CN109126624A - It is a kind of to prepare the dedicated filtrate prilling granulator of hydrogen fluoride moving bed filter - Google Patents
It is a kind of to prepare the dedicated filtrate prilling granulator of hydrogen fluoride moving bed filter Download PDFInfo
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- CN109126624A CN109126624A CN201811207290.1A CN201811207290A CN109126624A CN 109126624 A CN109126624 A CN 109126624A CN 201811207290 A CN201811207290 A CN 201811207290A CN 109126624 A CN109126624 A CN 109126624A
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- spray tower
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- hydrogen fluoride
- air
- moving bed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
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Abstract
本发明涉及氟化工技术领域，具体涉及一种制备氟化氢移动床过滤器专用滤料造粒装置。其特征是：包括喷塔、泵送组件、风送组件、袋滤器、加热器、罗茨风机。
The invention relates to the technical field of fluorine chemical industry, in particular to a special filter material granulation device for preparing hydrogen fluoride moving bed filters. It is characterized in that it includes a spray tower, a pumping component, an air supply component, a bag filter, a heater, and a Roots blower.
Description
Technical field
The present invention relates to technical field of fluorine chemical industry, and in particular to a kind of dedicated filtrate of hydrogen fluoride moving bed filter for preparing is made
Grain device.
Background technique
Hydrogen fluoride is widely used to the industries such as electronics, chemical industry, petroleum, is mainly used as producing villiaumite, fluorohaloparaffin, fluorine cause
Cryogen, etching glass, impregnated timber, electrolysis element fluorine etc., separation impurity purification is one of critical process after obtaining thick hydrogen fluoride,
The prior art generallys use the method despumation of washing, distillation, absorption, rectifying.Chinese invention patent (Patent No.
CN201310287202.4, patent name are a kind of anhydrous hydrogen fluoride production method) disclose a kind of anhydrous hydrogen fluoride producer
Method, which comprises the following steps: Fluorspar Powder and sulfuric acid are sent into pre-reactor；In pre-reactor, sulfuric acid and fluorite
Powder is sufficiently mixed while being reacted, and generates thick hydrogen fluoride gas；The thick hydrogen fluoride gas is removed through preliminary clearning tower, scrubbing tower
Then impurity passes sequentially through two condensers, most of hydrogen fluoride gas is frozen medium and is condensed, in first condenser
Obtained lime set flows back into preliminary clearning tower, is pumped to rectifying column essence by the second crude acid in the crude acid lime set that the second condenser obtains
System；Anhydrous hydrofluoric acid leaves the rectifying column by the pressure of tower itself, through finished product cooler to anhydrous hydrogen fluoride finished product storage tank；
The on-condensible gas of rectifying tower top and hydrogen fluoride condenser enters sulfuric acid absorption tower；Sulfuric acid absorbs in gas phase from tower top to flowing down
Hydrogen fluoride；The sulfuric acid containing hydrogen fluoride is sent back to scrubbing tower with pump；The gas for leaving sulfuric acid absorption tower top is obtained by water scrubber
Byproduct fluosilicic acid；The washed tower of sulfuric acid for absorbing hydrogen fluoride returns to pre-reactor.Chinese invention patent (Patent No. CN
201210506779.5, patent name is a kind of preparation method of anhydrous hydrogen fluoride) disclose a kind of preparation of anhydrous hydrogen fluoride
Method, which comprises the following steps: after a) heating mixing sulfuric acid and fluorspar powder respectively, according to certain charged material weight
Than the mixing progress pre-reaction in pre-reactor, mixed material is obtained, wherein the mixing sulfuric acid is the concentrated sulfuric acid and oleum
The mixture of acid, weight ratio are sulfuric acid: oleum=1:1.40~1.50；The heating time for mixing sulfuric acid is 7~8 points
Clock, heating temperature are 100~120 DEG C；B) mixed material is continuously fed into converter reactor, is in converter reactor revolving speed
Under conditions of 1.0r/min~2.0r/min and furnace pressure are -0.55~-0.45KPa, 550~650 DEG C and 700 are successively used
~800 DEG C of two kinds of temperature react mixed material, react 50~70 minutes, obtain thick hydrogen fluoride gas and solid material,
A part of obtained solid material is fed to converter reactor secondary response again by material-returning device, remaining solid material enters
Dihydrate gypsum process units；C) the washed tower of thick hydrogen fluoride gas, condenser, rectifying column and degassing tower processing, obtain pure
Hydrogen fluoride gas and residual gas；D) circulation and stress is carried out to residual gas using sulfuric acid, to absorb hydrogen fluoride gas；E) not by
The residual gas of circulation and stress is discharged after water scrubber processing and tail gas tower processing from tail gas tower top.
The prior art 1 and 2 hydrogen fluoride of prior art separation impurity refining plant are currently used preliminary clearning tower, washing
Tower, condenser, rectifying column and degassing tower, have a disadvantage in that: passing through the process means separation and purification such as washing, distillation, absorption, rectifying
Hydrogen fluoride, process flow is complex, the decline of product yield, energy consumption are higher, does not efficiently use and generates in production process
Byproduct.
Summary of the invention
In view of the deficiencies of the prior art, the dedicated filter of hydrogen fluoride moving bed filter is prepared the object of the present invention is to provide a kind of
Prilling granulator is expected, it is characterized in that: including spray tower, pump, wind sending component, bag hose, heater, roots blower.
The spray tower, bag hose, heater, roots blower form the outer closed type circulatory system, the hot wind gas of spray tower discharge
It is sent into heater heating after flowing through bag hose purification, spray tower bottom air compartment is then sent by roots blower and is recycled, to fill
Divide the waste heat using hot-air flow.
The spray tower includes nozzle component, sprays tower body, cyclone separator, material returning device, air distribution plate, material blanking tube, air compartment, described
Spray tower body, cyclone separator, material returning device, air compartment, air distribution plate form the interior closed type circulatory system, and anhydrite powder can be abundant
It is contacted with slurry particles and completes drying process, and prevent slurry particles to be adhered on spray each component of tower as interleaving agent.The spray
Tube assembly design is at the top of spray tower body, and air compartment, air distribution plate design are in spray tower body bottom.
The nozzle component includes delivery pipe, nozzle, mixing chamber, Venturi tube, jet pipe, nozzle exit, deflection cone.It is described
Pump, wind sending component are connect with nozzle, delivery pipe respectively, and fluorgypsum slurry and anhydrite powder are sent into mixing chamber and mixed
It closes, through enturi tube, jet pipe is sent out from nozzle exit along deflection cone to spray tower body after mixing strongly.
Inventors have found that preparing the fluorite (CaF of hydrogen fluoride2) and sulfuric acid (H2SO4) following main reaction: CaF occurs2+
2H2S04→2HF+CaSO4, the product into the subsequent processing stage mainly has heavy constituent impurity H2SO4、H2O, light component impurity
SO2、SiF4、CO2、H2S, byproduct include CaSO4、Fe2(SO4)3、H2SiF6.According to " anhydrous hydrogen fluoride for industrial use " GB 7746-
The requirement of 2011 national standards, to H2SO4、H2O、H2SiF6、SO2Content it is restricted, remove the above impurity and prepare anhydrous fluorine
The prior art for changing hydrogen mainly uses the process means such as purification, washing, condensation, rectifying, degassing, with water to dissolve, adsorb, wash
Main techniques medium, the specifically dedusting of prior art preparation hydrogen fluoride, condensation process such as wash, be desorbed, conveying, separating
The effect of middle water is in scrubbing tower with spray absorption method absorption CaSO4、Fe2(SO4)3Dust, while technique is realized in water heat absorption
Temperature decline.Due to this case recirculating fluidized bed reacting furnace with superheated vapour be main processing medium, be at this stage exactly to purify
The CaSO that superheated vapour carries4、Fe2(SO4)3Particulate matter, to make process flow become simple, product yield raising, energy consumption
Decline, using the technical solution of stratum granulosum moving bed filter.
Inventors have found that due to proprietary the setting that stratum granulosum moving bed filter is recirculating fluidized bed reacting furnace Aided design
It is standby, have a following characteristics: first, using prior art water washing wet dust removal method, i.e. dry dust removal method is different from, use
Filtrate trap particulate matter, arresting efficiency is quite even higher with bag hose, and the rate of filtration is much higher than bag hose, and pressure drop is filtered compared with bag
Device is low, and high temperature resistant, corrosion-resistant；Second, it can gather materials on the spot using using the byproduct in production process, stratum granulosum filtrate
Using fluorgypsum particle, it is well known that fluorite (CaF2) and sulfuric acid (H2SO4) main reaction: CaF occurs2+2H2S04→2HF+
CaSO4, byproduct CaSO4It is exactly the fluorgypsum that we are commonly called as, final products of the fluorgypsum as above-mentioned irreversible reaction, from
So have not by H2SO4, HF corrosion the advantages of, also achieve solid waste circulation comprehensive utilization；Third, stratum granulosum moving bed
Filter its to move bed be also the second reaction chamber, recirculating fluidized bed reacting furnace, which reacts incomplete fluorite particle, can adhere to
The reaction was continued for granulosa filter material surface, improves the yield of HF product.
Inventors have found that being attached to stratum granulosum filtrate table since recirculating fluidized bed reacting furnace reacts incomplete fluorite particle
The reaction was continued in face, and for the HF of generation with air-flow runaway, solid fluorgypsum, which is attached on filtering material particle surface, causes it to grow up, many
Well known, the factor for influencing granular-bed filter arresting efficiency mainly has filtering material particle diameter and bed height, therefore is designed as
Two-stage stratum granulosum, 8~10mm of particle diameter of filter medium of primary granule layer filling, main purpose is that incomplete fluorite particle is allowed to be attached to
The reaction was continued for stratum granulosum filter material surface, and causes filtering material particle long in view of solid fluorgypsum is attached on filtering material particle surface
Greatly, it fills mutual gap while improving arresting efficiency pressure drop will will increase, move whereabouts and be discharged to moving bed and become in vitro
Obtain the factors such as difficult；1~2mm of particle diameter of filter medium of secondary granule layer filling, mainly interception fine particle.
Inventors have found that the bed body of stratum granulosum moving bed filter is designed as U-shaped, main bed body and secondary bed body are well formula
Bed body, bottom are interconnected, and main bed body fills 8~10mm of particle diameter of filter medium, and airflow direction is identical as its moving direction, are cocurrent
Formula；Secondary bed body fills 1~2mm of particle diameter of filter medium, airflow direction with its moving direction on the contrary, be it is reverse-flow, purpose prevents air-flow band
From dust.
Inventors have found that the raw material fluorgypsum main component for preparing filtrate is anhydrous CaSO4Particle adds water hardening
Process is: CaSO anhydrous first4It is dissolved in water then CaSO4.2H2O is precipitated to form slurry, with the continuous progress of aquation, generates
CaSO4.2H2O colloidal particles are increasing, these particle specific surface areas are very big, adsorb many moisture, while in slurry
Free moisture constantly reduced due to aquation and evaporation, the consistency of slurry is continuously increased, and slurry gradually generates condensation, colloid turn
Become crystal, i.e. slurry produces hardening.
Water hardening is added to obtain the physicochemical property with some strength and hardness particle inventors have found that can use fluorgypsum
The filtrate of stratum granulosum moving bed filter is prepared, 60 mesh are screened to by fluorgypsum is broken first, according to weight ratio ingredient fluorite
It 100 parts of cream, 80~100 parts of deionized water, stirs evenly and slurry is made, be pumped to nozzle component, fluorgypsum slurry is sent from nozzle
It shrinks to form spherical particle due to surface tension after out, while anhydrite powder is also sent through delivery pipe to mixing chamber, wrap up
Slurry particles and absorb its free moisture, it is both above-mentioned constantly to grow up by Venturi tube and the strong mixture slurry particle of jet pipe
While due to moisture constantly reduce gradually generate condensation, through nozzle exit along deflection cone to spray tower body send out, via spray
The hot-air flow purging that tower bottom air compartment and air distribution plate conveying come up comes along spray tower body wall spiral from air-flow cross section transverse
Observation, air-flow form that periphery flow velocity is fast, center flow velocity is slow, the periphery feature big compared with center pressure, drive constantly grow up and
The slurry particles of solidification throw to spray tower body wall friction collision lose kinetic energy fall and to center assemble, and under the sweeping along of air-flow to
Top of tower flowing is sprayed, is in brief exactly that slurry particles flow in spray tower body in fluidized state, slurry particles are dry in continuous absorption
It grows up and solidifies under the action of fluorgypsum powder and hot wind evaporation, spray tower body center is gathered in after particle size growth to certain diameter simultaneously
It is separated under gravity with hot-air flow, enters vibrating screen sorting through material blanking tube；The nonadherent dry fluorite in slurry particles
Cream powder enters cyclone separator under the carrying of hot-air flow, through material returning device after separating in cyclone separator with hot-air flow
It is fed again into spray tower body and is mixed with slurry particles, hot-air flow is sent into heater heating after bag hose purifies, then by sieve
Thatch blower is sent into spray tower bottom air compartment and is recycled.
Inventors have found that spray tower, bag hose, heater, roots blower form the outer closed type circulatory system, spray tower discharge
Hot-air flow is sent into heater heating after bag hose purifies, and is then sent into spray tower bottom air compartment by roots blower and is recycled,
To make full use of the waste heat of hot-air flow.Spray the interior closed type that tower body, cyclone separator, material returning device, air compartment, air distribution plate are formed
The circulatory system, anhydrite powder, which can be contacted sufficiently with slurry particles, completes drying process, and prevents slurry as interleaving agent
Particle is adhered on spray each component of tower.
Inventors have found that can adjust the diameter and roots blower conveying air velocity of nozzle to obtain the filtrate of different-grain diameter.For
Guarantee that bag hose is not blocked, bag hose outlet temperature is not less than 110 DEG C, to guarantee that particle is in normal fluidisation shape in material returning device
State accelerates slurry particles solidification, and spray tower body should keep 135~150 DEG C of temperature.
Compared with the existing technology, the present invention, which at least contains, has the advantage that adding water hardening to obtain using fluorgypsum has centainly
The physicochemical property of intensity and hardness particle prepares the filtrate of stratum granulosum moving bed filter, can gather materials on the spot using using production
Byproduct in the process, stratum granulosum filtrate use fluorgypsum particle, it is well known that fluorite (CaF2) and sulfuric acid (H2SO4) lead
Reaction: CaF2+2H2S04→2HF+CaSO4, byproduct CaSO4Be exactly the fluorgypsum that we are commonly called as, fluorgypsum as it is above-mentioned not
The final products of reversible reaction have not by H naturally2SO4, HF corrosion the advantages of, also achieve solid waste circulation comprehensive benefit
With.
Detailed description of the invention
Fig. 1 is a kind of front view structure signal for preparing the dedicated filtrate prilling granulator of hydrogen fluoride moving bed filter of the present invention
Figure.
Fig. 2 is a kind of A enlarged structure signal for preparing the dedicated filtrate prilling granulator of hydrogen fluoride moving bed filter of the present invention
Figure.
Fig. 3 is a kind of B enlarged structure signal for preparing the dedicated filtrate prilling granulator of hydrogen fluoride moving bed filter of the present invention
Figure.
Fig. 4 is a kind of C enlarged structure signal for preparing the dedicated filtrate prilling granulator of hydrogen fluoride moving bed filter of the present invention
Figure.
Fig. 5 is a kind of D enlarged structure signal for preparing the dedicated filtrate prilling granulator of hydrogen fluoride moving bed filter of the present invention
Figure.
1- sprays tower 2- pump 3- wind sending component 4- bag hose 5- heater
6- roots blower 7- nozzle component 8- sprays tower body 9- cyclone separator 10- material returning device
11- air distribution plate 12- material blanking tube 13- air compartment 14- delivery pipe 15- nozzle
16- mixing chamber 17- Venturi tube 18- jet pipe 19- nozzle exit 20- deflection cone.
Specific embodiment
The present invention is described further with specific embodiment with reference to the accompanying drawing.
It is as shown in figure 1, figure 2, figure 3, figure 4 and figure 5, a kind of to prepare the dedicated filtrate prilling granulator of hydrogen fluoride moving bed filter,
It is characterized in that: including spray tower 1, pump 2, wind sending component 3, bag hose 4, heater 5, roots blower 6.
The spray tower 1, bag hose 4, heater 5, roots blower 6 form the outer closed type circulatory system, the heat that spray tower 1 is discharged
General mood, which flows through, is sent into the heating of heater 5 after bag hose 4 purifies, being then sent into spray 1 bottom plenum 13 of tower circulation by roots blower 1 makes
With to make full use of the waste heat of hot-air flow.
The spray tower 1 includes nozzle component 7, spray tower body 8, cyclone separator 9, material returning device 10, air distribution plate 11, material blanking tube
12, air compartment 13, the spray tower body 8, cyclone separator 9, material returning device 10, air compartment 13, air distribution plate 11 form interior closed type cyclic system
System, anhydrite powder, which can be contacted sufficiently with slurry particles, completes drying process, and prevents slurry particles viscous as interleaving agent
It is attached on the spray each component of tower 1.The design of nozzle component 7 is at 8 top of spray tower body, and air compartment 13, the design of air distribution plate 11 are in spray tower body 8
Bottom.
The nozzle component 7 includes delivery pipe 14, nozzle 15, mixing chamber 16, Venturi tube 17, jet pipe 18, nozzle exit
19, deflection cone 20.The pump 2, wind sending component 3 are connect with nozzle 15, delivery pipe 14 respectively, by fluorgypsum slurry and are done
Fluorgypsum powder be sent into mixing chamber 16 mix, through enturi tube 17, jet pipe 18 strongly mixing after from nozzle exit 19 along water conservancy diversion
Cone 20 is sent out to spray tower body 8.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and is modified.Therefore, the invention is not limited to the specific embodiments disclosed and described above, to of the invention
Some modifications and changes should also be as falling into the scope of the claims of the present invention.In addition, although being used in this specification
Some specific terms, these terms are merely for convenience of description, does not limit the present invention in any way.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811207290.1A CN109126624B (en) | 2018-10-17 | 2018-10-17 | A special filter material granulation device for preparing hydrogen fluoride moving bed filter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811207290.1A CN109126624B (en) | 2018-10-17 | 2018-10-17 | A special filter material granulation device for preparing hydrogen fluoride moving bed filter |
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| CN109126624A true CN109126624A (en) | 2019-01-04 |
| CN109126624B CN109126624B (en) | 2020-07-28 |
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| CN201811207290.1A Expired - Fee Related CN109126624B (en) | 2018-10-17 | 2018-10-17 | A special filter material granulation device for preparing hydrogen fluoride moving bed filter |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109731396A (en) * | 2019-03-11 | 2019-05-10 | 杨松 | It is a kind of to prepare roller kilns dedusting filtrate mixed fluidized bed |
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| EP0334982A1 (en) * | 1988-03-30 | 1989-10-04 | Ohkawara Kakohki Co., Ltd. | Spray-drying granulation apparatus |
| CN2668243Y (en) * | 2003-12-03 | 2005-01-05 | 上海化工研究院 | Internal return fluidized granulation device |
| CN1721327A (en) * | 2004-07-14 | 2006-01-18 | 淄博齐鲁乙烯化工有限公司 | Fluidized production process for granular calcium chloride |
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| CN109731396A (en) * | 2019-03-11 | 2019-05-10 | 杨松 | It is a kind of to prepare roller kilns dedusting filtrate mixed fluidized bed |
| CN109731396B (en) * | 2019-03-11 | 2021-12-24 | 林贤贵 | Preparation roller kilns removes dust and mixes fluidized bed with filter material |
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| CN109126624B (en) | 2020-07-28 |
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Effective date of registration: 20220106 Address after: 315000 room 306, No. 22, Chuang e Huigu, No. 777, Zhongguan West Road, Zhuangshi street, Zhenhai District, Ningbo City, Zhejiang Province Patentee after: NINGBO JIACHEN HUIGU NEW ENERGY TECHNOLOGY Co.,Ltd. Address before: 362000 the 2 floor of 32 new gate Street and 1916 Creative Industrial Park, Licheng District, Quanzhou, Fujian, China, 1916 Patentee before: Yang Song |
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Granted publication date: 20200728 |