Process for recovering phenol wastewater by ultrasonic impinging stream liquid-liquid extraction

Abstract

The application discloses a kind of ultrasonic wave impact flow liquid-liquid extraction recovery phenol wastewater process device, and relates to a kind of recovery phenol wastewater device.The device combines ultrasonic extraction technology with impact flow technology, and when extraction process is carried out, impact flow liquid-liquid extraction technology is mainly used, and is assisted by ultrasonic wave generating device.When working, wastewater and organic solvent are sprayed through the nozzles horizontally opposite in the impact flow reactor, pre-mixed in the nozzle, fully contacted in the reactor, and the liquid-liquid mixing is strengthened under the assistance of ultrasonic system, and the liquid-liquid extraction process occurs better.The method and device have high inter-transmission efficiency and good extraction effect, can effectively recover phenol-containing wastewater, and are widely applicable, and can be used in various industrial occasions.

Description

TECHNICAL FIELD

[0001] The present application relates to a kind of recovery phenol wastewater process device, especially to a kind of ultrasonic wave impact flow liquid-liquid extraction recovery phenol wastewater process device. BACKGROUND

[0002] Phenolic wastewater is a kind of widely-sourced, harmful industrial wastewater, which needs to be pretreated before being discharged. Especially its recycling and discharge have economic value and social significance.

[0003] At present, the pretreatment and recovery of phenolic wastewater are carried out by extraction method. Extraction method is an important separation technology developed rapidly in the twentieth century. It uses the different distribution coefficients of solutes between two mutually insoluble or partially soluble liquid phases to realize the separation or purification of one or more solutes. The appropriate extractant and process can be selected according to the separation object and requirements.

[0004] However, the conventional extraction method and extraction device for treating and recycling phenolic wastewater have the problems of small raw material processing capacity, low efficiency, difficulty in separating and purifying impurities and effective components, and relatively high process cost, which affects the comprehensive economic effect of phenolic wastewater treatment and recycling.

[0005] Impinging stream is a technology that can efficiently enhance the gas-liquid mass transfer characteristics. Its main principle is to use the highly turbulent region formed by the mutual impingement of two or more streams to enhance the mass transfer between two or more phases. Therefore, it is widely used in the fields of ultrafine powder preparation, combustion, drying, extraction and absorption, etc.

[0006] Compared with conventional extraction technologies such as water boiling and alcohol precipitation, ultrasonic wave extraction is fast, inexpensive and efficient. Moreover, the raw material processing capacity of medicinal materials is doubled or several times higher, and the impurities are less, the effective components are easy to separate and purify, the ultrasonic wave extraction has little relationship with the properties of solvent and target extract, the extraction process cost is low, and the comprehensive economic benefit is remarkable.

[0007] It is undoubtedly necessary to combine the impinging stream principle and the ultrasonic wave extraction principle to propose a process device for treating and recycling phenolic wastewater. SUMMARY

[0008] The present application aims to provide an ultrasonic wave impact flow liquid-liquid extraction recovery phenol wastewater process device. The device is designed with an internal mixing nozzle. Different inlets for phenolic wastewater and extractant are arranged inside the nozzle. Through the internal components and double-channel structure, the two are fully contacted and mixed. Under the action of the strong cavitation effect, mechanical vibration disturbance effect, high acceleration, emulsification, diffusion, crushing and stirring multi-level effects generated by ultrasonic wave radiation pressure, the molecular movement frequency and speed of the substances are increased, the solvent penetration is increased, and the extraction and recovery of phenol in phenolic wastewater are accelerated and promoted.

[0009] The purpose of the present application is achieved by the following technical solutions:

[0010] The device comprises an impinging stream reactor, a liquid level meter, an internal mixing nozzle, an electromagnetic flowmeter, an ultrasonic vibrator, a stop valve, a stirrer, an ultrasonic generator, a discharge barrel, a ball valve, a liquid inlet pump, a wastewater feeding barrel and an organic feeding barrel. The bottom of the impinging stream reactor is conical, the ultrasonic vibrator is arranged at the inclined edge of the cone, and the bottom of the cone is provided with a stirrer for stirring the mixed liquid. The two nozzles are internally mixed nozzles and are composed of a conical block, a fixed ring magnet, a ring baffle, a rotating blade, two liquid distribution pieces, a movable ring magnet, a fixed nail, a sealing cover and a fixed groove. The working state of the nozzle is as follows: the organic solvent and wastewater enter the nozzle from the inlet, are stirred by the internal rotating blade, are mixed by the two complementary liquid distribution pieces, the two channels are opened simultaneously under the action of the two annular magnets repelling each other, the materials are mixed by impingement in the nozzle, and then are sprayed out after mixing at the nozzle opening to realize partial extraction.

[0011] The movable ring magnet enters the internally mixed nozzle in the direction of magnetic repulsion with the fixed ring magnet under the limitation of the inner wall of the internally mixed nozzle, the liquid distribution piece one and the liquid distribution piece two are fixed in the internally mixed nozzle through the liquid distribution piece fixing block and the fixed groove, the conical block is inserted from the middle hole of the liquid distribution piece one and the liquid distribution piece two, the top of the conical block is on the movable ring magnet, and the tail is fixed by cooperating with the liquid distribution piece one through the middle fixed groove. The nozzle tail outer thread is connected with the wastewater pipe and the extractant pipe through the nozzle tail inner thread and the organic liquid inlet, and the nozzle is fixed on the impinging stream reactor through the nozzle tail outer thread.

[0012] The phenol-containing wastewater and the extraction solution are respectively pumped out from the wastewater feeding barrel and the organic feeding barrel by the liquid inlet pump, are mixed into the internally mixed nozzle after adjusting the flow by the electromagnetic flowmeter, are sprayed out from the nozzle opening after passing through the blade, the liquid distribution piece one and the liquid distribution piece two in sequence, and impinge in the impinging stream reactor.

[0013] The adopted extractant is heavy benzene N-503 stored in the organic feeding barrel.

[0014] The ultrasonic impinging stream liquid-liquid extraction recovery phenol wastewater process device, the wastewater, such as trinitrophenol, is extracted from the wastewater feed barrel by the liquid inlet pump, is adjusted in flow by the electromagnetic flowmeter, and then is entered into the internal mixing nozzle, simultaneously, the heavy benzene N-503 solvent is extracted from the organic feed barrel by the liquid inlet pump, is adjusted in flow by the electromagnetic flowmeter, and then is entered into the internal mixing nozzle and is mixed with the trinitrophenol-containing wastewater to react.

[0015] The ultrasonic impinging stream liquid-liquid extraction recovery phenol wastewater process device, the ultrasonic generator is disturbed by the ultrasonic vibrator; the situation is observed by the liquid level meter and the pressure gauge.

[0016] The ultrasonic impinging stream liquid-liquid extraction recovery phenol wastewater process device, the heavy benzene N-503 solvent is added from the extraction agent inlet.

[0017] The ultrasonic impinging stream liquid-liquid extraction recovery phenol wastewater process device, the mixed liquid of the heavy benzene N-503 solvent and water is entered into the discharge barrel from the side outlet, after the discharge barrel is placed for a period of time, the mixed liquid is separated after being layered.

[0018] The ultrasonic impinging stream liquid-liquid extraction recovery phenol wastewater process device, the recovered wastewater is sampled and detected to carry out the next step of treatment, the heavy benzene N-503 phenol-containing solution of the extraction phase is washed by the NaOH alkali washing tower, sodium phenol is obtained, and the recovery of phenol in the phenol-containing wastewater is realized.

[0019] The advantages and effects of the present application are:

[0020] 1. The nozzle of the present application is designed with different inlets for the phenol-containing wastewater and the extraction agent, the two are fully contacted and mixed through the special internal components and the double-channel structure, and the good mixing effect is realized after being sprayed out of the nozzle; the impinging stream liquid-liquid extraction process is used as the main extraction process, and the ultrasonic system is used for auxiliary extraction. After the phenol-containing wastewater and the extraction agent mixed liquid are sprayed out of the horizontally-opposed nozzles, impinging occurs in the impinging stream reactor, a highly turbulent zone is formed, the two are fully contacted, and the extraction process is promoted. The ultrasonic system is used as auxiliary, under the action of the multi-level effects such as the strong cavitation effect, mechanical vibration, disturbance effect, high acceleration, emulsification, diffusion, crushing and stirring effect generated by the ultrasonic radiation pressure, the motion frequency and speed of the material molecules are increased, the solvent penetration is increased, and thus the phenol in the phenol-containing wastewater is recovered into the extraction agent, the extraction is promoted.

[0021] 2. The impinging stream liquid-liquid extraction technology used in the present application is based on its high turbulence, high interfacial transfer effect and high velocity gradient, etc. characteristics, relying on the impinging stream reactor to greatly improve the fluid turbulence energy, liquid-liquid interfacial transfer efficiency, make the components uniform, greatly improve the extraction efficiency. The impinging stream reactor is installed with an internal mixing nozzle on both sides, which preliminarily mixes the organic extractant and the phenol-containing wastewater in the nozzle, uses the double-channel structure inside it to make the two more fully mixed, and the ratio and input of the two are controllable. At the same time, the ultrasonic extraction technology produces turbulent effect, perturbation effect, interface effect and other additional effects in the reactor internal environment under the action of elastic mechanical vibration wave, so as to promote the occurrence of the extraction process of the two, compared with the conventional extraction method, the extraction time is short, the extraction efficiency is high, and the extractant will not cause pollution to the extractant.

[0022] 3. The device of the present application is suitable for large-scale treatment of phenol-containing wastewater in industry, and the extractant can be reused to ensure extraction and prevent material waste. The overall cost of the device is low, easy to maintain, simple to operate, and high safety factor. The method and device can be extended to many industrial applications. It has high selectivity, good separation effect, strong adaptability, simple operation, high safety factor, low extraction process cost, and significant comprehensive economic benefit, and can be extended to many industrial applications. BRIEF DESCRIPTION OF DRAWINGS

[0023] Figure 1 : The overall device schematic diagram in the present application;

[0024] Figure 2 : The half-section structure diagram of the internal mixing nozzle of the impinging stream reactor used in the method of the present application; that is Figure 1 the cross-sectional view of component 6;

[0025] Figure 3 : Figure 2 the nozzle along the A-A cross-sectional view;

[0026] Figure 4 : The liquid separation piece diagram; that is Figure 2 the component 26 (left) and component 27 (right) in the middle.

[0027] Parts in the figure: 1-pressure gauge, 2-impinging stream reactor, 3-extractant inlet, 4-liquid level meter, 5-air hole, 6-inner mixing nozzle, 7-electromagnetic flow meter, 8-ultrasonic vibrator, 9-stop valve, 10-stirrer, 11-ultrasonic generator, 12-outlet barrel, 13-ball valve, 14-liquid inlet pump, 15-waste water inlet barrel, 16-organic material inlet barrel, 17-nozzle tail external thread, 18-separation piece fixing block, 19-conical block, 20-fixed ring magnet, 21-ring baffle, 22-nozzle tail internal thread, 23-nozzle mouth, 24-waste water inlet mouth, 25-blade, 26-separation piece one, 27-separation piece two, 28-movable ring magnet, 29-second channel, 30-fixed nail, 31-sealing cover, 32-organic material inlet mouth, 33-intermediate fixed groove, 34-fixed groove. DETAILED DESCRIPTION

[0028] The application will be described in detail below with reference to the embodiments shown in the drawings.

[0029] The device of the application comprises an impinging stream reactor, a liquid level meter, an internal mixing nozzle, an electromagnetic flowmeter, an ultrasonic transducer, a stop valve, a stirrer, an ultrasonic generator, a discharge barrel, a ball valve, a liquid inlet pump, a waste water inlet barrel and an organic material inlet barrel. The bottom of the barrel of the impinging stream reactor is conical, and an ultrasonic transducer is arranged at the conical inclined edge, and a stirrer is arranged at the conical bottom to continuously stir the mixed liquid. Two horizontally-opposed nozzles are arranged on the two sides of the barrel, and the nozzles are internal mixing nozzles. The internal mixing nozzle mainly comprises a conical block, a fixed ring-shaped magnet, a ring-shaped baffle, a rotating blade, two liquid distribution pieces, a movable ring-shaped magnet, a fixing nail, a sealing cover and a fixing groove. When the nozzle works, the organic solvent and the waste water enter the nozzle from different inlets, are stirred by the rotating blade, are mixed by the two complementary liquid distribution pieces, are simultaneously opened by the two ring-shaped magnets which repel each other, are mixed in the nozzle and are sprayed out of the nozzle, so that partial extraction is realized. The mixed liquid after being sprayed out enters the reactor to be further mixed by impinging, and the material is continuously reciprocatingly oscillated in the reactor under the action of the ultrasonic wave and the stirrer, so that the material is strongly mixed, the phase-to-phase transmission and the liquid-liquid extraction process are facilitated. The extraction process of the ultrasonic-assisted impinging stream extraction technology comprises two parts of the impinging stream liquid-liquid extraction technology and the ultrasonic extraction technology. The impinging stream liquid-liquid extraction process is the main extraction process, and the ultrasonic system is used for auxiliary extraction. After the horizontally-opposed nozzles spray out the mixed liquid of the waste water containing phenol and the extractant, impinging occurs in the impinging stream reactor, a highly turbulent zone is formed, the two are fully contacted, and the extraction process is promoted. The ultrasonic system is used as an auxiliary, under the action of the multi-stage effects of the strong cavitation effect, mechanical vibration, disturbance effect, high acceleration, emulsification, diffusion, crushing and stirring effect generated by the ultrasonic radiation pressure, the motion frequency and speed of the material molecules are increased, the solvent penetration is increased, and thus the phenol in the waste water containing phenol is recovered into the extractant. Embodiment

[0030] Firstly, the movable ring-shaped magnet 28 is entered into the internal mixing nozzle 6 under the restriction of the inner wall of the internal mixing nozzle 6 in the direction of repelling the fixed ring-shaped magnet 20, the liquid distribution piece one 26 and the liquid distribution piece two 27 are fixed in the internal mixing nozzle 6 through the liquid distribution piece fixing block 18 and the fixing groove 34, the conical block 19 is inserted from the middle hole of the liquid distribution piece one 26 and the liquid distribution piece two 27, the top of the conical block 19 is abutted on the movable ring-shaped magnet 28, and the tail of the conical block 19 is fixed with the liquid distribution piece one 26 by the middle fixing groove 33. The waste water pipe and the extractant pipe are respectively connected to the nozzle tail inner thread 22 and the organic liquid inlet 32. The nozzle is fixed on the impinging stream reactor 2 by the nozzle tail outer thread 17.

[0031] After preparation, the reaction begins. Open the stop valve 9, the wastewater containing phenol and the extraction solution are respectively drawn from the wastewater feed tank 15 and the organic feed tank 16 by the liquid inlet pump 14, and then are mixed in the inner mixing nozzle 6 after the flow is adjusted by the electromagnetic flow meter 7, and then are sprayed from the nozzle port 23 after successively passing through the vane 25, the first liquid separation piece 26 and the second liquid separation piece 27, and then are impacted in the impinging stream reactor 2.

[0032] During the reaction, the ultrasonic generator 11 is turned on to disturb by the ultrasonic vibrator 8, and the stirring machine 10 is turned on to rotate. The whole device begins to work, and during the working, the inlet 3 and the air hole 5 are used according to the requirement, and the situation is observed by the liquid level meter 4 and the pressure gauge 1. Finally, the mixed solution is introduced into the discharge tank 12 from the upper side outlet of the inner mixing nozzle 6, and then is separated after being left still.

[0033] Before the reaction begins, the inner mixing nozzle 6 is installed according to the sequence in the foregoing detailed description, and then the power is turned on after the line connection is determined to be safe and the pipeline connection is determined to be correct. The wastewater containing phenol to be treated is the wastewater containing trinitrophenol stored in the wastewater feed tank 15, and the extraction agent used is heavy benzene N-503 stored in the organic feed tank 16. After the stop valve 9 is opened, the wastewater containing trinitrophenol is drawn from the wastewater feed tank 15 by the liquid inlet pump 14, and then is introduced into the inner mixing nozzle 6 after the flow is adjusted by the electromagnetic flow meter 7, and at the same time, the heavy benzene N-503 solvent is drawn from the organic feed tank 16 by the liquid inlet pump 14, and then is introduced into the inner mixing nozzle 6 after the flow is adjusted by the electromagnetic flow meter 7 to be mixed with the wastewater containing trinitrophenol. The ultrasonic generator 11 is turned on to disturb by the ultrasonic vibrator 8. The situation is observed by the liquid level meter 4 and the pressure gauge. The heavy benzene N-503 solvent is added from the extraction agent inlet 3 according to the situation. Finally, the mixed solution of the heavy benzene N-503 solvent and water is introduced into the discharge tank 12 from the side outlet, and then is separated after the mixed solution is left still for a period of time and is layered. The recovered wastewater is sampled and detected for the next treatment, the heavy benzene N-503 containing phenol in the extraction phase is washed by the NaOH alkali washing tower, and finally, sodium phenol is obtained, so that the phenol in the wastewater containing phenol is recovered.

[0034] The above examples are only used to illustrate the technical solutions of the present application but not limit the present application. Although the present application is described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or replaced equivalently without departing from the purpose and scope of the present application, and all of them should be covered in the scope of the claims of the present application.

Claims

1. A process for the recovery of phenolic wastewater by ultrasonic impinging stream liquid-liquid extraction, characterized in that, The device comprises an impinging stream reactor, a liquid level meter, an internal mixing nozzle, an electromagnetic flowmeter, an ultrasonic transducer, a stop valve, a mixer, an ultrasonic generator, a discharge barrel, a ball valve, a liquid inlet pump, a wastewater feeding barrel, an organic material feeding barrel; wherein the bottom of the impinging stream reactor cylinder is conical, the conical slope is provided with an ultrasonic transducer, and the conical bottom is provided with a mixer for stirring the mixed liquid; two horizontally-opposed nozzles are arranged on the two sides of the cylinder, and the nozzles are internal mixing nozzles; the internal mixing nozzle mainly comprises a conical block, a fixed ring-shaped magnet, a ring-shaped baffle, a rotating blade, two liquid distribution pieces, a movable ring-shaped magnet, a fixing nail, a sealing cover, a fixed groove and two second channels; the working state of the nozzle is as follows: the extractant and the wastewater enter the nozzle from the inlet respectively, are stirred by the internal rotating blade, are mixed by the two complementary liquid distribution pieces, the two second channels are opened simultaneously under the action of the fixed ring-shaped magnet and the movable ring-shaped magnet which repel each other magnetically, the materials are mixed by impingement in the nozzle, and then are sprayed out after mixing at the nozzle opening, so that partial extraction is realized; then the mixed liquid after spraying enters the impinging stream reactor to further impinge and mix, under the action of the ultrasonic transducer and the mixer, the materials are continuously reciprocatingly oscillated in the reactor, are strongly mixed, and are transferred between phases, so that the liquid-liquid extraction process is completed. The movable ring-shaped magnet enters the internal mixing nozzle in the direction of magnetic repulsion with the fixed ring-shaped magnet under the limitation of the inner wall of the internal mixing nozzle, the liquid distribution piece one and the liquid distribution piece two are fixed in the internal mixing nozzle through the liquid distribution piece fixing block and the fixed groove, the conical block is inserted from the middle hole of the liquid distribution piece one and the liquid distribution piece two, the top of the conical block is abutted on the movable ring-shaped magnet, and the tail of the conical block is fixed by cooperation of the middle fixed groove and the liquid distribution piece one; the wastewater pipe and the extractant pipe are connected to the nozzle tail inner thread and the organic liquid inlet respectively; the internal mixing nozzle is fixed on the impinging stream reactor through the nozzle tail outer thread. The wastewater containing phenol and the extractant are respectively drawn out from the wastewater feeding barrel and the organic material feeding barrel by the liquid inlet pump, are mixed into the internal mixing nozzle after the flow is adjusted by the electromagnetic flowmeter, and then are sprayed out from the nozzle opening after passing through the rotating blade, the liquid distribution piece one and the liquid distribution piece two components to impinge in the impinging stream reactor. The ultrasonic generator disturbs through the ultrasonic transducer, and the mixer blade starts to rotate; the mixed liquid enters the discharge barrel from the upper part side outlet of the internal mixing nozzle, and is separated after standing.

2. The process for recovery of phenolic wastewater by ultrasonic impinging stream liquid-liquid extraction according to claim 1, wherein, The extractant is N-503 solvent which is stored in the organic material feeding barrel.

3. The process as claimed in claim 1, wherein the said process is an ultrasonic impinging stream liquid-liquid extraction process for recovery of phenolic wastewater. The wastewater is drawn out from the wastewater feeding barrel by the liquid inlet pump, is mixed into the internal mixing nozzle after the flow is adjusted by the electromagnetic flowmeter, and the N-503 solvent is drawn out from the organic material feeding barrel by the liquid inlet pump, is mixed into the internal mixing nozzle after the flow is adjusted by the electromagnetic flowmeter, and is mixed with the wastewater containing trinitrophenol.

4. The process as claimed in claim 1, wherein the said process is an ultrasonic impinging stream liquid-liquid extraction process for recovery of phenolic wastewater. The ultrasonic generator disturbs through the ultrasonic transducer, and the situation is observed through the liquid level meter and the pressure gauge.

5. The process as claimed in claim 2, wherein the said process is an ultrasonic impinging stream liquid-liquid extraction process for recovery of phenolic wastewater. The N-503 solvent is added from the extractant inlet.

6. The process as claimed in claim 2, wherein the said process is an ultrasonic impinging stream liquid-liquid extraction process for recovery of phenolic wastewater. The mixed liquid of the N-503 solvent and the wastewater enters the discharge barrel from the side outlet, the discharge barrel is left to stand, and the mixed liquid is separated after stratification.

7. The process as claimed in claim 1, wherein the said process is an ultrasonic impinging stream liquid-liquid extraction process for recovery of phenolic wastewater. The recovered waste water is sampled and detected for next step treatment, and the N-503 phenol-containing solution of the extraction phase is washed by a NaOH alkali washing tower to obtain sodium phenate, so as to realize phenol recovery of the waste water containing phenol.

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