on a pipeline between the heat exchanger (14) and the continuous centrifuge (15).

6. The neutralization mother liquor reaction rectification apparatus of trichlorogalactose according to claim 2, characterized by: The first rectification assembly (2) further comprises a second condenser (22) connected between the first rectification tower (21) and the first condenser (24) and a first reflux tank (23) connected between the first condenser (24) and the second condenser (22) and connected with the first rectification tower (21).

7. The neutralization mother liquor reaction rectification apparatus for trichloro sucrose according to claim 6, characterized by: The first rectification assembly (2) further comprises a first reboiler (25) installed at the bottom of the first rectification tower (21) and matched with the heat exchanger (14).

8. The neutralization mother liquor reaction rectification apparatus of trichlorogalactose according to claim 1, characterized by, The parameters of the first rectification tower (21) are as follows: the number of tower plates is 20-36, the tower top temperature is 100-145 DEG C, the tower bottom temperature is 160-190 DEG C, and the tower internal pressure is 8-15 bar.

Images