CN205501166U - Piece -rate system of 2 - methyl - 3 - crotononitrile isomerization production 3 - allyl acetonitrile in -process accessory substance 2 - methyl - 2 - crotononitrile - Google Patents
Piece -rate system of 2 - methyl - 3 - crotononitrile isomerization production 3 - allyl acetonitrile in -process accessory substance 2 - methyl - 2 - crotononitrile Download PDFInfo
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Abstract
The utility model provides one kind 2 the methyl 3 crotononitrile isomerization production 3 allyl acetonitrile in -process accessory substance 2 the methyl 2 the piece -rate system of crotononitrile, the utility model provides a 2 the methyl 3 does the crotononitrile isomerization generate 3 can the allyl acetonitrile in -process by -product 2 the methyl 2 the crotononitrile, and 2 the methyl 2 the crotononitrile can constantly accumulate in the system, restraines going on of isomerization reaction, through does the extractant increase by 2 the methyl 2 crotononitrile and 2 the methyl 3 does the relative volatility of crotononitrile accomplish 2 in the same rectifying column that has a baffle the methyl 2 crotononitrile and 2 the methyl 3 the separation of crotononitrile and the cyclic utilization of extractant, greatly reduced equipment cost with the operation degree of difficulty to can obtain 2 of high -purity the methyl 2 crotononitrile and 2 the methyl 3 the crotononitrile product.
Description
Technical field
This utility model belongs to technical field of chemical separation, particularly relates to a kind of 2-methyl-3-butene nitrile isomerization and produces the piece-rate system of 3 pentene nitrile byproduct in process thing 2-methyl-2-butene nitrile.
Background technology
3 pentene nitrile (3PN) is the intermediate preparing adiponitrile, and can continue hydrocyanation is adiponitrile, and adiponitrile is nylon66 fiber intermediate, belongs to important chemical products.2-methyl-3-butene nitrile (2M3BN) isomerization produces meeting by-product 2-methyl-2-butene nitrile (2M2BN) during 3 pentene nitrile (3PN), and 2-methyl-2-butene nitrile can constantly accumulate in response system, reaction conversion ratio and selectivity is caused to reduce, it is therefore desirable to 2-methyl-2-butene nitrile is continuously separated from response system extraction.But, the atmospheric boiling point difference of 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile is the least, less than 5 DEG C, needs high tower diameter and big reflux ratio by conventional distillation method, causes operating cost and operating cost higher.
The method of a patent CN201410052580.9 alkene nitrile mixed liquor direct isomerization synthesis 3 pentene nitrile proposes to add zero-valent nickel catalyst in 2-methyl-3-butene nitrile and 3 pentene nitrile, phosphorus-containing ligand and lewis acid, 2-methyl-3-butene nitrile can be isomerized to 3 pentene nitrile, the conversion ratio of 2-methyl-3-butene nitrile is more than 95%, the selectivity of 3 pentene nitrile is more than 95%, does not propose isomerization reaction and can produce 2-methyl-2-butene nitrile by-product in patent.
The method of a patent CN201410052751.8 alkene nitrile mixed liquor direct isomerization synthesis 2-methyl-2-butene nitrile proposes to add calcic inorganic base in 2-methyl-3-butene nitrile and 3 pentene nitrile, isomerization reaction can be occurred to generate 2-methyl-2-butene nitrile, this patent only shows that inorganic base can make 2-methyl-3-butene nitrile isomerization generate 3 pentene nitrile reaction and occur towards side reaction 2-methyl-2-butene nitrile direction, and the separation method of not mentioned 2-methyl-3-butene nitrile and 2-methyl-2-butene nitrile.
Summary of the invention
The utility model proposes use extractant, increase 2-methyl-2-butene nitrile and the boiling-point difference of 2-methyl-3-butene nitrile, the rectifying column of recycling ad hoc structure carries out continuous rectification, thus realizes 2-methyl-2-butene nitrile and the separation of 2-methyl-3-butene nitrile, and the concrete technical scheme of employing is as follows:
A kind of 2-methyl-3-butene nitrile isomerization produces the separation method of 3 pentene nitrile byproduct in process thing 2-methyl-2-butene nitrile, comprises the steps:
Step 1: dividing plate is set in rectifying column, tower body inside upper part is divided into two regions, left and right, tower body bottom is the public territory not separated, and 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile mixed material feed from rectifying column left field middle and lower part, and extractant is from rectifying column left field its top feed；
Step 2: rectifying column left field top obtains 2-methyl-2-butene nitrile, 2-methyl-3-butene nitrile enters tower reactor public territory with extractant；
Step 3: be circulated heating in public territory, enters the right side area of rectifying column, is separated with extractant by 2-methyl-3-butene nitrile, and rectifying column right side area top obtains 2-methyl-3-butene nitrile, and extractant returns to tower reactor public territory and is circulated utilization.
Rectifying tower pressure on top surface is 10-50kPaA, and column bottom temperature is 100-120 DEG C, rectifying column diameter 300mm, and tower height is not less than 6000mm, arranges the shared height in the public territory after dividing plate less than the 20% of rectifying column tower height in rectifying column.
Described extractant is the one in trimethyl phosphate or dimethyl sulfoxide.Extractant is bigger to the difference in solubility of two kinds of components, dissolubility to 2-methyl-3-butene nitrile is much larger than the dissolubility of 2-methyl-2-butene nitrile, and extractant is poorer than the volatility of 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile, 2-methyl-2-butene nitrile can be separated from isomerization reaction system by extraction rectifying method.
In described 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile mixture, 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile are according to mass ratio 1:1 proportioning.
A kind of 2-methyl-3-butene nitrile isomerization produces the piece-rate system of 3 pentene nitrile byproduct in process thing 2-methyl-2-butene nitrile, including tower bottom reboiler, tower top 2-methyl-3-butene nitrile cooler, tower top 2-methyl-2-butene nitrile cooler, rectifying column, head tank, feed pump, head tank is connected with rectifying column by feed pump, rectifier bottoms arranges tower bottom reboiler, dividing plate is set in rectifying column, tower body inside upper part is divided into two regions, left and right, tower body bottom is the public territory not separated, left field tower top arranges tower top 2-methyl-2-butene nitrile cooler, right side area tower top arranges tower top 2-methyl-3-butene nitrile cooler, rectifying column left field top arranges extractant feed mouth.
The shared height in public territory after dividing plate is set in described rectifying column less than the 20% of rectifying column tower height.Rectifying column diameter 300mm, tower height is not less than 6000mm.Head tank is connected with rectifying column left field middle and lower part by feed pump.
What in this utility model, 2-methyl-3-butene nitrile represented is 2-methyl-3-butene nitrile, and what 3 pentene nitrile represented is 3 pentene nitrile, and what 2-methyl-2-butene nitrile represented is 2-methyl-2-butene nitrile.This utility model uses the middle rectifying column arranging dividing plate, and region in tower is divided into left field, right side area and public territory, bottom by dividing plate.Left field realizes the extracting rectifying of 2-methyl-2-butene nitrile, and right side area realizes the rectification of 2-methyl-3-butene nitrile, and public territory, bottom is stripping region, completes the recovery of extractant.2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile left side central portion from tower enters, extractant adds from left side top of tower, owing to extractant is much larger than 2-methyl-2-butene nitrile to the dissolubility of 2-methyl-3-butene nitrile, left side top can obtain pure 2-methyl-2-butene nitrile, 2-methyl-3-butene nitrile enters tower reactor public territory with extractant, in public territory by circulating-heating, enter the right side area of tower, it is achieved 2-methyl-3-butene nitrile is with the separation of trimethyl phosphate.
The beneficial effects of the utility model are: the utility model proposes 2-methyl-3-butene nitrile isomerization and generate meeting by-product 2-methyl-2-butene nitrile during 3 pentene nitrile, and 2-methyl-2-butene nitrile can accumulate the most in systems, the carrying out of suppression isomerization reaction, 2-methyl-2-butene nitrile and the relative volatility of 2-methyl-3-butene nitrile is increased by extractant described in the utility model, recycling of 2-methyl-2-butene nitrile and the separation of 2-methyl-3-butene nitrile and extractant is completed in the same rectifying column with dividing plate, greatly reduce equipment cost and operation easier, and highly purified 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile product can be obtained.
Accompanying drawing explanation
Fig. 1 is to produce by-product 2-methyl-2-butene nitrile accumulation schematic diagram during 2-methyl-3-butene nitrile isomerization produces 3 pentene nitrile
Fig. 2 is that 2-methyl-3-butene nitrile isomerization described in the utility model produces 3 pentene nitrile byproduct in process thing 2-methyl-2-butene nitrile piece-rate system structure chart
Marginal data: 1, tower bottom reboiler, 2, tower top 2-methyl-3-butene nitrile cooler, 3, tower top 2-methyl-2-butene nitrile cooler, 4, rectifying column, 5, head tank, 6, feed pump, 7, dividing plate, 8, left field, 9, right side area, 10, public territory, 11, extractant feed mouth
A, 2-methyl-3-butene nitrile, B, 2-methyl-2-butene nitrile, C, 3 pentene nitrile, D, catalyst, E, extractant, F, left field top products, G, right side area top products
Detailed description of the invention
For the technological means making this utility model realize, creation characteristic, reach purpose and be easy to understand with effect; below detailed description of the invention of the present utility model is described further; but do not limit protection domain of the present utility model; it should be noted that; in the case of not conflicting, the embodiment in this utility model creation and the feature in embodiment can be mutually combined.
As it is shown in figure 1, be continuously added to 2-methyl-3-butene nitrile A and catalyst D in the carbon steel reactor of diameter 600mm, highly 800mm, catalyst D inlet amount 1kg/h, 2-methyl-3-butene nitrile A inlet amount 100kg/h, open stirring, reaction time about 2h.Sample at exit analysis, find that product has unreacted 2-methyl-3-butene nitrile, by-product 2-methyl-2-butene nitrile B and product 3 pentene nitrile C, 2-methyl-2-butene nitrile B content about 5w.t%, unreacted 2-methyl-3-butene nitrile content about 30w.t%, 3 pentene nitrile C content 65w.t%, it can be said that the generation having 2-methyl-2-butene nitrile B in bright reaction.
Separately carry out reaction as shown in Figure 1, in the carbon steel reactor of diameter 600mm, highly 800mm, add 2-methyl-3-butene nitrile A, control 2-methyl-3-butene nitrile A addition 200kg, it is simultaneously introduced catalyst D, control catalyst D addition 2kg, open stirring, measure under the differential responses time, 2-methyl-2-butene nitrile content, 2-methyl-3-butene nitrile content, 3 pentene nitrile content, measurement data is as shown in table 1.
Table 1 measurement data list
By table 1 it appeared that, prolongation along with the response time, in response system, the content of 2-methyl-2-butene nitrile is being continuously increased, and by-product 2-methyl-2-butene nitrile can suppress 2-methyl-3-butene nitrile isomerization reaction, and 3 pentene nitrile can inversely be converted into 2-methyl-2-butene nitrile as time went on.
Embodiment 1:
A kind of 2-methyl-3-butene nitrile isomerization produces the piece-rate system of 3 pentene nitrile byproduct in process thing 2-methyl-2-butene nitrile, including tower bottom reboiler 1, tower top 2-methyl-3-butene nitrile cooler 2, tower top 2-methyl-2-butene nitrile cooler 3, rectifying column 4, head tank 5, feed pump 6, head tank 5 is connected with rectifying column 4 by feed pump 6, tower bottom reboiler 1 is set bottom rectifying column 4, dividing plate 7 is set in rectifying column 4, tower body inside upper part is divided into left field 8 and right side area 9, tower body bottom is the public territory 10 not separated, left field 8 tower top arranges tower top 2-methyl-2-butene nitrile cooler 3, right side area 9 tower top arranges tower top 2-methyl-3-butene nitrile cooler 2, rectifying column 4 left field 8 top arranges extractant feed mouth 11.
nullRectifying column 4 diameter 300mm，Tower height 6000mm，Dividing plate 7 is inside set，Tower body inside upper part is divided into left field 8 and right side area 9，Tower body bottom is the public territory 10 not separated，Bottom rectifying column 4, the shared height in public territory 10 is the 20% of total tower height，By 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile according to mass ratio 1:1 proportioning in head tank 5，This rectifying column 4 left field 8 middle and lower part is sent into by feed pump 6，Extractant E trimethyl phosphate is by rectifying column 4 left field 8 its top feed，Control rectification amount 200kg/h，Vapo(u)rizing temperature 100 DEG C at the bottom of control tower，Tower top pressure 10kPaA，Use continuous distillation method，2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile mixed material middle and lower part on the left of tower adds，Extractant E trimethyl phosphate adds from tower left field 8 top，Control extractant addition 300kg/h,Owing to extractant E trimethyl phosphate is much larger than 2-methyl-2-butene nitrile to the dissolubility of 2-methyl-3-butene nitrile，Left field 8 top can obtain pure 2-methyl-2-butene nitrile，2-methyl-3-butene nitrile enters tower reactor public territory 10 with extractant E trimethyl phosphate，In public territory 10 by tower bottom reboiler 1 circulating-heating，Enter the right side area 9 of rectifying column，Realize the separation with trimethyl phosphate of the 2-methyl-3-butene nitrile.Respectively tower top left field 8 and right side area 9 top products are analyzed, find that in left field top products F, 2-methyl-2-butene nitrile content is more than 99.99w.t%, in right side area top products G, 2-methyl-3-butene nitrile content is more than 99.99wt%, show in this rectifying column 4, be successfully realized 2-methyl-2-butene nitrile and the separation of 2-methyl-3-butene nitrile, and extractant E trimethyl phosphate will not be entrained in product 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile.Extractant E trimethyl phosphate in tower reactor can feed back to extractant feed mouth 11, is circulated utilization.
Embodiment 2:
A kind of 2-methyl-3-butene nitrile isomerization produces the piece-rate system of 3 pentene nitrile byproduct in process thing 2-methyl-2-butene nitrile, including tower bottom reboiler 1, tower top 2-methyl-3-butene nitrile cooler 2, tower top 2-methyl-2-butene nitrile cooler 3, rectifying column 4, head tank 5, feed pump 6, head tank 5 is connected with rectifying column 4 by feed pump 6, tower bottom reboiler 1 is set bottom rectifying column 4, dividing plate 7 is set in rectifying column 4, tower body inside upper part is divided into left field 8 and right side area 9, tower body bottom is the public territory 10 not separated, left field 8 tower top arranges tower top 2-methyl-2-butene nitrile cooler 3, right side area 9 tower top arranges tower top 2-methyl-3-butene nitrile cooler 2, rectifying column 4 left field 8 top arranges extractant feed mouth 11.
nullRectifying column 4 diameter 300mm，Tower height 7000mm，Dividing plate 7 is inside set，Tower body inside upper part is divided into left field 8 and right side area 9，Tower body bottom is the public territory 10 not separated，Bottom rectifying column 4, the shared height in public territory 10 is less than the 20% of total tower height，By 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile according to mass ratio 1:1 proportioning in head tank 5，This rectifying column 4 left field 8 middle and lower part is sent into by feed pump 6，Extractant E dimethyl sulfoxide is by rectifying column 4 left field 8 its top feed，Control rectification amount 200kg/h，Vapo(u)rizing temperature 120 DEG C at the bottom of control tower，Tower top pressure 50kPaA，Use continuous distillation method，2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile mixed material middle and lower part on the left of tower adds，Extractant E dimethyl sulfoxide adds from tower left field 8 top，Control extractant addition 300kg/h,Owing to extractant E dimethyl sulfoxide is much larger than 2-methyl-2-butene nitrile to the dissolubility of 2-methyl-3-butene nitrile，Left field 8 top can obtain pure 2-methyl-2-butene nitrile，2-methyl-3-butene nitrile enters tower reactor public territory 10 with extractant E dimethyl sulfoxide，In public territory 10 by tower bottom reboiler 1 circulating-heating，Enter the right side area 9 of rectifying column，Realize the separation with dimethyl sulfoxide of the 2-methyl-3-butene nitrile.Respectively tower top left field 8 and right side area 9 top products are analyzed, find that in left field top products F, 2-methyl-2-butene nitrile content is more than 99.99w.t%, in right side area top products G, 2-methyl-3-butene nitrile content is more than 99.99wt%, show in this rectifying column 4, be successfully realized 2-methyl-2-butene nitrile and the separation of 2-methyl-3-butene nitrile, and extractant E dimethyl sulfoxide will not be entrained in product 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile.Extractant E dimethyl sulfoxide in tower reactor can feed back to extractant feed mouth 11, is circulated utilization.
Embodiment 3:
A kind of 2-methyl-3-butene nitrile isomerization produces the piece-rate system of 3 pentene nitrile byproduct in process thing 2-methyl-2-butene nitrile, including tower bottom reboiler 1, tower top 2-methyl-3-butene nitrile cooler 2, tower top 2-methyl-2-butene nitrile cooler 3, rectifying column 4, head tank 5, feed pump 6, head tank 5 is connected with rectifying column 4 by feed pump 6, tower bottom reboiler 1 is set bottom rectifying column 4, dividing plate 7 is set in rectifying column 4, tower body inside upper part is divided into left field 8 and right side area 9, tower body bottom is the public territory 10 not separated, left field 8 tower top arranges tower top 2-methyl-2-butene nitrile cooler 3, right side area 9 tower top arranges tower top 2-methyl-3-butene nitrile cooler 2, rectifying column 4 left field 8 top arranges extractant feed mouth 11.
nullRectifying column 4 diameter 300mm，Tower height 6500mm，Dividing plate 7 is inside set，Tower body inside upper part is divided into left field 8 and right side area 9，Tower body bottom is the public territory 10 not separated，Bottom rectifying column 4, the shared height in public territory 10 is less than the 20% of total tower height，By 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile according to mass ratio 1:1 proportioning in head tank 5，This rectifying column 4 left field 8 middle and lower part is sent into by feed pump 6，Extractant E trimethyl phosphate is by rectifying column 4 left field 8 its top feed，Control rectification amount 200kg/h，Vapo(u)rizing temperature 110 DEG C at the bottom of control tower，Tower top pressure is in 30kPaA scope，Use continuous distillation method，2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile mixed material middle and lower part on the left of tower adds，Extractant E trimethyl phosphate adds from tower left field 8 top，Control extractant addition 300kg/h,Owing to extractant E trimethyl phosphate is much larger than 2-methyl-2-butene nitrile to the dissolubility of 2-methyl-3-butene nitrile，Left field 8 top can obtain pure 2-methyl-2-butene nitrile，2-methyl-3-butene nitrile enters tower reactor public territory 10 with extractant E trimethyl phosphate，In public territory 10 by tower bottom reboiler 1 circulating-heating，Enter the right side area 9 of rectifying column，Realize the separation with trimethyl phosphate of the 2-methyl-3-butene nitrile.Respectively tower top left field 8 and right side area 9 top products are analyzed, find that in left field top products F, 2-methyl-2-butene nitrile content is more than 99.99w.t%, in right side area top products G, 2-methyl-3-butene nitrile content is more than 99.99wt%, show in this rectifying column 4, be successfully realized 2-methyl-2-butene nitrile and the separation of 2-methyl-3-butene nitrile, and extractant E trimethyl phosphate will not be entrained in product 2-methyl-2-butene nitrile and 2-methyl-3-butene nitrile.Extractant E trimethyl phosphate in tower reactor can feed back to extractant feed mouth 11, is circulated utilization.
Separation method described in the utility model and system are described by specific embodiment.Those skilled in the art can use for reference content of the present utility model and suitably change the links such as rectifying tower structure and realize other purpose corresponding; its relevant change is all without departing from content of the present utility model; within all spirit in this utility model creation and principle; the any modification, equivalent substitution and improvement etc. made, within should be included in the protection domain that this utility model is created.
Claims (3)
1. the piece-rate system of a 2-methyl-3-butene nitrile isomerization production 3 pentene nitrile byproduct in process thing 2-methyl-2-butene nitrile, it is characterized in that, dividing plate is set in rectifying column, tower body inside upper part is divided into two regions, left and right, tower body bottom is the public territory not separated, left field tower top arranges tower top 2-methyl-2-butene nitrile cooler, and right side area tower top arranges tower top 2-methyl-3-butene nitrile cooler, and rectifying column left field top arranges extractant feed mouth.
A kind of 2-methyl-3-butene nitrile isomerization produces the piece-rate system of 3 pentene nitrile byproduct in process thing 2-methyl-2-butene nitrile, it is characterized in that, the shared height in the public territory after dividing plate is set in described rectifying column less than the 20% of rectifying column tower height.
A kind of 2-methyl-3-butene nitrile isomerization produces the piece-rate system of 3 pentene nitrile byproduct in process thing 2-methyl-2-butene nitrile, it is characterised in that described rectifying column diameter 300mm, tower height is not less than 6000mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105367448A (en) * | 2015-12-04 | 2016-03-02 | 中国天辰工程有限公司 | Separation method and system for byproduct 2M2BN in course of producing 3PN by 2M3BN isomerization |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105367448A (en) * | 2015-12-04 | 2016-03-02 | 中国天辰工程有限公司 | Separation method and system for byproduct 2M2BN in course of producing 3PN by 2M3BN isomerization |
| CN105367448B (en) * | 2015-12-04 | 2017-07-28 | 中国天辰工程有限公司 | A kind of 2M3BN isomerization production 3PN byproduct in process things 2M2BN separation method and system |
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