CN103041705B - Device and method for coupling catalyst recovery process with dynamic disc membrane separation process - Google Patents
Device and method for coupling catalyst recovery process with dynamic disc membrane separation process Download PDFInfo
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- CN103041705B CN103041705B CN201210588126.6A CN201210588126A CN103041705B CN 103041705 B CN103041705 B CN 103041705B CN 201210588126 A CN201210588126 A CN 201210588126A CN 103041705 B CN103041705 B CN 103041705B
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Abstract
The invention relates to a device and method for coupling a catalyst recovery process with a dynamic disc membrane separation process. The device comprises a reaction kettle, a rotary device, a recoil tank, a clear liquid tank, a recoil tank feeding pump and a reaction kettle built-in dynamic disc separator body. The whole system is fully-closed, so that other impurities are prevented from being introduced; the cross-flow filtration operation is carried out by the adopted microfiltration or ultrafiltration dynamic disc, so that the permeation flux of the dynamic disc is high and the equipment investment cost is reduced while the technological process is shortened; the discharging effect is stable and the rejection rate of a superfine catalyst reaches more than 99%; the permeation flux recovery rate of the cleaned dynamic disc can reach more than 90%, the cleaning cycle is long, the integration level of a filter-recoil device structure is high, the continuous operation can be performed, and the economic benefit is also increased to a certain extent while the cost is saved; the dynamic disc is resistant to high temperature, acid, alkali and an organic solvent, and can be applied to various reactions; and the dynamic disc is low in running power consumption, small in occupied area and low in requirement on performance stability of feeding liquid.
Description
Technical field
The present invention relates to a kind of device and method, particularly relating to a kind ofly provides a kind of dynamic disc-type film device being applied to catalyst recovery for the defect existing for existing apparatus and technique, equipment rotates feed liquid by video disc and forms relative motion, separative efficiency is high, the device and method that the catalyst recovery overcoming the problem that internal circulating load is large, production cost is high of prior art is coupled with dynamic disc-type membrane separating process.
Background technology
Along with the development of chemical industry, petrochemical iy produced industry, the size of catalyst trends towards fine future development, the heterogeneous efficient separation of solid-liquid becomes very difficulty, traditional separation method such as plate-frame filtering, centrifugation are difficult to product and catalyst to separate completely, not only waste energy consumption, catalyst utilization is low, and catalyst content is too high in the product obtained, affect the quality of product, filter process is often intermittent filtration, be unfavorable for the sustainable development of enterprise from economic aspect, do not meet the call of country about energy-saving and emission-reduction from energy consumption aspect.
In recent years, also get more and more in industries such as petrochemical industry, fine chemistry industry, pharmacy, light industry, environmental protection and relate to micron and nano level solid catalyst, greatly can improve reaction rate, reduce catalyst amount, need this catalyst of separation and recovery after completion of the reaction, but bring difficulty to separation.In molecular sieve catalyst production process, what the generation of washing workshop section was a large amount of contains Catalyst waste water.The current domestic natural sedimentation that adopts reclaims catalyst more, but due to grain diameter little, cause that precipitation apparatus floor space is large, efficiency is low, recovery is incomplete, molecular sieve run off in a large number.Tradition sedimentation is inapplicable; And taking filter cloth as the various types of filtration technology of filter medium, separative efficiency is very low, and filter quality is difficult to ensure; Ultrafiltration centrifuge is extremely low to its separative efficiency of solution that solid content is lower.
The film catalyst filtering technique of current use mainly adopts cross-flow membrane tubular filter mode, needs larger internal circulating load to ensure cross-flow crossflow velocity.And catalyst content is general all lower in course of reaction, the energy consumption that causes of circulating in a large number is high, production cost rising.Meanwhile, it is cracked that a large amount of circulation makes catalyst collide, and causes catalyst loss.
Summary of the invention
For the problems referred to above, main purpose of the present invention is that providing a kind of provides a kind of dynamic disc-type film device being applied to catalyst recovery for the defect existing for existing apparatus and technique, equipment rotates feed liquid by video disc and forms relative motion, be cross-flow filtration, produce shearing force, the catalyst granules being trapped in film surface is pulled away, reduces film surface pollution, thus make film stabilized flux keep constant.Adopt this kind of filter type, do not need high-power pump to provide big cycle volume, solve the separative efficiency of conventional art low, the device and method that the catalyst recovery of the problem that the internal circulating load of prior art is large, production cost is high is coupled with dynamic disc-type membrane separating process.
The present invention solves above-mentioned technical problem by following technical proposals: the device that a kind of catalyst recovery is coupled with dynamic disc-type membrane separating process, and described device comprises reactor, tumbler, recoil tank, Clear liquid tank, recoil tank feed pump, described reactor built-in dynamic disc-type separator main body;
Described reactor has charging aperture and catalyst regeneration outlet, described tumbler and dynamic disc-type separator main body are separately installed with heavy motor and small machine, reactor is connected with Clear liquid tank by a Clear liquid tank charging autocontrol valve, and reactor is connected with recoil tank by a backwash liquid outlet autocontrol valve;
Described recoil tank is connected by the tank feed pump that recoils with Clear liquid tank, between recoil tank and recoil tank feed pump, recoil tank fluid infusion autocontrol valve and the tank feed pump check-valves that recoils also are installed, recoil tank is also connected with the blow-off line of blowdown by recoil tank blowoff valve, the top of recoil tank is also connected with air inlet pipe by recoil tank tonifying Qi autocontrol valve, and the top of recoil tank is also connected with blast pipe by recoil tank atmospheric valve;
The top of described Clear liquid tank is connected with air inlet pipe by Clear liquid tank tonifying Qi autocontrol valve, the top of Clear liquid tank is also connected with blast pipe by Clear liquid tank atmospheric valve, the bottom of Clear liquid tank is connected to the blow-off line of blowdown by Clear liquid tank blowoff valve, Clear liquid tank is also connected with clear liquid inputted subsequent treatment enter follow-up workshop section pipe, enter on follow-up workshop section pipe and Clear liquid tank purified liquor outlet autocontrol valve be installed.
In specific embodiments of the invention, in described dynamic disc-type separator main body, the quantity of dynamic video disc is 1-100 part.
In specific embodiments of the invention, described dynamic disc-type separator main body is dynamic video disc membrane module, and film surface apertures is 7nm ~ 30um, and disc diameter is at 50 ~ 400mm.
One utilizes said apparatus to carry out catalyst recovery and dynamic disc-type membrane separating process coupling process, and described method comprises the steps:
Treating capacity setting device in reactor according to reactant carries out filtration treatment with unit module form two or more sets dynamic disc-type separator main bodies in parallel, product product clear liquid after dynamic disc-type separator main body is separated containing catalyst is separated, catalyst is trapped within reactor and continues reaction, when catalyst needs regeneration, can discharge from the catalyst regeneration outlet bottom reactor.
In specific embodiments of the invention, dynamic disc-type separator main body is ceramic video disc, micro-filtration or the dynamic video disc of ultrafiltration is adopted to be filtered into cross-flow filtration mode, rotarily drive ceramic video disc by motor to rotate, the rotation of ceramic video disc and feed liquid form relative motion, are cross-flow filtration, due to the existence of shearing force, the catalyst granules on the film surface being trapped in dynamic disc-type separator main body is pulled away, reduces film surface pollution, thus make film stabilized flux keep constant.
In specific embodiments of the invention, catalyst recovery process is closed continuous print process.
In specific embodiments of the invention, when the clear liquid flux of setting filter element module drops to the 60%-80% of initial flux, start the dynamic video disc of backwash.
In specific embodiments of the invention, use the material of clear liquid for automatic backwash of filtration in reactor, recoil pressure reduction is 0.1 ~ 0.3MPa, and the recoil time is 1 ~ 60s.
In specific embodiments of the invention, the rotating speed 0 ~ 1000 rev/min of dynamic disc-type separator main body tumbler in filter process.
Positive progressive effect of the present invention is: the present invention and existing similar catalyst reclaim the device that is coupled with dynamic disc-type membrane separating process and technique compares, and whole system of the present invention is totally enclosed type, can not introduce other impurity; The micro-filtration taked or the dynamic video disc cross-flow filtration of ultrafiltration, dynamic video disc permeation flux is high, while shortened process, reduces equipment investment cost; Discharging effect stability, reaches more than 99% to superfine catalyst rejection; Dynamic video disc permeation flux recovery rate after cleaning can reach more than 90%, and the cleaning frequency is long, and the structure-integrated degree of filtration-recoiling device is high, and can carry out continued operation, while cost-saving, economic benefit also improves; Dynamic video disc is high temperature resistant, acid and alkali-resistance, organic solvent-resistant, can be used for all types of reaction; Dynamic video disc operation energy consumption is low, and floor space is little, less demanding to feeding liquid stability.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the Structure and energy flow process of apparatus of the present invention.
Detailed description of the invention
Present pre-ferred embodiments is provided, to describe technical scheme of the present invention in detail below in conjunction with accompanying drawing.
Fig. 1 is the schematic diagram of the Structure and energy flow process of apparatus of the present invention, as shown in Figure 1: the present invention includes reactor 15, tumbler 18, recoil tank 12, Clear liquid tank 3, recoil tank feed pump 11, described reactor 15 built-in dynamic disc-type separator main body 17;
Reactor 15 has charging aperture 151 and catalyst regeneration outlet 152, described tumbler 18 and dynamic disc-type separator main body 17 are separately installed with heavy motor 181 and small machine 171, reactor 15 is connected with Clear liquid tank 3 by a Clear liquid tank charging autocontrol valve 13, and reactor 15 is connected with recoil tank 12 by a backwash liquid outlet autocontrol valve 14;
Recoil tank 12 is connected by the tank feed pump 11 that recoils with Clear liquid tank 3, between recoil tank 12 and recoil tank feed pump 11, recoil tank fluid infusion autocontrol valve 8 and the tank feed pump check-valves 10 that recoils also are installed, recoil tank 12 is also connected with the blow-off line of blowdown by recoil tank blowoff valve 9, the top of recoil tank 12 is also connected with air inlet pipe by recoil tank tonifying Qi autocontrol valve 7, and the top of recoil tank 12 is also connected with blast pipe by recoil tank atmospheric valve 6;
The top of Clear liquid tank 3 is connected with air inlet pipe by Clear liquid tank tonifying Qi autocontrol valve 5, the top of Clear liquid tank 3 is also connected with blast pipe by Clear liquid tank atmospheric valve 4, the bottom of Clear liquid tank 3 is connected to the blow-off line of blowdown by Clear liquid tank blowoff valve 1, Clear liquid tank 3 is also connected with clear liquid inputted subsequent treatment enter follow-up workshop section pipe, enter on follow-up workshop section pipe and Clear liquid tank purified liquor outlet autocontrol valve 2 be installed.
In concrete implementation process, in dynamic disc-type separator main body 17, the quantity of dynamic video disc can elect 1-100 part as.
Described dynamic disc-type separator main body 17 is dynamic video disc membrane module, and film surface apertures is 7nm ~ 30um, and disc diameter is at 50 ~ 400mm.
One utilizes right said apparatus to carry out catalyst recovery and dynamic disc-type membrane separating process coupling process, and the method comprises the steps:
Treating capacity setting device in reactor 15 according to reactant carries out filtration treatment with unit module form two or more sets dynamic disc-type separator main bodies 17 in parallel, product product clear liquid after dynamic disc-type separator main body 17 is separated containing catalyst is separated, catalyst is trapped within reactor 15 and continues reaction, when catalyst needs regeneration, can discharge from the catalyst regeneration outlet 152 bottom reactor 15.
Dynamic disc-type separator main body 17 is ceramic video disc, micro-filtration or the dynamic video disc of ultrafiltration is adopted to be filtered into cross-flow filtration mode, rotarily drive ceramic video disc by motor to rotate, rotation and the feed liquid of pottery video disc form relative motion, be cross-flow filtration, due to the existence of shearing force, the catalyst granules on the film surface being trapped in dynamic disc-type separator main body 17 be pulled away, reduce film surface pollution, thus make film stabilized flux keep constant.
Catalyst recovery process is closed continuous print process.
When the clear liquid flux of setting filter element module drops to the 60%-80% of initial flux, start the dynamic video disc of backwash.
Use the material of clear liquid for automatic backwash of filtration in reactor 15, recoil pressure reduction is 0.1 ~ 0.3MPa, and the recoil time is 1 ~ 60s.
The rotating speed 0 ~ 1000 rev/min of dynamic disc-type separator main body 17 tumbler in filter process.
Here is specific embodiment:
Embodiment: in caprolactam production, oximate process catalyst reclaims
Current domestic use titanium molecular sieve catalysis preparing cyclohexanone oxime by ammoximation of cyclohexanone.The tert-butyl alcohol, ammonia, catalyst react in reactor 15, catalyst concn is 3%, after reacting completely, containing catalyst reactant liquor through ceramic video disc (the dynamic disc-type separator main body 17 in the present invention) be separated after, clear liquid enters Clear liquid tank 3 through Clear liquid tank charging autocontrol valve 13, obtain cyclohexanone oxime through subsequent technique, and then produce caprolactam.Catalyst is trapped within reactor 15 and continues reaction, until need regeneration, needs the catalyst of regeneration recycling after catalyst regeneration outlet 152 is discharged.
Filter process:
Material enters in reactor 15, carries out cyclohexanone oxamidinating reaction and generate cyclohexanone oxime under titanium-silicon molecular sieve catalyst catalysis.Question response contains the reactant liquor of catalyst completely afterwards after ceramic video disc (the dynamic disc-type separator main body 17 in the present invention) is separated, reaction clear liquid enters Clear liquid tank 3 through Clear liquid tank 3 charging autocontrol valve 13, Clear liquid tank 3 liquid level is controlled by Clear liquid tank purified liquor outlet autocontrol valve 2, setting operation pressure reduction is 0.2MPa, revolution 400 revs/min.Catalyst is trapped within reactor 15 and continues reaction, when needs regenerate, go catalyst regeneration system by catalyst regeneration outlet autocontrol valve 16.
Backwash process:
When flux drops to original flux 60-80% in the tank 12 that recoils, use the clear liquid of 1.0-1.5MPa to enter from purified liquor outlet and recoil.Backwash pressure tank is by source of the gas pressurize, and counter-flushing liquid is supplemented by recoil tank feed pump 11 by the clear liquid of Clear liquid tank 3, controls liquid level in recoil tank by recoil tank fluid infusion autocontrol valve 8.
Whole system of the present invention is totally enclosed type, can not introduce other impurity; The micro-filtration taked or the dynamic video disc cross-flow filtration of ultrafiltration, dynamic video disc permeation flux is high, while shortened process, reduces equipment investment cost; Discharging effect stability, reaches more than 99% to superfine catalyst rejection; Dynamic video disc permeation flux recovery rate after cleaning can reach more than 90%, and the cleaning frequency is long, and the structure-integrated degree of filtration-recoiling device is high, and can carry out continued operation, while cost-saving, economic benefit also improves; Dynamic video disc is high temperature resistant, acid and alkali-resistance, organic solvent-resistant, can be used for all types of reaction; Dynamic video disc operation energy consumption is low, and floor space is little, less demanding to feeding liquid stability.
More than show and describe general principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and application claims protection domain is defined by appending claims and equivalent thereof.
Claims (3)
1. catalyst recovery and a dynamic disc-type membrane separating process coupling process, the device of employing comprises reactor (15), tumbler (18), recoil tank (12), Clear liquid tank (3), recoil tank feed pump (11), described reactor (15) built-in dynamic disc-type separator main body (17);
Described reactor (15) has charging aperture (151) and catalyst regeneration outlet (152), described tumbler (18) and dynamic disc-type separator main body (17) are separately installed with heavy motor (181) and small machine (171), reactor (15) is connected with Clear liquid tank (3) by a Clear liquid tank charging autocontrol valve (13), and reactor (15) is connected with recoil tank (12) by backwash liquid outlet autocontrol valve (14);
Described recoil tank (12) is connected by the tank feed pump (11) that recoils with Clear liquid tank (3), between recoil tank (12) and recoil tank feed pump (11), recoil tank fluid infusion autocontrol valve (8) and the tank feed pump check-valves (10) that recoils also are installed, recoil tank (12) is also connected with the blow-off line of blowdown by recoil tank blowoff valve (9), the top of recoil tank (12) is also connected with air inlet pipe by recoil tank tonifying Qi autocontrol valve (7), the top of recoil tank (12) is also connected with blast pipe by recoil tank atmospheric valve (6),
The top of described Clear liquid tank (3) is connected with air inlet pipe by Clear liquid tank tonifying Qi autocontrol valve (5), the top of Clear liquid tank (3) is also connected with blast pipe by Clear liquid tank atmospheric valve (4), the bottom of Clear liquid tank (3) is connected to the blow-off line of blowdown by Clear liquid tank blowoff valve (1), Clear liquid tank (3) is also connected with clear liquid inputted subsequent treatment enter follow-up workshop section pipe, enter on follow-up workshop section pipe and Clear liquid tank purified liquor outlet autocontrol valve (2) is installed
In described dynamic disc-type separator main body (17), the quantity of dynamic video disc is 1-100 part,
Described dynamic disc-type separator main body (17) is dynamic video disc membrane module, and film surface apertures is 7nm ~ 30 μm, and disc diameter, at 50 ~ 400mm, is characterized in that: described method comprises the steps:
Treating capacity setting device in reactor (15) according to reactant carries out filtration treatment with unit module form two or more sets dynamic disc-type separator main bodies (17) in parallel, product product clear liquid after dynamic disc-type separator main body (17) is separated containing catalyst is separated, catalyst is trapped within reactor (15) and continues reaction, when catalyst needs regeneration, can discharge from catalyst regeneration outlet (152) of reactor (15) bottom, when the clear liquid flux of setting filter element module drops to the 60%-80% of initial flux, start the dynamic video disc of backwash, the material that the clear liquid filtered is automatic backwash is used in reactor (15), recoil pressure reduction is 0.1 ~ 0.3MPa, the recoil time is 1 ~ 60s, the rotating speed 0 ~ 1000 rev/min of dynamic disc-type separator main body (17) tumbler in filter process.
2. catalyst recovery according to claim 1 and dynamic disc-type membrane separating process coupling process, it is characterized in that: dynamically disc-type separator main body (17) is ceramic video disc, micro-filtration or the dynamic video disc of ultrafiltration is adopted to be filtered into cross-flow filtration mode, rotarily drive ceramic video disc by motor to rotate, rotation and the feed liquid of pottery video disc form relative motion, be cross-flow filtration, due to the existence of shearing force, the catalyst granules on the film surface being trapped in dynamic disc-type separator main body (17) is pulled away, reduce film surface pollution, thus make film stabilized flux keep constant.
3. catalyst recovery according to claim 1 and dynamic disc-type membrane separating process coupling process, is characterized in that: catalyst recovery process is closed continuous print process.
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| CN106166471A (en) * | 2016-08-11 | 2016-11-30 | 爱森（中国）絮凝剂有限公司 | The chemical reaction device that a kind of band catalyst reclaims |
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Address after: 201201 Shanghai, Pudong New Area Jin Tang Road, No. 2, block B, 145 Patentee after: SHANGHAI ANHORN ENVIRONMENTAL TECHNOLOGY CO., LTD. Address before: 201201 Shanghai, Pudong New Area Jin Tang Road, No. 2, block B, 145 Patentee before: Shanghai Anhorn Mechanical Equipment Co., Ltd. |