CN118594018A - System and method for preparing isononanoic acid by taking isononanal as raw material - Google Patents
System and method for preparing isononanoic acid by taking isononanal as raw material Download PDFInfo
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- CN118594018A CN118594018A CN202410592830.1A CN202410592830A CN118594018A CN 118594018 A CN118594018 A CN 118594018A CN 202410592830 A CN202410592830 A CN 202410592830A CN 118594018 A CN118594018 A CN 118594018A
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- XZOYHFBNQHPJRQ-UHFFFAOYSA-N 7-methyloctanoic acid Chemical compound CC(C)CCCCCC(O)=O XZOYHFBNQHPJRQ-UHFFFAOYSA-N 0.000 title claims abstract description 67
- JRPPVSMCCSLJPL-UHFFFAOYSA-N 7-methyloctanal Chemical compound CC(C)CCCCCC=O JRPPVSMCCSLJPL-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002994 raw material Substances 0.000 title claims abstract description 23
- 238000000926 separation method Methods 0.000 claims abstract description 38
- 238000001179 sorption measurement Methods 0.000 claims abstract description 34
- 238000007254 oxidation reaction Methods 0.000 claims description 69
- 239000000376 reactant Substances 0.000 claims description 63
- 238000007670 refining Methods 0.000 claims description 27
- 239000012535 impurity Substances 0.000 claims description 25
- 230000003647 oxidation Effects 0.000 claims description 21
- 239000003054 catalyst Substances 0.000 claims description 17
- 230000007704 transition Effects 0.000 claims description 14
- 239000000945 filler Substances 0.000 claims description 6
- 239000002638 heterogeneous catalyst Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229910052723 transition metal Inorganic materials 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011973 solid acid Substances 0.000 claims description 3
- 239000004927 clay Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 150000003624 transition metals Chemical group 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 13
- 238000000746 purification Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 description 18
- 239000000047 product Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 12
- 230000008569 process Effects 0.000 description 5
- 150000001299 aldehydes Chemical class 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- WTPYRCJDOZVZON-UHFFFAOYSA-N 3,5,5-Trimethylhexanal Chemical compound O=CCC(C)CC(C)(C)C WTPYRCJDOZVZON-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- -1 transition metal salts Chemical class 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a system and a method for preparing isononanoic acid by taking isononanal as a raw material, belonging to the field of chemical industry, the selectivity of isononanoic acid is preferably improved, and the isononanoic acid prepared based on tandem double rectification separation treatment and adsorption treatment has high purity without further purification treatment.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a system and a method for preparing isononanoic acid by taking isononanal as a raw material.
Background
Isononanoic acid is an important organic chemical raw material which has excellent wettability, permeability and emulsifying property, and is therefore widely used in the fields of lubricants, industrial detergents, cosmetics, medicines and the like. The isononanoic acid is prepared by directly oxidizing isononanal as a raw material, and the technology has the advantages of simple technological route, mild technological conditions, single raw material variety and the like.
The isononanoic acid preparation process by isononanal oxidation mainly uses transition metal salts such as manganese, cobalt, copper and the like as homogeneous catalysts, and the catalysts have the advantages of mild reaction conditions, high catalytic efficiency and the like; however, the catalyst also has the problems of high recycling difficulty and the like. Meanwhile, the process for preparing isononanoic acid by oxidizing isononanal has other problems, such as (1) isononanoic acid selectivity is not high, because the process has serious exothermic reaction, and the reaction is difficult to control along with the rapid progress of exothermic oxidation reaction, so that isononanoic acid selectivity is reduced; (2) The process has more byproducts, needs to further purify semi-finished products, and has high production cost.
Based on the technical problems, the process for preparing isononanoic acid by oxidizing isononanal is still difficult to realize industrialization on a large scale at present.
Disclosure of Invention
Based on the defects existing in the prior art, the invention aims to provide a system and a method for preparing isononanoic acid by taking isononanal as a raw material, the selectivity of isononanoic acid is preferably improved through the design of a sectional oxidation process, and meanwhile, the purity of the isononanoic acid obtained by preparation is high based on tandem double rectification separation treatment and adsorption treatment without further purification treatment.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the system for preparing isononanoic acid by taking isononanal as a raw material still comprises a serial oxidation reaction kettle, a filter, a serial double rectifying tower and an adsorption tower;
The series oxidation reaction kettles are two oxidation reaction kettles A1 and A2 which are arranged in series, and a transition radiator is arranged between the two oxidation reaction kettles;
the series double rectifying towers are a light component removing tower and a refining tower which are arranged in series;
The number of the tower plates of the light component removal tower is 8-18;
The number of the tower plates of the refining tower is 25-45;
and an adsorption filler is arranged in the adsorption tower.
Another object of the present invention is to provide a method for preparing isononanoic acid from isononanal as a raw material, comprising the steps of:
(1) Preheating isononanal, then sending the isononanal into the system of the invention, and carrying out a first-stage oxidation reaction at 40-60 ℃ in the oxidation reaction kettle A1 to obtain a reactant I;
(2) Delivering the reactant I into a transition radiator for cooling, and then delivering the reactant I into an oxidation reaction kettle A2 for performing two-stage oxidation treatment at 40-60 ℃ to obtain a reactant II; heterogeneous catalysts are arranged in the primary oxidation treatment and the secondary oxidation treatment;
(3) Delivering the reactant II into a filter for catalyst separation treatment to obtain a reactant III;
(4) Delivering the reactant III into a light component removal tower for first-stage impurity separation treatment, and then delivering the reactant III into a refining tower for second-stage impurity separation treatment to obtain a reactant IV;
(5) And (3) sending the reactant IV into an adsorption tower for adsorption and impurity removal treatment to obtain isononanoic acid.
The conventional isononanoic acid preparation process by isononanoic aldehyde oxidation has the defects of low recovery repetition rate of materials (particularly oxidation catalysts) and low isononanoic acid yield and low purity, so in the system and scheme of the invention, improvement is carried out on a traditional isononanoic acid preparation reaction kettle by isononanoic aldehyde oxidation reaction, a serial reaction kettle is arranged, meanwhile, a transition radiator is arranged between the two reaction kettles, isononanoic aldehyde is preheated and then enters a first reaction kettle in advance to carry out a first-stage reaction, then the transition radiator is adopted to carry out heat dissipation, and then the second-stage reaction is carried out in the other reaction kettle, so that the heat dissipation effect of the oxidation flow of the whole isononanoic acid is higher through sectional oxidation design, the yield of isononanoic acid is more facilitated to be improved, and the transition radiator can also be used for the preheating treatment of the isononanoic acid in the earlier stage based on the simplified design of a system line. After the crude isononanoic acid is generated, the heterogeneous catalyst is recovered by the filter, so that the utilization rate of the catalyst is effectively improved.
After the catalyst is recovered, the product is treated by a series-connected rectification double tower, the light component of the light component removing tower is separated, the heavy component of the light component removing tower is separated by a refining tower, and finally, the residual impurities are subjected to final adsorption separation by an adsorption tower, so that the purifying effect is higher compared with that of the traditional separation process. However, the number of trays in the two rectifying columns must be strictly limited, and if the number of trays is too large, the production energy consumption increases, but if the number of trays in any one of the rectifying columns is insufficient, the desired purification effect cannot be achieved.
Preferably, the pressure at the time of the primary oxidation reaction and the secondary oxidation reaction is 0.1 to 2MPa.
More preferably, the pressure at the time of the primary oxidation reaction and the secondary oxidation reaction is 0.4 to 0.8MPa.
The oxidation reaction of isononyl aldehyde under the pressure can be effectively controlled within a proper rate, and the condition that the reaction degree is difficult to control due to excessive heat generation is avoided.
Preferably, the heterogeneous catalyst is a transition metal element supported solid acid catalyst.
More preferably, the transition metal element is at least one of Fe, mn, co, cr.
Preferably, the filter is at least one of a bag filter, a basket filter, a plate filter, and a tube filter.
Preferably, the top temperature of the light component removal tower is 45-95 ℃ and the top pressure is 1-45 kPa.
More preferably, the separated substances are taken out from the top of the light ends column when the reactant II is fed into the light ends column.
In the light component separation in the specific tray number of the light component removal column of the present invention, the light component in the reactant II can be efficiently separated from the main body, and when the column top temperature and pressure are set within the above-mentioned preferred ranges, such light component impurities can be efficiently withdrawn from the column top.
Preferably, the temperature of the top of the refining tower is 110-180 ℃, and the pressure of the top of the refining tower is 1-45 kPa.
More preferably, the reactant IV is withdrawn from the top of the refining column.
Unlike the light fraction, since the heavy fraction has a larger molecular weight than isononanoic acid in the main body, it is more likely to accumulate at the bottom upon separation, and thus it is required to collect the separated target fraction at the top of the column as opposed to the light-removal column, whereas when the above-mentioned specific column top temperature and pressure setting are selected, the isononanoic acid content of the produced product is higher.
Preferably, the adsorption filler in the adsorption tower is at least one of clay, diatomite, molecular sieve and activated carbon fiber.
The invention has the beneficial effects that the invention provides the system and the method for preparing isononanoic acid by taking isononanal as the raw material, the selectivity of isononanoic acid is preferably improved (more than 95 percent) through the design of a sectional oxidation process, and meanwhile, the isononanoic acid prepared by series double rectification separation treatment and adsorption treatment has high purity (more than 99 percent) without further purification treatment.
Drawings
FIG. 1 is a schematic structural diagram of the isononanoic acid refining system described herein, comprising a serial oxidation reactor, a filter C, a serial double rectifying tower and an adsorption tower E, which are connected in sequence; the series oxidation reaction kettles are two oxidation reaction kettles A1 and A2 which are arranged in series, and a transition radiator B is arranged between the two oxidation reaction kettles; the tandem double rectifying towers are a light component removing tower D1 and a refining tower D2 which are arranged in series.
Detailed Description
The present invention will be further described with reference to specific examples and comparative examples for better illustrating the objects, technical solutions and advantages of the present invention, and the object of the present invention is to be understood in detail, not to limit the present invention. All other embodiments, which can be made by those skilled in the art without the inventive effort, are intended to be within the scope of the present invention. The experimental reagents and instruments involved in the practice of the present invention are common reagents and instruments unless otherwise specified. The isononanal used in each example and comparative example had the same mass, and was subjected to a preheating treatment using a transition radiator B at the time of preheating.
Example 1
The invention relates to an embodiment of a system and a method for preparing isononanoic acid by taking isononanal as a raw material, wherein the system is shown in figure 1, and comprises an isononanal oxidation unit and an isononanal refining unit, and specifically comprises a serial oxidation reaction kettle, a filter C, a serial double rectifying tower and an adsorption tower E which are sequentially connected; the series oxidation reaction kettles are two oxidation reaction kettles A1 and A2 which are arranged in series, a transition radiator B is arranged between the two oxidation reaction kettles, heterogeneous catalysts are arranged in the oxidation reaction kettles A1 and A2, the catalysts are solid acid catalysts loaded with Mn element, and the catalyst consumption is 1% of isononanal; the filter C is a bag filter; the series double rectifying towers are a light component removing tower D1 and a refining tower D2 which are arranged in series; in the adsorption tower E, all the filler is carclazyte.
The method for preparing isononanoic acid by taking isononanal as a raw material comprises the following steps:
(1) Preheating isononanal to 45 ℃, then feeding the isononanal into the system described in the embodiment, and setting 50 ℃ (the fluctuation range is 48-52 ℃) in the oxidation reaction kettle A1, and carrying out a first-stage oxidation reaction for 2 hours under 0.5MPa to obtain a reactant I;
(2) The reactant I is sent into a transition radiator B to be cooled to 50 ℃, then is sent into an oxidation reaction kettle A2 to be set to 50 ℃ (the fluctuation range is within 1 ℃), and is subjected to two-stage oxidation treatment for 2 hours under the pressure of 0.5MPa, so that a reactant II is obtained;
(3) Delivering the reactant II into a filter C for catalyst separation treatment to obtain a reactant III;
(4) Delivering the reactant III into a light component removal tower D1 for first-stage impurity separation treatment, extracting a product from a tower kettle, extracting a separation substance from the tower top, delivering the product into a refining tower D2 for second-stage impurity separation treatment to obtain a reactant IV, extracting the reactant IV from the tower top, and extracting the separation substance from the tower kettle; the tray number of the light component removal column D1 is 12, the column top temperature is 60 ℃, and the column top pressure is 5kPa; the tower plate number of the refining tower D2 is 30, the tower top temperature is 140 ℃, and the tower top pressure is 3kPa;
(5) And (3) sending the reactant IV into an adsorption tower E for adsorption and impurity removal treatment to obtain isononanoic acid.
Example 2
In one embodiment of the method and system for refining isononanoic acid, the system for refining isononanoic acid is the same as that in embodiment 1, but a plate filter is selected as the filter C, and all the fillers in the adsorption tower E are diatomite.
The method for preparing isononanoic acid by taking isononanal as a raw material comprises the following steps:
(1) Preheating isononanal to 45 ℃, then feeding the isononanal into the system described in the embodiment, and setting 50 ℃ (the fluctuation range value is 48-52 ℃) in the oxidation reaction kettle A1, and carrying out primary oxidation reaction for 2 hours under 0.6MPa to obtain a reactant I;
(2) The reactant I is sent into a transition radiator B to be cooled to 50 ℃, then is sent into an oxidation reaction kettle A2 to be set to 50 ℃ (the fluctuation range is within 1 ℃), and is subjected to two-stage oxidation treatment for 2 hours under the pressure of 0.6MPa, so that a reactant II is obtained;
(3) Delivering the reactant II into a filter C for catalyst separation treatment to obtain a reactant III;
(4) Delivering the reactant III into a light component removal tower D1 for first-stage impurity separation treatment, extracting a product from a tower kettle, extracting a separation substance from the tower top, delivering the product into a refining tower D2 for second-stage impurity separation treatment to obtain a reactant IV, extracting the reactant IV from the tower top, and extracting the separation substance from the tower kettle; the tray number of the light component removal column D1 is 15, the column top temperature is 60 ℃, and the column top pressure is 4kPa; the tower plate number of the refining tower D2 is 30, the tower top temperature is 140 ℃, and the tower top pressure is 3kPa;
(5) And (3) sending the reactant IV into an adsorption tower E for adsorption and impurity removal treatment to obtain isononanoic acid.
Comparative example 1
A system and a method for preparing isononanoic acid by taking isononanal as a raw material, wherein the system comprises an oxidation reaction kettle A, a filter C, a serial double rectifying tower and an adsorption tower E which are connected in sequence; the series double rectifying towers are a light component removing tower D1 and a refining tower D2 which are arranged in series; the arrangement of the corresponding parts of the system described in example 1 is the rest.
The method for preparing isononanoic acid by taking isononanal as a raw material comprises the following steps:
(1) Preheating isononanal to 45 ℃, then feeding the isononanal into the system, and setting 50 ℃ (the fluctuation range is 46-54 ℃) in the oxidation reaction kettle A, and carrying out oxidation reaction for 4 hours under 0.5MPa to obtain a reactant I;
(2) Sending the reactant I into a filter C for catalyst separation treatment to obtain a reactant II;
(3) Delivering the reactant II into a light component removal tower D1 for first-stage impurity separation treatment, extracting a product from a tower kettle, extracting a separation substance from the tower top, delivering the product into a refining tower D2 for second-stage impurity separation treatment to obtain a reactant III, extracting the reactant III from the tower top, and extracting the separation substance from the tower kettle; the tray number of the light component removal column D1 is 12, the column top temperature is 60 ℃, and the column top pressure is 5kPa; the tower plate number of the refining tower D2 is 30, the tower top temperature is 140 ℃, and the tower top pressure is 3kPa;
(4) And (3) sending the reactant III into an adsorption tower E for adsorption and impurity removal treatment to obtain isononanoic acid.
Comparative example 2
A system and a method for preparing isononanoic acid by taking isononanal as a raw material, wherein the system comprises a serial oxidation reaction kettle, a filter C and a serial double rectifying tower which are sequentially connected; the arrangement of the corresponding parts of the system described in example 1 is the same except for the specific explanation.
The method for preparing isononanoic acid by taking isononanal as a raw material comprises the following steps:
(1) Preheating isononanal to 45 ℃, then feeding the isononanal into the system described in the embodiment, and setting 50 ℃ (the fluctuation range is 48-52 ℃) in the oxidation reaction kettle A1, and carrying out a first-stage oxidation reaction for 2 hours under 0.5MPa to obtain a reactant I;
(2) The reactant I is sent into a transition radiator B to be cooled to 50 ℃, then is sent into an oxidation reaction kettle A2 to be set to 50 ℃ (the fluctuation range is within 1 ℃), and is subjected to two-stage oxidation treatment for 2 hours under the pressure of 0.5MPa, so that a reactant II is obtained;
(3) Delivering the reactant II into a filter C for catalyst separation treatment to obtain a reactant III;
(4) Delivering the reactant III into a light component removal tower D1 for first-stage impurity separation treatment, obtaining a product from a tower kettle, extracting a separation substance from the tower top, delivering the product into a refining tower D2 for second-stage impurity separation treatment to obtain isononanoic acid, obtaining isononanoic acid from the tower top, and extracting the separation substance from the tower kettle; the tray number of the light component removal column D1 is 12, the column top temperature is 60 ℃, and the column top pressure is 5kPa; the number of plates of the refining column D2 was 30, the column top temperature was 140℃and the column top pressure was 3kPa.
Comparative example 3
A system and a method for preparing isononanoic acid by taking isononanal as a raw material, wherein the system comprises a serial oxidation reaction kettle, a filter C, a single rectifying tower D and an adsorption tower E which are sequentially connected; the arrangement of the corresponding parts of the system described in example 1 is the same except for the specific explanation.
The method for preparing isononanoic acid by taking isononanal as a raw material comprises the following steps:
(1) Preheating isononanal to 45 ℃, then feeding the isononanal into the system described in the embodiment, and setting 50 ℃ (the fluctuation range is 48-52 ℃) in the oxidation reaction kettle A1, and carrying out a first-stage oxidation reaction for 2 hours under 0.5MPa to obtain a reactant I;
(2) The reactant I is sent into a transition radiator B to be cooled to 50 ℃, then is sent into an oxidation reaction kettle A2 to be set to 50 ℃ (the fluctuation range is within 1 ℃), and is subjected to two-stage oxidation treatment for 2 hours under the pressure of 0.5MPa, so that a reactant II is obtained;
(3) Delivering the reactant II into a filter C for catalyst separation treatment to obtain a reactant III;
(4) Feeding the reactant III into a single rectifying tower D for intermittent light-weight and impurity removal treatment, firstly carrying out light-weight and impurity removal separation treatment, extracting light component separation substances from the tower top, then carrying out heavy-weight and impurity removal separation treatment to obtain a reactant IV, extracting the reactant IV from the tower top, and extracting heavy component separation substances from the tower bottom; the tray number of the single rectifying tower is 32, the temperature of the tower top is 61 ℃ in the light component removing stage, and the temperature of the tower top is 142 ℃ in the heavy component removing stage.
(5) And (3) sending the reactant IV into an adsorption tower E for adsorption and impurity removal treatment to obtain isononanoic acid.
Comparative example 4
A method and a system for refining isononanoic acid differ from example 1 only in that the tray number of the light ends removal column D1 is 5.
Comparative example 5
A method and a system for purifying isononanoic acid were different from example 1 only in that the number of trays of the purifying column D2 was 20.
The purity of isononanoic acid refined in each example and comparative example is detected by gas chromatography, and the conversion rate of isononanoic aldehyde and the selectivity of isononanoic acid are counted, and the calculation formulas are respectively as follows:
isononanal conversion (%) = (isononanal molar amount before reaction-isononanal molar amount after reaction)/isononanal molar amount before reaction x 100%;
Isononanoic acid selectivity (%) = molar isononanoic acid after reaction/molar isononanal before reaction x 100%;
The results are shown in Table 1.
TABLE 1
From Table 1, the system and the method for preparing isononanoic acid by using isononanal as raw material can effectively improve the conversion rate of isononanal and the selectivity of isononanoic acid, and can ensure that the purity of the prepared product reaches more than 99%; in contrast, the scheme described in comparative example 1 does not employ a stepwise oxidation treatment step, the temperature stability of the isononaldehyde oxidation process is low, and although the purity of the prepared product is high, the selection of isononanoic acid is not high, and the product yield is not high; the scheme of comparative example 2 does not design a final adsorption tower, and the purity of the prepared product can not reach 99%; the product of comparative example 3 adopts a single rectifying tower to separate impurities, and the purity of the product is only 98%; comparative examples 4 and 5, although using a series-type double rectification column to separate impurities, it is also difficult to achieve high purity of the product based on the insufficient number of trays.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (8)
1. The system for preparing isononanoic acid by taking isononanal as a raw material is characterized by still comprising a serial oxidation reaction kettle, a filter, a serial double rectifying tower and an adsorption tower;
The series oxidation reaction kettles are two oxidation reaction kettles A1 and A2 which are arranged in series, and a transition radiator is arranged between the two oxidation reaction kettles;
the series double rectifying towers are a light component removing tower and a refining tower which are arranged in series;
The number of the tower plates of the light component removal tower is 8-18;
The number of the tower plates of the refining tower is 25-45;
and an adsorption filler is arranged in the adsorption tower.
2. The system for preparing isononanoic acid from isononanal as claimed in claim 1, wherein the filter is at least one of a bag filter, a basket filter, a plate filter, and a tube filter.
3. The system for preparing isononanoic acid by using isononanal as claimed in claim 1, wherein the top temperature of the light component removing tower is 45-95 ℃ and the top pressure is 1-45 kPa.
4. The system for preparing isononanoic acid by using isononanal as claimed in claim 1, wherein the top temperature of the refining tower is 110-180 ℃ and the top pressure is 1-45 kPa.
5. The system for preparing isononanoic acid by using isononanal as raw material according to claim 1, wherein the adsorption filler in the adsorption tower is at least one of clay, diatomite, molecular sieve and activated carbon fiber.
6. The method for preparing isononanoic acid by taking isononanal as a raw material is characterized by comprising the following steps:
(1) Preheating isononanal, then feeding the isononanal into the system of any one of claims 1-5, and carrying out a first-stage oxidation reaction at 40-60 ℃ in the oxidation reaction kettle A1 to obtain a reactant I;
(2) Delivering the reactant I into a transition radiator for cooling, and then delivering the reactant I into an oxidation reaction kettle A2 for performing two-stage oxidation treatment at 40-60 ℃ to obtain a reactant II; heterogeneous catalysts are arranged in the primary oxidation treatment and the secondary oxidation treatment;
(3) Delivering the reactant II into a filter for catalyst separation treatment to obtain a reactant III;
(4) Delivering the reactant III into a light component removal tower for first-stage impurity separation treatment, and then delivering the reactant III into a refining tower for second-stage impurity separation treatment to obtain a reactant IV;
(5) And (3) sending the reactant IV into an adsorption tower for adsorption and impurity removal treatment to obtain isononanoic acid.
7. The method for producing isononanoic acid as claimed in claim 6, wherein the pressure at the time of the primary oxidation reaction and the secondary oxidation reaction is 0.1 to 2MPa.
8. The method for producing isononanoic acid as claimed in claim 6, wherein the heterogeneous catalyst is a transition metal element-supported solid acid catalyst.
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