CN212246823U - System for isoflurane ketone hydrogenation production 3,3, 5-trimethyl cyclohexanol - Google Patents
System for isoflurane ketone hydrogenation production 3,3, 5-trimethyl cyclohexanol Download PDFInfo
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- CN212246823U CN212246823U CN202021550931.6U CN202021550931U CN212246823U CN 212246823 U CN212246823 U CN 212246823U CN 202021550931 U CN202021550931 U CN 202021550931U CN 212246823 U CN212246823 U CN 212246823U
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Abstract
The utility model discloses a system for producing 3,3, 5-trimethyl cyclohexanol by hydrogenation of isophorone, which comprises a hydrogenation reaction part and a separation circulation part, wherein the hydrogenation reaction part comprises an isophorone circulation tank, a feed pump, a raw material preheater, a hydrogenation reaction kettle and a hydrogen compressor, and the isophorone circulation tank, the feed pump, the raw material preheater and the hydrogenation reaction kettle are sequentially communicated; the separation circulation part comprises a cooler, a gas-liquid separation buffer tank, a first rectifying tower, a second rectifying tower and a final cooler which are sequentially communicated, the raw material preheater is communicated with the cooler, the first rectifying tower is communicated with the isophorone circulation tank through a desalted water circulating pump, and the second rectifying tower is communicated with the isophorone circulation tank through the isophorone circulating pump. The system can effectively solve the problems that the prior equipment cannot fully utilize heat, so that energy is wasted and continuous production cannot be realized.
Description
Technical Field
The utility model belongs to the technical field of fine chemical production, concretely relates to system for isoflurane ketone hydrogenation production 3,3, 5-trimethyl cyclohexanol.
Background
3,3, 5-Trimethylcyclohexanol (TMOL) is an important intermediate for synthesizing cyclanoate (vasodilator drug) in the medical field; and also for the synthesis of novel plasticizers, lubricants, dinitriles, diamines and alcohol intermediates.
At present, 3, 5-trimethylcyclohexanol is prepared by hydrogenation reaction of isophorone, the preparation process is usually carried out in a fixed bed reactor, in a gas-solid phase reaction, the gasification of raw material isophorone needs to reach a high temperature of over 240 ℃, and the problems of hydrogenation metal sintering, catalyst carrier carbon deposition and the like easily occur in a surface supported Ni and Cu based catalyst at the temperature, so that the conversion rate of isophorone and the selectivity of TMOL are reduced in the reaction process. For preparing 3,3, 5-trimethylcyclohexanol by using a high-pressure reaction kettle to carry out liquid-phase hydrogenation reaction, heating is needed in the reaction process, and after the reaction is finished, heat is generally dissipated, so that the heat is not fully utilized, and the waste of energy is caused; in addition, the existing equipment cannot carry out continuous batch production in the process of preparing the 3,3, 5-trimethylcyclohexanol, so that the preparation efficiency of the 3,3, 5-trimethylcyclohexanol is low.
SUMMERY OF THE UTILITY MODEL
To the above-mentioned not enough among the prior art, the utility model provides a system of isoflurane ketone hydrogenation production 3,3, 5-trimethyl cyclohexanol, this system can effectively solve the easy high temperature inactivation of catalyst that current production method exists, can't make full use of the heat, leads to the extravagant and unable continuous production's of energy problem.
In order to achieve the above object, the present invention provides a technical solution for solving the technical problem:
a system for producing 3,3, 5-trimethylcyclohexanol by hydrogenation of isophorone comprises a hydrogenation reaction part and a separation circulation part, wherein the hydrogenation reaction part comprises an isophorone circulation tank, a feed pump, a raw material preheater, a hydrogenation reaction kettle and a hydrogen compressor, the isophorone circulation tank, the feed pump, the raw material preheater and the hydrogenation reaction kettle are sequentially communicated, the hydrogen compressor is also communicated with the hydrogenation reaction kettle, a discharge port of the hydrogen compressor is also communicated with the raw material preheater, and an oil guide pipeline is also arranged on the hydrogenation reaction kettle;
the separation circulating part comprises a cooler, a gas-liquid separation buffer tank, a first rectifying tower, a second rectifying tower and a final cooler which are sequentially communicated, the raw material preheater is communicated with the cooler, the first rectifying tower is communicated with the isophorone circulating tank through a desalted water circulating pump, and the second rectifying tower is communicated with the isophorone circulating tank through an isophorone circulating pump;
hydrogenation cauldron includes the cauldron body, and the internal portion of cauldron is provided with spiral heating pipe and hydrogen distributor, and the hydrogen distributor sets up in the spiral heating pipe lower part, and cauldron body bottom is provided with the drain, and cauldron body upper portion is provided with hydrogen import and hydrogen discharge port, and cauldron body side wall is provided with conduction oil import, feed inlet, conduction oil export and reaction liquid export, and conduction oil import and conduction oil export are linked together with the both ends of spiral heating pipe respectively, and hydrogen import and hydrogen distributor intercommunication.
The beneficial effect that above-mentioned scheme produced does: heat conducting oil enters the spiral heating pipe through the heat conducting oil inlet to heat the interior of the kettle body, so that the isophorone hydrogenation reaction is promoted to be carried out, and the heat conducting oil in the spiral heating pipe is finally discharged through the heat conducting oil outlet; hydrogen enters the kettle body through the hydrogen inlet and enters the hydrogen distributor, the hydrogen is uniformly discharged through the hydrogen distributor, the hydrogen is uniformly contacted with the isophorone, the reaction effect is improved, and the reacted hydrogen is discharged through the hydrogen discharge port and collected; the isophorone and desalted water enter the kettle body through the feeding hole, and the mixture after reaction is discharged through the reaction liquid outlet; the continuous reaction can be realized by the device.
The feeding pump is used for conveying raw materials in the isophorone circulating tank into the raw material preheater, the temperature in the raw material preheater is used for exchanging heat of the entering raw materials to 60-100 ℃, the raw materials are preheated, the preheated raw materials enter the hydrogenation reaction kettle, heat conducting oil is continuously introduced into the hydrogenation reaction kettle to heat the hydrogenation reaction kettle, hydrogen is conveyed into the hydrogenation reaction kettle through the hydrogen compressor, and the hydrogen and the isophorone in the hydrogenation reaction kettle react to generate 3,3, 5-trimethyl cyclohexanol containing certain impurities.
Discharging the 3,3, 5-trimethylcyclohexanol mixed product generated in the hydrogenation reactor into a raw material preheater again through a discharge hole of the hydrogenation reactor, and recovering heat carried on the mixed product through the raw material preheater so as to preheat isophorone at the next time, thereby saving energy consumption and reducing energy loss; and continuously flowing the mixed product in the raw material preheater into a cooler for cooling to 38-45 ℃, feeding the cooled mixed product into a gas-liquid separation buffer tank, separating hydrogen in the mixed product through the gas-liquid separation buffer tank, continuously feeding the rest product into a first rectifying tower, distilling 3,3, 5-trimethylcyclohexanol out of a first tower kettle of the rectifying tower, feeding the distilled 3,3, 5-trimethylcyclohexanol into a 3,3, 5-trimethylcyclohexanol buffer tank for buffering, continuously feeding the 3,3, 5-trimethylcyclohexanol in the 3,3, 5-trimethylcyclohexanol buffer tank into a second rectifying tower for rectifying, and cooling the 3,3, 5-trimethylcyclohexanol separated from the tower top through a final cooler and discharging to obtain the product. The desalted water separated by the first rectifying tower is distilled off from the top of the first rectifying tower and pumped into an isophorone circulating tank through a desalted water circulating pump for recycling, the isophorone separated by the second rectifying tower is pumped into the isophorone circulating tank through the isophorone circulating pump for recycling, and heat in a mixed product can be exchanged with the isophorone and the desalted water through a raw material preheater by the device, so that the heat of the solution after reaction is recycled, and the energy consumption is saved; the desalted water pump that will separate out is gone into in the isophorone circulating tank through the desalted water circulating pump and is carried out reuse, and it is extravagant to reduce the raw materials, and simultaneously, be provided with gas-liquid separation buffer tank and 3,3, 5-trimethyl cyclohexanol buffer tank, can store a certain amount of product mixture, play the effect of buffering, has maintained the steady operation of rectifying column one and rectifying column two to a certain extent for it is rationally distributed between each device of this system, can realize continuous production.
Further, a hydrogen program control valve is arranged between the hydrogen compressor and the hydrogenation reaction kettle.
The beneficial effect that above-mentioned scheme produced does: after the pressure in the hydrogenation reaction kettle is too high, the opening degree of the hydrogen program control valve can be reduced, the dynamic stability of the reaction pressure is further maintained, the safety performance of the reaction is improved, and the device has the advantage of convenience in operation.
Furthermore, a conduction oil program control valve is arranged on the conduction oil pipeline.
The beneficial effect that above-mentioned scheme produced does: when the temperature in the hydrogenation reaction kettle is too high or too low, the adding amount of the heat conduction oil can be adjusted by controlling the opening of the heat conduction oil program control valve, so that the dynamic stability of the reaction temperature in the hydrogenation reaction kettle is maintained.
Furthermore, a raw material program control valve is arranged between the raw material preheater and the hydrogenation reaction kettle.
The beneficial effect that above-mentioned scheme produced does: when the liquid level in the hydrogenation reaction kettle is too high, the adding of raw materials can be reduced by controlling the opening degree of the raw material program control valve, and further the dynamic stability of the reaction liquid level is maintained.
Further, the upper part of the hydrogenation reaction kettle is provided with a safety valve.
The beneficial effect that above-mentioned scheme produced does: be connected with the hydrogen recovery pipeline on the relief valve, when the pressure in the hydrogenation cauldron was too big, the relief valve was opened, released the pressure in the hydrogenation cauldron to the hydrogen recovery pipeline in, and then guaranteed the holistic security of device.
Furthermore, the number of the trays in the first rectifying tower is 20-60.
Furthermore, the number of the trays in the second rectifying tower is 30-60.
The beneficial effect that above-mentioned scheme produced does: the purity of the finally obtained product is improved by adjusting the number of the tower plates in the first rectifying tower and the second rectifying tower.
The use method of the system for producing 3,3, 5-trimethylcyclohexanol by hydrogenation of isophorone comprises the following steps:
(1) conveying the isophorone and desalted water into an isophorone circulating tank together for mixing, pumping the mixture in the isophorone circulating tank into a raw material preheater by using a feed pump, and continuously feeding the mixture into a hydrogenation reaction kettle after preheating treatment;
(2) introducing hydrogen into the hydrogenation reaction kettle, simultaneously introducing heat-conducting oil to heat the hydrogenation reaction kettle, and reacting the hydrogen in the hydrogenation reaction kettle with the isophorone;
(3) after the reaction is finished, discharging the product mixed liquor back to the raw material preheater through the discharge port for cooling, conveying the product mixed liquor to a cooler through a pipeline, and conveying the product mixed liquor into a separation buffer tank after the product mixed liquor is cooled through the cooler;
(4) separating hydrogen dissolved in the product mixed solution by a separation buffer tank, feeding the residual product mixed solution into a first rectifying tower, separating desalted water and a mixed solution of 3,3, 5-trimethylcyclohexanol and isophorone by the first rectifying tower, conveying the separated desalted water to a isophorone circulating tank by a desalted water circulating pump, conveying the separated mixed solution of 3,3, 5-trimethylcyclohexanol and isophorone to a 3,3, 5-trimethylcyclohexanol buffer tank for buffering, conveying the mixed solution of 3,3, 5-trimethylcyclohexanol and isophorone to a second rectifying tower, discharging the distilled 3,3, 5-trimethylcyclohexanol at the top of the second rectifying tower after cooling by a final cooler, conveying the distilled isophorone at the bottom into the isophorone circulating tank by the isophorone circulating pump, can be repeatedly used
The beneficial effect that above-mentioned scheme produced does: the device can realize the continuous production of 3,3, 5-trimethylcyclohexanol, and simultaneously realize the heat exchange, thereby achieving the purposes of saving energy consumption, recycling desalted water and reducing cost.
Further, the heating temperature in the hydrogenation reaction kettle is 100-140 ℃.
The beneficial effect that above-mentioned scheme produced does: the temperature is most beneficial to the reaction of the isophorone and hydrogen, the hydrogenation effect of the isophorone is improved, and the purity of the 3,3, 5-trimethylcyclohexanol is further improved.
Further, the temperature of the product mixed liquor cooled by the cooler is 38-45 ℃.
The beneficial effect that above-mentioned scheme produced does: after the temperature is reduced to the temperature, the hydrogen in the product mixed liquid is easy to separate, and the separated hydrogen is recovered by the gas-liquid separation buffer tank, so that the waste of raw materials is reduced.
Further, the separation molar reflux ratio of the first rectifying tower is set to be 0.5-2.0, and the tower top pressure is set to be 0.01-1.0 MPa.
Further, the separation molar reflux ratio of the second rectifying tower is set to be 2.5-2.0, and the tower top pressure is set to be 0.01-0.5 MPa.
The beneficial effect that above-mentioned scheme produced does: the rectification effect is best under the parameter, and the purity of the rectified 3,3, 5-trimethylcyclohexanol is higher.
The utility model discloses produced beneficial effect does:
the system is internally provided with a raw material preheater, the product mixed solution, the isophorone and the desalted water can be subjected to heat exchange through the raw material preheater, and the heat in the product mixed solution is transferred to the isophorone and the desalted water, so that the heat consumption in the reaction process is reduced, and the energy consumption is saved; the device is provided with a gas-liquid separation buffer tank, the device can separate a small amount of hydrogen in a product mixed liquid, the hydrogen is recycled, the raw materials are saved, the production cost is reduced, meanwhile, the device can store a certain amount of the product mixed liquid and is used for maintaining the stable operation of the first rectifying tower, and then the continuous production of 3,3, 5-trimethylcyclohexanol is realized, the 3,3, 5-trimethylcyclohexanol buffer tank is arranged, the 3,3, 5-trimethylcyclohexanol mixed liquid can also be buffered, the 3,3, 5-trimethylcyclohexanol mixed liquid is rectified again through the second rectifying tower, the purity of the 3,3, 5-trimethylcyclohexanol is improved, and meanwhile, the continuous production is realized.
Drawings
Fig. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic structural diagram of a hydrogenation reactor;
reference numerals: v0101, an isophorone circulating tank; p0101, a feed pump; e0101, a raw material preheater; r0101 and a hydrogenation reaction kettle; c0101, a hydrogen compressor; e0102, a cooler; v0102, a gas-liquid separation buffer tank; t0101, a rectifying tower I; e0103, a final cooler; p0102, a desalted water circulating pump; VA0101, hydrogen program control valve; VA0103, a conduction oil program control valve; VA0102, raw material program control valve; SA0101, safety valve; a V0103, 3, 5-trimethylcyclohexanol buffer tank; t0102, a second rectifying tower; p0103, an isophorone circulating pump; 1. a spiral heating pipe; 2. a hydrogen distributor; 3. a sewage draining outlet; 4. a hydrogen inlet; 5. a hydrogen gas discharge port; 6. a heat conducting oil inlet; 7. a feed inlet; 8. a heat conducting oil outlet; 9. and (4) a reaction liquid outlet.
Detailed Description
The following detailed description of the embodiments of the present invention will be made with reference to the accompanying drawings.
The utility model discloses an embodiment, as shown in fig. 1-2, provide a system of isoflurane ketone hydrogenation production 3,3, 5-trimethyl cyclohexanol, including hydrogenation part and separation circulation part, hydrogenation part includes isoflurane ketone circulation tank V0101, charge pump P0101, raw materials pre-heater E0101, hydrogenation cauldron R0101 and hydrogen compressor C0101, isoflurane ketone circulation tank V0101, charge pump P0101, raw materials pre-heater E0101 and hydrogenation cauldron R0101 communicate in proper order, hydrogen compressor C0101 also communicates with hydrogenation cauldron R0101, hydrogenation cauldron R0101's discharge gate still is linked together with raw materials pre-heater E0101, still is provided with the oil guide pipeline on the hydrogenation cauldron R0101; optimally, a hydrogen program control valve VA0101 is arranged between a hydrogen compressor C0101 and a hydrogenation reaction kettle R0101. Optimally, a conduction oil program control valve VA0103 is arranged on the conduction oil pipeline. Optimally, a raw material program control valve VA0102 is also arranged between the raw material preheater E0101 and the hydrogenation reaction kettle R0101. Optimally, the upper part of the hydrogenation reactor R0101 is provided with a safety valve SA 0101. Optimally, the hydrogenation reaction kettle comprises a kettle body, a spiral heating pipe 1 and a hydrogen distributor 2 are arranged in the kettle body, the hydrogen distributor 2 is arranged on the lower portion of the spiral heating pipe 1, a drain outlet 3 is arranged at the bottom of the kettle body, a hydrogen inlet 4 and a hydrogen discharge outlet 5 are arranged on the upper portion of the kettle body, a conduction oil inlet 6 is formed in the side wall of the kettle body, a feed inlet 7, a conduction oil outlet 8 and a reaction liquid outlet 9 are formed in the side wall of the kettle body, the conduction oil inlet 6 and the conduction oil outlet 8 are respectively communicated with two ends of the spiral heating pipe 1, and the hydrogen.
The separation circulation part comprises a cooler E0102, a gas-liquid separation buffer tank V0102, a rectification tower I T0101, a rectification tower II T0102 and a final cooler E0103 which are sequentially communicated, wherein the raw material preheater E0101 is communicated with the cooler E0102, the rectification tower I T0101 is communicated with the isophorone circulation tank V0101 through a desalted water circulating pump P0102, and the rectification tower II T0102 is communicated with the isophorone circulation tank V0101 through the isophorone circulating pump P0103. Optimally, the number of the trays in the first rectifying tower T0101 is 20-60, and the number of the trays in the second rectifying tower T0102 is 30-60.
The use method of the system for producing 3,3, 5-trimethylcyclohexanol by hydrogenation of isophorone specifically comprises the following steps:
(1) conveying isoflurane ketone and desalted water from a plant area into an isoflurane ketone circulating tank V0101 together for mixing, then pressurizing to 3.0MPa by using a feed pump P0101, pumping the mixture in the isoflurane ketone circulating tank V0101 into a raw material preheater E0101, exchanging heat with a reacted product mixed solution to 100 ℃ for preheating treatment, and then continuously entering a hydrogenation reaction kettle R0101, and reducing the opening of a raw material program control valve when the liquid level of the mixed solution reaches 60% of the whole reaction kettle;
(2) introducing hydrogen into a hydrogenation reaction kettle R0101 through a hydrogen compressor C0101, and simultaneously introducing heat conduction oil at 200 ℃ to heat the interior of the hydrogenation reaction kettle R0101, optimally, the heating temperature in the hydrogenation reaction kettle R0101 is 120 ℃, starting a stirrer at the top of the hydrogenation reaction kettle, and enabling the hydrogen to react with the isophorone for 180min at the rotating speed of 600 rpm/min;
(3) after the reaction is finished, opening a hydrogen discharge valve at the top of the hydrogenation reaction kettle, reducing the pressure in the hydrogenation reaction kettle to 0.18MPa, then discharging the product mixed liquid back into the raw material preheater E0101 through a discharge port to cool to 80 ℃, then conveying the product mixed liquid to the cooler E0102 through a pipeline, conveying the product mixed liquid into the gas-liquid separation buffer tank V0102 after cooling through the cooler E0102, and optimally, controlling the temperature of the product mixed liquid cooled by the cooler E0102 to be 45 ℃;
(4) the gas-liquid separation buffer tank V0102 separates the hydrogen dissolved in the product mixed liquid, the separated hydrogen is recovered through a hydrogen pipeline, the rest of the product mixed liquid enters a rectification tower I T0101 with 50 trays, optimally, the separation molar reflux ratio of the rectification tower I T0101 is set to be 2.0, the pressure at the tower top is set to be 1.0MPa, desalted water and 3,3, 5-trimethylcyclohexanol are separated through the rectification tower I T0101, the separated desalted water is conveyed to an isoflurolone circulation tank V0101 through a desalted water circulation pump P0102, the separated 3,3, 5-trimethylcyclohexanol is conveyed to a 3,3, 5-trimethylcyclohexanol buffer tank V0103 for buffering, the 3,3, 5-trimethylcyclohexanol buffer tank V0103 in the 3,3, 5-trimethylcyclohexanol buffer tank V0103 is continuously conveyed to a rectification tower II T0102, and the 3 at the top of the rectification tower II T0102 is distilled out, the 3, 5-trimethylcyclohexanol is cooled by an end cooler E0103 through the end cooler E0103 and then discharged, and the isophorone distilled from the bottom is conveyed into an isophorone circulating tank V0101 through an isophorone circulating pump P0103 for recycling.
Claims (7)
1. The system for producing 3,3, 5-trimethylcyclohexanol by hydrogenation of isophorone is characterized by comprising a hydrogenation reaction part and a separation circulation part, wherein the hydrogenation reaction part comprises an isophorone circulation tank (V0101), a feed pump (P0101), a raw material preheater (E0101), a hydrogenation reaction kettle (R0101) and a hydrogen compressor (C0101), the isophorone circulation tank (V0101), the feed pump (P0101), the raw material preheater (E0101) and the hydrogenation reaction kettle (R0101) are sequentially communicated, the hydrogen compressor (C0101) is also communicated with the hydrogenation reaction kettle (R0101), a discharge hole of the hydrogenation reaction kettle (R0101) is also communicated with the raw material preheater (E0101), and an oil guide pipeline is further arranged on the hydrogenation reaction kettle (R0101);
the separation circulation part comprises a cooler (E0102), a gas-liquid separation buffer tank (V0102), a first rectifying tower (T0101), a 3,3, 5-trimethylcyclohexanol buffer tank (V0103), a second rectifying tower (T0102) and a final cooler (E0103), which are sequentially communicated, wherein the raw material preheater (E0101) is communicated with the cooler (E0102), the first rectifying tower (T0101) is communicated with the isoflurolone circulation tank (V0101) through a desalted water circulating pump (P0102), and the second rectifying tower (T0102) is communicated with the isoflurolone circulation tank (V0101) through an isoflurolone circulating pump (P0103);
hydrogenation cauldron (R0101) is including the cauldron body, the internal portion of cauldron is provided with spiral heating pipe (1) and hydrogen distributor (2), hydrogen distributor (2) set up in spiral heating pipe (1) lower part, cauldron body bottom is provided with drain (3), cauldron body upper portion is provided with hydrogen import (4) and hydrogen gas discharge port (5), cauldron body side wall is provided with conduction oil import (6), feed inlet (7), conduction oil export (8) and reaction liquid outlet (9), conduction oil import (6) and conduction oil export (8) respectively with the both ends of spiral heating pipe (1) are linked together, hydrogen import (4) with hydrogen distributor (2) intercommunication.
2. System for the hydrogenation of isophorone to 3,3, 5-trimethylcyclohexanol according to claim 1, wherein a hydrogen program control valve (VA0101) is disposed between the hydrogen compressor (C0101) and the hydrogenation reactor (R0101).
3. The system for producing 3,3, 5-trimethylcyclohexanol by hydrogenation of isophorone according to claim 1, wherein the conduction oil pipeline is provided with a conduction oil program control valve (VA 0103).
4. The system for producing 3,3, 5-trimethylcyclohexanol by hydrogenation of isophorone according to claim 1, wherein a feed programmable valve (VA0102) is further disposed between the feed preheater (E0101) and the hydrogenation reactor (R0101).
5. The system for producing 3,3, 5-trimethylcyclohexanol by hydrogenation of isophorone according to claim 1, wherein the upper part of hydrogenation reactor (R0101) is provided with a safety valve (SA 0101).
6. The system for producing 3,3, 5-trimethylcyclohexanol by hydrogenation of isophorone according to claim 1, wherein the number of plates in rectifying column one (T0101) is 20-60.
7. The system for producing 3,3, 5-trimethylcyclohexanol by hydrogenation of isophorone according to claim 1, wherein the number of plates in rectifying column two (T0102) is 30-60.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021550931.6U CN212246823U (en) | 2020-07-30 | 2020-07-30 | System for isoflurane ketone hydrogenation production 3,3, 5-trimethyl cyclohexanol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021550931.6U CN212246823U (en) | 2020-07-30 | 2020-07-30 | System for isoflurane ketone hydrogenation production 3,3, 5-trimethyl cyclohexanol |
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