CN218421084U - Preparation facilities of o-phenylphenol - Google Patents
Preparation facilities of o-phenylphenol Download PDFInfo
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- CN218421084U CN218421084U CN202222587280.3U CN202222587280U CN218421084U CN 218421084 U CN218421084 U CN 218421084U CN 202222587280 U CN202222587280 U CN 202222587280U CN 218421084 U CN218421084 U CN 218421084U
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Abstract
The utility model discloses a preparation facilities of o phenyl phenol relates to the preparation technical field of o phenyl phenol. The method comprises a first-stage reaction unit, a second-stage reaction unit, a third-stage reaction unit and a rectification unit, wherein the first-stage reaction unit is used for obtaining an intermediate product 2- (1-hydroxycyclohexyl) cyclohex-1-one by taking cyclohexanone as a raw material and performing condensation reaction; the second-stage reaction unit is used for performing dehydration-hydrogenation step of 2- (1-hydroxycyclohexyl) cyclohex-1-one and obtaining o-cyclohexylcyclohexanone (containing cis-trans isomers); the third-stage reaction unit is used for completing the dehydrogenation step of o-cyclohexyl cyclohexanone (cis-trans isomerization) and obtaining a crude o-phenylphenol product; the rectification unit is used for carrying out secondary rectification on the o-phenylphenol and obtaining the o-phenylphenol. The utility model discloses a device preparation o phenyl phenol has avoided unsaturated dimer isomer's formation to the device can realize continuous production, improves the production efficiency of o phenyl phenol.
Description
Technical Field
The utility model relates to a preparation technical field of o phenyl phenol, concretely relates to preparation facilities of o phenyl phenol.
Background
The preparation method of o-phenylphenol mainly comprises a dibenzopyran method, a biphenyl sulfonation method, a phenol method and a cyclohexanone condensation dehydrogenation method, wherein in the cyclohexanone condensation dehydrogenation method, the main process flow is as follows:
(1) Condensing and dehydrating cyclohexanone to generate unsaturated dimer, and rectifying the unsaturated dimer to remove unreacted cyclohexanone; (2) Then carrying out dehydrogenation reaction on the unsaturated dimer to obtain a crude product of o-phenylphenol; (3) And rectifying, crystallizing and slicing the crude product to obtain the finished product of the o-phenylphenol.
In the above process, unsaturated dimer comprising cyclohexenyl cyclohexanone and cyclohexenyl alkylidene cyclohexanone isomers can be generated, both isomers have carbon-carbon double bond in the molecule, and the isomers are unstable in chemical property, easy to generate self-polymerization, poor in storage stability, and can be slowly oxidized in air to show red color. Meanwhile, when the two isomers are dehydrogenated to prepare o-phenylphenol, side reactions such as cracking and polymerization are accompanied to generate impurities such as phenol, benzene and polymer, which adversely affects the quality of o-phenylphenol products, thereby resulting in low product yield and poor quality.
Therefore, the preparation device of the o-phenylphenol is improved, so that the process route of the preparation device is changed, and the generation of unsaturated dimers and other related technologies is avoided.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a preparation facilities of o-phenylphenol prepares o-phenylphenol through the device, has avoided unsaturated dimer isomer's formation, can improve the production efficiency of o-phenylphenol.
In order to realize the purpose, the utility model adopts the following technical scheme:
the preparation device of the o-phenylphenol comprises a first-stage reaction unit, a second-stage reaction unit, a third-stage reaction unit and a rectification unit, wherein the first-stage reaction unit is used for obtaining an intermediate product 2- (1-hydroxycyclohexyl) cyclohex-1-one by taking cyclohexanone as a raw material and carrying out condensation reaction;
the intermediate product obtained by the first-stage reaction unit is introduced into the second-stage reaction unit;
the second-stage reaction unit is used for performing dehydration-hydrogenation step of 2- (1-hydroxycyclohexyl) cyclohex-1-one and obtaining o-cyclohexylcyclohexanone;
introducing o-cyclohexyl cyclohexanone obtained by the second-stage reaction unit into the third-stage reaction unit;
the three-stage reaction unit is used for completing the dehydrogenation step of o-cyclohexyl cyclohexanone and obtaining a crude o-phenylphenol product;
the o-phenylphenol obtained by the third-stage reaction unit is introduced into the rectification unit;
the rectification unit is used for carrying out secondary rectification on the o-phenylphenol and obtaining the o-phenylphenol.
As a preferred scheme of the utility model, the first-stage reaction unit comprises a first fixed bed reaction tower, a condensation reaction liquid buffer tank, a first rectification tower and a condensation crude product buffer tank which are connected in sequence, the top of the first fixed bed reaction tower is provided with a feed inlet, the bottom of the first fixed bed reaction tower is provided with a discharge outlet, cyclohexanone enters from the feed inlet at the top of the first fixed bed reaction tower, the middle part of the first fixed bed reaction tower is provided with a first catalyst, condensation reaction occurs under the action of the first catalyst, and a mixed liquid obtained by reaction enters into the condensation reaction liquid buffer tank from the discharge outlet at the bottom of the first fixed bed reaction tower;
the condensation reaction liquid buffer tank is connected with the first rectifying tower, the condensation reaction liquid enters from the top of the first rectifying tower, and the 2- (1-hydroxycyclohexyl) cyclohex-1-one obtained by rectifying in the first rectifying tower is introduced into the condensation crude product buffer tank.
As another preferred scheme of the utility model, the second-stage reaction unit comprises a second fixed bed reaction tower, a first preheating heat exchanger, a second preheating heat exchanger, a first cooler and an o-cyclohexyl cyclohexanone (cis-trans isomerization) buffer tank; the first preheating heat exchanger is positioned between the condensation crude product buffer tank and the second fixed bed reaction tower and is used for preheating the 2- (1-hydroxycyclohexyl) cyclohex-1-one in the condensation crude product buffer tank to a certain temperature;
the 2- (1-hydroxycyclohexyl) cyclohex-1-one preheated by the first preheating heat exchanger enters from the top of the second fixed bed reaction tower;
the second preheating heat exchanger is connected with a hydrogen pipeline and is used for preheating hydrogen to a certain temperature, and the preheated hydrogen enters from the top of the second fixed bed reaction tower;
and a second catalyst is arranged in the middle of the second fixed bed reaction tower, dehydration-hydrogenation reaction is carried out under the action of the second catalyst, reaction liquid obtained after reaction is discharged from an outlet at the bottom of the second fixed bed reaction tower and enters the first cooler, the first cooler is used for cooling the reaction liquid, and the cooled o-cyclohexylcyclohexanone (cis-trans-isomerization) is introduced into the o-cyclohexylcyclohexanone (cis-trans-isomerization) buffer tank.
Preferably, the third preheating heat exchanger is connected with the o-cyclohexylcyclohexanone (cis-trans isomerization) buffer tank and is used for preheating the o-cyclohexylcyclohexanone (cis-trans isomerization) to a certain temperature;
and (2) feeding preheated cyclohexyl cyclohexanone (cis-trans-isomerization) from the top of the third fixed bed reaction tower, arranging a third catalyst in the middle of the third fixed bed reaction tower, carrying out dehydrogenation reaction under the action of the third catalyst, feeding reaction liquid obtained after the reaction into the second cooler for cooling, and introducing the obtained crude o-phenylphenol into the crude o-phenylphenol buffer tank after cooling.
Preferably, the rectification unit comprises a second rectification tower and a third rectification tower, the second rectification tower is connected with the o-phenylphenol crude product buffer tank, and the third rectification tower is connected with the second rectification tower;
the second rectifying tower is used for removing light components and water in the crude o-phenylphenol product;
and the third rectifying tower is used for collecting o-phenylphenol.
Preferably, the third fixed bed reaction tower comprises a gas diffusion zone, a gas buffer zone and a main reaction buffer zone, the gas diffusion zone is located at the top of the third fixed bed reaction tower, the gas buffer zone is of an inverted circular truncated cone structure, and gas diffusion holes are formed in the gas buffer zone and are communicated with the main reaction buffer zone through the gas diffusion holes.
Preferably, a gas diffuser is arranged in the gas diffusion area, and the gas diffuser is positioned at the top of the third fixed bed reaction tower.
Preferably, the outer wall of the main reaction buffer zone is provided with a heating coil, and the heating coil is used for providing the required temperature for the third fixed bed reaction tower.
Preferably, the main reaction buffer zone is provided with a plurality of equally spaced trays, and the catalyst III is arranged on each tray.
Preferably, a pressure measuring hole and a temperature measuring hole are arranged on the side wall of the middle part of the third fixed bed reaction tower; the o-cyclohexyl cyclohexanone comprises two cis-trans isomers.
In order to facilitate the control of the feeding amount, the above-mentioned device for preparing o-phenylphenol further comprises a metering pump, for example, a metering pump is arranged on a pipeline connected with the feeding port of the first fixed bed reaction tower, so that the feeding amount of cyclohexanone is conveniently controlled, and the metering pumps are arranged on a pipeline between the condensation reaction liquid buffer tank and the first rectifying tower, a pipeline between the condensation crude product buffer tank and the feeding port of the second fixed bed reaction tower, and a pipeline between the o-cyclohexylcyclohexanone (cis-trans-isomer) buffer tank and the third preheating heat exchanger.
The first catalyst is macroporous strong alkali type anion exchange resin which is one or the combination of two or three of IRA-900, PA 308 or MP-500.
The above-mentioned second catalyst is any one of 1% Ru-5% phosphotungstic acid/activated carbon, 1% Rh-5% phosphotungstic acid/activated carbon, 1% Pd-5% phosphotungstic acid/activated carbon.
The third catalyst is MgO-ZnO-gamma alumina or CuO-ZnO-gamma alumina.
Compared with the prior art, the utility model discloses following beneficial technological effect has been brought:
the utility model provides a preparation facilities of o-phenyl phenol, it includes the one-level reaction unit, second grade reaction unit, tertiary reaction unit and the rectification unit that connect gradually, utilizes cyclohexanone to take place condensation reaction as the raw materials in the one-level reaction unit, later in the second grade reaction unit, dewaters-hydrogenation step with 2- (1-hydroxycyclohexyl) cyclohexyl-1-ketone that obtains in the one-level reaction unit to obtain o-cyclohexyl cyclohexanone (cis-trans isomerism); introducing o-cyclohexyl cyclohexanone (cis-trans isomerization) into a three-stage reaction unit for dehydrogenation reaction to obtain a crude o-phenylphenol product; and finally, introducing the crude o-phenylphenol obtained in the third-stage reaction unit into a rectification unit, and carrying out secondary rectification on the o-phenylphenol through the rectification unit to obtain the o-phenylphenol. The utility model discloses a closely cooperate of each reaction unit and rectifying unit, in the preparation process of o-phenylphenol, can not generate unstable structures such as unsaturated dimer isomer, improved the product yield.
Through the utility model discloses o phenyl phenol that preparation facilities of o phenyl phenol prepared obtains saves the crystallization process, has consequently shortened process flow, has also reduced manufacturing cost.
The utility model provides a preparation facilities of o phenyl phenol can realize continuous production, has improved the production efficiency of o phenyl phenol.
Drawings
The present invention will be further explained with reference to the accompanying drawings:
FIG. 1 is a schematic structural diagram of an o-phenylphenol production apparatus of the present invention;
FIG. 2 is a schematic structural view of a third fixed bed reaction column of the present invention;
in the figure:
1. a first fixed bed reaction tower, 2, a second fixed bed reaction tower, 3, a third fixed bed reaction tower, 4, a first catalyst, 5, a second catalyst, 6, a third catalyst, 7, a first rectifying tower, 8, a second rectifying tower, 9, a third rectifying tower, 10, a condensation reaction liquid buffer tank, 11, a condensation crude product buffer tank, 12, a first preheating heat exchanger, 13 and a second preheating heat exchanger, 14, a third preheating heat exchanger, 15, a first cooler, 16, a second cooler, 17, a third cooler, 18, an o-cyclohexyl cyclohexanone buffer tank, 19, an o-phenyl phenol crude product buffer tank, 20, a gas diffuser, 21, a gas buffer zone, 22, gas diffusion holes, 23, a main reaction buffer zone, 24, a heating coil, 25, pressure measuring holes, 26, temperature measuring holes, 27 and a catalyst three-filling zone.
Detailed Description
The utility model provides an o phenyl phenol's preparation facilities, in order to make the utility model discloses an advantage, technical scheme are clearer, clear and definite, and it is right to combine specific embodiment below the utility model discloses do further the explanation.
As shown in figure 1, the utility model relates to a preparation device of o-phenylphenol, which comprises a first-stage reaction unit, a second-stage reaction unit, a third-stage reaction unit and a rectification unit.
Wherein, the first-stage reaction unit takes cyclohexanone as a raw material to carry out condensation reaction to obtain an intermediate product 2- (1-hydroxycyclohexyl) cyclohex-1-one; the first-stage reaction unit comprises a first fixed bed reaction tower 1, a condensation reaction liquid buffer tank 10, a first rectification tower 7 and a condensation crude product buffer tank 11 which are sequentially connected, the first fixed bed reaction tower comprises a tower body, the whole shape of the tower body is a cylinder, a feed inlet is formed in the top of the tower body, a discharge outlet is formed in the bottom of the tower body, materials enter from the feed inlet in the top, the materials pass through a reaction zone in the middle of the first fixed bed reaction tower, a catalyst I4 is arranged in the reaction zone, the catalyst I4 is macroporous strong alkali type anion exchange resin and is one or a combination of two or three of IRA-900, PA 308 or MP-500, and the reaction temperature of the first fixed bed reaction tower 1 is controlled to be 10-60 ℃ under the action of the catalyst, and the reaction is preferably carried out at 20-40 ℃.
The condensation reaction equation occurring in the first-order reaction unit is shown in formula (1).
After the reaction is finished, the condensation reaction liquid flowing out of a discharge port of the first fixed bed reaction tower 1 enters a condensation reaction liquid buffer tank 10 connected with the first fixed bed reaction tower 1, unreacted cyclohexanone is recycled from a first rectifying tower through a metering pump, a bottom material of the first rectifying tower enters a condensation crude product buffer tank 11, and the recycled cyclohexanone is recycled;
the temperature of 60-100 ℃ and the vacuum degree of 0.085-0.095 MPa under the condition of recovering the cyclohexanone.
Wherein: the second-stage reaction unit is used for carrying out dehydration-hydrogenation reaction, and o-cyclohexyl cyclohexanone (cis-trans isomerization) is obtained through the reaction;
the second-stage reaction unit comprises a second fixed bed reaction tower 2, a first preheating heat exchanger 12, a second preheating heat exchanger 13, a first cooler 15 and an o-cyclohexyl cyclohexanone buffer tank 18; the first preheating heat exchanger is positioned between the condensation crude product buffer tank and the second fixed bed reaction tower and is used for preheating the 2- (1-hydroxycyclohexyl) cyclohex-1-one in the condensation crude product buffer tank to a certain temperature;
the 2- (1-hydroxycyclohexyl) cyclohex-1-one preheated by the first preheating heat exchanger enters from the top of the second fixed bed reaction tower;
the second preheating heat exchanger is connected with a hydrogen pipeline and is used for preheating hydrogen to a certain temperature, and the preheated hydrogen enters from the top of the second fixed bed reaction tower;
and a second catalyst 5 is arranged in the middle of the second fixed bed reaction tower, dehydration-hydrogenation reaction is carried out under the action of the second catalyst, the reaction liquid obtained after the reaction is discharged from an outlet at the bottom of the second fixed bed reaction tower and enters the first cooler, the first cooler is used for cooling the reaction liquid, and the cooled o-cyclohexylcyclohexanone (cis-trans-isomerization) is introduced into the o-cyclohexylcyclohexanone (cis-trans-isomerization) buffer tank.
The second catalyst is selected from any one group of catalysts with the dewatering and hydrogenation catalytic performances, preferably 1-Ru-5% phosphotungstic acid/activated carbon, 1-Rh-5% phosphotungstic acid/activated carbon, and 1-Pd-5% phosphotungstic acid/activated carbon, and the addition amount is limited by cyclohexanone feeding mass space velocity;
the mass space velocity of the 2- (1-hydroxycyclohexyl) cyclohexyl-1-ketone relative to the catalyst II is 2-4 kg/h.kg; the feeding rate of the hydrogen is 10-20 ml/min; the temperature ranges of the first preheating heat exchanger and the second preheating heat exchanger are 60-100 ℃; the temperature range of the second fixed bed reaction tower is 100-140 ℃; the temperature range of the first cooler is 50-80 ℃;
the chemical reaction equation is shown as formula (2):
the o-cyclohexyl cyclohexanone obtained by the reaction comprises two cis-trans isomers, and has the following structure:
the third-stage reaction unit is used for completing the dehydrogenation step of o-cyclohexyl cyclohexanone (cis-trans isomerization), and obtaining the crude o-phenylphenol.
The third-stage reaction unit comprises a third preheating heat exchanger 14, a third fixed bed reaction tower 3, a second cooler 16 and an o-phenylphenol crude product buffer tank 19, wherein the third preheating heat exchanger is connected with the o-cyclohexylcyclohexanone (cis-trans isomerization) buffer tank and is used for preheating the o-cyclohexylcyclohexanone (cis-trans isomerization) to a certain temperature; the preheating temperature range of the third preheating heat exchanger is 330-360 ℃.
The preheated cyclohexyl cyclohexanone (cis-trans isomerization) enters from the top of a third fixed bed reaction tower, a catalyst III 6 is arranged in the middle of the third fixed bed reaction tower, the catalyst III is one of MgO-ZnO-gamma alumina and CuO-ZnO-gamma alumina, and the preferred mass ratio of MgO or CuO to ZnO and gamma alumina is 0.6-1; the mass space velocity of o-cyclohexylcyclohexanone (cis-trans-isomerization) relative to the catalyst III is 0.8-1.2 kg/h.kg, dehydrogenation reaction is carried out under the action of the catalyst III, reaction liquid obtained after reaction enters a second cooler for cooling, and the obtained o-phenylphenol crude product is introduced into an o-phenylphenol crude product buffer tank after cooling. The temperature range of the second cooler is 90-120 ℃; the reaction temperature range of the third fixed bed reaction tower is 330-400 ℃; the pressure of the reaction area of the third fixed bed reaction tower is 0.5-1.2 MPa.
The chemical reaction equation for dehydrogenation is shown in formula (3):
the rectifying unit comprises a second rectifying tower 8 and a third rectifying tower 9, the second rectifying tower is connected with an o-phenylphenol crude product buffer tank 19, and the third rectifying tower is connected with the second rectifying tower; the second rectifying tower is used for removing light components and water in the crude o-phenylphenol product; the third rectifying tower is used for collecting o-phenyl phenol, and an outlet pipeline of the third rectifying tower is connected with a third cooler 17.
Removing other light components such as water and the like through a second rectifying tower at the operating conditions of 40-60 Pa and 30-60 ℃, transferring the material at the bottom of the o-phenylphenol light-component removing tower to a third rectifying tower, rectifying and collecting fractions at the temperature of 40-60 Pa and 125-135 ℃, obtaining an o-phenylphenol finished product with the gas phase purity of more than 99.5%, and finally slicing the obtained o-phenylphenol to obtain the o-phenylphenol flaky solid.
As shown in fig. 2, the third fixed bed reaction column includes a gas diffusion zone located at the top of the third fixed bed reaction column, a gas buffer zone 21 having an inverted circular truncated structure, and a main reaction buffer zone 23 in which gas diffusion holes 22 are formed to maintain communication with the main reaction buffer zone through the gas diffusion holes.
On the tower plate of the third fixed bed reaction tower is a catalyst three-filling zone 27, the tower plates are uniformly arranged at intervals, and the catalyst three is filled in the catalyst three-filling zone.
A gas diffuser 20 is provided in the gas diffusion area, and the structure of the gas diffuser 20 can be realized by using the prior art. A gas diffuser is arranged at the top of the third fixed bed reaction tower, so that sufficient reaction is facilitated.
Be provided with heating coil 24 at the outer wall of main reaction buffer, through heating coil provide required temperature to the third fixed bed reaction tower, heating coil with the form cladding of coil pipe on the tower wall of third fixed bed reaction tower, can conveniently control its temperature, heating coil's main heating methods if adopt electric heating.
Preferably, the side wall of the middle part of the third fixed bed reaction tower is provided with a pressure measuring hole 25 and a temperature measuring hole 26, so that pressure measurement and temperature measurement are convenient.
In order to facilitate the control of the feeding amount, the above-mentioned device for preparing o-phenylphenol further comprises a metering pump, for example, a metering pump is arranged on a pipeline connected with the feeding port of the first fixed bed reaction tower, so that the feeding amount of cyclohexanone is conveniently controlled, and the metering pumps are arranged on a pipeline between the condensation reaction liquid buffer tank and the first rectifying tower, a pipeline between the condensation crude product buffer tank and the feeding port of the second fixed bed reaction tower, and a pipeline between the o-cyclohexylcyclohexanone (cis-trans-isomer) buffer tank and the third preheating heat exchanger. How to operate and control the metering pump is not described in detail herein, and can be implemented by those skilled in the art by using the prior art.
The following description will discuss a method for using the o-phenylphenol production apparatus of the present invention with reference to specific examples.
Example 1:
pumping cyclohexanone into a first fixed bed reaction tower filled with a hydrogen-oxygen type IRA-900A catalyst I by using a metering pump, wherein the cyclohexanone enters from the top of the first fixed bed reaction tower, the feeding mass space velocity of the cyclohexanone is 6kg/h.kg, the reaction temperature in the first fixed bed reaction tower is controlled to be 20-25 ℃, a condensation reaction liquid flows out from the bottom of the first fixed bed reaction tower and enters a condensation reaction liquid buffer tank through a U-shaped elbow, the reaction conversion rate of the cyclohexanone is 17.78%, and the selectivity of the 2- (1-hydroxycyclohexyl) cyclohexyl-1-ketone is 98.5%;
and continuously transferring the crude product of the reaction liquid in the condensation reaction liquid buffer tank to a first rectifying tower by using a metering pump, recovering unreacted cyclohexanone from the top of the first rectifying tower, collecting the component cyclohexanone at the temperature of 90-95 ℃ and under the pressure of-0.09 MPa, returning the component cyclohexanone to the condensation process for reuse, and feeding the material at the bottom of the first rectifying tower into a condensation crude product buffer tank 11. Transferring the 2- (1-hydroxycyclohexyl) cyclohexa-1-one in the condensation crude product buffer tank to a first preheating heat exchanger by using a metering pump, preheating to 80 ℃ by using the first preheating heat exchanger, continuously entering the top of a second fixed bed reaction tower, simultaneously preheating hydrogen to 70 ℃ by using a second preheating heat exchanger, entering the second fixed bed reaction tower, mixing and meeting in the second fixed bed reaction tower, entering the second fixed bed reaction tower, contacting with a catalyst II 1 Ru-5% phosphotungstic acid/active carbon, performing dehydration and hydrogenation reaction, wherein the temperature in the second fixed bed reaction tower is 110-120 ℃, the mass space velocity of the 2- (1-hydroxycyclohexyl) cyclohexa-1-one relative to the catalyst II is 2kg/h.kg, the hydrogen feeding rate is 10ml/min, cooling the reacted material to 50-60 ℃ by using a cooler, entering an o-cyclohexyl (cis-trans-iso) buffer tank for gas-liquid separation, treating and recycling the gas phase by using a hydrogen system, the liquid phase is a target product, the conversion rate of the 2- (1-hydroxycyclohexyl) cyclohexa cis-1-one is 97.5%, and the trans-iso cyclohexanone (trans-iso) selectivity is 98.1.1;
the o-cyclohexyl cyclohexanone (cis-trans isomerization) is vaporized at high temperature by a third preheating heat exchanger and then enters a third fixed bed reaction tower filled with a MgO-ZnO-gamma alumina composite catalyst, the vaporization temperature is 330 ℃, and the feeding mass space velocity of the o-cyclohexyl cyclohexanone (cis-trans isomerization) is 1.0kg/h.kg. Controlling the internal temperature of a third fixed bed reaction tower to be 370-380 ℃, cooling the dehydrogenation product to 90-95 ℃ to obtain an o-phenylphenol crude product, separating hydrogen, treating the hydrogen by a hydrogen system, and returning the hydrogen for reuse, wherein the conversion rate of o-cyclohexylcyclohexanone (cis-trans isomerization) is 96.8%, and the selectivity of o-phenylphenol is 98.7%;
rectifying the crude product of the o-phenylphenol, removing low-boiling-point substances such as water and the like through a second rectifying tower, transferring the material to a third rectifying tower from the tower bottom of the second rectifying tower, rectifying and collecting fractions at the temperature of between 130 and 132 ℃ under 50Pa, wherein GC =99.75%, and then cooling and slicing the obtained o-phenylphenol to obtain the o-phenylphenol flaky solid.
The utility model discloses the part that does not describe in can realize by reference prior art.
It is intended that any equivalents, or obvious variations, which may be made by those skilled in the art in light of the teachings herein, be considered within the scope of the present invention.
Claims (10)
1. The utility model provides a preparation facilities of o-phenylphenol, its includes one-level reaction unit, second grade reaction unit, tertiary reaction unit and rectification unit, its characterized in that:
the first-stage reaction unit is used for obtaining an intermediate product 2- (1-hydroxycyclohexyl) cyclohex-1-one by taking cyclohexanone as a raw material and carrying out condensation reaction;
the intermediate product obtained by the first-stage reaction unit is introduced into the second-stage reaction unit;
the secondary reaction unit is used for performing dehydration-hydrogenation step of 2- (1-hydroxycyclohexyl) cyclohex-1-one and obtaining o-cyclohexyl cyclohexanone;
the o-cyclohexyl cyclohexanone obtained by the second-stage reaction unit is introduced into the third-stage reaction unit;
the three-stage reaction unit is used for completing the dehydrogenation step of o-cyclohexyl cyclohexanone and obtaining a crude o-phenylphenol product;
the crude o-phenylphenol obtained in the third-stage reaction unit is introduced into the rectification unit;
the rectification unit is used for carrying out secondary rectification on the o-phenylphenol crude product and obtaining the o-phenylphenol.
2. The production apparatus of o-phenylphenol according to claim 1, wherein: the primary reaction unit comprises a first fixed bed reaction tower, a condensation reaction liquid buffer tank, a first rectification tower and a condensation crude product buffer tank which are sequentially connected, wherein a feed inlet is formed in the top of the first fixed bed reaction tower, a discharge outlet is formed in the bottom of the first fixed bed reaction tower, cyclohexanone enters from the feed inlet in the top of the first fixed bed reaction tower, a first catalyst is arranged in the middle of the first fixed bed reaction tower, condensation reaction is carried out under the action of the first catalyst, and a mixed liquid obtained by reaction enters the condensation reaction liquid buffer tank from the discharge outlet in the bottom of the first fixed bed reaction tower;
the condensation reaction liquid buffer tank is connected with the first rectifying tower, the condensation reaction liquid enters from the top of the first rectifying tower, and the 2- (1-hydroxycyclohexyl) cyclohex-1-one obtained by rectifying in the first rectifying tower is introduced into the condensation crude product buffer tank.
3. The production apparatus of o-phenylphenol according to claim 2, characterized in that: the second-stage reaction unit comprises a second fixed bed reaction tower, a first preheating heat exchanger, a second preheating heat exchanger, a first cooler and an o-cyclohexyl cyclohexanone buffer tank; the first preheating heat exchanger is positioned between the condensation crude product buffer tank and the second fixed bed reaction tower and is used for preheating the 2- (1-hydroxycyclohexyl) cyclohex-1-one in the condensation crude product buffer tank to a certain temperature;
the 2- (1-hydroxycyclohexyl) cyclohex-1-one preheated by the first preheating heat exchanger enters from the top of the second fixed bed reaction tower;
the second preheating heat exchanger is connected with a hydrogen pipeline and used for preheating hydrogen to a certain temperature, and the preheated hydrogen enters from the top of the second fixed bed reaction tower;
and a second catalyst is arranged in the middle of the second fixed bed reaction tower, dehydration-hydrogenation reaction is carried out under the action of the second catalyst, reaction liquid obtained after reaction is discharged from an outlet at the bottom of the second fixed bed reaction tower and enters the first cooler, the first cooler is used for cooling the reaction liquid, and cooled o-cyclohexylcyclohexanone is introduced into the o-cyclohexylcyclohexanone buffer tank.
4. The production apparatus of o-phenylphenol according to claim 3, wherein: the three-stage reaction unit comprises a third preheating heat exchanger, a third fixed bed reaction tower, a second cooler and an o-phenylphenol crude product buffer tank, wherein the third preheating heat exchanger is connected with the o-cyclohexylcyclohexanone buffer tank and is used for preheating the o-cyclohexylcyclohexanone to a certain temperature;
and (2) feeding preheated cyclohexyl cyclohexanone from the top of the third fixed bed reaction tower, arranging a third catalyst in the middle of the third fixed bed reaction tower, carrying out dehydrogenation reaction under the action of the third catalyst, feeding reaction liquid obtained after reaction into the second cooler for cooling, and introducing the obtained crude o-phenylphenol into the crude o-phenylphenol buffer tank after cooling.
5. The production apparatus of o-phenylphenol according to claim 4, wherein: the rectification unit comprises a second rectification tower and a third rectification tower, the second rectification tower is connected with the o-phenylphenol crude product buffer tank, and the third rectification tower is connected with the second rectification tower;
the second rectifying tower is used for removing light components and water in the crude o-phenylphenol;
and the third rectifying tower is used for collecting o-phenylphenol.
6. The production apparatus of o-phenylphenol according to claim 4, wherein: the third fixed bed reaction tower include gas diffusion zone, gas buffer area and main reaction buffer area, the gas diffusion zone be located the top of third fixed bed reaction tower, the gas buffer area be round platform structure the gas buffer area be provided with gas diffusion hole, through the gas diffusion hole keep with main reaction buffer area's intercommunication.
7. The production apparatus of o-phenylphenol according to claim 6, wherein: and a gas diffuser is arranged in the gas diffusion area and is positioned at the top of the third fixed bed reaction tower.
8. The production apparatus of o-phenylphenol according to claim 6, wherein: and the outer wall of the main reaction buffer zone is provided with a heating coil, and the required temperature is provided for the third fixed bed reaction tower through the heating coil.
9. The production apparatus of o-phenylphenol according to claim 6, wherein: the main reaction buffer zone is provided with a plurality of tower plates which are arranged at equal intervals, and the catalyst III is arranged on each tower plate.
10. The apparatus for producing an o-phenylphenol according to claim 6, wherein: a pressure measuring hole and a temperature measuring hole are arranged on the side wall of the middle part of the third fixed bed reaction tower; the o-cyclohexyl cyclohexanone comprises two cis-trans isomers.
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