CN111875471B - Catalyst circulation dehydration chloromethane synthesis process - Google Patents
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- CN111875471B CN111875471B CN202010736545.4A CN202010736545A CN111875471B CN 111875471 B CN111875471 B CN 111875471B CN 202010736545 A CN202010736545 A CN 202010736545A CN 111875471 B CN111875471 B CN 111875471B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/16—Preparation of halogenated hydrocarbons by replacement by halogens of hydroxyl groups
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- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/02—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention discloses a chloromethane synthesis process for catalyst cyclic dehydration. Hydrogen chloride and methanol react in a chloromethane reactor to generate chloromethane and water, the catalyst and the water are discharged from the bottom of the chloromethane reactor and enter a catalyst dehydration tank, the catalyst and the water are gasified and leave the system after being heated by a heat exchanger, and the catalyst returns to the chloromethane reactor through a catalyst circulating pump. Compared with the prior art, the process avoids the generation of a large amount of dilute hydrochloric acid in the synthesis of chloromethane through the dehydration of the catalyst, and the concentration of the catalyst in the reactor is accurately regulated through the regulation and control of the circulation quantity and the dehydration rate of the catalyst solution. Meanwhile, the reaction rate is improved by the countercurrent flow of the catalyst and the gas phase raw material.
Description
Technical Field
The invention belongs to the field of chloromethane synthesis, and particularly relates to a chloromethane synthesis process for catalyst cyclic dehydration.
Background
Methyl chloride is an important raw material for organosilicon, methylcellulose and quaternary ammonium compound products. At present, the chloromethane synthesis method comprises a methane chlorination method and a methanol hydrogen oxidation method. The principle of the methanol-hydrogen oxidation method is that methanol reacts with hydrogen chloride to produce chloromethane and water, which has industrial feasibility. The methanol hydrogen oxidation method can be divided into a gas-liquid non-catalytic process, a gas-solid catalytic process and a gas-liquid catalytic process with wide application. The gas-liquid catalytic process has mild reaction condition and high selectivity. The reaction equation is as follows:
hydrogen chloride + methanol = methyl chloride + water
There are three significant disadvantages to the gas-liquid catalytic process in industrial production. Firstly, the reaction product water is separated from the reaction system along with the gas phase, and a large amount of low-concentration hydrochloric acid is formed after condensation. The treatment process of the low-concentration hydrochloric acid is complex, and the investment and the energy consumption are high; secondly, the proportion of the catalyst to water in the catalyst aqueous solution is determined by the composition of the exhaust gas of the reactor, and the concentration of the catalyst cannot be independently regulated and controlled, so that the catalytic efficiency is affected; thirdly, when the catalyst solution is added into the reactor, the catalyst solution depends on gas-liquid contact formed by bubbling raw material gas, and the insufficient gas-liquid contact surface severely limits the production capacity and the industrial scale of a single device.
CN209010413U provides a chloromethane synthesis process in which two reaction kettles are connected in series, and the crude chloromethane gas in the first reaction kettle is compressed by a compressor and sent to the second reaction kettle. The addition of compressors increases the complexity and investment costs of the system.
CN209555111U provides a chloromethane synthesis apparatus without by-product hydrochloric acid. The problem that the wastewater in the pure water separator contains hydrochloric acid with low concentration cannot be avoided because of the azeotropic phenomenon of the aqueous hydrochloric acid solution. The treatment of salt-containing wastewater formed by a neutralization unit in the process is also a great difficulty in the chemical process.
Disclosure of Invention
The invention aims to provide a chloromethane synthesis process for catalyst cyclic dehydration, which fundamentally avoids the problems that a large amount of diluted hydrochloric acid is generated by mixing hydrogen chloride with water in chloromethane synthesis and the subsequent separation is difficult by a catalyst cyclic dehydration method.
The technical scheme of the invention is that the chloromethane synthesis process for catalyst cyclic dehydration is characterized by comprising the following steps:
1. the reaction raw materials of hydrogen chloride and methanol gas are heated and mixed and then sent to the bottom of a chloromethane reactor, and uniformly distributed by a gas distributor and then flow from bottom to top; the concentrated catalyst solution is sent to the top of a chloromethane reactor and flows from top to bottom after being distributed by a liquid distributor; the gas-liquid two-phase reverse flow fully contacts and reacts to generate chloromethane and water. The reaction temperature is 80-280 ℃, and the reaction pressure is-0.1-3.0 MPaG.
2. Due to the water absorption of the concentrated catalyst solution and the homoionic effect of chloride ions, unreacted hydrogen chloride and reaction product chloromethane are discharged from the top of the reactor, and water generated by the reaction is discharged from the bottom of the reactor along with the catalyst solution and enters a catalyst dehydration tank. Thus, the hydrogen chloride and the water are discharged in the form of gas phase and liquid phase respectively, and the generation of a large amount of dilute hydrochloric acid is fundamentally avoided.
3. The dilute catalyst solution is heated either before entering the dehydration tank or after entering the cargo removal tank, where the water evaporates and exits the top, the dilute catalyst solution changing to a concentrated catalyst solution. Because the bubble point of the catalyst solution is raised greatly after the concentration of the catalyst solution is raised, the heating before entering the tank has the advantages of large heat transfer temperature difference, effective energy utilization and no back mixing of the solution. The advantage of heating in the form of heat exchanger after entering the tank is that the material circulates in a large amount in the heat exchanger, the single gasification rate is small, the heat transfer coefficient is large, the dehydration speed is easy to control, and the heat exchanger is not easy to scale. The viscosity of the catalyst solution increases with the increase of the concentration, and is easy to crystallize or scale, so that compared with a jacket heating mode, the falling film type, rising film type and thermosiphon type applicability are better. In the invention, a proper scheme is selected according to the production scale, the industries and the like. The concentration of the concentrated catalyst generated after dehydration is 60-98 wt% and the temperature is 80-280 ℃.
4. The dehydrated catalyst solution is conveyed to a chloromethane reactor by a catalyst circulating pump, and the catalyst reacts with hydrogen chloride and methanol which newly enter the reactor to complete the circulation of the catalyst. Through regulating and controlling the dehydration temperature of the catalyst solution and the circulation quantity of the catalyst solution, the concentration of the catalyst solution in the catalyst can be well controlled, thereby realizing the accurate control of the reaction efficiency.
A chloromethane synthesis process for catalyst cyclic dehydration is characterized by comprising the following steps:
(1) The reaction raw materials of hydrogen chloride and methanol gas are heated and mixed and then sent to the bottom of a chloromethane reactor, and uniformly distributed by a gas distributor and then flow from bottom to top; the concentrated catalyst solution is sent to the top of a chloromethane reactor and flows from top to bottom; the gas-liquid two-phase countercurrent flows to fully contact and react to generate chloromethane and water;
(2) Unreacted hydrogen chloride and reaction product chloromethane are discharged from the top of the chloromethane reactor, and water generated by the reaction is discharged from the bottom of the chloromethane reactor along with the catalyst solution and enters a heat exchanger, so that the hydrogen chloride and the water are respectively discharged in the form of gas phase and liquid phase, thereby fundamentally avoiding the generation of a large amount of dilute hydrochloric acid;
(3) Heating the dilute catalyst solution in a heat exchanger, wherein water is evaporated, separated and discharged, the dilute catalyst solution is changed into a concentrated catalyst solution, the concentration of the concentrated catalyst generated after dehydration is 60-98wt% and the temperature is 80-280 ℃;
(4) The dehydrated catalyst solution is sent to a chloromethane reactor, and the catalyst reacts with hydrogen chloride and methanol which newly enter the chloromethane reactor to complete the circulation of the catalyst; through regulating and controlling the dehydration temperature of the catalyst solution and the circulation quantity of the catalyst solution, the concentration of the catalyst solution in the catalyst can be well controlled, thereby realizing the accurate control of the reaction efficiency.
The invention precisely regulates and controls the concentration of the catalyst in the reactor through the circulation volume of the aqueous solution of the catalyst and the dehydration temperature thereof, and improves the reaction efficiency and the reaction controllability. Meanwhile, the invention solves the problems of insufficient contact between the catalyst and the reaction raw materials and large-scale synthesis of chloromethane in a mode of reverse contact reaction of gas phase upward and liquid phase downward.
Drawings
FIG. 1 is one of the process diagrams for synthesizing chloromethane by catalyst cyclic dehydration.
FIG. 2 is a second diagram of a process for synthesizing chloromethane by cyclic dehydration of a catalyst.
FIG. 3 is a diagram of a process for synthesizing chloromethane using a catalyst cycle dehydration process using a rising film heat exchanger.
Fig. 4 is a diagram of a process for synthesizing methyl chloride by cyclic dehydration of a catalyst using a falling film heat exchanger.
Wherein: methyl chloride reactor (R-1), catalyst dehydration tank (V-1), heat exchanger (E-1), climbing film heat exchanger (E-2), falling film heat exchanger (E-3), catalyst circulating pump (P-1), catalyst solution dehydration circulating pump (P-2)
Detailed Description
The process operating characteristics according to the invention are further described below.
As shown in fig. 1, the process of the present invention is as follows:
1. the reaction raw materials of hydrogen chloride and methanol gas are heated and mixed and then sent to the bottom of a chloromethane reactor (R-1), and uniformly distributed by a gas distributor and then flow from bottom to top; the concentrated catalyst solution is sent to the top of a chloromethane reactor (R-1) and flows from top to bottom after being distributed by a liquid distributor; the gas-liquid two-phase reverse flow fully contacts and reacts to generate chloromethane and water. The reaction temperature is 80-250 ℃, and the reaction pressure is-0.1-3.0 MPaG.
2. Unreacted hydrogen chloride and reaction product chloromethane are discharged from the top of the chloromethane reactor (R-1) due to the water absorption of the concentrated catalyst solution and the homoionic effect of chloride ions, and water generated by the reaction is discharged from the bottom of the chloromethane reactor (R-1) along with the catalyst solution to enter a catalyst dehydration tank (V-1). Thus, the hydrogen chloride and the water are discharged in the form of gas phase and liquid phase respectively, and the generation of a large amount of dilute hydrochloric acid is fundamentally avoided.
3. The dilute catalyst solution is heated before entering the catalyst dehydration tank (V-1) or after entering the cargo removal tank, wherein the water evaporates and exits from the top, the dilute catalyst solution changing into a concentrated catalyst solution. Because the bubble point of the catalyst solution is raised greatly after the concentration of the catalyst solution is raised, the heating before entering the tank has the advantages of large heat transfer temperature difference, effective energy utilization and no back mixing of the solution. The advantage of heating in the form of a heat exchanger (E-1) after entering the tank is that the materials circulate in the heat exchanger in a large quantity, the single gasification rate is small, the heat transfer coefficient is large, the dehydration speed is easy to control, and the heat exchanger is not easy to scale. The viscosity of the catalyst solution increases with the increase of the concentration, and is easy to crystallize or scale, so that compared with a jacket heating mode, the falling film type, rising film type and thermosiphon type applicability are better. In the invention, a proper scheme is selected according to the production scale, the industries and the like. The concentration of the concentrated catalyst generated after dehydration is 60-98 wt% and the temperature is 90-280 ℃.
4. The dehydrated catalyst solution is conveyed to a chloromethane reactor (R-1) by a catalyst circulating pump (P-1), and the catalyst reacts with hydrogen chloride and methanol which newly enter the reactor to complete the circulation of the catalyst. Through regulating and controlling the dehydration temperature of the catalyst solution and the circulation quantity of the catalyst solution, the concentration of the catalyst solution in the catalyst can be well controlled, thereby realizing the accurate control of the reaction efficiency.
As shown in fig. 2, the process of the present invention may also employ the following means:
(1) The reaction raw materials of hydrogen chloride and methanol gas are heated and mixed and then sent to the bottom of a chloromethane reactor, and uniformly distributed by a gas distributor and then flow from bottom to top; the concentrated catalyst solution is sent to the top of a chloromethane reactor and flows from top to bottom after being distributed by a liquid distributor; the gas-liquid two-phase countercurrent flows to fully contact and react to generate chloromethane and water;
(2) Unreacted hydrogen chloride and reaction product chloromethane are discharged from the top of the chloromethane reactor, and water generated by the reaction is discharged from the bottom of the chloromethane reactor along with the catalyst solution and enters a heat exchanger, so that the hydrogen chloride and the water are respectively discharged in the form of gas phase and liquid phase, thereby fundamentally avoiding the generation of a large amount of dilute hydrochloric acid;
(3) Heating the dilute catalyst solution in a heat exchanger, wherein water is evaporated, separated and discharged, the dilute catalyst solution is changed into a concentrated catalyst solution, the concentration of the concentrated catalyst generated after dehydration is 70-98 wt% and the temperature is 90-280 ℃;
(4) The dehydrated catalyst solution is sent to a chloromethane reactor, and the catalyst reacts with hydrogen chloride and methanol which newly enter the chloromethane reactor to complete the circulation of the catalyst; through regulating and controlling the dehydration temperature of the catalyst solution and the circulation quantity of the catalyst solution, the concentration of the catalyst solution in the catalyst can be well controlled, thereby realizing the accurate control of the reaction efficiency.
As shown in fig. 3, the process of the present invention may also employ the following manner:
1. hydrogen chloride gas was fed from outside the boundary at 15312kg/h and methanol was fed from outside the boundary at 12807kg/h to the gas distributor at the bottom of the chloromethane reactor (R-1).
2. The dehydrated catalyst is sent to the top of a chloromethane reactor (R-1) and then falls into 8 layers of gas-liquid reaction trays in sequence after passing through a trough-tray type liquid distributor.
3. Methanol and hydrogen chloride continuously flow upwards in a chloromethane reactor (R-1) to continuously react to generate chloromethane and water. When the gas phase reaches the top of the chloromethane reactor (R-1), the methanol is basically completely reacted, the hydrogen chloride gas slightly remains, and the chloromethane concentration reaches the highest. The catalyst flows from top to bottom, continuously catalyzes the reaction and absorbs water which is a reaction product, and reaches the bottom of the chloromethane reactor (R-1).
4. After the dilute catalyst solution automatically flows into a catalyst dehydration tank (V-1), the dilute catalyst solution is sent to a climbing film heat exchanger (E-2) by a catalyst solution dehydration circulating pump (P-2). The catalyst solution flows from bottom to top in the climbing film heat exchanger (E-2), is continuously gasified after being heated by steam, and finally circularly enters the catalyst dehydration tank (V-1) for gas-liquid separation. The gas phase mainly comprising water is discharged from the top of the catalyst dehydration tank (V-1), and the concentrated catalyst is discharged from the bottom of the dehydration tank (V-1), wherein part of the catalyst exists in a crystalline form.
5. And the concentrated catalyst aqueous solution is conveyed to a chloromethane reactor (R-1) by a catalyst circulating pump (P-1) to complete the catalyst circulating dehydration process.
Compared with the traditional process, the chloromethane synthesis process adopting the catalyst for cyclic dehydration realizes the synthesis of chloromethane, and the yield of dilute hydrochloric acid is reduced by 96.95%. The concentration of the catalyst in the chloromethane reactor and the gas-liquid contact strength are improved, the reaction efficiency and the controllability are improved, and the reaction efficiency per unit volume is improved by 31.52 percent.
As shown in fig. 4, the process of the present invention may also employ the following manner:
1. hydrogen chloride gas was fed from outside the boundary at 1167kg/h and methanol was fed from outside the boundary at 896kg/h to the gas distributor at the bottom of the chloromethane reactor (R-1).
2. The dehydrated catalyst is sent to the top of a chloromethane reactor (R-1) and then falls into 5 layers of gas-liquid reaction trays in sequence after passing through an open-pore tray type liquid distributor.
3. Methanol and hydrogen chloride continuously flow upwards in a chloromethane reactor (R-1) to continuously react to generate chloromethane and water. When the gas phase reaches the top of the chloromethane reactor (R-1), the methanol is basically completely reacted, the hydrogen chloride gas slightly remains, and the chloromethane concentration reaches the highest. The catalyst flows from top to bottom, continuously catalyzes the reaction and absorbs water which is a reaction product, and reaches the bottom of the chloromethane reactor (R-1).
4. After the dilute catalyst solution automatically flows into a catalyst dehydration tank (V-1), the dilute catalyst solution is sent to a falling film heat exchanger (E-3) by a catalyst solution dehydration circulating pump (P-2). The dilute catalyst solution flows from top to bottom in the falling film heat exchanger (E-3), is continuously gasified after being heated by steam, and finally circularly enters the catalyst dehydration tank (V-1) for gas-liquid separation. The gas phase mainly composed of water is discharged from the top of the catalyst dehydration tank (V-1), and the concentrated catalyst is discharged from the bottom of the catalyst dehydration tank (V-1), wherein part of the catalyst exists in a crystalline form.
5. And the catalyst circulating pump (P-1) conveys the concentrated catalyst solution to the chloromethane reactor (R-1) to complete the catalyst circulating dehydration process.
Compared with the prior art, the chloromethane synthesis process adopting the catalyst for cyclic dehydration realizes the synthesis of chloromethane, and the yield of dilute hydrochloric acid is reduced by 93.27%. The concentration of the catalyst in the chloromethane reactor and the gas-liquid contact strength are improved, the reaction efficiency and the controllability are improved, and the reaction efficiency per unit volume is improved by 22.72%.
Claims (3)
1. A chloromethane synthesis process for catalyst cyclic dehydration is characterized by comprising the following steps:
(1) The reaction raw materials of hydrogen chloride and methanol gas are heated and mixed and then sent to the bottom of a chloromethane reactor, and uniformly distributed by a gas distributor and then flow from bottom to top; the concentrated catalyst solution is sent to the top of a chloromethane reactor and flows from top to bottom; the gas-liquid two-phase countercurrent flows to fully contact and react to generate chloromethane and water; the reaction temperature is 80-250 ℃, and the reaction pressure is-0.1-3.0 MpaG;
(2) Unreacted hydrogen chloride and reaction product chloromethane are discharged from the top of the chloromethane reactor, and water generated by the reaction is discharged from the bottom of the chloromethane reactor along with the catalyst solution to enter a catalyst dehydration tank, so that the hydrogen chloride and the water are respectively discharged in the form of gas phase and liquid phase, thereby fundamentally avoiding the generation of a large amount of dilute hydrochloric acid;
the water and the catalyst solution generated by the synthesis reaction are discharged from the bottom of the chloromethane reactor, and the chloromethane gas and the unreacted hydrogen chloride gas generated by the synthesis reaction are discharged from the top of the chloromethane reactor;
(3) Heating the dilute catalyst solution in a heat exchanger mode before entering a dehydration tank or after entering the dehydration tank, wherein water is evaporated, discharging the dilute catalyst solution from the top, changing the dilute catalyst solution into a concentrated catalyst solution, and generating a concentrated catalyst with the concentration of 60-98wt% after dehydration and the temperature of 80-280 ℃;
(4) The dehydrated catalyst solution is conveyed to a chloromethane reactor by a catalyst circulating pump, and the catalyst reacts with hydrogen chloride and methanol which newly enter the chloromethane reactor to complete the circulation of the catalyst; through regulating and controlling the dehydration temperature of the catalyst solution and the circulation quantity of the catalyst solution, the concentration of the catalyst solution in the catalyst can be well controlled, thereby realizing the accurate control of the reaction efficiency.
2. A chloromethane synthesis process for catalyst cyclic dehydration is characterized by comprising the following steps:
(1) The reaction raw materials of hydrogen chloride and methanol gas are heated and mixed and then sent to the bottom of a chloromethane reactor, and uniformly distributed by a gas distributor and then flow from bottom to top; the concentrated catalyst solution is sent to the top of a chloromethane reactor and flows from top to bottom; the gas-liquid two-phase countercurrent flows to fully contact and react to generate chloromethane and water; the reaction temperature is 80-250 ℃, and the reaction pressure is-0.1-3.0 MpaG;
(2) Unreacted hydrogen chloride and reaction product chloromethane are discharged from the top of the chloromethane reactor, and water generated by the reaction is discharged from the bottom of the chloromethane reactor along with the catalyst solution and enters a heat exchanger, so that the hydrogen chloride and the water are respectively discharged in the form of gas phase and liquid phase, thereby fundamentally avoiding the generation of a large amount of dilute hydrochloric acid;
the water and the catalyst solution generated by the synthesis reaction are discharged from the bottom of the chloromethane reactor, and the chloromethane gas and the unreacted hydrogen chloride gas generated by the synthesis reaction are discharged from the top of the chloromethane reactor;
(3) Heating the dilute catalyst solution in a heat exchanger, wherein water is evaporated, separated and discharged, the dilute catalyst solution is changed into a concentrated catalyst solution, the concentration of the concentrated catalyst generated after dehydration is 60-98wt% and the temperature is 80-280 ℃;
(4) The dehydrated catalyst solution is sent to a chloromethane reactor, and the catalyst reacts with hydrogen chloride and methanol which newly enter the chloromethane reactor to complete the circulation of the catalyst; through regulating and controlling the dehydration temperature of the catalyst solution and the circulation quantity of the catalyst solution, the concentration of the catalyst solution in the catalyst can be well controlled, thereby realizing the accurate control of the reaction efficiency.
3. A process for synthesizing methyl chloride by cyclic dehydration of a catalyst according to claim 1 or 2, characterized in that: the heat exchanger for heating is in the form of falling film type, rising film type, thermosiphon type, inner jacket, outer jacket, and combined type of inserting heat exchange tube and catalyst dehydration tank.
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