CN110627751B - Device and method for recycling bromine element in industrialized production of tetrahydrofurfuryl alcohol diethyl ether - Google Patents
Device and method for recycling bromine element in industrialized production of tetrahydrofurfuryl alcohol diethyl ether Download PDFInfo
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- C07C17/08—Preparation of halogenated hydrocarbons by addition of hydrogen halides to unsaturated hydrocarbons
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Abstract
The invention relates to a device and a method for recycling bromine in industrialized production of tetrahydrofurfuryl alcohol diethyl ether, wherein the device comprises a raw material storage-metering conveying system, a built-in bed reaction kettle, a hydrogen bromide absorption tank, a fixed bed reactor, a falling film evaporator, a condenser and a product tank which are sequentially connected, the device also comprises an ethylene storage-metering conveying unit and a potassium sulfate tank, the ethylene storage-metering conveying unit is connected with the fixed bed reactor, and the potassium sulfate tank is connected with the bottom of the built-in bed reaction kettle. The comprehensive yield of the bromoethane produced by the device and the method is 92-95%, the purity reaches 98.5-99.5%, the requirement of tetrahydrofurfuryl alcohol diethyl ether production on raw material quality can be met, the production cost of tetrahydrofurfuryl alcohol diethyl ether is greatly reduced, the recycling of high-value bromine elements is realized, the resources are saved, and the environment is friendly.
Description
Technical Field
The invention belongs to the technical field of preparation of halogenated hydrocarbon compounds, and particularly relates to a device and a method for recycling bromine element in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether.
Background
Bromoethane is also known as ethyl bromide and has the molecular formula C 2 H 5 B r . The invention patent with publication number of CN105503784A discloses a method for producing tetrahydrofurfuryl alcohol diethyl ether by industrialized ultrasonic reaction, which comprises the steps of mixing tetrahydrofurfuryl alcohol, bromoethane and aqueous potassium hydroxide solution, fully reacting under ultrasonic condition, removing most of water from the obtained reaction product, and carrying out reduced pressure distillation to obtain tetrahydrofurfuryl alcohol diethyl ether. In the method disclosed in CN105503784a, bromoethane is one of the main raw materials for industrial production of tetrahydrofurfuryl alcohol diethyl ether, but the bromine element which is the most valuable part of the bromoethane is produced as a byproduct of potassium bromide with low added value after the production process, resulting in great waste of resources.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a device and a method for recycling bromine elements in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether, which take byproduct potassium bromide aqueous solution and ethylene which is easy to obtain in a resource enrichment area in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether as main raw materials, convert the raw materials into the production raw material of tetrahydrofurfuryl alcohol diethyl ether, namely bromoethane, through a specific reaction process, comprehensively couple the production optimization of tetrahydrofurfuryl alcohol diethyl ether, realize the recycling of high-value bromine elements, save resources and are environment-friendly.
Specifically, the invention provides the following technical scheme.
The device for recycling bromine element in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether comprises a raw material storage-metering conveying system, a built-in bed reaction kettle 7, a hydrogen bromide absorption tank 8, a fixed bed reactor 12, a falling film evaporator 19, a condenser 16 and a product tank 17 which are connected in sequence;
a stirring paddle is arranged in the internal bed reaction kettle 7, and a fixed bed layer made of sintered ceramics is arranged above the stirring paddle;
the raw material storage-metering conveying system consists of a parallel potassium bromide aqueous solution storage-metering conveying unit, a concentrated sulfuric acid storage-metering conveying unit and a hydrogen storage-metering conveying unit;
the device also comprises an ethylene storage-metering and conveying unit and a potassium sulfate tank 20, wherein the ethylene storage-metering and conveying unit is connected with the fixed bed reactor 12, and the potassium sulfate tank 20 is connected with the bottom of the internal bed reaction kettle 7.
Preferably, in the above device, the potassium bromide aqueous solution storing-metering and conveying unit is composed of a potassium bromide solution storage tank 1 and a potassium bromide solution conveying pump 2 which are sequentially connected, the concentrated sulfuric acid storing-metering and conveying unit is composed of a concentrated sulfuric acid storage tank 3 and a concentrated sulfuric acid conveying pump 4 which are sequentially connected, the hydrogen storing-metering and conveying unit is composed of a hydrogen storage tank 5 and a hydrogen meter 6 which are sequentially connected, and the ethylene storing-metering and conveying unit is composed of an ethylene storage tank 10 and an ethylene meter 11 which are sequentially connected; the potassium bromide solution delivery pump 2, the concentrated sulfuric acid delivery pump 4 and the hydrogen meter 6 are respectively connected with the internal bed reaction kettle 7, and the ethylene meter 11 is connected with the fixed bed reactor 12.
Preferably, in the above device, as shown in fig. 2, two circles of through holes penetrating through the upper side and the lower side of the fixed bed layer are formed on the fixed bed layer of the internal bed reaction kettle 7, more preferably, the volume of the bed layer of the internal bed reaction kettle 7 is less than or equal to 20% of the volume of the reaction kettle, and most preferably, the volume of the internal bed reaction kettle 7 is less than or equal to 2000L. Because the reaction of the potassium bromide aqueous solution and sulfuric acid to generate hydrogen bromide is more severe and easy to generate the phenomenon of 'bumping' so as to occur unsafe conditions, the inventor of the patent designs a special built-in bed reaction kettle, a section of fixed bed made of sintered ceramics is arranged on the upper part of a stirring paddle, the porous structure of the fixed bed is favorable for overflowing hydrogen bromide, two circles of small-diameter through holes are arranged to facilitate liquid to pass through, and the special built-in bed reaction kettle has the functions of providing more reaction contact area and inhibiting 'bumping'.
Preferably, in the above device, the volume of the bed layer of the fixed bed reactor 12 is less than or equal to 70% of the reactor volume, the bed layer filling material is alumina porcelain balls, and more preferably, the volume of the fixed bed reactor 12 is less than or equal to 2000L.
Preferably, in the above device, a nozzle for spraying atomized water is provided in the hydrogen bromide absorption tank 8, and a hydrogen outlet for discharging hydrogen is provided in the hydrogen bromide absorption tank 8.
Preferably, in the above device, a circulation line is provided between the top and bottom of the fixed bed reactor 12.
Preferably, the device further comprises a crude bromoethane storage tank 14, wherein the crude bromoethane storage tank 14 is arranged between the fixed bed reactor 12 and a falling film evaporator 19.
Preferably, in the above device, the product tank 17 is connected with a product reflux pump 18 for refluxing to the falling film evaporator 19.
The invention also provides a method for recycling bromine element in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether by using the device, which comprises the following steps: the method comprises the steps of inputting a byproduct potassium bromide aqueous solution generated in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether and concentrated sulfuric acid into a reaction kettle 7 of an internal bed, reacting in the presence of hydrogen to obtain a gas-phase product, inputting the gas-phase product into a hydrogen bromide absorption tank 8, absorbing hydrogen bromide by spraying atomized water to obtain a hydrogen bromide solution, inputting the hydrogen bromide solution into a fixed bed reactor 12 for reaction with ethylene, and treating the reaction product by a falling film evaporator 19 to obtain the bromoethane product.
The reactions mainly occurring in the internal bed reactor 7 are:
H 2 SO 4 +2KBr→2HBr↑+K 2 SO 4
the main reaction mechanism of the above reaction is: potassium bromide is oxidized to hydrobromic acid in a strong acid environment.
The reactions that mainly take place in the fixed bed reactor 12 are:
HBr+C 2 H 4 →C 2 H 5 Br
the main reaction mechanism of the above reaction is: hydrobromic acid reacts with ethylene in a fixed bed to form bromoethane.
Preferably, the method comprises the steps of:
(1) Inputting a byproduct potassium bromide aqueous solution and hydrogen generated in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether into an internal bed reaction kettle 7, slowly adding concentrated sulfuric acid into the internal bed reaction kettle 7, and outputting a gas-phase product after full reaction;
(2) The gas-phase product in the step (1) is input into a hydrogen bromide absorption tank 8, hydrogen bromide is absorbed by spraying atomized water to obtain hydrogen bromide solution, the hydrogen bromide solution and ethylene are input into a fixed bed reactor 12 for cyclic reaction, and a reaction product is output after full reaction;
(3) Inputting the reaction product in the step (2) into a falling film evaporator 19, and collecting the fraction at 35-40 ℃ to obtain bromoethane;
(4) Recycling bromoethane back to the raw material system for producing tetrahydrofurfuryl alcohol diethyl ether, namely finishing recycling of bromine;
preferably, in the above method, the mass fraction of the aqueous potassium bromide solution is 25-35%, based on the total amount of the concentrated sulfuric acid fed, and in the internal bed reactor 7, the aqueous potassium bromide solution and the H in the concentrated sulfuric acid 2 SO 4 The molar ratio is 1.55-2.15: 0.75 to 1.65; the mass fraction of hydrogen bromide in the hydrogen bromide solution is 45-55%, and the mole ratio of hydrogen bromide and ethylene in the hydrogen bromide solution is fed into the fixed bed reactor 120.66-1.15:0.77-1.25.
Preferably, in the above method, the reaction temperature of the reaction kettle 7 with a built-in bed is 15-45 ℃, the hydrogen partial pressure is 500-750 Pa, the reaction temperature of the fixed bed reactor 12 is 45-70 ℃, and the reaction pressure is 0.2-0.3 Mpa; more preferably, the reaction temperature of the reaction kettle 7 with the built-in bed is 22-41 ℃, the reaction temperature of the fixed bed reactor 12 is 50-65 ℃, and the pressure is 0.22-0.3 Mpa; most preferably, the reaction temperature of the fixed bed reactor 12 is 55 to 65 ℃.
Preferably, in the above method, the stirring frequency of the internal bed reactor 7 is 10 to 20Hz, and the fixed bed reactor 12 has no stirring frequency.
Preferably, in the above method, in step (3), the bottom temperature of the falling film evaporator 19 should be controlled at 55-80 ℃, the top temperature of the falling film evaporator 19 should be controlled at 30-45 ℃, and the recovery is performed when the top temperature of the falling film evaporator 19 is stabilized at 35-40 ℃, and the component in this stage is the recovered bromine element product bromoethane. In order to ensure that the product quality is acceptable, the pressure of the falling film evaporator 19 is stabilized within the range of 1-1.5 Kpa.
In the case that the metering accuracy reaches the standard, the invention can add the raw materials in a manner of pressing and feeding by an electronic scale and a metering tank, and in a preferred embodiment, the metering manner of feeding the gas-phase product of the reaction kettle 7 of the built-in bed into the hydrogen bromide absorption tank 8 is carried out in the form of the metering tank.
The invention also provides application of the device or the method in recycling bromine element in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether.
The beneficial effects obtained by the invention are as follows:
the comprehensive yield of the bromoethane produced by the device and the method is 92-95%, the purity reaches 98.5-99.5%, the requirement of tetrahydrofurfuryl alcohol diethyl ether production on raw material quality can be met, the production cost of tetrahydrofurfuryl alcohol diethyl ether is greatly reduced, the recycling of high-value bromine elements is realized, the resources are saved, and the environment is friendly.
Drawings
FIG. 1 is a schematic view of the apparatus of example 1; wherein, 1 part of potassium bromide solution storage tank, 2 parts of potassium bromide solution delivery pump, 3 parts of concentrated sulfuric acid storage tank, 4 parts of concentrated sulfuric acid delivery pump, 5 parts of hydrogen storage tank, 6 parts of hydrogen meter, 7 parts of internal bed reaction kettle, 8 parts of hydrogen bromide absorption tank, 9 parts of hydrogen bromide solution meter, 10 parts of ethylene storage tank, 11, ethylene meters, 12, a fixed bed reactor, 13, a reaction liquid delivery pump, 14, a crude bromoethane storage tank, 15, a crude product delivery pump, 16, a condenser, 17, a product tank, 18, a product reflux pump, 19, a falling film evaporator, 20, a potassium sulfate tank, 21 and a potassium sulfate delivery pump.
FIG. 2 is a top view of the fixed bed layer of the present invention in-bed reactor; wherein 7-2 parts of fixed bed layer, 7-2-1 parts of through holes.
FIG. 3 is a schematic structural diagram of the reactor of the embodiment 1; wherein 7-1 parts of stirring paddles, 7-2 parts of fixed bed layers.
FIG. 4 is a cross-sectional view of the fixed bed layer of the internal bed reactor of example 1; wherein 7-2 parts of fixed bed layer, 7-2-1 parts of through holes.
FIG. 5 is a gas chromatogram of the final product of example 2.
Detailed Description
The present invention is described in further detail below with reference to specific examples, but is not intended to limit the scope of the present invention.
Example 1
The embodiment provides a device (shown in figure 1) for recycling bromine in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether, which comprises a raw material storage-metering conveying system, a built-in bed reaction kettle 7, a hydrogen bromide absorption tank 8, a hydrogen bromide solution meter 9, a fixed bed reactor 12, a reaction liquid conveying pump 13, a crude bromoethane storage tank 14, a crude product conveying pump 15, a falling film evaporator 19, a condenser 16 and a product tank 17 which are sequentially connected.
In the embodiment, the raw material storage-metering conveying system consists of a potassium bromide aqueous solution storage-metering conveying unit, a concentrated sulfuric acid storage-metering conveying unit and a hydrogen storage-metering conveying unit which are arranged in parallel; the potassium bromide aqueous solution storage-metering and conveying unit consists of a potassium bromide solution storage tank 1 and a potassium bromide solution conveying pump 2 which are sequentially connected, the concentrated sulfuric acid storage-metering and conveying unit consists of a concentrated sulfuric acid storage tank 3 and a concentrated sulfuric acid conveying pump 4 which are sequentially connected, and the hydrogen storage-metering and conveying unit consists of a hydrogen storage tank 5 and a hydrogen meter 6 which are sequentially connected; the potassium bromide solution delivery pump 2, the concentrated sulfuric acid delivery pump 4 and the hydrogen meter 6 are respectively connected with the reaction kettle 7 with a built-in bed.
In this embodiment, the apparatus further comprises an ethylene storage-metering and conveying unit and a potassium sulfate tank 20, wherein the ethylene storage-metering and conveying unit is composed of an ethylene storage tank 10 and an ethylene meter 11 which are sequentially connected, and the ethylene meter 11 is connected with the upper part of the fixed bed reactor 12; the potassium sulfate tank 20 is connected with the lower part of the internal bed reaction kettle 7 through a potassium sulfate delivery pump 21.
In this embodiment, as shown in fig. 3 and 4, the volume of the reaction kettle 7 with built-in bed is 1200L, a stirring paddle is arranged in the reaction kettle, a fixed bed layer with a volume of 240L is arranged above the stirring paddle, and the fixed bed layer is made of two semicircular sintered ceramics (sintered ceramics are provided by the scientific and technological company of wudong, wushan, wherein Al 2 O 3 85% of SiO 2 Content of 4.5%, zrO 2 The content is less than or equal to 1.2 percent, and the balance is clay), two circles of through holes penetrating through the upper side and the lower side of the fixed bed layer are arranged on the fixed bed layer, the distance between the two circles in the diameter direction is 150mm, 24 inner circle through holes and 24 outer circle through holes are respectively set, the aperture of any through hole is 4mm, and the pore canal and the horizontal direction form an inclined angle of 75 degrees.
In this embodiment, a nozzle for spraying atomized water is disposed in the hydrogen bromide absorption tank 8, and a hydrogen outlet for discharging hydrogen is disposed on the hydrogen bromide absorption tank 8.
In this embodiment, the volume of the fixed bed reactor 12 is 1200L, the volume of the packed bed layer of the fixed bed reactor 12 is 720L, and the packing is Dz-003 type alumina ceramic balls provided by wudong fine technologies, inc; a circulation line is provided between the top and bottom of the fixed bed reactor 12.
In this embodiment, the product tank 17 is connected to a product reflux pump 18 for refluxing to the falling film evaporator 19.
Example 2
The embodiment provides a method for recycling bromine in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether by using the device of the embodiment 1, which comprises the following steps:
(1) 2.2t of 30% potassium bromide aqueous solution by mass fraction is input into a reactor 7 with an internal bed, hydrogen is introduced, and the hydrogen partial pressure is kept at 650Pa. Inputting 0.3t of 98% concentrated sulfuric acid into the internal bed reaction kettle 7 at the flow rate of 0.3t/h at the temperature of 32-40 ℃, continuously reacting for 1.5 hours, and outputting a gas-phase product;
(2) The gas-phase product in the step (1) is input into a hydrogen bromide absorption tank 8, and is absorbed by spraying atomized water to obtain a hydrogen bromide solution with the mass fraction of 50%, and unabsorbed hydrogen is discharged through a hydrogen outlet;
(3) Feeding 0.7t of the hydrogen bromide solution of the step (2) and 0.5t of ethylene into the fixed bed reactor 12 at a flow rate of 0.35t/h and a flow rate of 0.33t/h respectively, at a temperature of 57-60 ℃, a pressure of 0.2-0.3 MPa.G and a space velocity of 0.5h -1 Synthesizing bromoethane by reaction under the condition, returning the reaction product to the fixed bed reactor 12 for cyclic reaction through the circulating pipeline, and delivering the reaction product to the crude bromoethane storage tank 14 after 4 hours;
(4) Inputting the reaction product in the crude bromoethane storage tank 14 into a falling film evaporation system at a flow rate of 0.65t/h, and collecting the fraction at 35-40 ℃ to obtain the final product bromoethane;
(5) And recycling bromoethane back to the raw material system for producing tetrahydrofurfuryl alcohol diethyl ether, so as to finish recycling of bromine.
The final product bromoethane obtained was further examined in this example. The detection specifically comprises the following steps:
the final product was measured using a North Rayleigh SP-3420A weather chromatograph according to the method specified by the HG20560-2006 national standard, and specific parameters include: TCD detector: 7X 10 -6 mg/ml, PEG-20M capillary column; column temperature: 40 ℃/4 to 80 ℃/8 minutes; rate of temperature rise: 20 ℃/min; vaporization chamber temperature: 138 ℃; split ratio: 4:1; the carrier gas is hydrogen. The chromatogram of the final product is shown in FIG. 5, in which the peaks from left to right are sequentially emptyThe gas peaks, diethyl ether, bromoethane and ethanol, and the specific content results are shown in Table 1.
The analysis results were: the purity of bromoethane in the final product is 99.22%; the yield of bromoethane was 93.6% based on potassium bromide.
TABLE 1 content of the substances in the end product
| Sequence number | Name of the name | Unit (B) | Content of |
| 1 | Bromoethane | ％(wt) | 99.22 |
| 2 | Diethyl ether | ％(wt) | 0.51 |
| 3 | Ethanol | ％(wt) | 0.27 |
While the invention has been described in detail in the foregoing general description, embodiments and experiments, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (13)
1. The device for recycling bromine element in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether is characterized by comprising a raw material storage-metering conveying system, an internal bed reaction kettle (7), a hydrogen bromide absorption tank (8), a fixed bed reactor (12), a falling film evaporator (19), a condenser (16) and a product tank (17) which are connected in sequence;
a stirring paddle is arranged in the internal bed reaction kettle (7), and a fixed bed layer made of sintered ceramics is arranged above the stirring paddle; two circles of through holes penetrating through the upper side and the lower side of the fixed bed layer are formed in the fixed bed layer of the built-in bed reaction kettle (7);
the raw material storage-metering conveying system consists of a potassium bromide aqueous solution storage-metering conveying unit, a concentrated sulfuric acid storage-metering conveying unit and a hydrogen storage-metering conveying unit which are arranged in parallel;
the device also comprises an ethylene storage-metering and conveying unit and a potassium sulfate tank (20), wherein the ethylene storage-metering and conveying unit is connected with the fixed bed reactor (12), and the potassium sulfate tank (20) is connected with the bottom of the internal bed reaction kettle (7).
2. The device according to claim 1, wherein the potassium bromide aqueous solution storage-metering delivery unit consists of a potassium bromide solution storage tank (1) and a potassium bromide solution delivery pump (2) which are connected in sequence, the concentrated sulfuric acid storage-metering delivery unit consists of a concentrated sulfuric acid storage tank (3) and a concentrated sulfuric acid delivery pump (4) which are connected in sequence, the hydrogen storage-metering delivery unit consists of a hydrogen storage tank (5) and a hydrogen meter (6) which are connected in sequence, and the ethylene storage-metering delivery unit consists of an ethylene storage tank (10) and an ethylene meter (11) which are connected in sequence; the potassium bromide solution delivery pump (2), the concentrated sulfuric acid delivery pump (4) and the hydrogen meter (6) are respectively connected with the internal bed reaction kettle (7), and the ethylene meter (11) is connected with the fixed bed reactor (12).
3. The apparatus according to claim 1 or 2, wherein the bed volume of the internal bed reactor (7) is equal to or less than 20% of the reactor volume.
4. The apparatus of claim 1 or 2, wherein the bed volume of the fixed bed reactor (12) is less than or equal to 70% of the reactor volume, and the bed packing is alumina porcelain spheres.
5. The device according to claim 1 or 2, wherein a spray head for spraying atomized water is arranged in the hydrogen bromide absorption tank (8), and a hydrogen outlet for discharging hydrogen is arranged on the hydrogen bromide absorption tank (8).
6. The apparatus according to claim 1 or 2, wherein a circulation line is provided between the top and bottom of the fixed bed reactor (12).
7. The apparatus according to claim 1 or 2, further comprising a crude bromoethane storage tank (14), the crude bromoethane storage tank (14) being provided between the fixed bed reactor (12) and a falling film evaporator (19).
8. A method for recycling bromine in the industrial production of tetrahydrofurfuryl alcohol diethyl ether by using the device of any one of claims 1 to 7, comprising the following steps: the method comprises the steps of inputting a byproduct potassium bromide aqueous solution and concentrated sulfuric acid generated in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether into a reaction kettle (7) with a built-in bed, reacting in the presence of hydrogen to obtain a gas-phase product, inputting the gas-phase product into a hydrogen bromide absorption tank (8), absorbing hydrogen bromide by spraying atomized water to obtain a hydrogen bromide solution, inputting the hydrogen bromide solution into a fixed bed reactor (12) for reaction with ethylene, and treating the reaction product by a falling film evaporator (19) to obtain a bromoethane product.
9. The method according to claim 8, wherein the method comprises the steps of:
(1) Inputting a byproduct potassium bromide aqueous solution and hydrogen generated in the process of industrially producing tetrahydrofurfuryl alcohol diethyl ether into an internal bed reaction kettle (7), slowly adding concentrated sulfuric acid into the internal bed reaction kettle (7), and outputting a gas-phase product after full reaction;
(2) Inputting the gas-phase product in the step (1) into a hydrogen bromide absorption tank (8), absorbing hydrogen bromide by spraying atomized water to obtain a hydrogen bromide solution, inputting the hydrogen bromide solution and ethylene into a fixed bed reactor (12) for cyclic reaction, and outputting a reaction product after full reaction;
(3) Inputting the reaction product in the step (2) into a falling film evaporator (19), and collecting the fraction at 35-40 ℃ to obtain bromoethane;
(4) And recycling bromoethane back to the raw material system for producing tetrahydrofurfuryl alcohol diethyl ether, namely finishing recycling of bromine.
10. The method according to claim 9, wherein the mass fraction of potassium bromide in the aqueous potassium bromide solution is 25-35%, based on the total amount of the concentrated sulfuric acid input, in the internal bed reactor (7), the potassium bromide in the aqueous potassium bromide solution and the H in the concentrated sulfuric acid 2 SO 4 The molar ratio is 1.55-2.15: 0.75 to 1.65; the mass fraction of hydrogen bromide in the hydrogen bromide solution is 45-55%, and the mole ratio of the hydrogen bromide to the ethylene in the input hydrogen bromide solution is 0.66-1.15:0.77-1.25 in the fixed bed reactor (12).
11. The process according to any one of claims 8 to 10, wherein the reaction temperature of the internal bed reactor (7) is 15 to 45 ℃, the hydrogen partial pressure is 500 to 750Pa, the reaction temperature of the fixed bed reactor (12) is 45 to 70 ℃, and the reaction pressure is 0.2 to 0.3Mpa.
12. The process according to claim 11, wherein the reaction temperature of the internal bed reactor (7) is 22 to 41 ℃, the reaction temperature of the fixed bed reactor (12) is 50 to 65 ℃ and the pressure is 0.22 to 0.3Mpa.
13. The process according to claim 12, wherein the reaction temperature of the fixed bed reactor (12) is 55-65 ℃.
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| CN1429799A (en) * | 2003-01-04 | 2003-07-16 | 大连理工大学 | Synthesis method of 1-bromoane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1429799A (en) * | 2003-01-04 | 2003-07-16 | 大连理工大学 | Synthesis method of 1-bromoane |
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| Title |
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| An Efficient Algorithm for Automating Classification of Chemical Reactions into Classes in Ugi’s Reaction Scheme;Sanjay Ram等;International Journal of Chemoinformatics and Chemical Engineering;第2卷(第2期);第1-14页 * |
| 制备干燥澳化氢的改良方法;邵建本等;药学通报;第19卷(第10期);第27-28页 * |
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