CN104606946B - In a kind of adiponitrile production process, separate the method for inactivation curing catalysts - Google Patents
In a kind of adiponitrile production process, separate the method for inactivation curing catalysts Download PDFInfo
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- CN104606946B CN104606946B CN201510011459.6A CN201510011459A CN104606946B CN 104606946 B CN104606946 B CN 104606946B CN 201510011459 A CN201510011459 A CN 201510011459A CN 104606946 B CN104606946 B CN 104606946B
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Abstract
The invention provides a kind of method that separates inactivation curing catalysts in adiponitrile production process, use the processing of level Four backwash filter, first the filtrate of containing the curing catalysts of inactivation enters from the lower side filtrate entrance of one-level backwash filter by pump, after the filtration of array filter assemblies, clear liquid part enters upper clear supernate district through filter assemblies, outlet from filtrate entrance offside under pressure and Action of Gravity Field is derived, simultaneously, successively through secondary backwash filter, three grades of backwash filters, the clear liquid of level Four backwash filter processing returns to clear liquid area and carries out backwash, filter residue is discharged and is delivered to collecting tank from bottom under pressure. process provided by the invention, compared with existing process, has realized catalyst circulation recovery, reduces energy consumption, cost-saving, meanwhile, taken out and solidified decaying catalyst by filtration, reactant liquor can meet the requirement of pipeline conveying and next step rectifying, has realized carrying out continuously smoothly of reaction.
Description
Technical field
The present invention relates to a kind of method that catalyst circulation is used, particularly in a kind of adiponitrile production process, separate inactivationThe method of curing catalysts.
Background technology
Adiponitrile (ADN, adiponitrile), water white oily liquids, has slight bitter taste, inflammable, molecular formula NC(CH2) 4CN, density is 962kg/m3,1 DEG C of fusing point, 295 DEG C of boiling points. Toxic and corrosivity, sucks or skin is inhaled by oral cavityReceipts all can cause poisoning. Be dissolved in methyl alcohol, ethanol, chloroform, be insoluble in water, cyclohexane, ether, carbon disulfide, carbon tetrachloride. Oneself is two years oldThe main application of nitrile is to produce hexamethylene diamine, and also there is wide application in this external electronics, light industry and other organic synthesis field.
The process route of adiponitrile mainly contains acrylonitrile (AN) Electrolytic Dimeric method, butadiene (BD) hydrocyanation method, adipic acid(ADA) catalytic ammoniation method and the caprolactam Hydrolyze method again of degrading. In the world today, the main technique of adiponitrile suitability for industrialized production isElectrolytic Dimeric Acrylonitrile method and butadiene hydrocyanation method. The reaction that the direct hydrocyanation method of butadiene is produced adiponitrile comprises one-level cyanogenChange, isomerization, three steps of secondary cyaniding, the method adopts transition-metal catalyst, and two molecular hydrogen cyanic acid are introduced to butadiene,Catalyst adopts the complex compound of the transition metal such as Ni, Rh, Ru conventionally. Wherein allyl acetonitrile (3-PN) is its important intermediate, anti-Answer equation as follows:
One-level cyaniding:
Isomerization:
Secondary cyaniding:
General equation formula: CH2＝CHCH＝CH2+2HCN→NC(CH2)4CN+4H2
One-level cyaniding is produced in the process of allyl acetonitrile (3PN), and the catalyst of inactivation forms the solid formation that is insoluble to reactant liquorMatter, therefore needs to adopt suitable equipment and process that it is separated from reaction system, has both been conducive to next step reactionCarry out continuously smoothly, also saved high catalyst cost, reduce energy consumption, met environmentally friendly enterprise simultaneously and producedRequirement.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art, provide a kind of stable operation, manufacturing process simple, saveCost of labor, the method for decaying catalyst is solidified in the recovery that reduces energy consumption, the present invention by the following technical solutions:
Use the processing of level Four backwash filter, the filtrate of curing catalysts of first containing inactivation is anti-from one-level by pumpThe lower side filtrate entrance of flush filter enters, and after the filtration of array filter assemblies, clear liquid part is through filteringAssembly enters upper clear supernate district, and described clear liquid area is on tower tray, and the clear liquid after filtration and lower floor's filter residue separate, at pressure and heavyOutlet from filtrate entrance offside under power effect is derived, and filter residue strong adsorption is being crossed on filter core, and filter residue is piled up and caused filtrate entrancePressure increases, and in the time that pressure is 0.4～0.48MpaG, filtration fraction completes, and closes filtrate entrance, is switched to reserve filter,Every one-level backwash filter has reserve filter, and backwash filter pressure is switched to stand-by equipment while reaching setting value and entersRow filters, and ensures to react to proceed, and filter starts to clean simultaneously, opens backwash filter bottom sludge outlet, topClear liquid area passes into nitrogen air blowing pressurization, meanwhile, successively through secondary backwash filter, three grades of backwash filters, level Four recoilThe clear liquid of washing filter process returns to clear liquid area and carries out backwash, and filter residue is discharged and delivered to collecting tank from bottom under pressureIn.
Further, described filter assemblies adopts 10～20 filter cores to be fixed on the tower tray parts of filter middle and upper part, filter coreThe mode that adopts spray welding filter element and the combination of wire-wound filter core, filtering accuracy is 1～10 μ m.
Further, described each backwash filter is equipped with reserve filter switching use.
Major advantage of the present invention has:
Process provided by the invention, compared with existing process, has realized catalyst circulation recovery, reduces energyConsumption, cost-saving; Meanwhile, taken out and solidified decaying catalyst by filtration, reactant liquor can meet pipeline and carry and next step rectifyingRequirement, realized carrying out continuously smoothly of reaction.
Brief description of the drawings
Fig. 1 is process chart of the present invention
1, one-level backwash filter 2, secondary backwash filter 3, three grades of backwash filters
4, level Four backwash filter 11, one-level backwash filter for 5, collecting tank
Use filter
6, filter assemblies 7, filtrate entrance 8, outlet
9, sludge outlet 22, secondary backwash filter for 33, three grades of backwash filters are standby
With filter filter
44, level Four backwash filter is standby
Use filter
Detailed description of the invention
The filter effect that the traditional level Four of embodiment 1 is filtered
The reactant liquor of four kinds of different solid contents is added respectively to same stream from backwash filter lower side filtrate entranceUnder amount (10kg/h) condition, solid content is respectively 20%wt, 15%wt, 10%wt, 5%wt. After every single filter, solid content numberAccording to listing in table 1. Solid content analyzer measurement category is 0.01～100%wt.
After measured, during actual adiponitrile is produced, range of solid content is about 6%wt～12%wt, requires to enter Distallation systmReactant liquor solid content≤0.03%. As can be seen from Table 1, filter through level Four at the reactant liquor of given four kinds of different solid contentsAfter, solid content is in the time of 8%wt～15%wt, and filter effect meets production requirement.
The filter effect that the traditional level Four of table 1 is filtered
Embodiment 2
As shown in Figure 1, in a kind of adiponitrile production process, separate the method for inactivation curing catalysts, use level Four backwashFilter process, the filtrate of curing catalysts of first containing inactivation is the lower side from one-level backwash filter 1 by pumpFiltrate entrance 7 enters, and after the filtration of array filter assemblies 6, clear liquid part enters upper clear supernate district through filter assemblies,Clear liquid area is above tower tray, and the clear liquid after filtration and lower floor's filter residue separate, under pressure and Action of Gravity Field from filtrate entrance 7 offsidesOutlet sequence number 8 derive, filter residue strong adsorption is being crossed on filter core, filter residue is piled up and is caused filtrate inlet pressure to increase, when pressure isWhen 0.4～0.48MpaG, filtration fraction completes, and closes filtrate entrance, is switched to reserve filter 11, every one-level backwash filterDevice has reserve filter, and backwash filter pressure is switched to stand-by equipment while reaching setting value and filters, and ensures reactionProceed, filter starts to clean simultaneously, opens backwash filter bottom sludge outlet 9, and upper clear supernate district passes into nitrogenBlow and pressurize, meanwhile, through 2, three grades of backwash filters 3 of secondary backwash filter, level Four backwash filter 4 is processed successivelyClear liquid return to clear liquid area and carry out backwash, filter residue is discharged and is delivered to collecting tank from bottom under pressure.
Adopt the process shown in Fig. 1 compared with traditional discontinuous operation, the reactant liquor processing that contains decaying catalystWhen amount is all 10kg/h, the method for the invention is obviously better than discontinuous operation.
The reaction raw materials that adiponitrile production process is related and intermediate product mostly are the hazardous chemical such as poisonous, inflammable and explosiveProduct, all operations requires isolated air to carry out, and therefore, selects device that a kind of closed can continued operation and process veryImportant, save time and manpower aspect with the obvious advantage, for further expanding the scale of production, improve product quality and yieldHaving supplied may.
The traditional level Four of table 2 is filtered the contrast with the present invention
Above embodiments of the invention are had been described in detail, but described content is only preferred embodiment of the present invention,Not in order to limit the present invention. All any amendments of making in application range of the present invention, be equal to and replace and improvement etc., all shouldWithin being included in protection scope of the present invention.
Claims (3)
1. a method that separates inactivation curing catalysts in adiponitrile production process, is characterized in that, uses level Four backwashFilter process, first contains filtrate lower side filter from one-level backwash filter by pump of the curing catalysts of inactivationLiquid entrance enters, and after the filtration of array filter assemblies, clear liquid part enters upper clear supernate district through filter assemblies, is pressingOutlet from filtrate entrance offside under power and Action of Gravity Field is derived, and filter residue strong adsorption is being crossed on filter core, and filter residue is piled up and caused filterLiquid inlet pressure increases, and in the time that pressure is 0.4～0.48MpaG, filtration fraction completes, and closes filtrate entrance, is switched to mistake for subsequent useFilter, opens backwash filter bottom sludge outlet, and upper clear supernate district passes into nitrogen air blowing pressurization, meanwhile, and successively through secondaryBackwash filter, three grades of backwash filters, the clear liquid of level Four backwash filter processing returns to clear liquid area and carries out backwash,Filter residue is discharged and is delivered to collecting tank from bottom under pressure.
2. according to the method that separates inactivation curing catalysts in a kind of adiponitrile production process claimed in claim 1, its featureBe, described filter assemblies adopts 10～20 filter cores to be fixed on the tower tray parts of filter middle and upper part, and filter core adopts spray fusing filterThe mode of core and the combination of wire-wound filter core, filtering accuracy is 1～10 μ m.
3. according to the method that separates inactivation curing catalysts in a kind of adiponitrile production process claimed in claim 1, its featureBe, described each backwash filter is equipped with reserve filter and switches use.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510011459.6A CN104606946B (en) | 2015-01-09 | 2015-01-09 | In a kind of adiponitrile production process, separate the method for inactivation curing catalysts |
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| CN201510011459.6A CN104606946B (en) | 2015-01-09 | 2015-01-09 | In a kind of adiponitrile production process, separate the method for inactivation curing catalysts |
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| CN104606946B true CN104606946B (en) | 2016-05-11 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106732198A (en) * | 2016-12-29 | 2017-05-31 | 杭州油脂化工有限公司 | A kind of oil hydrogenation catalyst recycle device and recoverying and utilizing method |
| CN106669279B (en) * | 2017-02-09 | 2022-04-22 | 无锡玖和隆工程科技有限公司 | Filtering equipment for realizing catalyst separation in polytetramethylene glycol production |
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| US3559809A (en) * | 1969-02-07 | 1971-02-02 | Amf Inc | Filter back wash means |
| CN2171403Y (en) * | 1993-08-07 | 1994-07-13 | 宜兴市华宜环保设备技术工程公司 | Multi-stage homogeneity anti-grading filter |
| CN201871489U (en) * | 2010-10-13 | 2011-06-22 | 中国石油化工股份有限公司 | Separator for separating catalysts with different inactive degree |
| CN102441446A (en) * | 2010-10-13 | 2012-05-09 | 中国石油化工股份有限公司 | Table separating method of catalysts with different inactivation degrees |
| CN102441527A (en) * | 2010-10-13 | 2012-05-09 | 中国石油化工股份有限公司 | Separation method for catalysts of different inactivation degrees |
| CN203316246U (en) * | 2013-06-25 | 2013-12-04 | 中国石油化工股份有限公司 | Separation device for separating catalysts with different inactivation degrees |
| CN103769248A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Separation method of boiling bed residual oil hydrogenation catalysts of different inactivation degrees |
| CN203598828U (en) * | 2013-10-31 | 2014-05-21 | 中国石油化工股份有限公司 | Multistage separation device for hydrogenation catalysts of different deactivation degrees |
-
2015
- 2015-01-09 CN CN201510011459.6A patent/CN104606946B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3559809A (en) * | 1969-02-07 | 1971-02-02 | Amf Inc | Filter back wash means |
| CN2171403Y (en) * | 1993-08-07 | 1994-07-13 | 宜兴市华宜环保设备技术工程公司 | Multi-stage homogeneity anti-grading filter |
| CN201871489U (en) * | 2010-10-13 | 2011-06-22 | 中国石油化工股份有限公司 | Separator for separating catalysts with different inactive degree |
| CN102441446A (en) * | 2010-10-13 | 2012-05-09 | 中国石油化工股份有限公司 | Table separating method of catalysts with different inactivation degrees |
| CN102441527A (en) * | 2010-10-13 | 2012-05-09 | 中国石油化工股份有限公司 | Separation method for catalysts of different inactivation degrees |
| CN103769248A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Separation method of boiling bed residual oil hydrogenation catalysts of different inactivation degrees |
| CN203316246U (en) * | 2013-06-25 | 2013-12-04 | 中国石油化工股份有限公司 | Separation device for separating catalysts with different inactivation degrees |
| CN203598828U (en) * | 2013-10-31 | 2014-05-21 | 中国石油化工股份有限公司 | Multistage separation device for hydrogenation catalysts of different deactivation degrees |
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