Device for rectifying and recycling sucralose neutralization mother liquor

Abstract

The utility model relates to a sucralose neutralization mother liquor rectifying and recycling device which comprises a first rectifying assembly, a second rectifying assembly and a third rectifying assembly, the first rectifying assembly comprises a first rectifying tower, a first condenser communicated with the top of the first rectifying tower and a first return tank connected with the first condenser and the first rectifying tower; the parameters of the first rectifying tower are as follows: the number of tower plates is 18-30, the tower top temperature is 20-40 DEG C, the tower bottom temperature is 80-100 DEG C, and the pressure in the tower is 8-15 bar; the byproduct utilization assembly comprises an ammonia distributor connected with the first reflux tank and a reactor communicated with the bottom of the first rectifying tower. The first rectification assembly with a specific structure is matched with the byproduct utilization assembly, so that ammonia water and dimethylamine hydrochloride with a specific concentration are obtained, the recycling of specific byproducts is realized, and the production profit is improved.

Description

Technical Field

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

[0002] Sucralose was approved as a food additive by the Food and Agriculture Organization of the United Nations (FAO) and the World Health Organization (WHO) in 1990, and as a sucralose by the U.S. Food and Drug Administration (FDA) in 1999. It is currently used as a sweetener in more than 80 countries worldwide. With increasing global consumption, the treatment of wastewater generated during the industrial production of sucralose has become an urgent problem to be solved.

[0003] The sucralose neutralization mother liquor contains high concentrations of salt, ammonia nitrogen, and COD, specifically sucrose and its derivatives, DMF, ammonium chloride, ammonium formate, dimethylamine salt, ethyl acetate, etc.; COD is approximately 80,000–150,000 mg / L, and Kjeldahl nitrogen is approximately 20,000–50,000 mg / L. Currently, the treatment method for this type of wastewater typically involves advanced oxidation pretreatment, 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. Summary of the Invention

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

[0005] To achieve the above objectives, the technical solution adopted by this utility model is: a sucralose neutralization mother liquor distillation and reuse device, which includes:

[0006] The first distillation assembly includes a first distillation column, a first condenser connected to the top of the first distillation column, and a first reflux tank connected to the first condenser and the first distillation column; the parameters of the first distillation column are: 18 to 30 trays, a top temperature of 20 to 40°C and a bottom temperature of 80 to 100°C, and an internal pressure of 8 to 15 bar.

[0007] The by-product utilization component includes an ammonia distributor connected to the first reflux tank and a reactor connected to the bottom of the first distillation column.

[0008] Optimally, the first distillation assembly further includes a first reboiler installed at the bottom of the first distillation column and cooperating with the reactor.

[0009] Furthermore, the by-product utilization component also includes a pressure reducing valve connected to the ammonia distributor.

[0010] Furthermore, the by-product utilization component also includes a dryer connected to the bottom of the reactor.

[0011] Ideally, the reflux ratio of the first reflux tank is 2:1.

[0012] Ideally, the ammonia concentration output by the ammonia distributor is 15-30%.

[0013] Furthermore, a crystallizer and a centrifuge are installed sequentially between the reactor and the dryer.

[0014] Due to the application of the above technical solution, this utility model has the following advantages compared with the prior art: The sucralose neutralization mother liquor distillation and recycling device of this utility model, by adopting a first distillation component with a specific structure and a by-product utilization component in combination, can realize the re-distillation treatment of the condensate at the top of the distillation column of the sucralose neutralization mother liquor reaction liquid (the mixture after the reaction of sucralose neutralization mother liquor and alkali solution), thereby obtaining ammonia water and dimethylamine hydrochloride of a specific concentration, realizing the recovery and utilization of specific by-products, thereby increasing production profits. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the structure of the sucralose neutralization mother liquor distillation and reuse device of this utility model. Detailed Implementation

[0016] The present invention will be further described below with reference to the embodiments shown in the accompanying drawings.

[0017] like Figure 1 The sucralose neutralization mother liquor distillation and recycling device shown mainly includes a first distillation component 3 and a by-product utilization component 4, etc.

[0018] The first distillation assembly 3 mainly includes a first distillation column 31, a first condenser 32, and a first reflux tank 34. The first distillation column 31 is connected to the condenser at its upper middle section, which receives the condensate from the condenser (the neutralized mother liquor reacts with sodium hydroxide solution, and is then distilled to obtain the top product; this top product is condensed at least once to obtain the aforementioned condensate) and performs distillation on it (distillation yields the top and bottom products). The parameters of the first distillation column 31 are: 18-30 trays, a top temperature of 20-40°C, a bottom temperature of 80-100°C, and an internal pressure of 8-15 bar. The first condenser 32 is connected to the top of the first distillation column 31 and receives the top product, condensing it into a liquid. The first reflux tank 34 is connected to the first condenser 32 and the first distillation column 31, and is used to transfer the liquid outlet from the first reflux tank 34 to the first distillation column 31 for circulating distillation. In this embodiment, the reflux ratio of the first reflux tank 34 is 2:1 (that is, the mass ratio or flow rate ratio between the product entering the first distillation column 31 and the product entering the ammonia distributor 41).

[0019] The by-product utilization component 4 mainly includes an ammonia distributor 41, a pressure reducing valve 42, a reactor 43, and a dryer 44. The ammonia distributor 41 is also connected to the first reflux tank 34, allowing the liquid output from the first reflux tank 34 to be transported to the first distillation column 31, while the remainder is introduced into the ammonia distributor 41. The pressure reducing valve 42 is connected to the ammonia distributor 41. Since the ammonia distributor 41 has a water inlet, water can be continuously added to it, thereby preparing ammonia water of a certain concentration in conjunction with the pressure reducing valve 42 (the final concentration of ammonia water can be controlled according to actual needs; ammonia water is typically 15-30% (mass concentration)). The reactor 43 is connected to the bottom of the first distillation column 31, used to receive the bottom product and can be infused with acid (hydrochloric acid in this application) to induce a reaction. The dryer 44 is connected to the bottom of the reactor 43, so that the product after the aforementioned acid reaction is separated and purified (preferably, a crystallizer and a centrifuge are installed between the reactor 43 and the dryer 44 in sequence to crystallize and centrifuge the product after the reaction, and the filter residue of the centrifuge is dried) and then enters the dryer 44 to obtain 99% dimethylamine hydrochloride.

[0020] In this embodiment, the first distillation component 3 also includes a first reboiler 33 installed at the bottom of the first distillation column 31 and cooperating with the reactor 43. At this time, the first reboiler 33 receives part of the bottom product of the first distillation column 31 and then transports it back to the first distillation column 31 for recycling. At this time, a flow distributor can be added to control the proportion of the bottom product entering the first reboiler 33 and the reactor 43 (which can be adjusted according to the actual situation to ensure the distillation effect).

[0021] The method of using the above-mentioned sucralose neutralization mother liquor distillation and reuse device includes the following steps:

[0022] (a) The product (i.e., the product obtained by distillation after the reaction of the sucralose neutralization mother liquor with sodium hydroxide solution) is condensed into a liquid phase and then introduced into the first distillation column 31 for distillation treatment to obtain the top product and the bottom product; the parameters of the first distillation column 31 are: 18 to 30 trays, top temperature of 20 to 40°C and bottom temperature of 80 to 100°C, and internal pressure of 8 to 15 bar; the bottom product is partially heated before being fed into the first distillation column 31.

[0023] (b) After condensing the top product of the column, part of it is refluxed for distillation, and the remaining part is prepared into ammonia water of a specified concentration; the bottom product of the column is reacted with acid to obtain a high-purity dimethylamine salt by-product, that is, after the bottom product of the column is reacted with acid, it is crystallized, washed, centrifuged and dried to obtain a 99% dimethylamine salt by-product.

[0024] Specifically as follows:

[0025] (1) The product is condensed and then enters the first distillation column 31. The first distillation column 31 is used in conjunction with the first reboiler 33 and the first condenser 32. The first distillation column 31 has 20 trays. The parameters of the bottom product are: 87℃, 10 bar, dimethylamine mass fraction 0.91, and flow rate 1.92 t / h. The parameters of the top condensed product are: 25℃, 10 bar, flow rate 0.77 t / h, and ammonia mass fraction greater than 0.99.

[0026] (2) The top product of the first distillation column 31 is condensed and refluxed through the first reflux tank 34 to obtain liquid product; the reflux ratio is controlled to be 2:1 (i.e., the mass or flow rate ratio between the product entering the first distillation column 31 and the product entering the ammonia distributor 41), so that part of it is refluxed into the first distillation column 31 for distillation, and the remaining part enters the ammonia distributor 41. By adding water and controlling the pressure reducing valve 42, 30% ammonia water (mass concentration, the same below) is made to meet the requirements of the recycling process, and the flow rate is 2.5t / h; if the reflux ratio here is adjusted, ammonia water of different concentrations (15~30%) can be obtained; the bottom product of the first distillation column 31 is fed into the reactor 43, and 30% hydrochloric acid is added to react it. After crystallization and purification, the reactants enter the dryer 44 to prepare high-purity dimethylamine salt by-product (purity 99.6%).

[0027] The above embodiments are only for illustrating the technical concept and features of this utility model, and are intended to enable those skilled in the art to understand the content of this utility model and implement it accordingly. They should not be construed as limiting the scope of protection of this utility model. All equivalent changes or modifications made in accordance with the spirit and essence of this utility model should be included within the scope of protection of this utility model.

Claims

1. A device for distilling and recycling sucralose neutralization mother liquor, characterized in that it The utility model relates to a kind of ammonia production system, including: First rectification component (3), the first rectification component (3) includes first rectification tower (31), first condenser (32) being communicated with the top of first rectification tower (31) and first reflux tank (34) being connected with first condenser (32) and first rectification tower (31);The parameters of the first rectification tower (31) are: tray number is 18~30, tower top temperature is 20~40 ℃ and tower bottom temperature is 80~100 ℃, tower internal pressure is 8~15bar; By-product utilization component (4), the by-product utilization component (4) includes ammonia distributor (41) being connected with the first reflux tank (34) and reactor (43) being communicated with the bottom of first rectification tower (31).

2. The neutralization mother liquor rectification reuse apparatus for trichloro sucrose according to claim 1, characterized by: The first rectification component (3) further includes first reboiler (33) being installed in the bottom of the first rectification tower (31) and cooperating with the reactor (43).

3. A trichlorosucrose neutralization mother liquor rectification reuse apparatus according to claim 1 or 2, characterized in that: The by-product utilization component (4) further includes pressure reducing valve (42) being connected with the ammonia distributor (41).

4. The trichlorosucrose neutralization mother liquor rectification reuse apparatus according to claim 3, characterized in that: The by-product utilization component (4) further includes drying machine (44) being communicated with the bottom of the reactor (43).

5. The neutralization mother liquor rectification reuse apparatus for trichloro sucrose according to claim 1, characterized by: The reflux ratio of the first reflux tank (34) is 2:

1.

6. The neutralization mother liquor rectification reuse apparatus for trichloro sucrose according to claim 1, characterized by: The mass concentration of ammonia water output by the ammonia distributor (41) is 15~30%.

7. The trichlorosucrose neutralization mother liquor rectification reuse apparatus of claim 4, characterized in that: Crystallizer and centrifuge are sequentially installed between the reactor (43) and the drying machine (44).

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