Hydrolysis concentration system
By designing a hydrolysis concentration system and utilizing multi-stage concentration and condensation technology, the problem of low purity in indigo production was solved, achieving efficient extraction and purification of indigo and reducing environmental pollution.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-30
- Publication Date
- 2026-04-07
AI Technical Summary
During the production of indigo, the solution generated after the hydrolysis of indigo precursors contains a large amount of water and impurities, resulting in low purity of indigo that is difficult to remove effectively.
A hydrolysis concentration system was designed, including a hydrolysis reactor and a multi-stage concentration device. The supernatant is evaporated sequentially by multiple concentrators. Combined with a condenser and a membrane reactor, multi-stage concentration and impurity removal are achieved to improve the purity of indigo.
It improved the yield and purity of indigo, enhanced the discharge and separation efficiency of the supernatant, reduced environmental pollution, and improved the extraction rate and solubility of indigo.
Smart Images
Figure CN224086706U_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of hydrolysis and concentration technology, and in particular to a hydrolysis and concentration system. Background Technology
[0002] Indigo, molecular formula C 16 H 10 N₂O₂ is a water-soluble non-azo colorant. Indigo pigments are among the oldest known pigments and are widely used in the food, pharmaceutical, and printing and dyeing industries.
[0003] The production of indigo involves the hydrolysis of its precursors (indoside or indorubane B) under acidic or alkaline conditions, releasing intermediates such as indophenol. Specifically, indoside hydrolyzes into glucose and indophenol under acidic conditions, while indorubane B hydrolyzes into indophenol under alkaline conditions. Indophenol is a key raw material for the production of indigo. Because the solution generated after the hydrolysis of indigo precursors typically contains a large amount of water and other impurities, the purity of indigo is low. Therefore, to remove excess water and impurities and improve the purity of indigo, this application proposes a hydrolysis concentration system suitable for indigo. Utility Model Content
[0004] This application provides a hydrolysis concentration system to solve the technical problems described in the background art.
[0005] To solve the above-mentioned technical problems, this application adopts the following technical solution:
[0006] This application provides a hydrolysis concentration system, including: a hydrolysis reactor and a concentration device interconnected by a first supernatant pipe;
[0007] The hydrolysis reactor is connected from top to bottom to multiple second supernatant pipes located below the first supernatant pipe. The first supernatant pipe is equipped with a first shut-off valve near the hydrolysis reactor. The ends of the multiple second supernatant pipes away from the hydrolysis reactor are all connected to the first supernatant pipe and are all equipped with a second shut-off valve.
[0008] The concentration device includes a plurality of concentrators connected in series along a first direction via a concentration tube; the end of the first supernatant tube away from the hydrolysis reactor is connected to the first concentrator in the first direction;
[0009] The concentration temperature of the plurality of concentrators along the first direction gradually increases.
[0010] Optionally, a condenser may also be included;
[0011] The tops of all the concentrators are connected to the steam inlet of the condenser via a first condenser tube.
[0012] Optionally, it also includes a membrane reactor and a return water tank that are interconnected via a first pipe;
[0013] The condensate outlet of the condenser is connected to the inlet of the membrane reactor via a second condenser tube.
[0014] Optionally, the bottom of the last concentrator along the first direction is connected to a concentration storage tank via a second pipe, and a first discharge valve is provided on the second pipe near the concentrator.
[0015] Optionally, the bottom of the hydrolysis reactor is connected to a filter press via a third pipe, the solid material outlet of the filter press is connected to a dryer via a conveyor, and its water outlet is connected to the first supernatant pipe via a fourth pipe.
[0016] A second discharge valve is installed on the third pipe near the hydrolysis reactor.
[0017] Optionally, a first delivery pump is provided on the first supernatant tube near the first concentrator in the first direction.
[0018] Optionally, a second delivery pump is provided on the concentration tube between the last two concentrators in the first direction.
[0019] The hydrolysis and concentration system provided in this application hydrolyzes the raw materials used for indigo production in a hydrolysis reactor to obtain indigo precipitate and supernatant. The supernatant is discharged into a concentration device through a first supernatant pipe and multiple second supernatant pipes. The concentration device contains multiple concentrators arranged along a first direction, which sequentially evaporate various impurities in the supernatant with increasing boiling points until the supernatant is concentrated to the required concentration, thereby obtaining indigo precipitate and a highly pure indigo solution, thus improving the indigo yield. The arrangement of the first supernatant pipe and multiple second supernatant pipes located below it enables the simultaneous discharge of supernatant from multiple heights. This allows the supernatant in the hydrolysis reactor to be discharged through the first supernatant pipe into the first concentrator arranged along the first direction, improving the discharge efficiency of the supernatant in the hydrolysis reactor and the separation efficiency of the supernatant from the indigo precipitate. At the same time, the arrangement of multiple concentrators with progressively increasing concentration temperatures along the first direction enables multi-stage concentration of the supernatant, removing as many impurities as possible from the supernatant, resulting in a higher purity indigo solution after concentration. This also improves the extraction rate and efficiency of indigo from the supernatant, leading to a higher concentration of indigo in the extracted indigo solution. Attached Figure Description
[0020] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0021] Figure 1 This is a schematic diagram of the structure of a hydrolysis concentration system provided in an embodiment of this application;
[0022] Figure 2 This is a schematic diagram of the structure of a hydrolysis concentration system provided in another embodiment of this application;
[0023] Figure 3 This is a schematic diagram of the structure of a hydrolysis concentration system provided in another embodiment of this application.
[0024] In the diagram: 101, First supernatant pipe; 1011, First shut-off valve; 1012, First transfer pump; 102, Second supernatant pipe; 1021, Second shut-off valve; 103, Concentrator pipe; 1031, Second transfer pump; 104, First condenser pipe; 105, First pipeline; 106, Second condenser pipe; 107, Second pipeline; 1071, Concentrator storage tank; 1072, First discharge valve; 108, Third pipeline; 1081, Filter press; 1082, Second discharge valve; 109, Fourth pipeline; 200, Hydrolysis reactor; 300, Concentrator device; 301, Concentrator; 400, Condenser; 500, Membrane reactor; 600, Return water tank; 700, Conveyor; 701, Dryer. Detailed Implementation
[0025] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application are described clearly and completely below. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without creative effort are also within the scope of protection of this application.
[0026] refer to Figures 1 to 3This application provides a hydrolysis concentration system, comprising: a hydrolysis reactor 200 and a concentration device 300 interconnected via a first supernatant pipe 101; Indigo, due to its chemical structure, low water solubility, and redox properties, produces a precipitate as its final product during synthesis, necessitating a precipitation step for separation. Specifically, the hydrolysis reactor 200 synthesizes indigo and generates an upper supernatant and a lower precipitate therein. The lower precipitate is indigo, while the upper supernatant may contain some incompletely precipitated indigo. The concentration device 300 concentrates the upper supernatant, recovering the indigo, organic solvents, and water. It should be noted that the specific raw materials for indigo synthesis can be selected according to the specific synthesis process, and this application does not impose specific limitations on them. The hydrolysis reactor 200 is connected from top to bottom to multiple second supernatant pipes 102 located below the first supernatant pipe 101. The first supernatant pipe 101 is equipped with a first shut-off valve 1011 near the hydrolysis reactor 200. The ends of the multiple second supernatant pipes 102 away from the hydrolysis reactor 200 are all connected to the first supernatant pipe 101 and are all equipped with a second shut-off valve 1021. In order to accurately separate the supernatant from the precipitate in the hydrolysis reactor 200, a visual observation window is provided on the hydrolysis reactor 200. The first supernatant pipe 101 and the multiple second supernatant pipes 102 below it can separate the supernatant at different liquid levels, thereby achieving high separation efficiency of the supernatant.
[0027] The concentration device 300 includes a plurality of concentrators 301 connected in series along a first direction via a concentration tube 103; the end of the first supernatant tube 101 away from the hydrolysis reactor 200 is aligned with the first direction (wherein, the first direction is as follows). Figure 1 The first concentrator 301 is connected to the (shown); since there are multiple reactants used to produce indigo and byproducts are generated during its hydrolysis reaction, various substances in the supernatant can be separated and recovered by multiple concentrators 301.
[0028] In this process, the concentration temperatures of the multiple concentrators 301 along the first direction gradually increase. This allows for the separation of substances with increasing boiling points from the supernatant, ultimately yielding indigo precipitate with high purity. Furthermore, concentration helps improve the solubility and stability of indigo, making it more suitable for subsequent dyeing and applications.
[0029] The hydrolysis and concentration system provided in this application hydrolyzes the raw materials used for indigo production in a hydrolysis reactor 200 to obtain indigo precipitate and supernatant. The supernatant is discharged into a concentration device 300 through a first supernatant pipe 101 and multiple second supernatant pipes 102. The concentration device 300 includes multiple concentrators 301 arranged along a first direction, which sequentially evaporate various impurities in the supernatant with boiling points from low to high until the supernatant is concentrated to the required concentration, thereby obtaining indigo precipitate and a high-purity indigo solution, thus improving the yield of indigo. The arrangement of the first supernatant pipe 101 and multiple second supernatant pipes 102 located below the first supernatant pipe 101 enables the simultaneous discharge of supernatant from multiple heights. This allows the supernatant in the hydrolysis reactor 200 to be discharged through the first supernatant pipe 101 into the first concentrator 301 arranged along the first direction, improving the discharge efficiency of the supernatant in the hydrolysis reactor 200 and the separation efficiency of the supernatant from the indigo precipitate. At the same time, the arrangement of multiple concentrators 301 with progressively increasing concentration temperatures along the first direction enables multi-stage concentration of the supernatant, removing as many impurities as possible from the supernatant, resulting in a higher purity indigo solution after concentration. This also improves the extraction rate and efficiency of indigo from the supernatant, leading to a higher concentration of indigo in the extracted indigo solution.
[0030] In some embodiments, reference Figure 2 and Figure 3 The hydrolysis concentration system in this application also includes a condenser 400; the specifications and model of the condenser 400 can be set according to actual needs, and this application does not specifically limit it.
[0031] Furthermore, the tops of the multiple concentrators 301 are all connected to the steam inlet of the condenser 400 via the first condenser pipe 104. Since the temperatures of the multiple concentrators 301 gradually increase along the first direction, during the actual concentration and condensation process, the mixture in the first concentrator 301 along the first direction concentrates for a preset time (this time refers to evaporating the substance at the temperature corresponding to the concentrator 301 as completely as possible). The mixture then enters the next concentrator 301, and the steam generated during this concentration process first enters the condenser 400 for condensation, and so on.
[0032] In the above embodiments, since the aqueous solution after separating the indigo precipitate during the indigo production process contains various organic substances and reaction byproducts, directly discharging the clear liquid from the upper layer of indigo may pollute the aquatic environment due to the presence of these organic substances and reaction byproducts. By concentrating the liquid and condensing the steam generated from these organic substances and reaction byproducts through a condenser 400, and then treating it centrally before discharging it, the environmental harm caused by direct discharge of the indigo production aqueous solution is reduced, and the purity of the indigo precipitate is improved.
[0033] In some embodiments, reference Figure 2 and Figure 3 The hydrolysis and concentration system in this application also includes a membrane reactor 500 and a return water tank 600 that are interconnected by a first pipe 105; wherein the membrane reactor 500 is a membrane bioreactor (MBR).
[0034] Specifically, the condensate outlet of the condenser 400 is connected to the inlet of the membrane reactor 500 through the second condenser tube 106.
[0035] In the above embodiment, the condensate after being condensed by the condenser 400 enters the membrane reactor 500 through the second condenser tube 106. The membrane reactor 500 removes various organic substances and reaction byproducts, reducing the content of various organic substances and reaction byproducts in the aqueous solution. The water treated by the membrane reactor 500 is then discharged into the return water tank for reuse, thereby improving the water recycling rate, reducing the pollution to the environment caused by the direct discharge of aqueous solution generated in the indigo production process, and also improving the recovery rate and purity of indigo precipitate.
[0036] In some embodiments, reference Figure 2 and Figure 3 In this application, the bottom of the last concentrator 301 along the first direction is connected to a concentration storage tank 1071 via a second pipe 107. A first discharge valve 1072 is installed on the pipe of the second pipe 107 near the concentrator 301. The supernatant obtained after the reaction in the hydrolysis reactor 200 contains indigo dye and organic macromolecules (e.g., nitrophenol, dimethylformamide, etc., depending on the raw materials and processes used in indigo production, which are specifically defined in this application). The boiling point of indigo is 400.4°C (at 760 mmHg), the boiling point of nitrophenol is approximately 202°C, and the boiling point of dimethylformamide is 153°C. That is to say, compared with the organic matter and by-products in the supernatant, the boiling point of indigo is relatively high.
[0037] In the above embodiment, the first discharge valve 1072 on the second pipeline 107 is opened to discharge the indigo precipitate deposited at the bottom of the last concentrator 301 along the first direction out of the concentrator 301 and collect it through the concentration storage tank 1071, thereby improving the collection efficiency of indigo.
[0038] In some embodiments, reference Figure 3 In this application, the bottom of the hydrolysis reactor 200 is connected to a filter press 1081 via a third pipe 108. The solid material outlet of the filter press 1081 is connected to a dryer 701 via a conveyor 700, and its water outlet is connected to a second condenser 106 via a fourth pipe 109. The models and specifications of the filter press 1081, the conveyor 700, and the dryer 701 can be set according to actual needs, and this application does not impose specific limitations on them.
[0039] In addition, a second discharge valve 1082 is installed on the pipe of the third pipe 108 near the hydrolysis reactor 200.
[0040] In the above embodiment, the second discharge valve 1082 is opened, and the indigo precipitate in the hydrolysis reactor 200 is discharged to the filter press 1081 through the third pipe 108. After filtration by the filter press 1081, an aqueous solution and indigo precipitate are obtained. The aqueous solution enters the second condenser 106 through the fourth pipe 109, and then enters the membrane reactor 500 through the second condenser 106. The membrane reactor 500 filters out the indigo dye and organic macromolecules (such as nitrophenol, dimethylformamide, etc.) contained in the aqueous solution. Finally, the water treated by the membrane reactor 500 is discharged to the return water tank 600 for later use, which improves the water recovery efficiency. The indigo precipitate is conveyed to the dryer 701 through the conveyor 700, and the indigo precipitate is dried by the dryer 701 to obtain the finished indigo product for subsequent use.
[0041] In some embodiments, reference Figures 1 to 3 In this application, a first transfer pump 1012 is provided on the first supernatant pipe 101 near the first concentrator 301 in the first direction. The specifications and model of the first transfer pump 1012 can be set according to actual needs, and this application does not specifically limit it.
[0042] In the above embodiment, after the reaction is completed in the hydrolysis reactor 200 and indigo precipitate and supernatant are formed, the first transfer pump 1012 is turned on. The first transfer pump 1012 provides the power to transport the supernatant in the hydrolysis reactor 200 to the first concentrator 301 in the first direction, thus ensuring the effective progress of the concentration process.
[0043] In some embodiments, reference Figures 1 to 3In this application, a second transfer pump 1031 is provided on the concentration pipe between the last two concentrators 301 in the first direction. The specifications and model of the second transfer pump 1031 can be set according to actual needs, and this application does not impose specific limitations on it.
[0044] In the above embodiment, the second transfer pump 1031 is turned on to provide the power for conveying the supernatant in the hydrolysis reactor 200 between the first supernatant pipe 101, the second supernatant pipe 102 and the multiple concentrators 301, thereby ensuring the continuity of the concentration process.
[0045] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.
Claims
1. A hydrolysis concentration system, characterized in that, include: The hydrolysis reactor (200) and the concentration device (300) are interconnected by the first supernatant pipe (101). The hydrolysis reactor (200) is connected from top to bottom to a plurality of second supernatant pipes (102) located below the first supernatant pipe (101). The first supernatant pipe (101) is provided with a first shut-off valve (1011) near the hydrolysis reactor (200). The ends of the plurality of second supernatant pipes (102) away from the hydrolysis reactor (200) are all connected to the first supernatant pipe (101) and are all provided with a second shut-off valve (1021). The concentration device (300) includes a plurality of concentrators (301) connected in series along a first direction via a concentration tube (103); the end of the first supernatant tube (101) away from the hydrolysis reactor (200) is connected to the first concentrator (301) in the first direction. The concentration temperature of the plurality of concentrators (301) along the first direction gradually increases.
2. The hydrolysis concentration system according to claim 1, characterized in that, It also includes a condenser (400); The tops of the multiple concentrators (301) are connected to the steam inlet of the condenser (400) via a first condenser tube (104).
3. The hydrolysis concentration system according to claim 2, characterized in that, It also includes a membrane reactor (500) and a return water tank (600) that are interconnected by a first pipe (105). The condensate outlet of the condenser (400) is connected to the inlet of the membrane reactor (500) through a second condenser tube (106).
4. The hydrolysis concentration system according to claim 1, characterized in that, The bottom of the last concentrator (301) along the first direction is connected to a concentration storage tank (1071) via a second pipe (107), and a first discharge valve (1072) is provided on the second pipe (107) near the concentrator (301).
5. The hydrolysis concentration system according to claim 3, characterized in that, The bottom of the hydrolysis reactor (200) is connected to a filter press (1081) via a third pipe (108); the solid material outlet of the filter press (1081) is connected to a dryer (701) via a conveyor (700), and its outlet is connected to the second condenser (106) via a fourth pipe (109); The third pipe (108) is equipped with a second discharge valve (1082) near the hydrolysis reactor (200).
6. The hydrolysis concentration system according to any one of claims 1 to 5, characterized in that, A first transfer pump (1012) is provided on the tube of the first supernatant tube (101) near the first concentrator (301) in the first direction.
7. The hydrolysis concentration system according to any one of claims 1 to 5, characterized in that, A second delivery pump (1031) is provided on the concentration tube (103) between the last two concentrators (301) in the first direction.