CN113072522B - Method for removing ethylbenzene hydroperoxide in mixed organic phase - Google Patents
Method for removing ethylbenzene hydroperoxide in mixed organic phase Download PDFInfo
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Abstract
The application relates to the field of organic impurity removal, and particularly discloses a method for removing ethylbenzene hydroperoxide in a mixed organic phase, which comprises the following steps: s1: adding NaOH solution into the organic phase, stirring for 30-60min to make ethylbenzene hydroperoxide in the organic phase completely react, and fully washing the oil phase to obtain reaction liquid; s2: after the reaction and the washing are finished, introducing the reaction liquid into a settling tank provided with a special settling plate for settling separation, and discharging a water phase to obtain a primary oil phase separation liquid; s3: adding external water into the first oil phase separation liquid, introducing the first oil phase separation liquid into a separation tank with a special settling plate after a certain oil-water ratio is reached, carrying out secondary settling separation, and discharging a water phase to obtain the oil phase separation liquid. By controlling the process parameters and specially designing the settling plates, the ethylbenzene hydroperoxide in the mixed organic phase of the styrene/propylene oxide co-production process can be removed, and a good oil-water separation effect is achieved.
Description
Technical Field
The application relates to the technical field of organic impurity removal, in particular to a method for removing ethylbenzene hydroperoxide in a mixed organic phase.
Background
In chemical production, a styrene/propylene oxide co-production process is provided, and can be used for simultaneously preparing styrene and propylene oxide, so that the production benefit is good. The technological process is that ethylbenzene is used as material and reacts with air to prepare intermediate product ethylbenzene hydroperoxide (EBHP), which is condensed and epoxidated with propylene to produce first product propylene oxide and alpha-phenylethyl alcohol, and after propylene and propylene oxide are separated, the alpha-phenylethyl alcohol is refined and dehydrated to obtain second product styrene.
In the above step, after the separation of propylene and propylene oxide, an organic peroxide containing R-OOH may remain in the remaining mixed organic phase. Since the compound containing peroxy groups is generally active in chemical property, the compound is easy to decompose and explode, and potential safety hazards exist. It is therefore necessary to remove the ethylbenzene hydroperoxide before proceeding to the next step.
The existing removal method mostly adopts an alkali liquor reaction method to convert ethylbenzene hydroperoxide into acetophenone, but has the defects that water phase and alkali liquor impurities can be introduced, and the a-phenethyl alcohol in the mixed organic phase is easy to form stable emulsion with the water phase, so that the separation of oil and water after the alkali liquor reaction is always difficult. There is therefore a need for a process for the removal of ethylbenzene hydroperoxide from the mixed phase for use in a styrene/propylene oxide co-production process.
Disclosure of Invention
In order to remove ethylbenzene hydroperoxide in the mixed organic phase of the styrene/propylene oxide co-production process and achieve a good oil-water separation effect, the application provides a method for removing ethylbenzene hydroperoxide in the mixed organic phase.
The application provides a method for removing ethylbenzene hydroperoxide in a mixed organic phase, which comprises the following steps:
s1: adding NaOH solution into the organic phase, stirring for 30-60min to ensure that ethylbenzene hydroperoxide in the organic phase completely reacts, and fully washing the oil phase to obtain reaction liquid;
s2: after the reaction and the washing are finished, introducing the reaction liquid into a settling tank for settling separation, and discharging a water phase to obtain a primary oil phase separation liquid;
s3: adding external water into the first oil-phase separation liquid, introducing the first oil-phase separation liquid into a separation tank for secondary sedimentation separation after a certain oil-water ratio is achieved, and discharging a water phase to obtain an oil-phase separation liquid;
the sedimentation tank and the separation tank are internally provided with V-shaped sedimentation plates, each sedimentation plate comprises an upper plate and a lower plate, the lower plate is obliquely arranged relative to the vertical direction, the inclination angle is 9-12 degrees, the included angle between the upper plate and the lower plate is 150-160 degrees, the length of the lower plate is 130-140mm, and the length of the upper plate is 25-30 mm;
a plurality of groups of separation holes are arranged on the settling plate along the horizontal direction, and each group of separation holes comprises a top hole, a tear hole and a tail hole; the top hole, the tear hole and the tail hole are sequentially arranged on the vertical surface from top to bottom, the top hole is formed in the top of the settling plate, the tear hole is formed in the joint of the upper plate and the lower plate, and the tail hole is formed in the bottom of the settling plate; the distance between each group of separation holes is 23-27 mm;
step S2, arranging 30-35 sedimentation plates in the sedimentation tank, wherein the diameter of a top hole is 13-15mm, the diameter of a tear hole is 11-13mm, and the diameter of a tail hole is 13-15 mm;
and step S3, 37-40 settling plates are arranged in the separating tank, the diameter of the top hole is 12-14mm, the diameter of the tear hole is 9-11mm, and the diameter of the tail hole is 12-14 mm.
By adopting the technical scheme, in the step S1, NaOH is used as alkali liquor to perform the function of washing the organic phase after reaction by using the NaOH as alkali liquor, and long-time stirring is performed, so that Na ions brought by the reaction in the organic phase are returned to the water phase, and the primary layering of oil and water is realized. Then, the oil phase separated from the separation tank finally has low water entrainment and Na ion entrainment values by sequentially carrying out two times of sedimentation in steps S2 and S3 to separate liquid drops with critical diameters of 50 μm and 30 μm respectively.
The key of the settling separation in steps S2 and S3 is a special settling plate, the settling plate is in a V shape with a short top and a long bottom, the oil-water mixture flows through the settling plate transversely from the opening direction of the V shape, when the mixture hits the settling plate, the light oil phase moves upwards along the inclined surface of the lower plate and gradually forms a continuous phase, the heavy water phase stays below the lower plate, finally the oil phase flows to the next settling plate through the top hole and the tear hole, and the water phase flows through the tail hole of the lower plate. All be equipped with a plurality of settlement plates in settling cask and the knockout drum, according to "shallow layer theory", the separation efficiency of subsiding can be improved to the multilayer settlement plate, reduces the required volume of settling cask and knockout drum. In the process, part of the water phase droplets can be carried in the oil phase moving upwards, and the continuous oil phase at the top can pass through the top holes and the residual water phase droplets can pass through the tear holes by separately arranging the top holes and the tear holes, so that the water phase droplets are prevented from continuously moving upwards to pollute the oil phase at the top layer, the continuity of the oil phase at the top layer is ensured, and the water phase droplets passing through the tear holes can be continuously separated on the next settling plate.
By controlling the diameters of the top, tear and tail holes of the settling plates in steps S2 and S3, the minimum separation diameter of the droplets can be controlled, thereby achieving progressive separation during settling on both sides, respectively. And because the liquid drops have certain demulsification effect in the process of flowing through the separation holes, the settling plate is used for settling separation, and the phenethyl alcohol can be effectively prevented from forming stable emulsion in a water phase, so that the oil-water separation effect is better.
Preferably, the tail hole on the settling plate is a long round hole; the diameter of a tail hole on a settling plate in the settling tank is 13-15mm, and the length of the tail hole is 25-28 mm; the diameter of a tail hole on a settling plate of the separation tank is 12-14mm, and the length of the tail hole is 22-25 mm.
By adopting the technical scheme, the tail hole is positioned at the bottom of the settling plate, and the water phase is a more uniform continuous phase at the position, so that the long round hole with larger circulation can be adopted on the premise of keeping the diameter (namely the width) unchanged, the passing of the water phase is accelerated, the settling efficiency is improved, and a small amount of residual oil phase liquid drops in the water phase cannot pass through due to overlarge diameter.
Preferably, the settling temperature in the settling tank and the separating tank is 38-43 ℃, and the settling time is 30-50 min.
By adopting the technical scheme, better settling efficiency and separation effect can be achieved at the settling temperature and further settling time of the optimal scheme.
Preferably, the reaction and washing temperature in step S1 is 30-50 deg.C, and the stirring speed is 60-80 r/min.
By adopting the technical scheme, the alkali liquor and the ethylbenzene hydroperoxide can be fully reflected at the temperature, so that the ethylbenzene hydroperoxide can be more thoroughly removed, and Na ions can be returned to the water phase after the reaction is completed. In the process, the low-speed stirring of 60-80r/min is adopted, so that the phenylethanol can be further prevented from forming stable emulsion in the water phase before the sedimentation is carried out.
Preferably, the aqueous phase discharged in steps S2 and S3 is continuously used as circulating water, the NaOH solution in step S1 is prepared by diluting high-concentration NaOH alkaline solution with the circulating water, and the dosage ratio of the high-concentration NaOH alkaline solution to the circulating water is controlled so that the content of NaOH in the mixed solution after the NaOH solution is added is 1-2 wt%.
By adopting the technical scheme, the efficiency of phase separation is improved by adding slightly excessive alkali liquor. And the separated water phase is recycled, so that the utilization rate of resources is improved, and the process is more environment-friendly.
Preferably, the addition amount of the circulating water and the external make-up water is controlled so that the oil-water ratio of the mixed liquid entering the settling tank and the separating tank is 4 (0.8-1.2).
By adopting the technical scheme, the oil-water ratio is kept in the separation process, and the oil phase can be helped to form a more stable continuous phase by matching with the settling plate.
Preferably, the water phase discharged from the settling tank and the separating tank is removed as part of the circulating water, and the rest is fed into an extraction tower, and ethylbenzene is used as an extraction liquid for extraction, so that the residual phenethyl alcohol and acetophenone in the water phase are recovered.
By adopting the technical scheme, a small amount of 2 percent of phenethyl alcohol and acetophenone still remain in the water phase after the settling separation is carried out, so the phenethyl alcohol and the acetophenone can be recycled by extraction, and the extracted ethylbenzene can be used as a raw material to continue the coproduction of styrene/propylene oxide, so that the organic phase is fully utilized, and the more green production is realized.
Preferably, the extraction temperature is 35-50 ℃, and the extraction time is 70-100 min.
By adopting the technical scheme, a better extraction effect can be achieved at the extraction temperature and the extraction time.
In summary, the present application includes at least one of the following beneficial technical effects:
1. according to the method, after the ethylbenzene hydroperoxide in the organic phase is reacted by using the alkali liquor and washed for a long time, the reaction liquid containing the organic phase and the water phase is obtained, then the reaction liquid is settled twice by using the settling tank and the separating tank respectively, the separation of the oil phase and the water phase is realized, and a good separation effect is achieved by adopting a special settling plate.
2. In the preferred scheme of this application, the tail hole adopts the slotted hole, has further improved sedimentation separation's efficiency.
3. In the preferred scheme of the application, preferred technological parameters in reaction washing and twice sedimentation separation processes are also provided, so that the sedimentation separation effect is further improved.
4. In the preferred scheme of this application, through carry out cyclic utilization and to the recovery of remaining organic matter in aqueous phase to the aqueous phase after the separation, improved the utilization ratio of raw materials, realize green production.
Drawings
FIG. 1 is a process flow diagram of examples and comparative examples;
fig. 2 is a schematic diagram of the structure of the settling plate of example 1;
fig. 3 is a schematic diagram of the structure of the settling plate of examples 3-4.
In the figure, 1, a settlement plate; 2. an upper plate; 3. a lower plate; 4. a separation well; 5. a top hole; 6. a tear hole; 7. a tail hole.
Detailed Description
The present application is described in further detail below with reference to the attached drawings.
Examples
Example 1: a method for removing ethylbenzene hydroperoxide in a mixed organic phase,
the process steps are as follows:
s1: as shown in figure 1, the organic phase of ethylbenzene hydroperoxide remained in the styrene/propylene oxide coproduction process is sent into a mixing tank, NaOH solution prepared from high-concentration NaOH alkali liquor and circulating water is added into the mixing tank, and the mixture is stirred for 30min at the temperature of 30 ℃ at the stirring speed of 80r/min, so as to obtain reaction liquid. The oil-water ratio in the mixing tank is 4:0.5, and the content of free NaOH after reaction is 0.5 wt%;
the NsOH reacts with ethylbenzene hydroperoxide to convert the ethylbenzene hydroperoxide into acetophenone, the water phase actually washes the oil phase in the subsequent stirring process, and Na ions brought into the oil phase in the reaction process are returned to the water phase again.
S2: and (3) conveying the reaction liquid in the mixing tank into a settling tank, arranging 30V-shaped settling plates 1 in the settling tank along the horizontal direction, enabling the reaction liquid to transversely flow through each settling plate 1 from the V-shaped opening for primary settling, wherein the settling temperature is 30 ℃, the settling time is 50min, and discharging the water phase after primary settling is finished to obtain primary oil phase separation liquid.
As shown in fig. 2, the settling plate 1 comprises an upper plate 2 and a lower plate 3, the lower plate 3 is arranged obliquely relative to the vertical direction, the inclination angle is 9 degrees, the included angle between the upper plate 2 and the lower plate 3 is 150 degrees, the length of the lower plate 3 is 130mm, and the length of the upper plate 2 is 25 mm; the settling plates 1 are provided with a plurality of groups of separation holes 4 arranged along the horizontal direction, the distance between each group of separation holes 4 is 23mm, and each settling plate 1 is provided with 100 groups of separation holes 4. Each set of separation holes 4 comprises a top hole 5, a tear hole 6 and a tail hole 7; the top hole 5, the tear hole 6 and the tail hole 7 are sequentially arranged on the vertical surface from top to bottom, the top hole 5 is arranged at the top of the settling plate 1, the tear hole 6 is arranged at the joint of the upper plate 2 and the lower plate 3, and the tail hole 7 is arranged at the bottom of the settling plate 1.
The diameter of a top hole 5 in each group of separation holes 4 on a settling plate 1 in the settling tank is 13mm, the diameter of a straight tear hole 6 is 11mm, and the diameter of a tail hole 7 is 13 mm.
S3: and (4) sending the oil-phase separation liquid obtained in the step (S2) into a separation tank, and synchronously introducing external water so as to keep the oil-water ratio in the separation tank at 4: 0.5. The separating tank is also provided with V-shaped settling plates 1 along the horizontal direction, and the number of the settling plates 1 is 37. Similarly, the liquid transversely flows through each settling plate 1 from the V-shaped opening to perform secondary settling at the settling temperature of 30 ℃ for 50min, and the water phase is discharged after the secondary settling is finished to obtain the oil phase separation liquid.
The diameter of a top hole 5 in each group of separation holes 4 on a settling plate 1 in the separation tank is 12mm, the diameter of a tear hole 6 is 9mm, and the diameter of a tail hole 7 is 12 mm.
And pumping the water phase discharged from the settling tank and the separating tank in the steps S2 and S3, returning one part of the water phase serving as circulating water to the mixing tank to mix and dilute the high-concentration NaOH alkali liquor, and pumping the other part of the water phase to the extraction tower for extraction.
The extraction is carried out by adopting ethylbenzene as extraction liquid, the extraction temperature is 35 ℃, and the extraction time is 70 min.
Example 2: a method for removing ethylbenzene hydroperoxide in a mixed organic phase,
the differences from example 1 are that the process parameters in steps S1, S2, S3 and extraction, and the design parameters of the settling tank and the settling plate in the knockout drum are different, as shown in table 1 and table 2 below.
Examples 3 to 4: a method for removing ethylbenzene hydroperoxide in a mixed organic phase,
the difference from example 1 is that the tail holes 7 of the settling plates used in the settling tank and the separation tank are oblong, the settling plate has a schematic structure as shown in fig. 3, and the diameters and lengths of the tail holes 7 are shown in table 2 below. In addition, the process parameters of the steps S1, S2, S3 and extraction are shown in table 1 below.
Examples 5 to 6: a method for removing ethylbenzene hydroperoxide in a mixed organic phase,
the difference from example 1 is that the settling temperatures in steps S2 and S3 are different, and the process parameters are specifically shown in table 1 below. In addition, the design parameters of the settling tank and the settling plate in the separation tank are shown in table 2 below.
Examples 7 to 8: a method for removing ethylbenzene hydroperoxide in a mixed organic phase,
the difference from example 1 is that the free NaOH content after the reaction of step S1 is different, and the specific parameters are shown in Table 1 below. In addition, the design parameters of the settling tank and the settling plate in the separation tank are shown in table 2 below.
Examples 9 to 10: a method for removing ethylbenzene hydroperoxide in a mixed organic phase,
the difference from example 1 is that the oil-water ratio during the sedimentation process is different, and the specific parameters are shown in table 1 below. Further the design parameters of the settling tank and the settling plate in the separation tank are shown in table 2 below.
Table 1: examples 1-10 Process parameters in Steps S1, S2, S3 and extraction
Table 2: examples 1-10 design parameters for settling plates
Comparative example
Comparative example 1: a method for removing ethylbenzene hydroperoxide in a mixed organic phase,
the difference from example 1 is that the settling tank and the separating tank used therein were straight plates disposed obliquely at an angle of 9 ° to the vertical plane, 100 groups of separation holes were horizontally arranged on the straight plates at a distance of 23mm from each other, the separation holes included a top hole at the top of the settling plate and a tail hole at the bottom of the settling plate. During the sedimentation process, the liquid flows through the sedimentation plate transversely along the inclined direction of the sedimentation plate.
30 settling plates are arranged in the settling tank, the diameter of a top hole is 13mm, and the diameter of a tail hole is 13 mm;
37 sedimentation plates are arranged in the separation tank, the diameter of a top hole is 12mm, and the diameter of a tail hole is 12 mm;
the remaining process steps are the same as in example 1.
Comparative example 2: a method for removing ethylbenzene hydroperoxide in a mixed organic phase,
the difference from example 1 is that the settlement plate is not perforated with tear holes. The design parameters of the settling tank and the settling plate in the knockout drum are shown in table 3 below.
The process steps are the same as in example 1.
Comparative examples 3 to 8: a method for removing ethylbenzene hydroperoxide in a mixed organic phase,
the difference from example 1 is that the settling plates have different design parameters, and the specific parameters are shown in table 3 below.
The process steps are the same as in example 1.
Table 3: design parameters for comparative examples 2-8 settling plates
Performance test
Test one: principle of water entrainment test in oil phase separation liquid: the water entrainment in the oil phase separation liquid is measured by adopting a Karl Fischer method, and the separation effect can be judged by comparing the water entrainment.
Test subjects: the oil-phase separation liquids of examples 1 to 10 and comparative examples 1 to 8.
The test steps are as follows: according to the national standard GB/T6283-2008 of the people's republic of China, the water content of the oil phase separation liquid of each embodiment and the comparative example is measured by a direct coulometry method, the results are expressed in a mass percentage mode, two effective values are reserved, and the test results are shown in the following table 4.
Table 4: the amount (wt%) of water entrained in the oil-phase separation liquids obtained in examples 1 to 10 and comparative examples 1 to 8
And (2) test II: principle of Na ion content test in oil phase separation liquid: the method adopts an atomic absorption spectrometry to measure the sodium content in the oil phase separation liquid, and the separation effect can be judged by comparing the sodium ion carrying capacity.
Test subjects: the oil-phase separation liquids of examples 1 to 10 and comparative examples 1 to 8.
The test steps are as follows: the Na ion content in each of the examples and comparative examples was measured by flame atomic absorption spectrometry, with reference to the general atomic absorption spectrometry rule of national Standard of the people's republic of China GB/T15337-1994, and the results were expressed as mass fractions with the result of retaining one decimal place and the test results are shown in Table 5 below.
Table 5: the amount (ppm) of sodium ions entrained in the oil-phase separation liquids obtained in examples 1 to 10 and comparative examples 1 to 8
Now the following analyses are performed in combination with the test results of test one and test two:
comparing the contents of water and sodium ions in the oil-phase separation liquids of examples 1-2 and comparative example 1 in tables 4 and 5, it can be seen that the contents of water and sodium ions in the oil-phase separation liquids of examples 1-2 are much lower than that of comparative example 1. This can show that the settling plates used in examples 1-2 have a prominent and effective separation effect compared to comparative example 1. The effective application of the V-shaped settling plate in the method for removing ethylbenzene hydroperoxide in the styrene/propylene oxide coproduction process is shown.
The oil-water mixed liquid flows through the settling plates from the V-shaped opening direction transversely during settling, when the mixed liquid meets the settling plates, the light oil phase moves upwards along the inclined surface of the lower plates and gradually forms a continuous phase, the heavy water phase stays below the lower plates, finally the oil phase flows to the next settling plate through the top holes and the tear holes, and the water phase flows through the tail holes of the lower plates. In the process, the upper plate can block the water phase droplets which are carried in the oil phase and move upwards, so that the carried water phase is discharged from the lacrimal holes, and the continuity of the upper oil phase is ensured. However, if the straight plate is adopted, the above effect cannot be achieved, and fine water phase is still mixed in the mailbox at the upper layer, so that the oil-water separation effect is poor.
Comparing the contents of water and sodium ions in the oil-phase separation liquids of examples 1-2 and comparative example 2 in tables 4 and 5, it can be seen that the contents of water and sodium ions in the oil-phase separation liquids of examples 1-2 are much lower than that of comparative example 2. This may indicate that the placement of the tear holes in the settlement plate has an important role. The reason is that during the process of sedimentation, the oil phase will gradually move upwards along the lower plate, part of the aqueous phase droplets will be carried in the upwards-moving oil phase, through the separate arrangement of the top holes and the tear holes, the continuous oil phase at the top can pass through the top holes, and the residual aqueous phase droplets can pass through the tear holes, so that the aqueous phase droplets are prevented from continuously moving upwards to pollute the oil phase at the top layer, thereby ensuring the continuity of the oil phase at the top layer, and the aqueous phase droplets passing through the tear holes can be continuously separated on the next sedimentation plate.
Comparing the contents of water and sodium ions in the oil-phase-separated liquids of examples 1-2 and comparative examples 3-8 in tables 4 and 5, it can be seen that the contents of water and sodium ions in the oil-phase-separated liquids of examples 1-2 are much lower than those of comparative examples 3-8. This indicates that the distances between the top holes, the tear holes, the tail holes, and the separation holes are in the optimum parameter range in examples 1 to 2, and a more effective oil-water separation effect can be obtained within this parameter range.
Comparing the contents of water and sodium ions in the oil-phase separation liquids of examples 1-2 and examples 3-4 in tables 4 and 5, it can be seen that the contents of water and sodium ions in the oil-phase separation liquids of examples 3-4 are lower than those of examples 1-2. This indicates that the oblong tail holes used in examples 3 to 4 can further improve the oil-water separation effect.
Comparing the contents of water and sodium ions in the oil-phase separation liquids of examples 1-2 and examples 5-6 in tables 4 and 5, it can be seen that the contents of water and sodium ions in the oil-phase separation liquids of examples 5-6 are lower than those of examples 1-2. This indicates that the settling temperature and settling time used in examples 5 to 6 are more preferable parameter ranges, and that a better oil-water separation effect can be obtained at these temperatures. This may be due to the effect of temperature on oil water surface tension and activity. The operation temperature is properly increased, which is beneficial to the digestion of small liquid drops.
Comparing the contents of water and sodium ions in the oil-phase separation liquids of examples 1-2 and examples 7-8 in tables 4 and 5, it can be seen that the contents of water and sodium ions in the oil-phase separation liquids of examples 7-8 are lower than those of examples 1-2. This indicates that the free NaOH content used in examples 7-8 is a more optimal parameter range. This is because an appropriate excess of NaOH improves the oil-water separation effect.
Comparing the contents of water and sodium ions in the oil-phase separation liquids of examples 1-2 and examples 9-10 in tables 4 and 5, it can be seen that the contents of water and sodium ions in the oil-phase separation liquids of examples 9-10 are lower than those of examples 1-2. This indicates that the oil-water ratio used for the separation in examples 9 to 10 is in a more preferable parameter range, and the use of an appropriate oil-water ratio contributes to further improvement in the oil-water separation effect.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. A method for removing ethylbenzene hydroperoxide in a mixed organic phase is characterized by comprising the following steps: the method comprises the following steps:
s1: adding NaOH solution into the organic phase, stirring for 30-60min to make ethylbenzene hydroperoxide in the organic phase completely react, and fully washing the oil phase to obtain reaction liquid;
s2: after the reaction and the washing are finished, introducing the reaction liquid into a settling tank for settling separation, and discharging a water phase to obtain a primary oil phase separation liquid;
s3: adding external water into the first oil-phase separation liquid, introducing the first oil-phase separation liquid into a separation tank for secondary sedimentation separation after a certain oil-water ratio is achieved, and discharging a water phase to obtain an oil-phase separation liquid;
the sedimentation tank and the separation tank are internally provided with V-shaped sedimentation plates (1), each sedimentation plate (1) comprises an upper plate (2) and a lower plate (3), each lower plate (3) is obliquely arranged relative to the vertical direction, the inclination angle is 9-12 degrees, the included angle between each upper plate (2) and each lower plate (3) is 150-160 degrees, the length of each lower plate (3) is 130-140mm, and the length of each upper plate (2) is 25-30 mm;
a plurality of groups of separation holes (4) are arranged on the settling plate (1) along the horizontal direction, and each group of separation holes (4) consists of a top hole (5), a tear hole (6) and a tail hole (7); the top hole (5), the tear hole (6) and the tail hole (7) are sequentially arranged on a vertical plane from top to bottom, the top hole (5) is formed in the top of the sedimentation plate (1), the tear hole (6) is formed in the joint of the upper plate (2) and the lower plate (3), and the tail hole (7) is formed in the bottom of the sedimentation plate (1); the distance between each group of separation holes (4) is 23-27 mm;
step S2, arranging 30-35 sedimentation plates (1) in the sedimentation tank, wherein the diameter of the top hole (5) is 13-15mm, the diameter of the tear hole (6) is 11-13mm, and the diameter of the tail hole (7) is 13-15 mm;
step S3, 37-40 sedimentation plates (1) are arranged in the separation tank, the diameter of the top hole (5) is 12-14mm, the diameter of the tear hole (6) is 9-11mm, and the diameter of the tail hole (7) is 12-14 mm;
the reaction solution in step S2 and the oil-water mixture solution in step S3 flow laterally through the settling plate from the V-shaped opening direction of the settling plate.
2. The method of claim 1 for removing ethylbenzene hydroperoxide from the mixed organic phase, wherein: the tail hole (7) on the settling plate (1) is a long round hole; the diameter of a tail hole (7) on a settling plate (1) in the settling tank is 13-15mm, and the hole length is 25-28 mm; the diameter of a tail hole (7) on a settling plate (1) of the separating tank is 12-14mm, and the hole length is 22-25 mm.
3. The method of claim 1 for removing ethylbenzene hydroperoxide from the mixed organic phase, wherein: the settling temperature in the settling tank and the separating tank is 38-43 ℃, and the settling time is 30-50 min.
4. The method of claim 1 for removing ethylbenzene hydroperoxide from the mixed organic phase, wherein: the reaction and washing temperature in the step S1 is 30-50 ℃, and the stirring speed is 60-80 r/min.
5. The method of claim 1 for removing ethylbenzene hydroperoxide from the mixed organic phase, wherein: and (3) continuously using the water phase part discharged in the steps S2 and S3 as circulating water, diluting the NaOH solution in the step S1 by using the high-concentration NaOH alkali solution and the circulating water, and controlling the dosage ratio of the high-concentration NaOH alkali solution to the circulating water so that the content of free NaOH in the mixed solution is 1-2wt% after the NaOH solution is added and the reaction is completed.
6. The method of claim 5 for removing ethylbenzene hydroperoxide from the mixed organic phase, wherein: the oil-water ratio of the mixed liquid entering the settling tank and the separating tank is controlled to be 4 (0.8-1.2) by controlling the addition amount of the circulating water and the external water.
7. The method of claim 5 for removing ethylbenzene hydroperoxide from the mixed organic phase, wherein: and removing the water phase discharged from the settling tank and the separating tank to obtain part of circulating water, introducing the rest into an extraction tower, extracting with ethylbenzene as an extraction liquid, and recovering the residual phenethyl alcohol and acetophenone in the water phase.
8. The method of claim 7, wherein the method comprises the steps of: the extraction temperature is 35-50 deg.C, and the extraction time is 70-100 min.
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| US5210354A (en) * | 1992-05-08 | 1993-05-11 | Arco Chemical Technology, L.P. | Propylene oxide-styrene monomer process |
| ES2197663T3 (en) * | 1998-07-20 | 2004-01-01 | Shell Internationale Research Maatschappij B.V. | PREPARATION PROCEDURE FOR STYRENE AND PROPYLENE OXIDE. |
| JP2005145880A (en) * | 2003-11-14 | 2005-06-09 | Mitsubishi Chemicals Corp | Method and apparatus for producing vinyl aromatic compound |
| CN101148278B (en) * | 2006-09-19 | 2010-11-03 | 威海广泰环保科技有限公司 | Oil-water purifying method and equipment thereof |
| CN108751512A (en) * | 2018-07-19 | 2018-11-06 | 上海洁鹿环保科技有限公司 | A kind of oil-water separation system |
| CN112010823B (en) * | 2019-05-29 | 2022-08-12 | 中国石油化工股份有限公司 | Alkylene oxide separation and benzyl alcohol purification method |
| CN110672547B (en) * | 2019-11-08 | 2022-07-12 | 万华化学集团股份有限公司 | Method for measuring content of ethylbenzene hydroperoxide |
| CN111620759B (en) * | 2020-05-21 | 2022-04-08 | 常州瑞华化工工程技术股份有限公司 | Method for preparing styrene by gas phase dehydration of phenethyl alcohol |
| CN112107886A (en) * | 2020-08-07 | 2020-12-22 | 青岛科技大学 | Separation and purification device for oil phase in oil, water and solid three-phase mixture |
| CN112174914B (en) * | 2020-10-09 | 2023-07-28 | 常州瑞华化工工程技术股份有限公司 | Method for gas phase epoxidation of olefins with hydroperoxides |
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