CN202962433U - Ammoximation reactor - Google Patents

Ammoximation reactor Download PDF

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Publication number
CN202962433U
CN202962433U CN 201220696701 CN201220696701U CN202962433U CN 202962433 U CN202962433 U CN 202962433U CN 201220696701 CN201220696701 CN 201220696701 CN 201220696701 U CN201220696701 U CN 201220696701U CN 202962433 U CN202962433 U CN 202962433U
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filter
reaction
outlet
ammoximation
reaction unit
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赵承军
赵云
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Hangzhou Xiangyun Chemical Co ltd
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DONGMING TIANJUN CHEMICAL Co Ltd
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Abstract

The utility model discloses an ammoximation reactor. The ammoximation reactor is characterized by comprising a reaction device (1) and a filtering device (2), wherein the reaction device (1) comprises a reactor, a raw material inlet (11), a product outlet (12) and a hollow guide cylinder (13); the raw material inlet (11) and the product outlet (12) are formed on the reactor; the hollow guide cylinder (13) is arranged in the reactor; the product outlet (12) is communicated with the filtering device (2); the hollow guide cylinder (13) is provided with a cooling medium inlet (14) and a cooling medium outlet (15); and the cooling medium inlet (14) and the cooling medium outlet (15) are both communicated with the outside. The ammoximation reactor disclosed by the utility model is not easy to block and is easy to clean.

Description

A kind of Ammoximation reaction device
Technical field
The utility model relates to a kind of Ammoximation reaction device.
Background technology
Cyclohexanone oxime is the key intermediate of synthetic Caprolactam, is a kind of important industrial chemicals, mainly as the raw material of raw material nylon 6 monomers that prepare fiber and nylon 6 and engineering plastics.At present, cyclohexanone oxime mainly utilizes cyclohexanone oxamidinating to react to prepare, and its course of reaction is as follows:
Figure BDA00002588807800011
The standby cyclohexanone oxime of cyclohexanone oxamidinating legal system is proposed by Italian ENI company the earliest.So far successively built up nearly 10 cover commercial plants in Japan and China, total productive capacity is near 1,000,000 tons.All there are some problems in commercial plant ruuning situation from building up both at home and abroad at present.Be built-in as existing catalyst separation device, that is, be built in reaction kettle body.After oximation reaction is completed, directly product is separated with solid catalyst.Yet built-in catalyst separation device easily stops up, and therefore needing stops production completely cleans and keep in repair, and not only treatment cycle is longer, and numerous and diverse and dangerous.
In addition, from the present domestic amidoxime chemical industry device ruuning situation of building up, also there is the problem that reaction temperature is wayward and reaction heat can not take full advantage of.For example, because Ammoximation reaction is exothermic reaction, in course of reaction, obvious rising may appear in temperature, thereby makes reaction temperature wayward under optimal reaction temperature and impact reaction.In addition, also caused the loss of this part reaction heat.This shows, at present amidoxime chemical industry device has the separation process complexity, reaction temperature is wayward and reaction heat such as can not take full advantage of at the drawback.Therefore, amidoxime chemical industry device being improved, is to reduce urgent problem in the Caprolactam production process.
The utility model content
The purpose of this utility model is in order to solve that existing Ammoximation reaction device easily stops up and the defective of easy cleaning not, and the Ammoximation reaction device that a kind of difficult obstruction is provided and easily cleans.
The utility model provides a kind of Ammoximation reaction device, wherein, described Ammoximation reaction device comprises reaction unit and filter, described reaction unit comprises reaction kettle body, is arranged on feed(raw material)inlet and the product outlet on reaction kettle body and is arranged on the interior hollow flow-guiding cylinder of reaction kettle body, the product outlet of described reaction kettle body is communicated with described filter, described hollow flow-guiding cylinder comprises cooling medium entrance and cooling medium outlet, and described cooling medium entrance and cooling medium outlet all are in communication with the outside.
Preferably, described filter comprises built-in film pipe filter, purified liquor outlet and the outlet of turbid liquid, and described turbid liquid outlet is arranged on the bottom of described filter and is communicated with the circulation fluid entrance at described reaction unit top by circulating pump.
Preferably, described film pipe filter is metal film pipe filter and/or ceramic-film tube filter; The bore dia of described metal film pipe filter is 0.1 μ m-10 μ m; The bore dia of described ceramic-film tube filter is 10nm-10 μ m.
Preferably, the quantity of described filter is 2-12; The quantity of the film pipe filter that arranges in each filter is 2-5 independently of one another.
Preferably, take the height H of described reaction unit as benchmark, the distance at the top of described hollow flow-guiding cylinder and the top of described reaction unit is 1/4H-1/3H; The distance of the bottom of described hollow flow-guiding cylinder and the bottom of described reaction unit is 1/5H-1/4H.
Preferably, described hollow flow-guiding cylinder is suspended on the center of described reaction unit by supporter.
Preferably, described reaction unit also comprises the circulation fluid outlet that is arranged on described reaction unit bottom, and described circulation fluid outlet is communicated with described circulation fluid entrance by circulating pump.
Preferably, described reaction unit also comprises the first distributor and the second distributor, and described the first distributor is communicated with the feed(raw material)inlet, and described the second distributor is communicated with the circulation fluid entrance.
Inventor of the present utility model finds, existing filter directly is placed in reaction kettle body, and the reaction in described reaction kettle body is normally carried out under the condition that stirs, thereby has increased the probability that described oximate catalyst contacts with filter, makes filter be easy to stop up.In addition, it is very inconvenient that described filter is cleaned, and needs to stop completely, thereby caused the waste of device resource and increased production cost.And the filter that the utility model provides is external, is not easy to stop up.This is because: the product that will contain the oximate catalyst is introduced when carrying out the separating of product and oximate catalyst in the filter of external, to carry out under the state that does not stir, described oximate catalyst is due to the bottom that has larger density and be easy to be deposited in filter, therefore, can reduce the probability that contacts with filter, thereby make filter be difficult for stopping up.In addition, because filter of the present utility model is external, easily clean.Described reaction unit also comprises the hollow flow-guiding cylinder that comprises cooling medium entrance and cooling medium outlet that is arranged in reaction kettle body, described cooling medium entrance and cooling medium outlet all are in communication with the outside, at this moment, can be when amount of heat be emitted in reaction, pass into cooling medium in the hollow flow-guiding cylinder, thereby reaction temperature not only can be maintained comparatively stable level, can also take full advantage of reaction heat cooling medium is heated, realize taking full advantage of of reaction heat.
According to a kind of preferred embodiment of the present utility model, when the quantity of described filter is 2-12, can also realizes in the situation that do not stop and clean in turn, thereby reduce the loss of stopping.
Other feature and advantage of the present utility model will partly be described in detail in the specific embodiment subsequently.
Description of drawings
Accompanying drawing is to be used to provide further understanding of the present utility model, and consists of the part of specification, is used from explanation the utility model with the following specific embodiment one, but does not consist of restriction of the present utility model.In the accompanying drawings:
Fig. 1 is the structural representation according to the Ammoximation reaction device of a kind of specific embodiment of the present utility model;
Fig. 2 is the structural representation according to the reaction unit of a kind of specific embodiment of the present utility model.
Description of reference numerals
The 1-reaction unit; The 11-feed(raw material)inlet; The outlet of 12-product; 13-hollow flow-guiding cylinder; 14-cooling medium entrance; The outlet of 15-cooling medium; 16-circulation fluid entrance; The outlet of 17-circulation fluid; The 18-agitator; The 19-motor; 110-the first distributor; 111-the second distributor; The 2-filter; 21-film pipe filter; The 22-purified liquor outlet; The turbid liquid outlet of 23-; The 24-clean-up line; The 3-circulating pump
The specific embodiment
Below the specific embodiment of the present utility model is elaborated.Should be understood that, the specific embodiment described herein only is used for description and interpretation the utility model, is not limited to the utility model.
In the utility model, in the situation that do not do opposite explanation, the noun of locality that uses typically refers to reaction unit 1 of the present utility model and the direction of filter 2 under working condition, the namely direction shown in accompanying drawing as " upper and lower, left and right, the end, top ".
As shown in Figure 1, the Ammoximation reaction device that the utility model provides comprises reaction unit 1 and filter 2, described reaction unit 1 comprises reaction kettle body, is arranged on feed(raw material)inlet 11 and product outlet 12 on reaction kettle body, and described product outlet 12 is communicated with described filter 2.
Wherein, the kind of described reaction unit 1 can be selected for the routine of this area, usually with agitator.That is, as shown in Figure 1, described reaction unit 1 comprises motor 19 and the agitator 18 that is connected with motor, raw material can be mixed more equably like this, and the even distribution of heat in more favourable whole reaction system, thereby make reacting balance ground carry out.In addition, because Ammoximation reaction may carry out at higher temperature, therefore, described reaction unit 1 also comprises heating element heater.Described heating element heater usually can be for being arranged on the heating jacket of reaction kettle body outside.
According to the utility model, above-mentioned Ammoximation reaction device is being used for the process of amidoxime production, Ammoximation reaction material such as cyclohexanone, ammonia, hydrogen peroxide or aqueous hydrogen peroxide solution (being hydrogen peroxide) and oximate catalyst are introduced in reaction kettle body by feed(raw material)inlet 11 continuously, complete reaction under the Ammoximation reaction condition after, the product that obtains is introduced in filters 2 continuously by described product outlet 12, with most of product and oximate catalyst separation.Wherein, described feed(raw material)inlet 11 and product outlet 12 optional positions that can be arranged on reaction kettle body, but in order to make reaction more abundant, under preferable case, as shown in Figure 1, described feed(raw material)inlet 11 is arranged on the bottom of reaction kettle body, and described product outlet 12 is arranged on the sidewall of described reaction kettle body, and take the total height L of described reaction kettle body as benchmark, described product outlet 12 is arranged on apart from the position of reaction kettle body bottom 1/3L-2/3L.
Preferably, described filter 2 comprises built-in film pipe filter 21, purified liquor outlet 22 and turbid liquid outlet 23, and described turbid liquid outlet 23 is arranged on the bottoms of described filter 2 and is communicated with the circulation fluid entrance 16 at described reaction unit 1 top by circulating pump 3.
In one embodiment, filter 2 can be upper and lower two parts by baffle for separating, and these two parts only end of logical filmed passing tube filter 21 are communicated with, and wherein, film pipe filter 21 is arranged on the bottom, and reaction unit 1 is communicated with the bottom of filter 2; The top of described dividing plate and filter 2 consists of stillness of night collecting zone, and described purified liquor outlet 22 is arranged on sidewall or the top of described stillness of night collecting zone.
As a rule, described film pipe filter 21 is enclosed construction, its membrane structure allow liquid material by and do not allow solid shape material to pass through.The product of Ammoximation reaction is liquid, and the oximate catalyst is the solid shape.The product that will contain the oximate catalyst exports 12 continuous introducings by product and is built-in with in the filter 2 of film pipe filter 21, liquid product can penetrate in film pipe filter 21 at an easy rate, and enter the clear liquid collecting region that is positioned at filter 2 tops, and then draw continuously by purified liquor outlet 22; It is outer and be circulated back in reaction unit 1 by the turbid liquid outlet 23 that is arranged on described filter 2 bottoms that the oximate catalyst of solid shape is blocked in described film pipe filter 21, to realize the recycling of oximate catalyst.
The kind of described film pipe filter 21 can be selected for the routine of this area, for example, can be metal film pipe filter and/or ceramic-film tube filter.Wherein, the particle diameter of the oximate catalyst that the bore dia of above-mentioned film pipe filter can use according to reality is reasonably selected, and for example, the bore dia of described metal film pipe filter can be for 0.1 μ m-10 μ m, be preferably 0.3 μ m-3 μ m.The bore dia of described ceramic-film tube filter can be for 10nm-10 μ m, be preferably 50nm-5 μ m.In addition, the quantity of the described film pipe filter 21 that arranges in each filter 2 also can reasonably be selected according to actual conditions, can for one or more, be preferably 2-5.Can be communicated with, also can not be communicated with between a plurality of film pipe filters 21.
Preferably, described filter 2 also comprises clean-up line 24, and the entrance of described clean-up line 24 is arranged on sidewall or the top of described filter 2, can realize so described filter 2 is carried out on-line cleaning.In one embodiment, as mentioned above, filter 2 is upper and lower two parts by baffle for separating, these two parts only end of logical filmed passing tube filter 21 are communicated with, reaction unit 1 is communicated with the bottom of filter 2, the top of described dividing plate and filter 2 consists of stillness of night collecting zone, and at this moment, the entrance of described clean-up line 24 can be arranged on sidewall or the top of described stillness of night collecting zone.
Preferably, the quantity of described filter 2 is 2-12.Need to prove, 2-12 filter 2 is communicated with respectively at reaction unit 1.Can realize like this in the situation that do not stop described filter 2 is cleaned in turn, thereby reduce the loss of stopping.
Preferably, described reaction unit 1 also comprises the built-in hollow flow-guiding cylinder 13 that comprises cooling medium entrance 14 and cooling medium outlet 15, and described cooling medium entrance 14 and cooling medium outlet 15 all are in communication with the outside.Wherein, described cooling medium entrance 14 is in communication with the outside to typically refer to the cooling medium source and is communicated with, and described cooling medium outlet 15 is in communication with the outside to typically refer to the cooling medium collector and is communicated with.
The utility model is not particularly limited the shape of described hollow flow-guiding cylinder 13, can be existing various shapes, for example, cylindrical, arc, star etc., but in order to increase the contact area of itself and kettle internal reaction material, described hollow flow-guiding cylinder 13 is for having the cannula-like of hollow tube wall.At this moment, described cooling medium entrance 14 and cooling medium outlet 15 all are arranged on the tube wall of sleeve pipe, described cooling medium after carrying out heat exchange with described reaction system, is drawn from cooling medium outlet 15 in the hollow tube wall of the hollow flow-guiding cylinder 13 of cooling medium entrance 14 lead-in bushing shapes.
Preferably, the ratio of the volume of the volume of described hollow flow-guiding cylinder 13 and reaction unit 1 is 1/8-1/3:1, more preferably 1/6-1/4:1.
Preferably, the wall thickness of described hollow flow-guiding cylinder 13 is 0.2-2 centimetre, more preferably 0.5-1 centimetre, so not only can avoid because the too thick heat exchange that causes of wall thickness is insufficient, but also can avoid due to the inadequate problem of the too thin mechanical strength that causes of wall thickness.
Preferably, take the height H of described reaction unit 1 as benchmark, the distance at the top of the top of described hollow flow-guiding cylinder 13 and described reaction unit 1 is 1/4H-1/3H; The distance of the bottom of the bottom of described hollow flow-guiding cylinder 13 and described reaction unit 1 is 1/5H-1/4H.
Preferably, described hollow flow-guiding cylinder 13 is suspended on the center of described reaction unit 1 by supporter.In the process of Ammoximation reaction, the oximate catalyst of part solid shape can be deposited on the bottom of reaction kettle body, in order to make this part oximate catalyst to react by attend fully, preferably, described reaction unit 1 also comprises the circulation fluid outlet 17 that is arranged on described reaction unit 1 bottom, the outlet 17 of described circulation fluid is communicated with described circulation fluid entrance 16 by circulating pump 3, can return to reaction unit 1 and be dispersed in that in reaction system, sustainable participation reacts being deposited on oximate catalyst bottom reaction kettle body like this.
According to the utility model, in order to make material to mix more equably, preferably, as shown in Figure 2, described reaction unit 1 also comprises the first distributor 110 and the second distributor 111, described the first distributor 110 is communicated with feed(raw material)inlet 11, and described the second distributor 111 is communicated with circulation fluid entrance 16.Wherein, described the first distributor 110 and the second distributor 111 can be fastened in reaction kettle body by any-mode, for example, can be connected on the reaction kettle body inwall by supporter.
The kind of described the first distributor 110 and the second distributor 111 can be selected for the routine of this area, for example, can be calandria distributor, annular tube type distributor, porose disc formula distributor, weir disc type distributor etc. independently of one another.
More than describe preferred embodiment of the present utility model in detail; but; the utility model is not limited to the detail in above-mentioned embodiment; in technical conceive scope of the present utility model; can carry out multiple simple variant to the technical solution of the utility model, these simple variant all belong to protection domain of the present utility model.
Need to prove that in addition each the concrete technical characterictic described in the above-mentioned specific embodiment in reconcilable situation, can make up by any suitable mode.For fear of unnecessary repetition, the utility model is to the explanation no longer separately of various possible combinations.
In addition, also can carry out any combination between various embodiment of the present utility model, as long as it is without prejudice to thought of the present utility model, it should be considered as content disclosed in the utility model equally.

Claims (9)

1. Ammoximation reaction device, it is characterized in that, described Ammoximation reaction device comprises reaction unit (1) and filter (2), described reaction unit (1) comprises reaction kettle body, be arranged on feed(raw material)inlet (11) and the product outlet (12) on reaction kettle body and be arranged on the interior hollow flow-guiding cylinder (13) of reaction kettle body, the product outlet (12) of described reaction kettle body is communicated with described filter (2), described hollow flow-guiding cylinder (13) comprises cooling medium entrance (14) and cooling medium outlet (15), described cooling medium entrance (14) and cooling medium outlet (15) all are in communication with the outside.
2. Ammoximation reaction device according to claim 1, it is characterized in that, described filter (2) comprises built-in film pipe filter (21), purified liquor outlet (22) and turbid liquid outlet (23), and described turbid liquid outlet (23) is arranged on the bottom of described filter (2) and is communicated with the circulation fluid entrance (16) at described reaction unit (1) top by circulating pump (3).
3. Ammoximation reaction device according to claim 2, is characterized in that, described film pipe filter (21) is metal film pipe filter and/or ceramic-film tube filter; The bore dia of described metal film pipe filter is 0.1 μ m-10 μ m; The bore dia of described ceramic-film tube filter is 10nm-10 μ m.
4. according to claim 2 or 3 described Ammoximation reaction devices, is characterized in that, the quantity of described filter (2) is 2-12; The quantity of the film pipe filter (21) that arranges in each filter (2) is 2-5 independently of one another.
5. according to claim 1,2 or 3 described Ammoximation reaction devices, is characterized in that, take the height H of described reaction unit (1) as benchmark, the distance at the top of the top of described hollow flow-guiding cylinder (13) and described reaction unit (1) is 1/4H-1/3H; The distance of the bottom of the bottom of described hollow flow-guiding cylinder (13) and described reaction unit (1) is 1/5H-1/4H.
6. Ammoximation reaction device according to claim 5, is characterized in that, described hollow flow-guiding cylinder (13) is suspended on the center of described reaction unit (1) by supporter.
7. according to claim 1,2 or 3 described Ammoximation reaction devices, it is characterized in that, described reaction unit (1) also comprises the circulation fluid outlet (17) that is arranged on described reaction unit (1) bottom, and described circulation fluid outlet (17) is communicated with described circulation fluid entrance (16) by circulating pump (3).
8. Ammoximation reaction device according to claim 7, it is characterized in that, described reaction unit (1) also comprises the first distributor (110) and the second distributor (111), described the first distributor (110) is communicated with feed(raw material)inlet (11), and described the second distributor (111) is communicated with circulation fluid entrance (16).
9. according to claim 2 or 3 described Ammoximation reaction devices, is characterized in that, described filter (2) also comprises clean-up line (24), and the arrival end of described clean-up line (24) is arranged on sidewall or the top of described filter (2).
CN 201220696701 2012-12-14 2012-12-14 Ammoximation reactor Expired - Lifetime CN202962433U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104001461A (en) * 2014-04-24 2014-08-27 金华精锐制药机械有限公司 Detachable multifunctional kettle internal jacket easy to clean
CN105268389A (en) * 2014-06-26 2016-01-27 东至天孚化工有限公司 Shock-absorbing rotary heating reaction kettle

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104001461A (en) * 2014-04-24 2014-08-27 金华精锐制药机械有限公司 Detachable multifunctional kettle internal jacket easy to clean
CN105268389A (en) * 2014-06-26 2016-01-27 东至天孚化工有限公司 Shock-absorbing rotary heating reaction kettle

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Effective date of registration: 20160920

Address after: 310000, room 532, 325 Shiqiao Road, Xiacheng District, Zhejiang, Hangzhou

Patentee after: Hangzhou Xiangyun Chemical Co.,Ltd.

Address before: 274500 west section of 38 Road, Dongming County, Shandong, Heze

Patentee before: DONGMING TIANJUN CHEMICAL Co.,Ltd.

CX01 Expiry of patent term
CX01 Expiry of patent term

Granted publication date: 20130605