CN101074194A - Carboxide synthesis and synthesizer - Google Patents
Carboxide synthesis and synthesizer Download PDFInfo
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- CN101074194A CN101074194A CN 200710069429 CN200710069429A CN101074194A CN 101074194 A CN101074194 A CN 101074194A CN 200710069429 CN200710069429 CN 200710069429 CN 200710069429 A CN200710069429 A CN 200710069429A CN 101074194 A CN101074194 A CN 101074194A
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Abstract
Process for synthesizing carboxide and its apparatus are disclosed. The process is carried out by putting liquid-phase olefin, alcohol or liquid-phase raw material CO and catalyst into synthetic reactor proportionally, carboxide synthetic reacting to carboxide synthetics, extracting carboxide synthetics from top or bottom of reactor, and returning un-reacted CO to reactor under action of double-Venturi circulation jetter. The apparatus consists of synthetic reactor, liquid circulation pump, temperature-controlled heat exchanger, condensing system and synthetic extracting system. Double-Venturi circulation jetter is arranged at lower part of synthetic reactor, light-component separating zone is arranged at upper part of synthetic reactor. It's simple and cheap, has higher synthetic rate and less consumption.
Description
Technical field
The present invention relates to a kind of chemical synthesis process method and device, more particularly, relate to a kind of processing method and device of new oxo process.
Background technology
Oxo process mainly is to carry out building-up reactions with raw material such as alkene, alcohol, amine and CO gas, generates synthetic products such as aldehyde, ester, acid amides.Along with the development of chemical industry, oxo process industry is constantly developed, and product scope constantly enlarges.
At present, oxo process generally is that raw material such as hydro carbons, alcohol or amine and CO gas with liquid phase carries out building-up reactions under the effect of catalyzer.Liquid phase feed adds reactor from top, the phase feed of reactor from the bottom of reactor, facilitates the form adding reactor of the catalyzer of building-up reactions with solution or suspension, and synthetic product is from the liquid phase extraction mouth extraction of reactor bottom.In the gas-circulating system of existing production equipment, work by equipment such as gas circulating compressors realizes unreacted CO gas is turned back in the synthesis reactor, thereby increased the energy consumption of the facility investment of production equipment and system's operation, the global reliability of equipment operation decreases, and has increased the maintenance cost of system.In the extraction system, no matter products of oxo synthesis is light constituent or heavy constituent, all is with the bottom extraction of liquid form from reactor.Owing to be subjected to the restriction of molecular balance, the partial reaction product is from recycle stock during extraction, exist in the extraction material product content low, circulating load is big, catalyzer is discharged synthesis system with material, and the catalyst consumption height causes production equipment huge, usefulness is low, and the production cost height of unit product.
Summary of the invention
Technical problem to be solved by this invention is: at the deficiencies in the prior art, provide a kind of facility investment less, running maintenance is convenient, product content height in the production, catalyst consumption is low, and the synthesis system circulating load is little, processing method that the production cost of unit product is low and device.
Technical scheme of the present invention is:
A kind of processing method of new oxo process comprises:
(1) liquid phase feed such as alkene, alcohol or amine and catalyzer and phase feed CO are added synthesis reactor according to a certain percentage, under certain process conditions, carry out carbongl group synthesis reaction, generate products of oxo synthesis;
(2) products of oxo synthesis that generates in step (1) is with the light-component separating zone of reactive system mixture steam by reactor top, after the condenser system condensation, get the products of oxo synthesis mixed solution, the extraction from system of a part in the mixed solution, another part refluxes; Unreacted CO gets back to reactor under the effect of double-venturi cyclic spray device, reaction end gas emptying after the condenser system condensation;
(3) the system's still liquid after separating is from the output of synthesis reactor bottom in step (1), and behind the liquid circulation pumping action, a part is got back to reactor through double-venturi cyclic spray device, and a part is got back to reactor after the temperature-controlled heat exchanger heat exchange;
(4) the still liquid of getting back to CO, the products of oxo synthesis mixed solution of reactor and get back to reactor in step (2) in step (3) is proceeded carbongl group synthesis reaction with the raw material that adds in the step (1), generates products of oxo synthesis.
An example as above-mentioned processing method, a part of unreacted CO is inhaled into reactor by the pressure reduction of the still liquid generation of the first order jet nozzle of the double-venturi cyclic spray device of flowing through in step (2), and passes through the effect and the reactor liquid uniform mixing of the secondary nozzle of double-venturi cyclic spray device.
A kind of processing method of new oxo process can also be to comprise:
(1) liquid phase feed such as alkene, alcohol or amine and catalyzer and phase feed CO are added synthesis reactor according to a certain percentage, under certain process conditions, carry out carbongl group synthesis reaction, generate products of oxo synthesis;
(2) unreacted CO gets back to reactor under the effect of double-venturi cyclic spray device in step (1), reaction end gas emptying after the condenser system condensation;
(3) the products of oxo synthesis mixed solution that generates in step (1) is from the output of synthesis reactor bottom, a part is by extraction behind the liquid circulation pumping action, a part is got back to reactor through the double-venturi injector, and some gets back to reactor after the temperature-controlled heat exchanger heat exchange in addition;
(4) mixed solution of get back to the CO of reactor in step (2), getting back to reactor in step (3) is proceeded carbongl group synthesis reaction with the raw material that adds in the step (1), generates products of oxo synthesis.
An example as above-mentioned processing method, a part of unreacted CO is inhaled into reactor by the pressure reduction of the mixed solution generation of the first order jet nozzle of the double-venturi cyclic spray device of flowing through in step (2), and passes through the effect and the reactor liquid uniform mixing of the secondary nozzle of double-venturi cyclic spray device.
As the device of realizing above-mentioned first kind of processing method be:
A kind of oxo process device comprises synthesis reactor, liquid circulating pump, temperature-controlled heat exchanger, condenser system and synthetic product extraction system; The bottom of described synthesis reactor is provided with double-venturi cyclic spray device; Described condenser system is to be located at the built-in condenser at synthesis reactor top, described synthetic product extraction system is the phlegma catch tray of built-in condenser below, the phlegma catch tray is provided with phlegma extraction mouth, the top exit of synthesis reactor is communicated with the circulation gas import of the double-venturi cyclic spray device of reactor bottom, and the top exit of reactor also is communicated with the tail gas blowdown system; Perhaps described condenser system comprises external condenser and tail condenser, the synthesis reactor top exit is communicated with condenser, the gaseous phase outlet of condenser is communicated with the gas phase import of tail condenser, the gaseous phase outlet of condenser is communicated with the circulation gas import of the double-venturi injector of synthesis reactor bottom, the gaseous phase outlet of tail condenser is communicated with the tail gas blowdown system, and the liquid phase outlet of condenser and the liquid phase outlet of tail condenser are communicated with; Described synthetic product extraction system is a medial launder, and described medial launder is communicated with the liquid phase outlet of tail condenser and condenser, and medial launder is provided with extraction mouth and refluxing opening, and the refluxing opening of medial launder is communicated with synthesis reactor; The top of synthesis reactor is provided with light-component separating zone; The synthesis reactor outlet at bottom is communicated with liquid circulating pump, and in the described liquid circulating pump one is communicated with temperature-controlled heat exchanger, and temperature-controlled heat exchanger is communicated with synthesis reactor; In the described liquid circulating pump another is communicated with the import of the double-venturi cyclic spray device of synthesis reactor bottom.
As an example of above-mentioned oxo process device, described double-venturi cyclic spray device comprises first order jet nozzle and secondary nozzle, and first order jet nozzle and secondary nozzle are on same axial line.。
Another example as above-mentioned oxo process device is provided with structured packing or column plate in the light-component separating zone of described synthesis reactor.
As the device of realizing above-mentioned second kind of processing method be:
A kind of oxo process device comprises synthesis reactor, liquid circulating pump, temperature-controlled heat exchanger and condenser system; The bottom of described synthesis reactor is provided with double-venturi cyclic spray device; Described condenser system is to be located at the built-in condenser at synthesis reactor top, and the top exit of synthesis reactor is communicated with the circulation gas import of the double-venturi cyclic spray device of reactor bottom, and the top exit of reactor also is communicated with the tail gas blowdown system; Perhaps described condenser system comprises external condenser and tail condenser, the synthesis reactor top exit is communicated with condenser, the gaseous phase outlet of condenser is communicated with the gas phase import of tail condenser, the gaseous phase outlet of condenser is communicated with the circulation gas import of the double-venturi injector of synthesis reactor bottom, the gaseous phase outlet of tail condenser is communicated with the tail gas blowdown system, the liquid phase outlet of condenser and the liquid phase outlet of tail condenser are communicated with, and are communicated with synthesis reactor; The top of synthesis reactor is provided with light-component separating zone; The synthesis reactor outlet at bottom is communicated with liquid circulating pump, and in the described liquid circulating pump one is communicated with temperature-controlled heat exchanger, and temperature-controlled heat exchanger is communicated with synthesis reactor; In the described liquid circulating pump another is communicated with the import of the double-venturi cyclic spray device of synthesis reactor bottom.
As an example of above-mentioned oxo process device, described double-venturi cyclic spray device comprises first order jet nozzle and secondary nozzle, and first order jet nozzle and secondary nozzle are on same axial line.
Another example as above-mentioned oxo process device is provided with structured packing or column plate in the light-component separating zone of described synthesis reactor.
Beneficial effect of the present invention is:
Adopt processing method and device among the present invention, can reduce facility investment, running maintenance is convenient; Product content height when being applied to the light constituent synthetic product, catalyst consumption is low, and the synthesis system circulating load is little, and the production cost of unit product reduces greatly.
Description of drawings
The present invention is further illustrated below in conjunction with accompanying drawing.
Fig. 1 is applicable to that products of oxo synthesis is the processing method and the schematic representation of apparatus of light constituent;
Fig. 2 is applicable to that products of oxo synthesis is the another kind of processing method and the schematic representation of apparatus of light constituent;
Fig. 3 is applicable to that products of oxo synthesis is the processing method and the schematic representation of apparatus of heavy constituent;
Fig. 4 is applicable to that products of oxo synthesis is the another kind of processing method and the schematic representation of apparatus of heavy constituent;
Fig. 5 is a double-venturi cyclic spray device structural representation.
Among the figure:
The built-in condenser 12-of 1-synthesis reactor 11-phlegma catch tray 13-light-component separating zone 14-double-venturi injector 141-circulation gas import 142-first order jet nozzle 143-secondary nozzle 15-synthesis reactor cylindrical shell 2-temperature-controlled heat exchanger 3-liquid circulating pump 4-medial launder 5-tail condenser 6-condenser
Fig. 1 is applicable to that products of oxo synthesis is the process of light component and the schematic diagram of device. Among Fig. 1 Comprise synthesis reactor, liquid circulation pump and temperature-controlled heat exchanger; The top of synthesis reactor is provided with built-in Condenser, this condenser is the condenser system of this device; The bottom is provided with double-venturi cyclic spray device; The top exit of reactor is communicated with the circulating air import of the double-venturi cyclic spray device of reactor bottom, The top exit of reactor also is communicated with the tail gas blowdown system, and this blowdown system is through artificial setting technique ginseng Automatic control system behind the number is used for discharging reaction end gas according to the ruuning situation of this device. Built-in cold The below of condenser is provided with the condensed fluid collection dish, and catch tray is provided with condensate liquid extraction mouth, and this catch tray is The synthetic product extraction system of this device; The below of catch tray is provided with the light component with structured packing or column plate The Disengagement zone; The synthesis reactor outlet at bottom is communicated with two liquid-circulating pump inlets, a liquid circulation pump Outlet links to each other with temperature-controlled heat exchanger. The liquid circulation pump rear section extraction of flowing through of part still liquid, residue Part behind the temperature-controlled heat exchanger heat-shift, get back to synthesis reactor, another part still liquid is at another liquid Synthesis reactor is got back in still liquid import through double-venturi cyclic spray device under the effect of body circulating pump. Perhaps A still liquid part of coming out from the reactor bottom liquid circulation pump rear section extraction of flowing through, remaining section Synthesis reactor is got back in the still liquid import of lease making double-venturi injector, and another part is handed over through temperature-controlled heat exchanger Get back to synthesis reactor after the heat exchange amount.
According to a certain percentage upper from synthesis reactor with the raw materials such as alkene, alcohol or the amine of liquid phase and catalyst Section adds synthesis reactor, and phase feed CO adds synthesis reactor from the bottom of synthesis reactor, one Under the fixed process conditions, carry out carbongl group synthesis reaction, generate the products of oxo synthesis of light component; Light component Products of oxo synthesis with the light-component separating zone of reaction system mixture steam by reactor top, warp Get the synthetic product mixed liquor after the condenser system condensation, the part in the mixed liquor is cold from the condensed fluid collection dish The extraction of lime set extraction mouth, another part refluxes, and controls reflux ratio by the height of setting the extraction mouth. Not The CO of reaction is by the pressure reduction sucting reaction of the still liquid generation of the first order jet nozzle of the double-venturi cyclic spray device of flowing through Device, and evenly mix with reactor liquid by the effect of double-venturi cyclic spray device secondary nozzle. Reaction Tail gas is discharged from blowdown system after condenser system is condensation and separation of synthetic product, comprise in this tail gas CO, Inert gas etc. System's still liquid is from synthesis reactor bottom output, and a part of still liquid liquid of flowing through follows The rear section extraction of ring pump at this moment, can give catalyst according to ruuning situation and the actual needs of system Recycling; Another part still liquid is got back to synthesis reactor behind the temperature-controlled heat exchanger heat-shift, also have one Part is got back to synthesis reactor through the still liquid import of double-venturi cyclic spray device.
Because synthetic target product difference is divided by boiling point, the boiling point of synthetic product is lower than liquid phase feed , be called the light component synthetic product; Otherwise, the component of attaching most importance to synthetic product. Because synthetic target product Difference, thereby need the liquid phase feed that adds, kind and the ratio of phase feed, and the product of catalyst Kind, model comprise that the technological parameters such as reaction temperature, synthesis pressure are also different, according to target product Actual conditions determine.
Fig. 2 is applicable to that products of oxo synthesis is the another kind of process of light component and the schematic diagram of device. Different from Fig. 1 is, this condenser system comprises tail condenser and condenser, and this synthetic product extraction system comprises Medial launder. The synthesis reactor top exit is communicated with condenser, the gaseous phase outlet of condenser and tail condenser The gas phase import is communicated with; The liquid-phase outlet of the liquid-phase outlet of condenser and tail condenser advances through U-shaped pipe and medial launder Mouth is communicated with, and medial launder is provided with extraction mouth and refluxing opening. After the condenser system condensation, get the synthetic product mixed liquor, Part in the mixed liquor is from the extraction mouth extraction of medial launder, and another part refluxes. Reaction end gas is through condensation System condensing is discharged from blowdown system after isolating synthetic product, comprises CO, inert gas in this tail gas Deng. 1 different is, divides because products of oxo synthesis is restructuring, and synthetic product is with the end of liquid form from reactor Section's extraction is not so arrange the condensed fluid collection dish in the device.
Fig. 4 is applicable to products of oxo synthesis the attach most importance to another kind of process of component and the schematic diagram of device. What Fig. 4 was different from Fig. 2 is divide because products of oxo synthesis is restructuring, synthetic product with liquid form from instead Answer the bottom extraction of device, so in the device medial launder is not set, condensate liquid is through liquid-phase outlet and the tail of condenser The liquid-phase outlet of condenser directly all refluxes through U-shaped pipe.
Fig. 5 is double-venturi cyclic spray device structural representation. Double-venturi cyclic spray device is installed in synthetic The below of reactor shell. Double-venturi cyclic spray device comprises first order jet nozzle and secondary nozzle, the one-level spray Mouth and secondary nozzle are on same axial line.
Embodiment
With the synthetic preparation of methyl alcohol and carbon monoxide methyl-formiate, the boiling point of methyl alcohol is that 64.7 ℃, the boiling point of methyl-formiate are 31.8 ℃, and the boiling point of methyl-formiate is lower than methyl alcohol boiling point, and methyl-formiate belongs to the light constituent product.As building the production equipment that production capacity reaches 10kt/a, the processing condition of building-up reactions are: pressure is 1.5MPa～2.5MPa, reaction zone temperature is 70 ℃～90 ℃, separating the extraction temperature is 85 ℃～110 ℃, as adopt Fig. 1 or device shown in Figure 2 among the present invention, then compare the synthesis system facility investment with conventional apparatus with traditional technology and reduce 20～40%, product content can improve 1～2 times in the production, and catalyst consumption can reduce by 20～70%.
Adopt the synthetic monomethyl methane amide of single stage method with Monomethylamine and carbon monoxide.The processing condition of building-up reactions are: pressure is 1.0MPa～2.5MPa, and reaction zone temperature is 70 ℃～130 ℃.Produce 10kt/a monomethyl methane amide device per year by Fig. 3 among the present invention or construction shown in Figure 4, compare the synthesis system facility investment with conventional apparatus with traditional technology and can reduce 10～40%, the synthesis system energy consumption reduces by 20～30%, and equipment maintenance cost reduces by 30～50%.
Claims (10)
1, a kind of processing method of new oxo process comprises:
(1) liquid phase feed such as alkene, alcohol or amine and catalyzer and phase feed CO are added synthesis reactor according to a certain percentage, under certain process conditions, carry out carbongl group synthesis reaction, generate products of oxo synthesis;
(2) products of oxo synthesis that generates in step (1) is with the light-component separating zone of reactive system mixture steam by reactor top, after the condenser system condensation, get the products of oxo synthesis mixed solution, the extraction from system of a part in the mixed solution, another part refluxes; Unreacted CO gets back to reactor under the effect of double-venturi cyclic spray device, reaction end gas emptying after the condenser system condensation;
(3) the system's still liquid after separating is from the output of synthesis reactor bottom in step (1), and behind the liquid circulation pumping action, a part is got back to reactor through double-venturi cyclic spray device, and a part is got back to reactor after the temperature-controlled heat exchanger heat exchange;
(4) the still liquid of getting back to CO, the products of oxo synthesis mixed solution of reactor and get back to reactor in step (2) in step (3) is proceeded carbongl group synthesis reaction with the raw material that adds in the step (1), generates products of oxo synthesis.
2, processing method according to claim 1, it is characterized in that a part of unreacted CO is inhaled into reactor by the pressure reduction of the still liquid generation of the first order jet nozzle of the double-venturi cyclic spray device of flowing through in step (2), and pass through the effect and the reactor liquid uniform mixing of the secondary nozzle of double-venturi cyclic spray device.
3, processing method according to claim 1 can also be to comprise:
(1) liquid phase feed such as alkene, alcohol or amine and catalyzer and phase feed CO are added synthesis reactor according to a certain percentage, under certain process conditions, carry out carbongl group synthesis reaction, generate products of oxo synthesis;
(2) unreacted CO gets back to reactor under the effect of double-venturi cyclic spray device in step (1), reaction end gas emptying after the condenser system condensation;
(3) the products of oxo synthesis mixed solution that generates in step (1) is from the output of synthesis reactor bottom, a part is by extraction behind the liquid circulation pumping action, a part is got back to reactor through the double-venturi injector, and some gets back to reactor after the temperature-controlled heat exchanger heat exchange in addition;
(4) mixed solution of get back to the CO of reactor in step (2), getting back to reactor in step (3) is proceeded carbongl group synthesis reaction with the raw material that adds in the step (1), generates products of oxo synthesis.
4, processing method according to claim 3, it is characterized in that a part of unreacted CO is inhaled into reactor by the pressure reduction of the mixed solution generation of the first order jet nozzle of the double-venturi cyclic spray device of flowing through in step (2), and pass through the effect and the reactor liquid uniform mixing of the secondary nozzle of double-venturi cyclic spray device.
5, realize the device of claim 1 or 2 described processing methodes, comprise synthesis reactor, liquid circulating pump, temperature-controlled heat exchanger, condenser system and synthetic product extraction system; The bottom that it is characterized in that described synthesis reactor is provided with double-venturi cyclic spray device; Described condenser system is to be located at the built-in condenser at synthesis reactor top, described synthetic product extraction system is the phlegma catch tray of built-in condenser below, the phlegma catch tray is provided with phlegma extraction mouth, the top exit of synthesis reactor is communicated with the circulation gas import of the double-venturi cyclic spray device of reactor bottom, and the top exit of reactor also is communicated with the tail gas blowdown system; Perhaps described condenser system comprises external condenser and tail condenser, the synthesis reactor top exit is communicated with condenser, the gaseous phase outlet of condenser is communicated with the gas phase import of tail condenser, the gaseous phase outlet of condenser is communicated with the circulation gas import of the double-venturi cyclic spray device of synthesis reactor bottom, the gaseous phase outlet of tail condenser is communicated with the tail gas blowdown system, the liquid phase outlet of condenser and the liquid phase outlet of tail condenser are communicated with, described synthetic product extraction system is a medial launder, described medial launder is communicated with the liquid phase outlet of tail condenser and condenser, medial launder is provided with extraction mouth and refluxing opening, and the refluxing opening of medial launder is communicated with synthesis reactor; The top of synthesis reactor is provided with light-component separating zone; The synthesis reactor outlet at bottom is communicated with liquid circulating pump, and in the described liquid circulating pump one is communicated with temperature-controlled heat exchanger, and temperature-controlled heat exchanger is communicated with synthesis reactor; In the described liquid circulating pump another is communicated with the import of the double-venturi cyclic spray device of synthesis reactor bottom.
6, device according to claim 5 is characterized in that described double-venturi cyclic spray device comprises first order jet nozzle and secondary nozzle, and first order jet nozzle and secondary nozzle are on same axial line.
7,, it is characterized in that being provided with structured packing or column plate in the light-component separating zone of described synthesis reactor according to claim 5 or 6 described devices.
8, realize the device of claim 3 or 4 described processing methodes, comprise synthesis reactor, liquid circulating pump, temperature-controlled heat exchanger and condenser system; The bottom that it is characterized in that described synthesis reactor is provided with double-venturi cyclic spray device; Described condenser system is to be located at the built-in condenser at synthesis reactor top, and the top exit of synthesis reactor is communicated with the circulation gas import of the double-venturi cyclic spray device of reactor bottom, and the top exit of reactor also is communicated with the tail gas blowdown system; Perhaps described condenser system comprises external condenser and tail condenser, the synthesis reactor top exit is communicated with condenser, the gaseous phase outlet of condenser is communicated with the gas phase import of tail condenser, the gaseous phase outlet of condenser is communicated with the circulation gas import of the double-venturi injector of synthesis reactor bottom, the gaseous phase outlet of tail condenser is communicated with the tail gas blowdown system, the liquid phase outlet of condenser and the liquid phase outlet of tail condenser are communicated with, and are communicated with synthesis reactor; The top of synthesis reactor is provided with light-component separating zone; The synthesis reactor outlet at bottom is communicated with liquid circulating pump, and in the described liquid circulating pump one is communicated with temperature-controlled heat exchanger, and temperature-controlled heat exchanger is communicated with synthesis reactor; In the described liquid circulating pump another is communicated with the import of the double-venturi cyclic spray device of synthesis reactor bottom.
9, device according to claim 8 is characterized in that described double-venturi cyclic spray device comprises first order jet nozzle and secondary nozzle, and first order jet nozzle and secondary nozzle are on same axial line.
10, according to Claim 8 or 9 described devices, it is characterized in that being provided with structured packing or column plate in the light-component separating zone of described synthesis reactor.
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| CN 200710069429 CN101074194A (en) | 2007-06-25 | 2007-06-25 | Carboxide synthesis and synthesizer |
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| CN 200710069429 CN101074194A (en) | 2007-06-25 | 2007-06-25 | Carboxide synthesis and synthesizer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951558A (en) * | 2014-04-10 | 2014-07-30 | 中国科学院福建物质结构研究所 | Device for producing methyl formate by gas phase methanol carbonylation, process and catalyst on-line evaluation method |
| CN110975770A (en) * | 2019-12-23 | 2020-04-10 | 中冶焦耐(大连)工程技术有限公司 | Decomposition process and device of phenate in coal tar processing process |
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2007
- 2007-06-25 CN CN 200710069429 patent/CN101074194A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951558A (en) * | 2014-04-10 | 2014-07-30 | 中国科学院福建物质结构研究所 | Device for producing methyl formate by gas phase methanol carbonylation, process and catalyst on-line evaluation method |
| CN110975770A (en) * | 2019-12-23 | 2020-04-10 | 中冶焦耐(大连)工程技术有限公司 | Decomposition process and device of phenate in coal tar processing process |
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