CN202376991U - Molecular sieve synthesis reaction kettle - Google Patents

Molecular sieve synthesis reaction kettle Download PDF

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Publication number
CN202376991U
CN202376991U CN2011204757173U CN201120475717U CN202376991U CN 202376991 U CN202376991 U CN 202376991U CN 2011204757173 U CN2011204757173 U CN 2011204757173U CN 201120475717 U CN201120475717 U CN 201120475717U CN 202376991 U CN202376991 U CN 202376991U
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China
Prior art keywords
paddle
molecular sieve
reaction kettle
synthesis reaction
sieve synthesis
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Expired - Fee Related
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CN2011204757173U
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Chinese (zh)
Inventor
庞新梅
潘慧芳
张茵
罗琛
丁冠正
王晓化
刘其武
王骞
朴佳锐
李发永
阎立军
朱晓晓
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Petrochina Co Ltd
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Petrochina Co Ltd
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Priority to CN2011204757173U priority Critical patent/CN202376991U/en
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Abstract

The utility model relates to a molecular sieve synthesis reaction kettle, which is characterized in that the reaction kettle is a jacket type reaction kettle, the bottom of the reaction kettle is spherical, a stirring paddle is arranged in the reaction kettle, a stirring shaft seal is double-end-face mechanical seal, two feed inlets, a safety valve and an emptying valve are arranged at the upper part of the reaction kettle, a discharge hole is arranged at the bottom, and a kettle bottom valve is arranged at the bottom of the reaction kettle; the stirring adopts three layers of combined stirring paddles at the upper part, the middle part and the lower part, and the lower part is a semi-anchor type stirring paddle. The molecular sieve synthesis reaction kettle has controllable temperature rising and falling speed and high temperature control precision; the materials are fully stirred and uniformly mixed, and the mass transfer and heat transfer effects are good; the solid content of the material is high (more than 55 percent), the dosage of the template agent can be saved, the crystallization speed is improved, and the cost of raw materials is reduced; the method has the advantages of more material feeding in a single kettle, high yield and capability of improving the production efficiency, and is particularly suitable for the reaction process of synthesizing the zeolite molecular sieve by a solid-like phase method.

Description

The molecular sieve synthesis reaction vessel
Technical field
The utility model belongs to the technical field of manufacture of materials process equipment, production equipment---the agitated reactor that particularly a kind of zeolite molecular sieve is synthetic.
Technical background
Synthesis method of zeolite molecular sieve mainly contains three kinds: traditional hydro-thermal method, gas solid method and type solid phase method (also being called dampening).Gas solid method be a kind of new synthesis zeolite that grew up in nearly ten years method [Dong Jinxiang, Dong Ping. the technical progress of Zeolite Synthesis with Vapor Phase Method [J] petrochemical industry, 1995, (03); Sun Xiuliang. Theoretical Calculation research [D] Beijing University of Chemical Technology of synthetic beta-molecular sieve of solid phase and synthesis mechanism thereof; 2009]; Be that with the main distinction of traditional water thermal synthesis method gas solid method is as solid phase, then with steam effect crystallization formation zeolite with the silica-alumina gel that contains organic template.For example, people such as Chen Tiehong are template with TEAOH, and waterglass or Ludox are alkali source, and aluminum nitrate is the aluminium source, and NaOH is alkali source, adopt the synthetic β zeolite of gas solid method.Method is: in agitated reactor, add a certain amount of waterglass, add sodium hydroxide solution and organic ammonium template in the stirring, add aluminum nitrate and water then, be stirred to dry state under the proper temperature, process the silica-alumina gel that contains TEAOH; The dry state silica-alumina gel is placed a self-control porous screen cloth, be placed in another stainless steel cauldron, a certain amount of water is housed at the bottom of the still, sealing is placed in the baking oven; Gel in agitated reactor under the self-generated pressure with the steam effect, 170 ℃ of following crystallization 5d; Crystallization product is dried in air after washing.Type solid-phase synthesis, concrete grammar are to be template with organic ammonium salt (like TEAOH), and the solid silochrom is the silicon source, and sodium aluminate is the aluminium source, and NaOH is alkali source.At first with a certain amount of organic ammonium salt, NaOH (Gu) and NaAlO2 (Gu) add in the entry and stir, heating, and dissolving is prepared into work alkali lye; In agitated reactor, add a certain amount of silochrom, add the work alkali lye for preparing while stirring, strong agitation is even then; Heat up in kettle cover sealing back, certain rotating speed constantly stirs 120 ℃ of-170 ℃ of following crystallization 2-3d down; Crystallization product is dried in air after washing.Compare with the traditional water thermal synthesis method, a type solid-phase synthesis not only can reduce the template consumption, and can accelerate crystallization rate, improves single-autoclave yield rate.
CN200720173192.1 discloses the synthetic revolving reaction still system of a kind of molecular sieve; Comprise electric heating bellows (1), agitated reactor (2), rotatable parts (4), control assembly (6) etc.; Agitated reactor support (3) is installed in the electric heating bellows (1), and agitated reactor (2) is fixedly connected with agitated reactor support (3), and outer support frame (5) is connected with rotatable parts (4); Be provided with control assembly (6) in the bottom of electric heating bellows (1); Reaction mixes, easy to operate, be easy to control, device structure is simple, efficient is high, do not have to reveal reaction temperature, pressure, the equal scalable of rotational frequency; The molecular sieve that can next time synthesize several kinds of different formulations in same reaction conditions; Also can once synthesize the molecular sieve of several kinds of same recipe, differential responses condition, thus use this system's synthesis of molecular sieve can conservation, shorten test period, increase work efficiency, and can guarantee the repeatability of synthesis of molecular sieve.
CN200710172524.9 discloses a kind of method that in the horizontal reacting still, prepares molecular sieve.This horizontal reacting still is applicable to that hydro-thermal method or sol-gel process and other relate to the molecular sieve synthetic method of liquid, solid mixed system, can be used for synthetic various micro porous molecular sieves, mesopore molecular sieve and microporous-mesoporous composite molecular sieve.Defectives such as this invention has overcome the existing liquid of synthesis of molecular sieve, solid phase mixing weak effect in the vertical response still, and the pore passage structure of products obtained therefrom, particle diameter and particle diameter distribution are wayward.The paddle of this horizontal reacting still is distortion turbine oar, and paddle diameter and agitated reactor internal diameter ratio are 0.4~0.85, and the long ratio of the axial width of paddle and kettle is 0.11~0.35.
The production equipment that different synthetic methods are suitable for is different.It is the crystallization device that the tradition hydro-thermal method adopts autoclave pressure, static state or dynamic crystallization; It is the crystallization device that gas solid method adopts autoclave pressure, static crystallization; The class solid-phase synthesis, adopting autoclave pressure is the crystallization device, dynamic crystallization needs special stirring.
The utility model content
The utility model purpose is to provide a kind of molecular sieve synthesis reaction vessel, and particularly a kind of synthetic reaction device of suitable type of solid phase method synthesis zeolite can be practiced thrift the production time, improves single-autoclave yield rate.
To achieve these goals, the molecular sieve synthesis reaction vessel of the utility model is characterized in that agitated reactor is a chuck type agitated reactor; The agitated reactor bottom is sphere; In establish paddle, shaft envelope is double mechanical seal, two charging apertures and safety valve and atmospheric valve are arranged at still top; Discharging opening is established in the bottom, joins the still bottom valve; Stir and adopt upper, middle and lower portion three layers of combination paddle, the bottom is half anchor formula paddle.
Last, middle part paddle can be typical solid-liquid suspension paddle, and like straight leaf formula oar, oblique leaf formula oar, hinging type oar, two hinging type oar, four oblique leaf formula oar unlatchings, six leaf formula oars etc., in order to prevent the blade sizing, blade section is preferably triangle.The shape of top paddle and middle part paddle can be identical, and being preferably in the end of blade place increases and scrape wallboard, can be one or more.
In order to reduce the material wall built-up, to be convenient to clean, polishing is preferably all done on still inwall, shaft and paddle surface.
Two general one of charging apertures are liquid inlet openings, and one is the feeding-in solid body mouth, and the liquid feed pipe line extend into the charge level top in the still, and nozzle is installed in the end.
General admittance deep fat carries out heating and cooling in the chuck.
The bottom of three layers of combination paddle is half anchor formula paddle, is preferably 10~30mm with bottom gap.
Class solid phase method synthesis zeolite process characteristic is: 140~180 ℃ of reaction temperatures, and reaction pressure 1.0~2.0MPa, the material solid content can be greater than 55% (being solid phase) basically.The variation of the proterties of material is divided into three phases in the course of reaction, initial period, and material (silica gel) is the solid of wetting attitude, and is inviscid, stirs easily; Along with temperature raises and the reaction time prolongation, the viscosity of material increases, and the stirring resistance is big, needs bigger power of agitator this moment, and in order not destroy crystal growth, mixing speed need strictly be controlled simultaneously; When reaction finished, what obtain was molecular sieve pulp (for the Ben-Hur thixotropic fluid), does not stop as long as stirring in the process, then is easy to stir, and this moment, power of agitator can be less.The difference of itself and traditional hydro-thermal method technology is that the material solid content is high, mixes difficulty, and mass transfer, heat transfer problem are the subject matter that realizes this technology.
Characteristics according to material proterties variation in the above-mentioned type of solid phase method synthesis zeolite reaction process process; With traditional water thermal synthesis still is that the crystallization device is obviously inapplicable; Because its material solid content generally is not more than 20%; Material is slurries, liquid-phase mixing and solid phase mixing to agitator shape, structure etc. require different.So the utility model provides the molecular sieve synthesis reaction vessel, production that can type of realization solid phase method synthesis zeolite.
With the molecular sieve synthesis reaction vessel is matching used alkali lye feed pump, heating system and control system etc. should be arranged also.Heating system can be selected cold-hot integrated machine for use.
The wallboard 7 of scraping of bottom anchor formula paddle I and top paddle III has taken into full account at initial period solid material is fully mixed; Basically there is not the dead angle; Liquid is sprayed onto the surface of solids equably by the top charging aperture, through stirring solid-liquid two phase materials is evenly mixed.The powder that certain jet flow property is arranged for particle diameter is thin, tack is little after mixing speed is elevated to a certain degree, has a large amount of gas and is stirred impeller and is brought into powder inside; Or in powder, stir out a cavity, and make impeller idle running, therefore half anchor formula paddle I is installed in the bottom; Preferably be equipped with and scrape wallboard 7 at agitator end of blade place, top, can destroy the bubble in the powder, and mixing speed should not be too high in actual the use; The top end of blade is scraped wallboard 7 for removable; In use, according to the material proterties, can not install if can reach mixed effect yet.
The utility model is compared with traditional hydro-thermal law technology, and have the following advantages: warming and cooling rate is controlled, and temperature-controlled precision is high; Material stirs fully, mixes, and mass transfer, heat-transfer effect are good; Material solid content high (can greater than 55%) can be practiced thrift the template consumption, improves crystallization rate, reduces the cost of raw material; That single still feeds intake is many, productive rate is high, can enhance productivity.
Description of drawings
Fig. 1 is a molecular sieve synthesis reaction vessel sketch map.
Be labeled as among the figure: 1. half anchor formula paddle I, 2. holding screw, 3. key, 4. paddle II, 5. shaft, 6. paddle III 7. scrapes wallboard, 8. pin.
Fig. 2 is a paddle II sketch map.
Fig. 3 is a paddle II generalized section.
Fig. 4 is the sketch map of a complete set of system of synthesis zeolite device, is labeled as among the figure: metering of A. alkali lye and feed system, B. molecular sieve crystallizing kettle system, C. cold-hot integrated machine system.
The specific embodiment
Contrast accompanying drawing below,, like interaction, operation principle, manufacturing process between the shape of each related member, structure, the each several part and manipulate method etc., be described further the specific embodiment of the utility model.
A is alkali lye metering and feed system, and B is a molecular sieve crystallizing kettle system, and C is that cold-hot integrated machine system three parts are formed (see figure 4).Because the alkali lye metering is all similar with routine techniques with feed system, autoclave pressure and cold-hot integrated machine system, does not do special instruction.
Embodiment:
Agitated reactor: pressure 2.5MPa, 200 ℃ of temperature, V=55L, in establish paddle, agitator speed 30~150r/min, power of motor 4.0KW (stirring motor band frequency converter).Heating of admittance deep fat or cooling in the equipment chuck.
Axially establish in the still, in two points for measuring temperature, the still wall is established two temperature controlling points.A liquid inlet opening and a feeding-in solid body mouth are arranged at still top, and the liquid feed pipe line extend into the charge level top in the still, and nozzle is installed in the end.Discharging opening is established in the bottom, joins the still bottom valve, and buildup must not be arranged at valve top.Still top is furnished with safety valve and atmospheric valve.
The described stirring system (see figure 1) of the utility model adopts three layers of combination paddle, and the bottom is half anchor formula paddle I, with oval bottom gap 20mm.Middle part paddle II is typical solid-liquid suspension paddle (4 leaf oars is seen Fig. 2), and in order to prevent the blade sizing, blade section is the triangle (see figure 3).Top paddle III is identical with middle part paddle II, and just increase by two and scrape wallboard at the end of blade place, length 170mm, width 30mm is apart from still wall 10mm.
This combination paddle fully takes into account the initial mix stages of solid powder and the stirring in the plaster material stage of reaction medium-high viscosity.The plaster material stage of reaction medium-high viscosity; The emphasis that stirs is to obtain required mixed effect like how minimum energy consumption; This stage has good mixed with the paddle III combination on middle part paddle II and top, compares with 45 ° of four oblique oar of leaf of independent use; When reaching same mixed effect, can save energy about 50%.
The blade tip of the impeller of middle part paddle II is narrower, can reduce the impact damage crystallization, is main with the axial flow impeller, has strengthened axial mixing, is convenient to the homogeneous of temperature and concentration.Scraping wallboard 7 can in time scrape material from the still wall, has prevented that material from gluing wall, avoids temperature of charge inhomogeneous.
The course of work of the utility model is: solid material is added in the still by the top charging aperture, and liquid material is squeezed in the still on the solid material by pump, opens agitating device; After fully stirring, start the cold-hot integrated machine system, be heated to design temperature; Begin reaction, continue to stir, after question response finishes; Cool to design temperature, material is drawn off from the still lower part outlet, promptly accomplish the course of work that the molecular sieve crystallization is produced.

Claims (7)

1. a molecular sieve synthesis reaction vessel is characterized in that agitated reactor is a chuck type agitated reactor, and the agitated reactor bottom is sphere; In establish paddle, shaft envelope is double mechanical seal, two charging apertures and safety valve and atmospheric valve are arranged at still top; Discharging opening is established in the bottom, joins the still bottom valve; Stir and adopt upper, middle and lower portion three layers of combination paddle, the bottom is half anchor formula paddle.
2. molecular sieve synthesis reaction vessel according to claim 1 is characterized in that top paddle or middle part paddle are the solid-liquid suspension paddle.
3. molecular sieve synthesis reaction vessel according to claim 1 is characterized in that top paddle or middle part paddle are straight leaf formula oar, oblique leaf formula oar, hinging type oar, two hinging type oar, four oblique leaf formula oars or six leaf formula oars.
4. molecular sieve synthesis reaction vessel according to claim 1 is characterized in that half anchor formula paddle of three layers of combination paddle bottom and gap, agitated reactor bottom are 10~30mm.
5. molecular sieve synthesis reaction vessel according to claim 1 is characterized in that the agitator end of blade place, top of three layers of combination paddle is equipped with and scrapes wallboard (7).
6. molecular sieve synthesis reaction vessel according to claim 1 is characterized in that in two charging apertures, one is liquid inlet opening, and one is the feeding-in solid body mouth, and the liquid feed pipe line extend into the charge level top in the still, and nozzle is installed in the end.
7. molecular sieve synthesis reaction vessel according to claim 1 is characterized in that middle part stirrer paddle section is a triangle.
CN2011204757173U 2011-11-25 2011-11-25 Molecular sieve synthesis reaction kettle Expired - Fee Related CN202376991U (en)

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Application Number Priority Date Filing Date Title
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103007810A (en) * 2012-11-11 2013-04-03 浙江长城减速机有限公司 Stirrer suitable for agglomerating and washing
WO2014023072A1 (en) * 2012-08-09 2014-02-13 Wen Xia Sludge solidification system
CN103693656A (en) * 2013-12-20 2014-04-02 济南大学 Directly-heated type 4A zeolite crystallization reaction kettle
CN107715743A (en) * 2017-10-31 2018-02-23 中国船舶重工集团公司第七0研究所 A kind of frame-type stickiness paint mixing device
CN108246230A (en) * 2018-04-01 2018-07-06 中鸿纳米纤维技术丹阳有限公司 A kind of silica aerogel production reaction kettle
CN108246229A (en) * 2018-04-01 2018-07-06 中鸿纳米纤维技术丹阳有限公司 A kind of silica aerogel production reaction kettle fast reaction component
CN108967505A (en) * 2018-05-30 2018-12-11 安徽省好再来食品有限公司 Drying unit is used in a kind of processing of bacon
CN112221463A (en) * 2020-09-30 2021-01-15 中触媒新材料股份有限公司 Efficient continuous molecular sieve adsorbent post-treatment device and use method

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014023072A1 (en) * 2012-08-09 2014-02-13 Wen Xia Sludge solidification system
CN103007810A (en) * 2012-11-11 2013-04-03 浙江长城减速机有限公司 Stirrer suitable for agglomerating and washing
CN103007810B (en) * 2012-11-11 2015-05-13 浙江长城减速机有限公司 Stirrer suitable for agglomerating and washing
CN103693656A (en) * 2013-12-20 2014-04-02 济南大学 Directly-heated type 4A zeolite crystallization reaction kettle
CN107715743A (en) * 2017-10-31 2018-02-23 中国船舶重工集团公司第七0研究所 A kind of frame-type stickiness paint mixing device
CN107715743B (en) * 2017-10-31 2023-07-28 中国船舶重工集团公司第七0一研究所 Frame-type viscous paint mixing device
CN108246230A (en) * 2018-04-01 2018-07-06 中鸿纳米纤维技术丹阳有限公司 A kind of silica aerogel production reaction kettle
CN108246229A (en) * 2018-04-01 2018-07-06 中鸿纳米纤维技术丹阳有限公司 A kind of silica aerogel production reaction kettle fast reaction component
CN108967505A (en) * 2018-05-30 2018-12-11 安徽省好再来食品有限公司 Drying unit is used in a kind of processing of bacon
CN112221463A (en) * 2020-09-30 2021-01-15 中触媒新材料股份有限公司 Efficient continuous molecular sieve adsorbent post-treatment device and use method
CN112221463B (en) * 2020-09-30 2022-04-26 中触媒新材料股份有限公司 Efficient continuous molecular sieve adsorbent post-treatment device and use method

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CF01 Termination of patent right due to non-payment of annual fee
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Granted publication date: 20120815

Termination date: 20201125