CN211339351U - Cyclohexanone ammoximation reaction separator - Google Patents
Cyclohexanone ammoximation reaction separator Download PDFInfo
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- CN211339351U CN211339351U CN201921685845.3U CN201921685845U CN211339351U CN 211339351 U CN211339351 U CN 211339351U CN 201921685845 U CN201921685845 U CN 201921685845U CN 211339351 U CN211339351 U CN 211339351U
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Abstract
The utility model discloses a cyclohexanone ammoximation reaction separator comprises ammoximation reation kettle, cauldron liquid circulating pump, circulating liquid cooler, reaction liquid filtering separation ware, one upgrades and expects blender and two upgrades and expect the blender. The cyclohexanone ammoximation reaction is carried out in an oximation reaction kettle, a low-frequency stirrer is arranged in the kettle, reaction circulating liquid is forcibly mixed, a hydrogen peroxide feeding and spraying ring pipe is arranged in the kettle, high-concentration hydrogen peroxide is uniformly distributed in the reaction circulating liquid, and the reaction is controlled to be carried out. The utility model discloses set up two and upgrade the material blender, set up the hydrogen peroxide solution injection feeding ring canal in the reation kettle, with hydrogen peroxide solution substep feeding, the part mixes with the material in two upgrade material blenders, and the feeding sprays the ring canal directly and gets into ammoximation reation kettle in the cauldron most, is adapted to the safe needs of high concentration hydrogen peroxide solution like this, has improved the selectivity of hydrogen peroxide solution simultaneously, and the hydrogen peroxide solution selectivity can reach more than 90%.
Description
Technical Field
The invention belongs to the technical field of caprolactam production, and mainly relates to a cyclohexanone ammoximation reaction separation device.
Background
Caprolactam is a main raw material for producing nylon fibers and engineering plastics, and the preparation of cyclohexanone oxime is a key step for producing caprolactam. At present, methods for preparing cyclohexanone oxime mainly comprise a Raschig method, an NO catalytic reduction method, a hydroxylamine phosphate method and an ammoximation method. Among them, the ammoximation method has become the mainstream of caprolactam equipment development in recent years due to the advantages of simple preparation method and safe process, and the research on improvement of the cyclohexanone ammoximation method is continuously carried out.
Chinese patent CN1324684 discloses a method for circularly separating catalyst in titanium-silicon molecular sieve catalytic reaction, which comprises the steps of adding reaction materials containing titanium-silicon molecular sieve catalyst into a membrane separator by a pump, controlling the membrane surface flow rate of the materials in the membrane separator, obtaining clear liquid from the permeation side of the membrane separator, obtaining trapped liquid from the outlet of the membrane separator, and circulating the trapped liquid to a material tank.
Chinese patent ZL02100227.4 discloses a separation method of a titanium-silicon molecular sieve in a ketone ammoximation reaction system. In the technical scheme, the external settler is used for realizing the continuous separation of the titanium silicalite molecular sieve and the reaction product ketoxime.
Chinese patent ZL02100228.2 discloses a method for preparing cyclohexanone oxime by ammoximation of cyclohexanone. In the technical scheme, the external settler is used for realizing the continuous separation of the titanium silicalite molecular sieve and the reaction product ketoxime.
Chinese patent ZL200510133880.0 discloses a method for preparing cyclohexanone oxime. The technical scheme mainly comprises the steps that a reaction mixture forms a circulating flow, and the addition position scheme of cyclohexanone, ammonia and hydrogen peroxide in a reactor does not relate to the separation scheme of reaction materials and a catalyst.
Chinese patent application CN200810227656.1 discloses an ammoximation reaction of a ketone or aldehyde. The method adopts the technical scheme that reaction slurry is subjected to multistage liquid-solid separation through a hydrocyclone and an inorganic membrane or a metal sintering pipe, wherein the hydrocyclone, the inorganic membrane or the metal sintering pipe and the like are external filter elements of a reactor and are arranged behind a circulating pump.
Chinese patent ZL201020046146.7 discloses a cyclohexanone ammoximation reactor. The core of the patent is that the separation of the filtrate and the catalyst is accomplished by a membrane filter installed inside the ammoximation reactor.
Chinese patent ZL201120054873.2 discloses a cyclohexanone ammoximation reaction catalyst separation device. The technical scheme is mainly characterized in that the built-in and external filters of the reactor are connected in series for two-stage step-by-step filtration, filtrate of the built-in filter is directly sent to the external filter for further filtration, and the pore diameter of a membrane tube of the external filter is smaller than that of a membrane tube of the built-in filter.
Chinese patent application CN201110209393.3 discloses an ammoximation reactor for producing cyclohexanone oxime, which claims mainly the internal structure of the reactor, including internal filtering system, liquid ammonia evaporating coil, annular distributor, cylindrical drainage tube, etc.
Chinese patent application CN201210016278.9 discloses a method for preparing cyclohexanone oxime by ammoximation of cyclohexanone, which is characterized in that: the reaction temperature is controlled by a reactant external circulation heat taking mode, and a reaction product is separated from the titanium silicalite molecular sieve in a filter. The scheme also completes the separation of the filtrate and the catalyst by arranging the external filter behind the circulating pump.
Chinese patent ZL201220142109.5 discloses an external inorganic membrane ammoximation catalytic reaction separation device, wherein the reaction materials are subjected to a large circulation among a reaction tank, a feed pump, an external inorganic membrane cross-flow filter and a mixer, and a part of the materials are subjected to a small circulation in a closed loop composed of a feed pipeline, a circulation pump, an external inorganic membrane cross-flow filter, a small circulation pipeline and the like. The scheme is also a scheme that an external filter is arranged behind a circulating pump to complete the separation of the filtrate and the catalyst, and the removal of reaction heat is not involved.
Chinese patent ZL201220294588.2 relates to a cyclohexanone ammoximation catalyst dynamic separation device. The technical scheme realizes the separation of the catalyst and the feed liquid through a disc membrane filter element in a dynamic separator tank body, and the scheme is also that
By providing a dynamic separator after the circulation pump, the separation of the filtrate from the catalyst is accomplished and no solution is involved to remove the heat of reaction.
Chinese patent application CN201210328123.9 relates to a method for filtering and separating catalyst in a reaction system for preparing cyclohexanone oxime, and the core of the method is that the catalyst in the reaction system is filtered and separated by combining two steps of a catalyst pre-separator and a catalyst precision filter to continuously complete the whole separation process. This solution places the catalyst pre-separator after the circulation pump and does not involve a solution to remove the heat of reaction.
Chinese patent application CN200410018607.9 relates to a process for producing acetone oxime or butanone oxime by oxidizing acetone or butanone. The main emphasis is on the description of the reaction parameters, and no specific process description is included.
Chinese patent application CN201110374542.1 relates to a device for preparing acetoxime, which comprises a condenser, an integral reactor, and an external circulating pump. Wherein the integral reactor is a tower reactor.
Chinese patent application CN201010229701.4 relates to a process for the preparation of acetoxime, characterized in that acetone and ammonia are contacted in the presence of a solvent, an oxidant, a surfactant and a catalyst. The claims are primarily directed to the selection of solvents, oxidants, surfactants and catalysts.
The technical schemes provided by the above documents are cyclohexanone, solvent and H2O2The catalyst is directly added into a reactor, is not suitable for the application of high-concentration hydrogen peroxide, and has low effective conversion rate and low selectivity of the hydrogen peroxide.
SUMMERY OF THE UTILITY MODEL
Aims to solve the problem of using high-concentration hydrogen peroxide H in the cyclohexanone ammoximation reaction process2O2The invention provides a cyclohexanone ammoximation reaction device with an increased feed mixer, which solves the problem of low effective conversion rate.
The technical scheme of the utility model is that:
a cyclohexanone ammoximation reaction separation device comprises an ammoximation reaction kettle, a kettle liquid circulating pump, a circulating liquid cooler and a reaction liquid filtering separator, the ammonia oximation reaction kettle is connected with an inlet of a kettle liquid circulating pump, an outlet of the kettle liquid circulating pump is connected with an inlet of a circulating liquid cooler, an outlet of the circulating liquid cooler is connected with an inlet of a reaction liquid filtering separator, the reaction liquid filtering separator is provided with two outlets, namely a clear liquid outlet, namely a circulating liquid outlet, the circulating liquid outlet of the reaction liquid filtering separator is connected with a progressive material mixer, the first progressive material mixer is respectively connected with the ammonia oximation reactor and a second progressive material mixer, the first-order feeding mixture is provided with cyclohexanone, a solvent and a liquid ammonia feeding pipeline, the second progressive material mixer is provided with a hydrogen peroxide feeding pipeline, and the ammonia oximation reaction kettle is provided with a hydrogen peroxide feeding pipeline.
The reaction solution filtering separator is a membrane filter or a metal sintering filter, preferably a ceramic membrane filter; the reaction liquid filter is provided with a reaction flushing pipeline.
The ammoximation reaction kettle is provided with a catalyst replenishing pipeline.
The two-stage feed mixer is provided with a catalyst replenishing pipeline.
The solvent is mainly a lower alcohol, preferably tert-butanol.
The ammoximation reaction kettle is a stirring reaction kettle with a jacket, the stirrer is a low-frequency stirrer, and reaction circulating liquid is forcibly mixed; a hydrogen peroxide feeding and spraying ring pipe is arranged in the kettle, and the high-concentration hydrogen peroxide is uniformly distributed in the reaction circulating liquid to control the reaction.
The cyclohexanone ammoximation reaction separation device is applied to cyclohexanone ammoximation reaction:
adding cyclohexanone, liquid ammonia and tert-butyl alcohol into a first-grade feed mixer, mixing with the filtered and separated circulating liquid, mixing with part of hydrogen peroxide in a second feeder, feeding into an ammoximation reaction kettle for reaction, and feeding most of hydrogen peroxide into the kettle through a feeding and spraying ring pipe in the reaction kettle to be mixed with materials.
The molar ratio of hydrogen peroxide to cyclohexanone in the reaction feed is 1.0-1.2: 1, preferably 1.02 to 1.10: 1; the molar ratio of ammonia to cyclohexanone is 1.1-3.5: 1, preferably 1.3 to 1.8: 1; the reaction temperature is 50-100 ℃, preferably 60-90 ℃; the reaction pressure is higher than the liquid phase equilibrium pressure of the reaction feed liquid, preferably from normal pressure to 0.8MPa, and more preferably from 0.2 to 0.4 MPa; the residence time of the reaction mass is from 20 to 120 minutes, preferably from 40 to 80 minutes.
And pumping the reacted material into a circulating liquid cooler for heat exchange, separating the heat-exchanged material in a filter to obtain clear liquid, introducing the clear liquid into a separation and purification process, and separating and purifying to obtain the cyclohexanone-oxime.
After separating clear liquid, the circulating liquid and fresh feed are mixed in a first-stage feed mixer and then enter an ammoximation reaction kettle.
Has the advantages that:
the invention is provided with two stages of feed mixers, a hydrogen peroxide spraying feeding ring pipe is arranged in the reaction kettle, hydrogen peroxide is fed step by step, part of hydrogen peroxide is mixed with materials in the two stages of feed mixers, and most hydrogen peroxide directly enters the ammoximation reaction kettle through the feeding spraying ring pipe in the kettle, so that the invention is suitable for the safety requirement of high-concentration hydrogen peroxide, and simultaneously improves the selectivity of hydrogen peroxide, and the selectivity of hydrogen peroxide can reach more than 90 percent.
Drawings
FIG. 1A cyclohexanone ammoximation reaction separation device of the present invention
1-ammoximation reaction kettle; 2-a kettle liquid circulating pump; 3-a circulating liquid cooler; 4-reaction liquid filtering separator; 5-a progressive feed mixer; 6-two-stage feed mixer
A-tert-butanol; b-cyclohexanone; c-liquid ammonia; d-hydrogen peroxide; e-clear liquid
Detailed Description
The invention will be further illustrated by the following examples, to which, however, the invention is not restricted.
Example 1:
adding cyclohexanone, liquid ammonia and tert-butyl alcohol into a first-stage feed mixer, mixing with the filtered and separated circulating liquid, mixing with 10-20% of 50-70% hydrogen peroxide in a second-stage feed mixer, feeding into an ammoximation reaction kettle for reaction, and feeding 80-90% of high-concentration hydrogen peroxide into the kettle through a feeding injection ring pipe in the reaction kettle to be mixed with materials.
The molar ratio of hydrogen peroxide to cyclohexanone in the reaction feed is 1.02-1.10: 1; the molar ratio of ammonia to cyclohexanone is 1.3-1.8: 1; the reaction temperature is 60-90 ℃; the reaction pressure is 0.2-0.4 MPa; the concentration of the catalyst is 3-5 percent, and the residence time of the reaction materials is 40-80 minutes.
And pumping the reacted material into a circulating liquid cooler for heat exchange, separating the heat-exchanged material in a reaction liquid separation filter to obtain clear liquid, introducing the clear liquid into a separation and purification process, and separating and purifying to obtain the cyclohexanone-oxime.
After separating clear liquid, the circulating liquid and fresh feed are mixed in a first-stage feed mixer and then enter a second-stage feed mixer.
The detection shows that the effective selectivity of the hydrogen peroxide is 90.1%.
Claims (8)
1. The utility model provides a cyclohexanone ammoximation reaction separator, by ammoximation reation kettle, cauldron liquid circulating pump, circulation liquid cooler, reaction liquid filtering separator, one grade of feed blender and two grades of feed blenders constitute, its characterized in that: ammoximation reation kettle links to each other with cauldron liquid circulating pump import, cauldron liquid circulating pump export and circulation liquid cooler access connection, circulation liquid cooler export and reaction liquid filter separator access connection, reaction liquid filter separator has two exports, firstly, the clear liquid export, firstly, the circulation liquid export, reaction liquid filter separator circulation liquid export and a feed mixer are connected, a upgrades feed mixer and is connected with two grades of feed mixer with ammoximation reactor respectively, one-level feeding mixture is equipped with cyclohexanone, the solvent, liquid ammonia feed line, two grades of feed mixer and is equipped with hydrogen peroxide solution feed line, ammoximation reation kettle is equipped with hydrogen peroxide solution feed line.
2. The cyclohexanone ammoximation reaction separation apparatus of claim 1, wherein the reaction liquid filtering separator is a membrane filter or a metal sintered filter.
3. The cyclohexanone ammoximation reaction separation apparatus of claim 1, wherein the reaction liquid filter is provided with a reaction flushing line.
4. The cyclohexanone ammoximation reaction separation apparatus of claim 1, wherein the two-stage feed mixer is provided with a catalyst replenishment line.
5. The cyclohexanone ammoximation reaction separation device of claim 1, wherein the ammoximation reaction kettle is provided with a catalyst replenishing pipeline.
6. The cyclohexanone ammoximation reaction separation device of claim 1, wherein the ammoximation reaction kettle is a jacketed stirred tank reactor.
7. The cyclohexanone ammoximation reaction separation apparatus of claim 1, wherein the ammoximation reaction vessel is provided with a hydrogen peroxide injection feeding loop.
8. The cyclohexanone ammoximation reaction separation apparatus of claim 2, wherein the membrane filter is a ceramic membrane filter.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112426958A (en) * | 2020-12-31 | 2021-03-02 | 湖南中天元环境工程有限公司 | Ammoximation reaction separation device and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112426958A (en) * | 2020-12-31 | 2021-03-02 | 湖南中天元环境工程有限公司 | Ammoximation reaction separation device and method |
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