CN203700237U - Reaction system for synthesizing isobutyl isobutyrate through isobutanol - Google Patents
Reaction system for synthesizing isobutyl isobutyrate through isobutanol Download PDFInfo
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- CN203700237U CN203700237U CN201420032118.8U CN201420032118U CN203700237U CN 203700237 U CN203700237 U CN 203700237U CN 201420032118 U CN201420032118 U CN 201420032118U CN 203700237 U CN203700237 U CN 203700237U
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Abstract
The utility model discloses a reaction system for synthesizing isobutyl isobutyrate through isobutanol. The reaction system comprises a primary reaction system and a secondary reaction system, wherein the primary reaction system comprises a primary feed pump, a primary heat exchanger, a primary preheater, a primary fixed bed reactor, a gas-liquid separator, a primary cooler and a primary coarse product tank, wherein the primary heat exchanger is connected with the feed pipe of the primary feed pump; the primary preheater is connected with the feed pipe of the primary heat exchanger; the primary fixed bed reactor is connected with one pipe of the primary preheater; the discharge pipe of the primary fixed bed reactor is connected with the primary heat exchanger; the discharge pipe of the primary heat exchanger is connected with the gas-liquid separator; a liquid outlet pipe at the bottom of the gas-liquid separator is connected with the primary cooler; the primary cooler is connected with the primary coarse product tank. The secondary reaction system comprises a secondary heat exchanger, a secondary preheater, a secondary fixed bed reactor, a secondary cooler and a secondary coarse product tank, wherein the secondary heat exchanger is connected with an air outlet pipe at the top end of the gas-liquid separator; the secondary preheater is connected with the feed pipe of the secondary heat exchanger; the secondary fixed bed reactor is connected with a pipe of the secondary preheater; the discharge pipe of the secondary fixed bed reactor is connected with the secondary heat exchanger; the discharge pipe of the secondary heat exchanger is connected with the secondary cooler; the secondary cooler is connected with the secondary coarse product tank. The reaction system has the benefits that the yield of isobutyl isobutyrate is higher, and the amount of isobutyraldehyde as a by-product is very small.
Description
Technical field
The utility model belongs to fine chemical product production technical field, refers in particular to a kind of two-stage reaction system and method thereof for the synthetic isobutyl isobutyrate of isopropylcarbinol.
Background technology
Isobutyl isobutyrate is a kind of fine chemicals of safety and environmental protection, and its most general synthetic method is the esterification process take isopropylformic acid and isopropylcarbinol as raw material, also has in addition the condensation method take isobutyric aldehyde as raw material, and discrimination method take isopropylcarbinol as raw material.Patent CN101711983 discloses a kind of catalyzer for the synthetic isobutyl isobutyrate of isopropylcarbinol disproportionation, but this catalyst activity is not high, and generally making isobutyl isobutyrate yield is 70-80%, and generates approximately 2% isobutyric aldehyde by product.
Summary of the invention
The utility model, just in order to overcome the deficiency of above-mentioned catalyst for synthesizing, provides a kind of and makes isobutyl isobutyrate yield higher for two-stage reaction system and method thereof by the synthetic isobutyl isobutyrate of isopropylcarbinol, and isobutyric aldehyde by product is little.
In order to solve above-mentioned technical problem, the technical scheme the utility model proposes is: a kind of reactive system for the synthetic isobutyl isobutyrate of isopropylcarbinol, it is characterized in that comprising one section of reactive system and second-stage reaction system, described one section of reactive system comprises a section feeding pump, the one section of interchanger being connected with a section feeding pump feed pipe, the one section of preheater being connected with one section of interchanger feed pipe, the one section of fixed-bed reactor being connected with one section of preheater pipeline, gas-liquid separator, one section of water cooler and one section of thick products pot, described one section of fixed-bed reactor discharge pipe connects one section of interchanger, described one section of interchanger discharge pipe connects gas-liquid separator, gas-liquid separator bottom liquid outlet pipeline connects one section of water cooler, one section of water cooler connects one section of thick products pot, described second-stage reaction system comprises two sections of interchanger that are connected with air outlet, gas-liquid separator top pipeline, two sections of preheaters that are connected with two sections of interchanger feed pipes, the two sections of fixed-bed reactor, two-step cooling device and the two sections of thick products pots that are connected with two sections of preheater pipelines, described two sections of fixed-bed reactor discharge pipes connect two sections of interchanger, two sections of interchanger discharge pipes connect two-step cooling device, and two-step cooling device connects two sections of thick products pots.Described one section, two sections interchanger are double-pipe exchanger.
A kind of reaction method of the reactive system for the synthetic isobutyl isobutyrate of isopropylcarbinol, it is characterized in that comprising the following steps: first raw material one section feeding pump is pumped into one section of interchanger and carry out heat exchange with the discharging of reacting of one section of fixed-bed reactor, then the raw material after heat exchange is entered to one section of preheater and carry out preheating, then enter one section of fixed-bed reactor and carry out one section of catalyzed reaction, after one section of catalyzed reaction from one section of fixed-bed reactor discharge pipe material out through one section of interchanger and raw material heat exchange rear section condensation, enter gas-liquid separator and carry out gas-liquid separation, isolated liquid reactant enters one section of water cooler and carries out cooling, finally enter one section of thick products pot and obtain one section of thick product, heat exchange is carried out in the discharging that gaseous reactant enters after two sections of interchanger and two sections of fixed-bed reactor catalyzed reactions, then enter two sections of preheaters and carry out preheating, then enter two sections of fixed-bed reactor and carry out catalyzed reaction, discharging after catalyzed reaction due to the heat exchange condensation of gaseous reactant, enter again two-step cooling device and carry out condensation, finally enter two sections of thick products pots and obtain two sections of thick products.
As another key problem in technology of the utility model, the catalyzer of described one section, two sections catalyzed reaction is solid composite oxide catalysts.In one section of catalyzed reaction oxide compound, each component is made up of 5wt% neodymium, 15wt% zinc, 80wt% zirconium load 0.1wt% palladium in metal content.In two sections of catalyzed reaction oxide compounds, each component is made up of 5wt% neodymium, 15wt% copper, 20wt% zinc, 60%wt% aluminium load 0.1wt% palladium in metal content.
As preferably, one section of reaction raw materials temperature after heat exchange, preheating is 280 ℃, and the temperature of reaction of one section of fixed-bed reactor is 280 ℃, and the drop temperature after one section of catalyzed reaction is 280 ℃, and the temperature of discharging after one section of heat exchange is 135 ℃; The temperature of second-stage reaction raw material after heat exchange, preheating is 320 ℃, and the temperature of reaction of two sections of fixed-bed reactor is 320 ℃, and the drop temperature of two sections of catalyzed reactions is 320 ℃, and the temperature after two sections of heat exchange is 159 ℃.
The beneficial effects of the utility model: in this production system, one section of a small amount of isobutyric aldehyde that catalyzed reaction generates, in two sections of catalytic reaction processes, react, part is finally converted into target product isobutyl isobutyrate, reacts like this by two-stage catalytic, makes isopropylcarbinol feed stock conversion high, isobutyl isobutyrate selectivity is higher, and isobutyric aldehyde by product is less.Greatly improve reaction efficiency, improved finished product production rate.
Accompanying drawing explanation
Fig. 1 is system schematic of the present utility model.
Embodiment
As shown in Figure 1, a kind of reactive system for the synthetic isobutyl isobutyrate of isopropylcarbinol, comprise one section of reactive system and second-stage reaction system, described one section of reactive system comprises a section feeding pump 1, the one section of interchanger 2 being connected with section feeding pump 1 feed pipe, the one section of preheater 3 being connected with one section of interchanger 2 feed pipe, the one section of fixed-bed reactor 4 being connected with one section of preheater 3 pipeline, gas-liquid separator 5, one section of water cooler 6 and one section of thick products pot 7, described one section of fixed-bed reactor, 4 discharge pipes connect one section of interchanger 2, described one section of interchanger, 2 discharge pipes connect gas-liquid separator 5, gas-liquid separator 5 bottom liquid outlet pipelines connect one section of water cooler 6, one section of water cooler 6 connects one section of thick products pot 7, described second-stage reaction system comprises two sections of interchanger 8 that are connected with gas-liquid separator 5 air outlet, top pipelines, two sections of preheaters 9 that are connected with two sections of interchanger 8 feed pipes, the two sections of fixed-bed reactor 10, two-step cooling device 11 and the two sections of thick products pots 12 that are connected with two sections of preheater 9 pipelines, described two sections of fixed-bed reactor, 10 discharge pipes connect two sections of interchanger 8, two sections of interchanger 8 discharge pipes connect two-step cooling device 11, and two-step cooling device 11 connects two sections of thick products pots 12.Described one section, two sections interchanger (2,8) are double-pipe exchanger.
A kind of reaction method of the reactive system for the synthetic isobutyl isobutyrate of isopropylcarbinol, comprise the following steps: first raw material one section feeding pump 1 is pumped into one section of interchanger 2 and carry out heat exchange with the discharging of reacting of one section of fixed-bed reactor 4, then the raw material after heat exchange is entered to one section of preheater 3 and carry out preheating, then enter one section of fixed-bed reactor 4 and carry out one section of catalyzed reaction, after one section of catalyzed reaction from one section of fixed-bed reactor 4 discharge pipe material out through one section of interchanger 2 and raw material heat exchange rear section condensation, enter gas-liquid separator 5 and carry out gas-liquid separation, isolated liquid reactant enters one end water cooler 6 and carries out cooling, finally enter one section of thick products pot 7 and obtain one section of thick product, heat exchange is carried out in the discharging that gaseous reactant enters after two sections of interchanger 8 and two sections of fixed-bed reactor 10 catalyzed reactions, then enter two sections of preheaters 9 and carry out preheating, then enter two sections of fixed-bed reactor 10 and carry out catalyzed reaction, discharging after catalyzed reaction due to the heat exchange condensation of gaseous reactant, enter again two-step cooling device 11 and carry out condensation, finally enter two sections of thick products pots 12 and obtain two sections of thick products.
The catalyzer of one section of reaction is by 5wt% neodymium, 15wt% zinc, 80wt% zirconium load 0.1wt% palladium composition, loaded catalyst is 600kg, isopropylcarbinol inlet amount is 300kg/h, material temperature is 20 ℃, one section of reaction raw materials temperature after heat exchange is 109 ℃, temperature after preheating is 280 ℃, the temperature of reaction at one section of fixed-bed reactor middle part is 280 ℃, reactor upper pressure is 0.012 MPa, the drop temperature of one section of reaction is 280 ℃, discharging consists of: isobutyl isobutyrate 77.02%, isopropylcarbinol 20.52%, isobutyric aldehyde 2.07%, other impurity 0.39%, temperature after heat exchange partial condensation is 135 ℃, wherein liquid isobutyl isobutyrate crude product flow is 237kg/h, consist of: isobutyl isobutyrate 97.04%, isopropylcarbinol 2.62%, isobutyric aldehyde 0.02%, other impurity 0.32%, be cooled to 40 ℃ of left and right by water cooler again, enter thick products pot, the mass flow-rates such as the unreacted isopropylcarbinol of gaseous state are 63kg/h, consist of: isobutyl isobutyrate 1.7%, isopropylcarbinol 87.91%, isobutyric aldehyde 9.78%, other impurity 0.61%.
The catalyzer of second-stage reaction is by 15wt% copper, 20wt% zinc, 60%wt% aluminium, 5wt% neodymium load 0.1wt% palladium composition, loaded catalyst is 150kg, the material inlet amounies such as the unreacted isopropylcarbinol of gaseous state are 63kg/h, the temperature of second-stage reaction raw material after heat exchange is 154 ℃, temperature after preheating is 320 ℃, the temperature of reaction at two sections of fixed-bed reactor middle parts is 320 ℃, reactor upper pressure is 0.005 MPa, the drop temperature of second-stage reaction is 320 ℃, discharging consists of: isobutyl isobutyrate 77.85%, isopropylcarbinol 18.68%, isobutyric aldehyde 2.52%, other impurity 0.95%, it is 159 ℃ through the cooled temperature of heat exchange, be cooled to 40 ℃ of left and right by water cooler again, enter thick products pot.
Table 1 reaction result
Claims (2)
1. the reactive system for the synthetic isobutyl isobutyrate of isopropylcarbinol, it is characterized in that comprising one section of reactive system and second-stage reaction system, described one section of reactive system comprises a section feeding pump, the one section of interchanger being connected with a section feeding pump feed pipe, the one section of preheater being connected with one section of interchanger feed pipe, the one section of fixed-bed reactor being connected with one section of preheater pipeline, gas-liquid separator, one section of water cooler and one section of thick products pot, described one section of fixed-bed reactor discharge pipe connects one section of interchanger, described one section of interchanger discharge pipe connects gas-liquid separator, gas-liquid separator bottom liquid outlet pipeline connects one section of water cooler, one section of water cooler connects one section of thick products pot, described second-stage reaction system comprises two sections of interchanger that are connected with air outlet, gas-liquid separator top pipeline, two sections of preheaters that are connected with two sections of interchanger feed pipes, the two sections of fixed-bed reactor, two-step cooling device and the two sections of thick products pots that are connected with two sections of preheater pipelines, described two sections of fixed-bed reactor discharge pipes connect two sections of interchanger, two sections of interchanger discharge pipes connect two-step cooling device, and two-step cooling device connects two sections of thick products pots.
2. a kind of reactive system for the synthetic isobutyl isobutyrate of isopropylcarbinol according to claim 1, is characterized in that described one section, two sections interchanger are double-pipe exchanger.
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| CN201420032118.8U CN203700237U (en) | 2014-01-20 | 2014-01-20 | Reaction system for synthesizing isobutyl isobutyrate through isobutanol |
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| CN201420032118.8U CN203700237U (en) | 2014-01-20 | 2014-01-20 | Reaction system for synthesizing isobutyl isobutyrate through isobutanol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103848737A (en) * | 2014-01-20 | 2014-06-11 | 宜兴市恒兴精细化工有限公司 | Reaction system and method for synthesizing isobutyl isobutyrate by utilizing isobutanol |
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2014
- 2014-01-20 CN CN201420032118.8U patent/CN203700237U/en not_active Withdrawn - After Issue
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103848737A (en) * | 2014-01-20 | 2014-06-11 | 宜兴市恒兴精细化工有限公司 | Reaction system and method for synthesizing isobutyl isobutyrate by utilizing isobutanol |
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| C14 | Grant of patent or utility model | ||
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Granted publication date: 20140709 Effective date of abandoning: 20150916 |
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