CN108569704A - A kind of Zeolite synthesis equipment - Google Patents

A kind of Zeolite synthesis equipment Download PDF

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Publication number
CN108569704A
CN108569704A CN201710139429.2A CN201710139429A CN108569704A CN 108569704 A CN108569704 A CN 108569704A CN 201710139429 A CN201710139429 A CN 201710139429A CN 108569704 A CN108569704 A CN 108569704A
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CN
China
Prior art keywords
reaction kettle
mother liquor
hydrothermal reaction
zeolite synthesis
synthesis equipment
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710139429.2A
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Chinese (zh)
Inventor
宋兰兰
于跃
王绍著
郭川
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Linyi University
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Linyi University
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Publication date
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Priority to CN201710139429.2A priority Critical patent/CN108569704A/en
Publication of CN108569704A publication Critical patent/CN108569704A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/006Processes utilising sub-atmospheric pressure; Apparatus therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B37/00Compounds having molecular sieve properties but not having base-exchange properties
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/129Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Materials Engineering (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The present invention relates to a kind of Zeolite synthesis equipment, including hydrothermal reaction kettle and condensing plant, hydrothermal reaction kettle top is equipped with steam port and is connect with condensing plant, and connecting pipe is equipped with solenoid valve.Condensing plant is made of condenser and Liquid acquisition tank, and gap section is all connected with condensed water between serpentine coil and tubular quill housing inside condenser, and Liquid acquisition tank top is equipped with exhaust-valve and vacuum tube, and vacuum tube is connect with vacuum pump.The present invention can be evaporated under reduced pressure to obtain concentrated mother liquor after the completion of Crystallization of Zeolite using a large amount of waste heat in hydrothermal reaction kettle, and the mother liquor after concentration is directly inputted to the synthesis that next step molecular sieve is participated in hydrothermal reaction kettle, active ingredient in mother liquor adequately is utilized, realize the zero-emission of mother liquor, shorten technological process, the energy has been saved, cost is reduced, has improved production efficiency.

Description

A kind of Zeolite synthesis equipment
Technical field
The invention belongs to the technical fields of material producing process equipment, are related to the production equipment of zeolite molecular sieve synthesis.
Background technology
Molecular sieve refers to having uniform micropore, aperture and the comparable substance of general molecular size.Molecular sieve It is widely used general, efficient drying agent, selective absorbent, catalyst, ion-exchanger etc. can be made.Commonly molecular sieve is The silicate or alumino-silicate of crystalline state are to form molecule ruler by being connected by oxygen bridge key by oxygen-octahedron or aluminum-oxygen tetrahedron The duct of very little size and cavity system have screening fluid molecule of different sizes because binding molecule size and shape is different Ability.Molecular screen material has a wide range of applications in many fields, if micro porous molecular sieve is as main catalysis material, absorption point From material and ion exchange material, played in PETROLEUM PROCESSING, petrochemical industry, fine chemistry industry and daily-use chemical industry more and more important Effect.
Currently, the synthesis of molecular sieve mainly uses hydrothermal synthesis method, but since this method is relatively low to the utilization rate of raw material, institute To contain largely unreacted raw materials and the largely water containing template in mother liquor after the completion of Crystallization of Zeolite.And in industry In production, the direct emission of mother liquor not only results in the waste of raw material, but also prodigious pollution can be caused to environment.Therefore, The concern of more and more people is received for the recycling processing of molecular sieve mother liquor.However it is a large amount of due to containing in mother liquor Moisture so that mother liquor all can not be utilized once in the industrial production, this needs the later stage to handle mother liquor(Such as in mother liquor After recycling, raw material or concentrated mother liquor are supplemented in proportion)It is used again afterwards, greatly reduces production efficiency in this way, increase life Produce cost.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and provide a kind of Zeolite synthesis equipment.
In order to solve the above technical problems, the present invention adopts the following technical scheme that:
A kind of Zeolite synthesis equipment, it is characterised in that:Including hydrothermal reaction kettle(1)And condensing plant;The hydrothermal reaction kettle (1)There are heating device and agitating device, there are two feed inlets on top(4), safety valve(5)And blow valve(13), discharging is arranged at lower part Mouthful(10);The hydrothermal reaction kettle(1)Top is additionally provided with steam (vapor) outlet(7)And pass through pipeline(25)It is linked with condensing plant, and Pipeline(25)It is equipped with solenoid valve(17);The condensing plant includes condenser(2)With Liquid acquisition tank(3);The condenser (2)Shell is made of inside and outside two layers of casing, and there is a serpentine coil in inside, and serpentine coil and tubular quill housing gap portion be all connected with it is cold Condensate;The Liquid acquisition tank(3)Top is equipped with blow valve(14)And vacuum tube(15), wherein vacuum tube(15)Connect with vacuum pump It connects and is equipped with solenoid valve(16), lower part is equipped with liquid emission valve(22).
Preferably, the hydrothermal reaction kettle(1)Lower part discharge port(10)It is sequentially connected solid-liquid separator(11), mother liquor storage Tank(27)And infusion pump(12), infusion pump(12)With hydrothermal reaction kettle(1)The one of feed inlet in top(4)It is connected, and institute State discharge port(10), solid-liquid separator(11), mother liquor storage tank(27), infusion pump(12), feed inlet(4)Between be equipped with electromagnetism Valve.
Preferably, in steam (vapor) outlet(7)With solenoid valve(17)Between be additionally provided with demister(8).
Preferably, in the reaction kettle(1)Top is additionally provided with pressure detecting and automatic control device(6), to automatically control The opening and closing of vacuum pump are adjusted, the vacuum state inside Zeolite synthesis equipment is kept.
Preferably, the pipeline(25)On be additionally provided with flow controller(9), to control steam from hydrothermal reaction kettle to condensation The flow velocity of equipment.
Preferably, the solid-liquid separator(11)It is to be separated by solid-liquid separation by centrifugal method.
Preferably, the solid-liquid separator(11)It is to filter or be filtered by vacuum by normal pressure to be separated by solid-liquid separation.
Due to the implementation of above technical scheme, the present invention has the following advantages that compared with prior art:
The present invention makes reaction kettle be connected with condensing plant after the completion of Crystallization of Zeolite, utilizes a large amount of waste heats in hydrothermal reaction kettle It is evaporated under reduced pressure, then the mother liquor after separation of solid and liquid obtains molecular sieve and concentration, concentration Mother liquor can be added directly into The synthesis that next round molecular sieve is carried out in reaction system, is adequately utilized the active ingredient in mother liquor, realizes the zero of mother liquor Discharge, shortens technological process, has saved the energy, improve production efficiency, reduce production cost.
Description of the drawings
The present invention will be further described in detail with specific embodiment below in conjunction with the accompanying drawings.
Fig. 1 is the structural schematic diagram of Zeolite synthesis equipment of the present invention;
Wherein:1- hydrothermal reaction kettles;2- condenser pipes;3- Liquid acquisition tanks;4- feed inlets;5- safety valves;6- pressure detectings and from Dynamic control device;7- steam (vapor) outlets;8- demisters;9- flow controllers;10- discharge ports;11- solid-liquid separators;12- is infused Pump;13,14- blow valves;15- vacuum tubes;16,17,18,19,20,21,26- solenoid valves;22- liquid emission valves;23- condensed waters Outlet;24- condenses water inlet;25- pipelines;27- mother liquor storage tanks
Specific implementation mode
As shown in Figure 1, according to the present embodiment Zeolite synthesis equipment comprising hydrothermal reaction kettle and condensing plant, condensation Equipment is equipped with condenser and Liquid acquisition tank, and more detailed structure is as follows.
Hydrothermal reaction kettle has heating device and agitating device, and there are two feed inlet, safety valve, blow valve, steam to go out on top Mouth and pressure detecting and automatic control device, lower part have discharge port, steam (vapor) outlet to be linked by pipeline and condensing plant, and successively Equipped with demister, solenoid valve and flow controller.Discharge port is connected with solid-liquid separator and infusion pump, infusion pump and hydro-thermal in turn The one of feed inlet in reaction kettle top is connected, and between discharge port and solid-liquid separator, between infusion pump and feed inlet Equipped with solenoid valve.Condenser casing is made of inside and outside two layers of casing, there is serpentine coil, and serpentine coil and shell inside condenser Shell clearance part is all connected with condensed water.Liquid acquisition tank top is equipped with blow valve and vacuum tube, and lower part is equipped with liquid emission valve, Wherein, vacuum tube is connected with vacuum pump.Pressure detecting and automatic control device are sieved for detection molecules inside synthesis device Pressure, and the opening and closing of vacuum pump are automatically controlled during mother liquor concentrations, to keep inside Zeolite synthesis equipment Vacuum state.
In this example, solenoid valve 17 is opened after the completion of Crystallization of Zeolite, so that reaction kettle is connected with condensing plant, utilizes water A large amount of waste heats are evaporated under reduced pressure in thermal response kettle, are obtained molecular sieve and are concentrated the mixture of Mother liquor, saved the energy, improve Production efficiency, reduces cost.
In addition, the solid-liquid separator and infusion pump that are arranged below reaction kettle, it can be direct by isolated concentrated mother liquor Be input in hydrothermal reaction kettle and participate in next round reaction system, shorten technological process, improve raw material utilization rate and Production efficiency reduces cost.
The present invention is described in detail above, its object is to allow be familiar with that be the personage of field technology can know about hair Bright content is simultaneously implemented, and it is not intended to limit the scope of the present invention, and all Spirit Essences according to the present invention are made Equivalent change or modification, should all cover within the scope of the present invention.

Claims (7)

1. a kind of Zeolite synthesis equipment, it is characterised in that:Including hydrothermal reaction kettle(1)And condensing plant;The hydro-thermal reaction Kettle(1)There are heating device and agitating device, there are two feed inlets on top(4), safety valve(5)And blow valve(13), lower part has Material mouth(10);The hydrothermal reaction kettle(1)Top is additionally provided with steam (vapor) outlet(7)And pass through pipeline(25)It is linked with condensing plant, And pipeline(25)It is equipped with solenoid valve(17);The condensing plant includes condenser(2)With Liquid acquisition tank(3);The condensation Device(2)Shell is made of inside and outside two layers of casing, and there is serpentine coil in inside, and serpentine coil and tubular quill housing gap portion are all connected with Condensed water;The Liquid acquisition tank(3)Top is equipped with blow valve(14)And vacuum tube(15), lower part is equipped with liquid emission valve (22), wherein vacuum tube(15)It is connect with vacuum pump and is equipped with solenoid valve(16).
2. Zeolite synthesis equipment according to claim 1, it is characterised in that:The hydrothermal reaction kettle(1)Lower part discharges Mouthful(10)It is sequentially connected solid-liquid separator(11), mother liquor storage tank(27)And infusion pump(12), infusion pump(12)With hydro-thermal reaction Kettle(1)The one of feed inlet in top(4)It is connected, and the discharge port(10), solid-liquid separator(11), mother liquor storage tank (27), infusion pump(12), feed inlet(4)Between be equipped with solenoid valve.
3. Zeolite synthesis equipment according to claim 1 or 2, it is characterised in that:In steam (vapor) outlet(7)With solenoid valve (17)Between be additionally provided with demister(8).
4. Zeolite synthesis equipment according to claim 1 or 2, it is characterised in that:The reaction kettle(1)Top is additionally provided with Pressure detecting and automatic control device(6), with the opening and closing of automatic control and adjustment vacuum pump.
5. Zeolite synthesis equipment according to claim 1 or 2, it is characterised in that:The pipeline(25)On be additionally provided with stream Amount controller(9).
6. Zeolite synthesis equipment according to claim 2, it is characterised in that:The solid-liquid separator(11)Be by from Heart method is separated by solid-liquid separation.
7. Zeolite synthesis equipment according to claim 2, it is characterised in that:The solid-liquid separator(11)It is by normal Pressure filters or vacuum filtration is separated by solid-liquid separation.
CN201710139429.2A 2017-03-10 2017-03-10 A kind of Zeolite synthesis equipment Pending CN108569704A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710139429.2A CN108569704A (en) 2017-03-10 2017-03-10 A kind of Zeolite synthesis equipment

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Application Number Priority Date Filing Date Title
CN201710139429.2A CN108569704A (en) 2017-03-10 2017-03-10 A kind of Zeolite synthesis equipment

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CN108569704A true CN108569704A (en) 2018-09-25

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109675514A (en) * 2019-01-04 2019-04-26 南京工业大学 Preparation device of surface layer assembled flame retardant

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101489677A (en) * 2006-07-28 2009-07-22 埃克森美孚化学专利公司 A mcm-22 family molecular sieve composition, its method of making, and use for hydrocarbon conversions
CN201485399U (en) * 2009-04-27 2010-05-26 南通泰利达化工有限公司 Methanol recovery device of esterification reaction kettle
CN102351211A (en) * 2011-08-01 2012-02-15 大连理工大学 Synthesis method of MCM-22 family molecular sieve
WO2012171447A1 (en) * 2011-06-17 2012-12-20 宜昌五帝机电有限公司 Method for synthesizing acetyl tri-n-butyl citrate using composite ionic liquid catalyst
CN203123960U (en) * 2013-03-28 2013-08-14 神华集团有限责任公司 Reaction kettle and reaction kettle system for synthesizing molecular sieve catalyst
CN105753010A (en) * 2014-12-19 2016-07-13 中国石油化工股份有限公司 Preparation method of MWW structure molecular sieve
CN105936620A (en) * 2016-05-23 2016-09-14 山东成武易信环保科技有限公司 Ethylene glycol purifying apparatus in environmentally-friendly plasticizer DOTP preparation process, and purifying technology thereof
CN106430228A (en) * 2016-09-08 2017-02-22 中国石油化工股份有限公司 Molecular sieve crystallization mother liquor treatment method
CN206553201U (en) * 2017-03-10 2017-10-13 临沂大学 A kind of Zeolite synthesis equipment

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101489677A (en) * 2006-07-28 2009-07-22 埃克森美孚化学专利公司 A mcm-22 family molecular sieve composition, its method of making, and use for hydrocarbon conversions
CN201485399U (en) * 2009-04-27 2010-05-26 南通泰利达化工有限公司 Methanol recovery device of esterification reaction kettle
WO2012171447A1 (en) * 2011-06-17 2012-12-20 宜昌五帝机电有限公司 Method for synthesizing acetyl tri-n-butyl citrate using composite ionic liquid catalyst
CN102351211A (en) * 2011-08-01 2012-02-15 大连理工大学 Synthesis method of MCM-22 family molecular sieve
CN203123960U (en) * 2013-03-28 2013-08-14 神华集团有限责任公司 Reaction kettle and reaction kettle system for synthesizing molecular sieve catalyst
CN105753010A (en) * 2014-12-19 2016-07-13 中国石油化工股份有限公司 Preparation method of MWW structure molecular sieve
CN105936620A (en) * 2016-05-23 2016-09-14 山东成武易信环保科技有限公司 Ethylene glycol purifying apparatus in environmentally-friendly plasticizer DOTP preparation process, and purifying technology thereof
CN106430228A (en) * 2016-09-08 2017-02-22 中国石油化工股份有限公司 Molecular sieve crystallization mother liquor treatment method
CN206553201U (en) * 2017-03-10 2017-10-13 临沂大学 A kind of Zeolite synthesis equipment

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109675514A (en) * 2019-01-04 2019-04-26 南京工业大学 Preparation device of surface layer assembled flame retardant

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