Phase separation apparatus for continuous deacidification of acid-containing flavor intermediates

Abstract

A phase separation device for continuous deacidification of acidic fragrance intermediates includes a horizontal container with an inlet perforated plate distributor, a downstream fiber mesh disc, a V-shaped stratified plate assembly, and a heavy phase cylinder in the settling section. The device utilizes laminar flow uniform distribution → wetting and collision of the fiber mesh disc to promote droplet coarsening → accelerated settling by the stratified plate assembly → automatic drainage via a valve linked to the interface meter in the heavy phase cylinder to complete the continuous separation of the acidic and light phases. This device eliminates the need for sodium hydroxide alkaline washing and static separation, avoiding emulsification risks, achieving residual sulfuric acid <200ppm, reducing wastewater discharge by over 90%, reducing footprint by 30%, consuming near-zero energy, and having a service life of up to 10 years. Equipped with dual differential pressure monitoring and online drainage control, it ensures continuous and efficient operation and stable product quality. It is suitable for deacidification of various acidic oil-phase systems and can be widely applied in fragrance, fine chemical, and related mixed liquid separation processes.

Description

Technical Field

[0001] This utility model belongs to the field of chemical separation technology, and in particular relates to a phase separation device for continuous deacidification of acidic fragrance intermediates. Background Technology

[0002] In the production of fragrances, 72% sulfuric acid is required to react with raw materials to generate fragrance intermediates (homologues of benzene) containing 15% C10 olefins and 85% benzene series materials. The fragrance intermediates produced in this reaction carry a large amount of sulfuric acid. The traditional treatment method involves first removing the sulfuric acid from the fragrance intermediates using an alkaline washing tower, then separating the alkaline solution and the fragrance intermediates by settling. The upper layer (fragrance intermediates after sulfuric acid removal) is then used for final purification in a distillation tower, while the lower layer (alkaline wastewater) is sent to wastewater treatment plants.

[0003] Traditional methods of handling this issue have the following problems:

[0004] 1. A large amount of sodium hydroxide is consumed in the alkaline washing tower section;

[0005] 2. The static separation section generates a large amount of alkaline wastewater;

[0006] 3. There is a risk of emulsification of fragrance intermediates in the static separation process (emulsification of fragrance intermediates will lead to poor quality of the final fragrance, or even the formation of the final fragrance). Utility Model Content

[0007] To address the problems of existing fragrance desulfurization processes that rely heavily on alkaline washing towers and settling separation, resulting in high sodium hydroxide consumption, large amounts of alkaline wastewater discharge, high risk of emulsification during settling, large equipment footprint, and high energy consumption, this invention proposes a novel physical phase separation device. This device uses a horizontal container as a carrier, with a perforated plate distributor, a fiber mesh module, and a stratification plate module sequentially arranged inside the container inlet. A settling zone and a heavy phase cylinder are located downstream. The acidic fragrance intermediate first achieves laminar flow uniformity through the perforated plate distributor, then undergoes acid droplet coarsening through wetting and collision with the fiber mesh module, followed by accelerated settling and stratification through the V-shaped stratification plate assembly. Finally, the acidic phase and the deacidified fragrance intermediate are continuously discharged from the heavy phase outlet and light phase outlet. The entire process requires no chemical reagents and achieves efficient and continuous physical deacidification through gravity and interface automatic control.

[0008] To achieve the above-mentioned technical objectives, the technical solution adopted by this utility model is as follows:

[0009] A phase separation apparatus for continuous deacidification of acidic flavor intermediates, comprising a horizontal container, the horizontal container including:

[0010] At least one orifice plate distributor is disposed inside the inlet of the horizontal container to ensure that the incoming acidic fragrance intermediate is uniformly distributed in a laminar flow manner.

[0011] A fiber mesh module, located downstream of the perforated plate distributor, is used to capture and aggregate coarsely dispersed acid droplets;

[0012] A layered plate module, located downstream of the fiber mesh module, comprises multiple rows of folded plate groups for accelerating the stratified sedimentation of coalesced droplets;

[0013] A settling zone is located downstream of the layered plate module. A heavy phase cylinder is provided in the settling zone, and the heavy phase cylinder is connected to the interior of the horizontal container.

[0014] The heavy phase outlet is located at the bottom of the heavy phase cylinder and is used to discharge the separated acid phase.

[0015] The light phase outlet, located on the side of the settling zone, is used to discharge the deacidified fragrance intermediates.

[0016] In some technical solutions, the orifice plate distributor has an opening ratio of 30% to 60%.

[0017] In some technical solutions, the fiber mesh module adopts a mechanically woven fiber mesh disc, and the mesh size of the fiber mesh disc is less than 200um.

[0018] In some technical solutions, the layered plate module includes at least 10 columns of folded plate groups, with a spacing of 10 to 30 mm between adjacent folded plate groups. Each column of folded plate groups consists of several vertically and parallelly arranged V-shaped plate groups with their openings facing upwards. The spacing between adjacent V-shaped plate groups is 5 to 30 mm.

[0019] Some technical solutions also include a first pressure transmitter and a second pressure transmitter, which are respectively installed between the orifice plate distributor and the fiber mesh module and between the fiber mesh module and the layered plate module, for monitoring the pressure difference before and after the fiber mesh module.

[0020] In some technical solutions, the heavy phase cylinder is equipped with two sight glasses and an interface gauge, and the interface gauge is linked with an automatic drain valve to automatically open or close the heavy phase outlet according to the heavy phase liquid level.

[0021] In some technical solutions, the automatic drain valve is driven by an electric actuator or a pneumatic actuator to achieve online control of heavy phase draining.

[0022] Some technical solutions also include a backwashing pipeline and a cleaning valve connected to the fiber mesh module for online cleaning or replacement of the fiber mesh module.

[0023] In some technical solutions, the horizontal container has a material inlet in front of the orifice plate distributor, a material outlet behind the settling zone, an exhaust port at the top, and a drain port at the bottom.

[0024] In some technical solutions, the horizontal container is cylindrical and its axis is set horizontally.

[0025] The present invention, by adopting the above technical solution, has at least the following beneficial effects:

[0026] 1. This utility model device adopts a purely physical separation method, eliminating the need for any sodium hydroxide or other chemical reagents, to achieve the deacidification and separation of high-concentration sulfuric acid and fragrance intermediates, completely eliminating the dependence of traditional alkaline washing processes on alkali solutions and wastewater. Compared with existing technologies, this utility model can reduce wastewater discharge by more than 90%, significantly reducing environmental disposal costs and meeting the requirements of green production and clean processes.

[0027] 2. Since the deacidification process is carried out continuously in a dynamic flow state, the emulsification risk and oleic acid interface instability caused by static separation are avoided, ensuring that the particle size distribution and physical properties of the fragrance intermediates are not damaged. The color, aroma and purity of the final product can be maintained at the best state, which significantly improves the quality of fragrance and the reliability of the process.

[0028] 3. This invention achieves rapid coarsening and stratification of acid droplets through a three-stage synergistic structure: perforated plate distributor → fiber mesh aggregation → V-shaped stratified plate sedimentation. This results in extremely high deacidification efficiency, and the residual sulfuric acid content in fragrance intermediates can be stably controlled at <200ppm. Compared with single sedimentation or coarse separation technologies, this device reduces processing time by more than 50% for the same throughput, significantly accelerating the production cycle.

[0029] 4. The entire unit is compactly integrated into a single horizontal container, reducing the floor space by more than 30% compared to traditional alkaline washing towers and settling tanks; and all separation units are driven by gravity and intelligent liquid level valves, requiring no additional power source, with energy consumption close to zero, significantly reducing operating costs and making it suitable for rapid deployment in small and medium-sized factories.

[0030] 5. The device is equipped with two-stage differential pressure transmitters, upper and lower sight glasses of the heavy phase cylinder, and an interface gauge, which can monitor wire mesh blockage and heavy phase liquid level in real time, and automatically open / close the acid drain valve to achieve unattended continuous online operation; all liquid-contacting parts are made of sulfuric acid corrosion-resistant materials, with an expected service life of up to 10 years, effectively ensuring the long-term stability and safety of production. Attached Figure Description

[0031] Figure 1 This is a schematic diagram of the phase separation device for continuous deacidification of acidic fragrance intermediates as described in an embodiment of the present invention.

[0032] Icon labels:

[0033] N1—Material inlet, N2—Material outlet, N3—Dense phase outlet, N4—First discharge port, N5—Second discharge port, N6—First differential pressure gauge port, N7—Second differential pressure gauge port, N8—First level gauge port, N9—Second level gauge port, N10—Exhaust port;

[0034] 11—Perforated plate distributor, 12—Fiber mesh disc, 13—Layered plate assembly, 14—Settling section. Detailed Implementation

[0035] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the specific implementation methods of the present invention will be described below with reference to the accompanying drawings. Obviously, the drawings described below are merely some embodiments of the present invention. For those skilled in the art, other drawings and other implementation methods can be obtained based on these drawings without any creative effort.

[0036] To keep the drawings concise, each figure only schematically shows the parts relevant to the invention, and these do not represent the actual structure of the product. Furthermore, to facilitate understanding, in some figures, only one of components with the same structure or function is schematically depicted, or only one is labeled. In this document, "one" not only means "only one," but can also mean "more than one."

[0037] It should also be further understood that the term “and / or” as used in this application specification and the appended claims means any combination of one or more of the associated listed items and all possible combinations, and includes such combinations.

[0038] In this document, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to mechanical connections or electrical connections; they can refer to direct connections or indirect connections through an intermediate medium; and they can refer to the internal communication between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0039] Furthermore, in the description of this application, the terms "first," "second," etc., are used only to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0040] In this embodiment, as Figure 1This invention provides a phase separation device for continuous deacidification of acidic fragrance intermediates. The entire device is supported by a horizontal cylindrical container. One end of the container is connected to a material inlet N1 via a flange pipe for receiving fragrance intermediates containing 72% sulfuric acid. An exhaust port N10 is located at the top of the container to release the gas phase within the system and maintain pressure balance within the container. A material outlet N2 is located in the middle of the container side wall, connected via a flange to a subsequent distillation column or storage tank for continuous output of the deacidified fragrance intermediates. A heavy phase outlet N3, a first clean outlet N4, and a second clean outlet N5 are arranged side-by-side at the bottom of the container. All three are connected to an acid recovery pipeline via valves for quantitative or continuous discharge of the separated acid phase. A first differential pressure gauge N6, a second differential pressure gauge N7, a first level gauge N8, and a second level gauge N9 are respectively installed on the upper part and tail of the container wall, and pressure sensors, interface gauges, and sight glasses are installed to achieve online monitoring of the pressure drop before and after the wire mesh coalescing module and the liquid level in the heavy phase cylinder.

[0041] After the acidic fragrance intermediate enters through the material inlet N1, it first encounters the perforated plate distributor 11 fixed inside the container inlet. The perforated plate distributor 11 is connected to the inlet pipe via a flange, and its opening ratio can be adjusted within the range of 30% to 60%, converting turbulent flow into laminar flow and achieving uniform distribution across the container cross-section, ensuring the uniformity of subsequent fiber mesh module processing. After flowing out of the perforated plate distributor 11, the fluid enters the fiber mesh disc 12 via a stainless steel support ring and clamp fixing mechanism. The fiber mesh disc 12 is mechanically woven from polypropylene or stainless steel wire with a mesh size <200μm and acid-loving filaments. The outer edge of the disc is clamped within the support ring, and a cleaning flange is located in the center, allowing for quick connection to the backwash pipeline for online rinsing or backwashing to maintain the coalescence effect. Through wetting, collision, and coalescence mechanisms, the dispersed acid droplets on the fiber surface of the fiber mesh disc 12 repeatedly impact and grow. Once they reach the threshold particle size, they detach under gravity and enter the stratification zone.

[0042] The downstream layered plate assembly 13 is bolted to the fiber mesh tray support, and the bottom of the support is connected to the flange of the settling section 14. The layered plate assembly 13 contains at least 10 rows of V-shaped folded plates, each row consisting of several vertically parallel V-shaped plates. The plate spacing is adjustable from 10mm to 30mm, and the intraplate spacing is 5mm to 30mm. All plates have their openings facing upwards, forming an umbrella-like shape to maximize the plate surface impact area and shorten the droplet sliding distance. The coalesced acid droplets that detach quickly slide along the folded plates towards the settling section 14 and concentrate in the heavy phase cylinder at the bottom of the settling zone.

[0043] During operation, the control system starts the feed pump to input material into the material inlet N1 at a preset flow rate (e.g., 150 m³ / h), while simultaneously opening the material outlet N2 valve and maintaining it at 80% opening, and closing the first discharge port N4 and the second discharge port N5. The system monitors the pressure drop at the first differential pressure gauge port N6 and the second differential pressure gauge port N7 in real time. When the pressure drop exceeds 50 kPa, the PLC is triggered to automatically interrupt the feeding and switch to backwashing: the valve of the material inlet N1 is closed, the channel of the first discharge port N4 or the second discharge port N5 is opened, and cleaning fluid is introduced to backwash the fiber mesh disc 12 at 50 L / min until the pressure drop returns to normal, after which feeding is resumed. The interface gauge (sight glass) inside the heavy phase cylinder provides feedback on the liquid level through the first level gauge port N8 and the second level gauge port N9. When the liquid level rises to the position of the first level gauge port N8, the PLC drives the electric drain valve to open automatically, discharging the acid phase from the heavy phase outlet N3 at a rate of 20L / min. The valve automatically closes when the liquid level drops to the position of the second level gauge port N9, ensuring continuous and accurate drainage of the acid phase. The exhaust port N10 at the top of the system remains slightly open to prevent negative pressure and gas retention.

[0044] To adapt to different working conditions, the structural parameters of the preferred orifice plate distributor 11, fiber mesh disc 12, and layered plate assembly 13 in this embodiment can be replaced as follows: the orifice plate distributor 11 can be a bubble cap type or annular porous tube type structure to cope with high viscosity systems; the fiber mesh disc 12 can also be replaced with structured packing, static mixer, or porous media packing module; the layered plate assembly 13 can be an inclined plate internal or honeycomb metal packing to obtain the same layering performance; the settling section 14 can be changed to an elliptical end cap with an inclined bottom plate or a rectangular cross-section container for more flexible docking with existing tank farms; the automatic valve actuator can be electric, pneumatic, or hydraulic, and a manual bypass device can be added to enhance on-site emergency response capabilities.

[0045] Through the above embodiments, the device can deacidify fragrance intermediates containing 72% sulfuric acid to residual acid <200ppm without any chemical reagents, a settling section, or additional energy consumption. This achieves a comprehensive and excellent effect, including eliminating emulsification risk, reducing wastewater discharge by 90%, reducing floor space by 30%, near-zero energy consumption, online monitoring, and long-life operation.

[0046] The above-described embodiments are merely illustrative of several implementations of this utility model, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of this utility model patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this utility model, and these all fall within the protection scope of this utility model. Therefore, the protection scope of this utility model should be determined by the appended claims.

Claims

1. A phase separation apparatus for continuous deacidification of acid-containing flavour intermediate, characterized in that, A horizontal container is provided, the horizontal container comprising: At least one orifice plate distributor is disposed inside the inlet of the horizontal container to ensure that the incoming acidic fragrance intermediate is uniformly distributed in a laminar flow manner. A fiber mesh module, located downstream of the perforated plate distributor, is used to capture and aggregate coarsely dispersed acid droplets. The fiber mesh module is a mechanically woven fiber mesh disc, which is made of polypropylene or stainless steel wire with a mesh size of less than 200μm and acid-loving filaments. It is used to make the dispersed acid droplets grow by impact on the fiber surface and fall off under the action of gravity. A layered plate module, located downstream of the fiber mesh module, comprises multiple rows of folded plate groups for accelerating the stratified sedimentation of coalesced droplets; A settling zone, located downstream of the layered plate module, is used to receive the acid phase and the deacidified fragrance intermediate after settling and stratification by the layered plate module. The settling zone is equipped with a heavy phase cylinder, which is connected to the interior of the horizontal container. The heavy phase cylinder is equipped with two sight glasses and an interface gauge. The interface gauge is linked to an automatic drain valve, which is used to automatically open or close the heavy phase outlet according to the heavy phase liquid level. The automatic drain valve is driven by an electric actuator or a pneumatic actuator. The heavy phase outlet is located at the bottom of the heavy phase cylinder and is used to discharge the separated acid phase. The light phase outlet, located on the side of the settling zone, is used to discharge the deacidified fragrance intermediates.

2. The phase separation device of claim 1, wherein, The orifice plate distributor has an opening ratio of 30% to 60%.

3. The phase separation device of claim 1, wherein, The layered plate module includes at least 10 columns of folded plate groups, with a spacing of 10-30mm between adjacent folded plate groups. Each column of folded plate groups consists of several vertically and parallelly arranged V-shaped plate groups with the openings facing upwards. The spacing between adjacent V-shaped plate groups is 5-30mm.

4. The phase separation device of claim 1, wherein, It also includes a first pressure transmitter and a second pressure transmitter, which are respectively installed between the orifice plate distributor and the fiber mesh module and between the fiber mesh module and the layered plate module, for monitoring the pressure difference before and after the fiber mesh module.

5. The phase separation device of claim 1, wherein, It also includes a backwashing pipeline and a cleaning valve connected to the fiber mesh module for online cleaning or replacement of the fiber mesh module.

6. The phase separation device of claim 1, wherein, The horizontal container has a material inlet in front of the perforated plate distributor, a material outlet behind the settling zone, an exhaust port at the top, and a drain port at the bottom.

7. The phase separation device of claim 1, wherein, The horizontal container is cylindrical and its axis is set horizontally.

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