CN201988375U - Cyclohexanone ammonia oximation reaction catalyst separation device - Google Patents

Cyclohexanone ammonia oximation reaction catalyst separation device Download PDF

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Publication number
CN201988375U
CN201988375U CN2011200548732U CN201120054873U CN201988375U CN 201988375 U CN201988375 U CN 201988375U CN 2011200548732 U CN2011200548732 U CN 2011200548732U CN 201120054873 U CN201120054873 U CN 201120054873U CN 201988375 U CN201988375 U CN 201988375U
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filter
reaction
built
catalyst
distributor
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Expired - Lifetime
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CN2011200548732U
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Chinese (zh)
Inventor
张玉新
赵承军
魏佩显
王庆响
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Hebei Mei Bang engineering science and technology limited-liability company
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HEBEI MEIBANG ENGINEERING TECHNOLOGY Co Ltd
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Abstract

The utility model discloses a cyclohexanone ammonia oximation reaction catalyst separation device which comprises a reaction tank body provided with a built-in filter, wherein the inner bottom of the reaction tank body is provided with a material inlet distributor, and the top of the reaction tank body is provided with a material circulating distributor, and the device is characterized in that the clear liquid outlet of the built-in filter is connected with the inlet of an external filter, and the outlet of the external filter is connected with a storage tank. The bore diameter of a filter membrane pipe ranges from 0.05 micron to 1 micron. The bore diameter of an external filter membrane pipe ranges from 0.01 micron to 0.05 micron. The material distributor and the material circulating distributor have an annular pipe structure respectively, and distributed holes are arranged on the annular pipe. As the built-in filter and the external filter are adopted by a catalytic reaction device for filtering by steps, catalyst leaking phenomenon during the running process of the filters is avoided, the safety is improved, the filtering area of the filters is reduced, the equipment investment is lowered, the energy consumption during reaction and catalyst running is reduced, the catalyst separating flow is simplified, and the cyclohexanone ammonia oximation reaction catalyst separation device has the characteristics of simple separation process, long equipment running period, reasonable reaction heat utilization and the like.

Description

A kind of cyclohexanone oxamidinating catalysts separator
Technical field
The utility model relates to a kind of Ammoximation reaction device of heterogeneous suspension catalystic converter system.
Background technology
Cyclohexanone oxime is an a kind of important intermediate of producing caprolactam, is made by hydroxylamine salt and cyclohexanone generation oximation reaction, and the cyclohexanone oxime of generation obtains caprolactam through Beckmann rearrangement again.At present, the method for preparing cyclohexanone oxime mainly contains Raschig process (HSO), NO catalytic reduction method (NO method), phosphatic hydroxylamine method (HPO), cyclohexanone oxamidinating method (HAO).The sulphur ammonium of HSO method, NO method complex process and by-product low value wherein; Though the HPO method is by-product sulphur ammonium not, technical process requires meticulous, and operation easier is big, and has NOx to produce, and has an environmental protection difficult problem.Have the problem that the amidoxime method has overcome above-mentioned three aspects only, the preparation method is simple, by-product sulphur ammonium not, and therefore a no environmental protection difficult problem quite is subjected to the favor of caprolactam industry in recent years.
The amidoxime legal system is equipped with cyclohexanone oxime at first by the invention of Italian ENI company, and at first set up and produce 10000 tons amidoxime experimental rig per year in Italy, built up in Japan in 2003 and produce 60000 tons amidoxime chemical industry device per year, the domestic amidoxime chemical industry device of producing 70000 tons per year and producing 100000 tons per year that also built up respectively.
From the present domestic amidoxime chemical industry device ruuning situation of building up, all there are some problems.Behind Ammoximation reaction, product need be transported to carries out separating of cyclohexanone oxime and catalyst in the filter, and filter needs regular online regeneration and irregular regenerated offline, and the cycle of operation is short; Simultaneously, for guaranteeing the tangent line linear speed of filter, reactor material self-loopa amount is bigger, has increased energy consumption, and in the filter running, also is prone to the catalyst leakage phenomenon.Because catalyst interception rate is had relatively high expectations, the filter area of filter is bigger, and the filter apparatus investment is bigger.This shows that at present the Ammoximation reaction separation equipment has drawbacks such as separation process complexity, utilization of Heat of Reaction are unreasonable.
In sum, for solving all difficult problems in the caprolactam production process amidoxime chemical industry preface, energy savings reduces production costs, and amidoxime chemical industry device is improved, and is to reduce caprolactam production cost urgent problem.
The utility model content
The utility model is at the deficiency of existing Ammoximation reaction technology, Ammoximation reaction device and catalysts thereof separated improve, and adopts connect with the external filter mode of cascade filtration of built-in filter to carry out catalyst separation.
For realizing the utility model purpose, this cyclohexanone oxamidinating catalysts separator comprises the reacting tank body that is equiped with built-in filter, the reacting tank body inner bottom part is provided with the raw material feed distributor, the top is provided with the recycle stock distributor, it is characterized in that described built-in filter purified liquor outlet connects external filter inlet, external filter outlet connects storage tank.
Described built-in filter film pore directly is 0.05~1 μ m.
Described external filter film tube aperture is 0.01~0.05 μ m.
Described feed distribution device and recycle stock distributor are respectively the endless tube structure, have the distribution hole on the endless tube.
The technological progress that the utility model is obtained: because the catalyst reaction device that adopts built-in and external filter to filter step by step, avoided the catalyst leakage phenomenon in the filter running, increased security, reduced the filter area of filter, reduced equipment investment, reduce the energy consumption of reaction and catalyst operation, simplified the flow process of catalyst separation, and had characteristics such as separation process is simple, the equipment cycle of operation is long, utilization of Heat of Reaction is reasonable.
Description of drawings
Fig. 1 is the utility model structural representation.
Fig. 2 is a reacting tank body structural representation among Fig. 1.
Fig. 3 is the vertical view of Fig. 2.
The specific embodiment
As Fig. 1, Fig. 2, shown in Figure 3, the utility model cyclohexanone oxamidinating catalysts separator comprises the reacting tank body 2 that is equiped with built-in filter 3, reacting tank body 2 inner bottom parts are provided with raw material feed distributor 8, the top is provided with recycle stock distributor 7, feed distribution device 8 and recycle stock distributor 7 are the endless tube structure, all have the distribution hole on endless tube.The purified liquor outlet of built-in filter 3 connects the inlet of external filter 4, and the outlet of external filter 4 connects storage tank 5.The film pore of built-in filter 3 directly is 0.05~1 μ m, and the film pore of the built-in filter 3 of present embodiment directly is 0.08 μ m; The film pore of external filter 4 directly is 0.01~0.05 μ m, and the film pore of the external filter 4 of present embodiment directly is 0.03 μ m.
The utility model technical process is: reaction raw materials, solvent tertiary butanol and enter respectively in the reacting tank body 2 that contains catalyst and reaction mass after mixed fast and raw material feed distributor 8 and recycle stock distributor 7 distribute through blender 1 at the reactor inlet pipeline from the recycle stock of reactor, under the effect of agitator 6, carry out Ammoximation reaction then, reacted reaction mass directly is that the built-in filter 3 of 0.05~1 μ m is carried out the one-level coarse filtration by reacting tank body 2 inner membrance pores, the suspended state catalyst that filters is trapped within and continues to participate in reaction in the outer reacting tank body of filter assemblies 2, it directly is that the external filter 4 of 0.01~0.05 μ m further filters that the filtrate of containing a certain amount of catalyst enters the film pore, filtrate after catalyst granules further is trapped enters in the storage tank 5, finish the separation of catalyst, the catalyst that cascade filtration is trapped turns back to blender 1 and advances into and participate in catalytic reaction in the reacting tank body 2 once more.

Claims (4)

1. cyclohexanone oxamidinating catalysts separator, it comprises the reacting tank body that is equiped with built-in filter, the reacting tank body inner bottom part is provided with the raw material feed distributor, the top is provided with the recycle stock distributor, it is characterized in that the built-in filter purified liquor outlet connects external filter inlet, external filter outlet connects storage tank.
2. cyclohexanone oxamidinating catalysts separator according to claim 1 is characterized in that described built-in filter film pore directly is 0.05~1 μ m.
3. cyclohexanone oxamidinating catalysts separator according to claim 1 is characterized in that described external filter film tube aperture is 0.01~0.05 μ m.
4. according to claim 1,2 or 3 described cyclohexanone oxamidinating catalysts separators, it is characterized in that described feed distribution device and recycle stock distributor are respectively the endless tube structure, have the distribution hole on the endless tube.
CN2011200548732U 2011-03-04 2011-03-04 Cyclohexanone ammonia oximation reaction catalyst separation device Expired - Lifetime CN201988375U (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
CN2011200548732U CN201988375U (en) 2011-03-04 2011-03-04 Cyclohexanone ammonia oximation reaction catalyst separation device

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012152600A1 (en) * 2011-05-09 2012-11-15 Versalis S.P.A. Ammoximation reactor for cyclohexanone oxime production
CN102838510A (en) * 2012-09-07 2012-12-26 福建锦江石化有限公司 Method and device for filtering and separating reaction system catalyst for preparing cyclohexanone-oxime
CN103214393A (en) * 2013-04-27 2013-07-24 湖南百利工程科技股份有限公司 Oximation method of ketone
CN103521142A (en) * 2013-11-05 2014-01-22 浙江华亿工程设计有限公司 Equipment and method for applying catalyst circularly and downwards
US8927770B2 (en) 2011-05-10 2015-01-06 Salpem, S.P.A. High-yield process for the synthesis of urea

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012152600A1 (en) * 2011-05-09 2012-11-15 Versalis S.P.A. Ammoximation reactor for cyclohexanone oxime production
US10525429B2 (en) 2011-05-09 2020-01-07 Versalis S.P.A. Ammoximation reactor for cyclohexanone oxime production
US8927770B2 (en) 2011-05-10 2015-01-06 Salpem, S.P.A. High-yield process for the synthesis of urea
CN102838510A (en) * 2012-09-07 2012-12-26 福建锦江石化有限公司 Method and device for filtering and separating reaction system catalyst for preparing cyclohexanone-oxime
CN102838510B (en) * 2012-09-07 2015-05-27 福建锦江石化有限公司 Method and device for filtering and separating reaction system catalyst for preparing cyclohexanone-oxime
CN103214393A (en) * 2013-04-27 2013-07-24 湖南百利工程科技股份有限公司 Oximation method of ketone
CN103214393B (en) * 2013-04-27 2014-08-20 湖南百利工程科技股份有限公司 Oximation method of ketone
CN103521142A (en) * 2013-11-05 2014-01-22 浙江华亿工程设计有限公司 Equipment and method for applying catalyst circularly and downwards
CN103521142B (en) * 2013-11-05 2015-05-27 浙江华亿工程设计有限公司 Equipment and method for applying catalyst circularly and downwards

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C56 Change in the name or address of the patentee
CP03 Change of name, title or address

Address after: 12, building 050035, Yee Yee building, 98 the Yellow River Avenue, Hebei, Shijiazhuang

Patentee after: Hebei Mei Bang engineering science and technology limited-liability company

Address before: 050035 construction hi tech international 17L, 9 Changjiang Road, Shijiazhuang, Hebei

Patentee before: Hebei Meibang Engineering Technology Co., Ltd.

CX01 Expiry of patent term

Granted publication date: 20110928

CX01 Expiry of patent term