CN104606946A - Method for separating inactivated curing catalyst in adiponitrile production process - Google Patents
Method for separating inactivated curing catalyst in adiponitrile production process Download PDFInfo
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- CN104606946A CN104606946A CN201510011459.6A CN201510011459A CN104606946A CN 104606946 A CN104606946 A CN 104606946A CN 201510011459 A CN201510011459 A CN 201510011459A CN 104606946 A CN104606946 A CN 104606946A
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Abstract
The invention provides a method for separating an inactivated curing catalyst in the adiponitrile production process. The method comprises the following steps: treating by using a four-stage back wash filter, that is, firstly, feeding a filtrate with the inactivated curing catalyst from a lower side surface filtrate inlet of a first-stage back wash filter, filtering by using a plurality of groups of filtering components, passing the clear liquid through the filtering components to enter an upper clear liquid area, under the action of pressure and gravity, leading out from an outlet in the side opposite to the filtrate inlet, at the same time, feeding back clear liquids which are treated by using a second-stage back wash filter, a third-stage back wash filter and a fourth-stage back wash filter to the clear liquid area for back wash, under the action of pressure, and discharging filter residues into a collecting tank from the lower part. Compared with a conventional process method, the method provided by the invention achieves circulation and recycling of the catalyst, reduces the energy consumption and lowers the cost; meanwhile, the inactivated curing catalyst can be filtered out, the reaction liquid can meet the requirements of pipeline conveying and distillation in later steps, and smooth and continuous operation of the reaction can be achieved.
Description
Technical field
The present invention relates to the method being separated inactivation curing catalysts in a kind of method, particularly adiponitrile production process of a kind of catalyst circulation use.
Background technology
Adiponitrile (ADN, adiponitrile), water white oily liquids, has slight bitter taste, inflammable, molecular formula NC (CH2) 4CN, and density is 962kg/m3, fusing point 1 DEG C, boiling point 295 DEG C.Toxic and corrosivity, sucked by oral cavity or skin absorb all can cause poisoning.Be dissolved in methyl alcohol, ethanol, chloroform, be insoluble in water, cyclohexane, ether, carbon disulfide, carbon tetrachloride.Hexamethylene diamine is produced in the main application of adiponitrile, 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 process, adipic acid (ADA) catalytic ammoniation method and caprolactam and to degrade Hydrolyze method again.In the world today, the main technique of adiponitrile suitability for industrialized production is Electrolytic Dimeric Acrylonitrile method and butadiene hydrocyanation process.The reaction that the direct hydrocyanation process of butadiene produces adiponitrile comprises one-level cyaniding, isomerization, secondary cyaniding three steps, the method adopts transition-metal catalyst, two molecular hydrogen cyanic acid are introduced butadiene, and catalyst adopts the complex compound of the transition metal such as Ni, Rh, Ru usually.Wherein allyl acetonitrile (3-PN) is its important intermediate, and reaction equation is as follows:
One-level cyaniding:
Isomerization:
Secondary cyaniding:
General equation: CH
2=CHCH=CH
2+ 2HCN → NC (CH
2)
4cN+4H
2
One-level cyaniding is produced in the process of allyl acetonitrile (3PN), the catalyst of inactivation forms the solid matter being insoluble to reactant liquor, therefore need to adopt suitable instrument and supplies method it to be separated from reaction system, both carrying out continuously smoothly of next step reaction had been conducive to, also save high catalyst cost, reduce energy consumption, meet the requirement that environment-friendly enterprise is produced simultaneously.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art, provide a kind of stable operation, manufacturing process simple, save labour turnover, reduce the method for the recovery solidification decaying catalyst of energy consumption, the present invention by the following technical solutions:
Use the process of level Four backwash filter, the filtrate of the curing catalysts first containing inactivation is entered by the lower side filtrate inlet of pump from one-level backwash filter, after the filtration of array filter assemblies, supernatant fraction enters upper clear supernate district through filter assemblies, described clear liquid area is at tray thereabove, clear liquid after filtration and lower floor's filter residue separate, derive from the outlet of filtrate inlet offside under pressure and Action of Gravity Field, filter residue strong adsorption is on filtration core, filter residue is piled up and is caused filtrate inlet pressure to increase, when pressure is 0.4 ~ 0.48MpaG, filtration fraction completes, close filtrate import, be switched to reserve filter, every one-level backwash filter has reserve filter, backwash filter pressure is switched to stand-by equipment when reaching setting value and filters, guarantee reaction proceeds, filter starts cleaning simultaneously, open backwash filter bottom sludge outlet, upper clear supernate district passes into nitrogen air blowing pressurization, simultaneously, successively through secondary backwash filter, three grades of backwash filters, the clear liquid of level Four backwash filter process returns to clear liquid area and carries out backwash, filter residue is discharged from bottom under pressure and is delivered to collecting tank.
Further, described filter assemblies adopts 10 ~ 20 filter cores to be fixed on the tower tray parts of filter middle and upper part, the mode that filter core adopts spray welding filter element and Wire-wound filter core to combine, and filtering accuracy is 1 ~ 10 μm.
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, achieves catalyst circulation and reclaims, reduce energy consumption, cost-saving; Meanwhile, take out solidification decaying catalyst by filtering, reactant liquor can meet the requirement of Cemented filling and next step rectifying, achieves carrying out continuously smoothly of reaction.
Accompanying drawing explanation
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 inlet 8, outlet
9, sludge outlet 22, secondary backwash filter are standby for 33, three grades of backwash filters
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
Added respectively from backwash filter lower side filtrate inlet by the reactant liquor of four kinds of different solid contents, under same traffic (10kg/h) condition, solid content is respectively 20%wt, 15%wt, 10%wt, 5%wt.After every single filter, solid content data are listed 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 reactant liquor solid content≤0.03% entering Distallation systm.As can be seen from Table 1, given four kinds of different solid contents reactant liquor through level Four filter after, solid content is when 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, the method of inactivation curing catalysts is separated in a kind of adiponitrile production process, use the process of level Four backwash filter, the filtrate of the curing catalysts first containing inactivation is entered by the lower side filtrate inlet 7 of pump from one-level backwash filter 1, after the filtration of array filter assemblies 6, supernatant fraction enters upper clear supernate district through filter assemblies, clear liquid area is tray thereabove, clear liquid after filtration and lower floor's filter residue separate, derive from the outlet sequence number 8 of filtrate inlet 7 offside under pressure and Action of Gravity Field, filter residue strong adsorption is on filtration core, filter residue is piled up and is caused filtrate inlet pressure to increase, when pressure is 0.4 ~ 0.48MpaG, filtration fraction completes, close filtrate import, be switched to reserve filter 11, every one-level backwash filter has reserve filter, backwash filter pressure is switched to stand-by equipment when reaching setting value and filters, guarantee reaction proceeds, filter starts cleaning simultaneously, open backwash filter bottom sludge outlet 9, upper clear supernate district passes into nitrogen air blowing pressurization, simultaneously, successively through secondary backwash filter 2, three grades of backwash filters 3, the clear liquid that level Four backwash filter 4 processes returns to clear liquid area and carries out backwash, filter residue is discharged from bottom under pressure and is delivered to collecting tank.
Adopt the process shown in Fig. 1 compared with traditional discontinuous, when the reactant liquor treating capacity containing decaying catalyst is all 10kg/h, the method for the invention is obviously better than discontinuous.
Reaction raw materials involved by adiponitrile production process and intermediate product mostly are the hazardous chemical such as poisonous, inflammable and explosive, all operations requires that isolated air carries out, therefore, select a kind of closed can the device of continued operation and process extremely important, save time and manpower in the obvious advantage, for expanding the scale of production further, improving product quality and yield and providing possibility.
The traditional level Four of table 2 is filtered and is contrasted with the present invention
Above embodiments of the invention have been described in detail, but described content is only preferred embodiment of the present invention, not in order to limit the present invention.All make in application range of the present invention any amendment, equivalent to replace and improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. in an adiponitrile production process, be separated the method for inactivation curing catalysts, it is characterized in that, use the process of level Four backwash filter, the filtrate of the curing catalysts first containing inactivation is entered by the lower side filtrate inlet of pump from one-level backwash filter, after the filtration of array filter assemblies, supernatant fraction enters upper clear supernate district through filter assemblies, derive from the outlet of filtrate inlet offside under pressure and Action of Gravity Field, filter residue strong adsorption is on filtration core, filter residue is piled up and is caused filtrate inlet pressure to increase, when pressure is 0.4 ~ 0.48MpaG, filtration fraction completes, close filtrate import, be switched to reserve filter, open backwash filter bottom sludge outlet, upper clear supernate district passes into nitrogen air blowing pressurization, simultaneously, successively through secondary backwash filter, three grades of backwash filters, the clear liquid of level Four backwash filter process returns to clear liquid area and carries out backwash, filter residue is discharged from bottom under pressure and is delivered to collecting tank.
2. according to the method being separated inactivation curing catalysts in a kind of adiponitrile production process according to claim 1, it is characterized in that, described filter assemblies adopts 10 ~ 20 filter cores to be fixed on the tower tray parts of filter middle and upper part, the mode that filter core adopts spray welding filter element and Wire-wound filter core to combine, filtering accuracy is 1 ~ 10 μm.
3. according to the method being separated inactivation curing catalysts in a kind of adiponitrile production process according to claim 1, it is characterized in that, described each backwash filter is equipped with reserve filter and switches use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN104606946A true CN104606946A (en) | 2015-05-13 |
| CN104606946B CN104606946B (en) | 2016-05-11 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106669279A (en) * | 2017-02-09 | 2017-05-17 | 无锡玖和隆工程科技有限公司 | Filtering equipment for realizing separation of catalyst in production of polytetramethylene ether glycol |
| 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 |
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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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106669279A (en) * | 2017-02-09 | 2017-05-17 | 无锡玖和隆工程科技有限公司 | Filtering equipment for realizing separation of catalyst in production of polytetramethylene ether glycol |
| 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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| Publication number | Publication date |
|---|---|
| CN104606946B (en) | 2016-05-11 |
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