CN203359979U - Device for preparing hydrogen fluoride - Google Patents

Device for preparing hydrogen fluoride Download PDF

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CN203359979U
CN203359979U CN 201320407180 CN201320407180U CN203359979U CN 203359979 U CN203359979 U CN 203359979U CN 201320407180 CN201320407180 CN 201320407180 CN 201320407180 U CN201320407180 U CN 201320407180U CN 203359979 U CN203359979 U CN 203359979U
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opening
reactor
conversion zone
pipeline
hydrogen fluoride
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应盛荣
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Dingsheng Chemical & Technology Co Ltd
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Dingsheng Chemical & Technology Co Ltd
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Abstract

The utility model provides a device for preparing hydrogen fluoride, which comprises a reactor, a superheat steam generator and a heating device used for heating calcium fluoride; the reactor comprises a reaction section and a gas collection section, and the gas collection section is arranged at the upper part of the reaction section; the reactor comprises at least a first opening, a second opening and a third opening, the first opening is positioned in the middle upper part of the reaction section, the second opening is positioned in the lower part of the reaction section and the third opening is positioned in the upper part of the gas collection section; the first opening is communicated and hermetically connected with a calcium fluoride conveying pipeline; and the second opening is communicated and hermetically connected with the superheat steam generator through a pipeline. According to the device provided by the utility model, the quantity of devices is small, a production control device is simple, large-scale equipment such as a converter is no longer adopted, the equipment investment is lowered, and energy conservation and consumption reduction are obvious; hydrogen fluoride gas leakage is avoided; and the coefficient of safety is increased greatly.

Description

For the preparation of hydrofluoric device
Technical field
The utility model relates to the chemical reaction equipment field, refers to especially a kind of for the preparation of hydrofluoric device.
Background technology
Hydrogen fluoride (HF) is the basic material of fluorine chemical, is the starting point of most of fluorine chemical product.Can be used for manufacturing the organic or inorganic fluorochemical, as aluminum fluoride, sodium aluminum fluoride, fluorohydrocarbon, anhydrous hydrogen fluoride, organic fluorocompound etc.Hydrogen fluoride mainly makes by fluorite (CaF2) and sulfuric acid reaction, and it reacts as shown in (I): CaF2(s)+H2SO4(l) → 2HF(g)+CaSO4(s) (I)
Owing to there being the impurity such as CaCO3, SiO2 in fluorite, also following side reaction can occur: SiO2(s)+4HF(g) → SiF4(g)+2H2O(g) (II) simultaneously in process of production
SiF4(g)+2HF(g)→H2SiF6(g)(Ⅲ)
CaCO3(s)+H2SO4(l)→CaSO4(s)+H2O(g)(Ⅳ)
Sulfuric acid in raw material and the generation of side reaction all can produce a large amount of water, make the moisture in system more and more, and production can't be carried out.Therefore, traditional hydrogen fluoride gas preparation technology adopts 98% sulfuric acid and oleum (more than 100%) to be mixed with mixing acid and uses, and reaches the purpose of moisture in the balanced production process.But, in such technique, 98% sulfuric acid and oleum price are higher, need it is carried out to accurate-metering, control and corresponding storage, handling equipment simultaneously, make this process costs increase, complex process.Also produced gypsum containing fluorine slag (calcium sulfate), needed to process.And it is complicated to produce equipment, investment is large.
The reference prepared about hydrogen fluoride or hydrofluoric acid is as follows:
Publication number is CN101913565A, and open day is 2010.12.15;
Publication number is CN102471059A, and open day is 2012.5.23;
Publication number CN101214925A, open day is 2008.7.9;
Prior art also has with Fluorspar Powder, sulphur trioxide and water vapour produces hydrogen fluoride (a kind of Fluorspar Powder is produced hydrofluoric method 201210276366.2) in the fluidized state reaction, there is no at present production equipment.
Adopted sulfuric acid or sulphur trioxide, dangerous large, cost is high.Produced gypsum containing fluorine slag (calcium sulfate), needed to process.And it is complicated to produce equipment, investment is large.
Prior art be take in addition silicofluoric acid and sodium sulfate and is prepared hydrofluoric acid (publication number is CN101134561A, open day be 2008.3.5) as raw material, and reaction formula is as follows:
Figure BDA00003483451100021
The method is due to silicofluoric acid at the system internal recycle, and the internal circulating load of material is a lot, so that equipment is huge; Need high temperature when Sodium Silicofluoride decomposes, energy consumption is very large, and resolving device very easily corrodes, and the life-span is very short, so the method does not have practical value.
The utility model content
The utility model proposes a kind ofly for the preparation of hydrofluoric device, solved the problem of production unit complexity in the prior art.
The technical solution of the utility model is achieved in that
A kind ofly for the preparation of hydrofluoric device, comprise,
Reactor, overheating steam generator and be used for heating the heating unit of Calcium Fluoride (Fluorspan);
Described reactor comprises conversion zone and gas collecting segment, and described gas collecting segment is arranged on the top of described conversion zone;
Described reactor comprises at least the first opening, the second opening and the 3rd opening, and described the first opening is positioned at the middle and upper part of described conversion zone, and described the second opening is positioned at the bottom of described conversion zone, and described the 3rd opening is positioned at the top of described gas collecting segment; Described the first opening communicates and is tightly connected with the pipeline of delivery of fluorinated calcium; Described the second opening communicates and is tightly connected with the superheated vapo(u)r hair device by pipeline; The delivery port that described the 3rd opening is hydrogen fluoride gas;
The bottom of described conversion zone is provided with is with foraminate grid distributor.
As preferred technical scheme, the gas collecting segment of described reactor is inverted cone-shaped structure.
As preferred technical scheme, the conversion zone of described reactor is cylindrical structural.
As preferred technical scheme, the bottom of described reactor, the top of grid distributor are provided with for discharging the 4th opening of calcium oxide.
As preferred technical scheme, described device also comprises washing tower and condensing equipment, and described the 3rd opening, washing tower, condensing equipment communicate and are tightly connected by pipeline successively.
As preferred technical scheme, described device also comprises absorption tower, and described absorption tower communicates and is tightly connected by pipeline with described the 3rd opening.
Beneficial effect
(1) appliance arrangement quantity of the present utility model is few, and the production control device is simple, no longer adopts the main equipments such as converter, and the facility investment volume reduces, obviously energy-saving and cost-reducing.
(2) device of the present utility model can not produce the hydrogen fluoride gas leakage; Safety coefficient improves greatly.
The accompanying drawing explanation
In order to be illustrated more clearly in the utility model embodiment or technical scheme of the prior art, below will the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described, apparently, accompanying drawing in the following describes is only embodiments more of the present utility model, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1: a kind of structure iron for the preparation of hydrofluoric device of the present utility model;
Fig. 2: another kind of the present utility model is for the preparation of the structure iron of hydrofluoric device;
Fig. 3: the third structure iron for the preparation of the device that water hydrofluoric acid is arranged of the present utility model.
Embodiment
Below will the technical scheme in the utility model embodiment be clearly and completely described, obviously, described embodiment is only the utility model part embodiment, rather than whole embodiment.Embodiment based in the utility model, those of ordinary skills are not making under the creative work prerequisite the every other embodiment obtained, and all belong to the scope of the utility model protection.
The utility model be take Calcium Fluoride (Fluorspan) as raw material, is decomposed into hydrogen fluoride and calcium oxide in high-temperature vapor, and hydrogen fluoride is the purpose product, and calcium oxide can be used for the raw material that cement is manufactured.
Chemical equation:
CaF 2+H 2O→CaO+2HF↑
As shown in Figure 1: for the preparation of hydrofluoric device 1, comprise reactor 11, overheating steam generator 12 and be used for heating the heating unit 13 of Calcium Fluoride (Fluorspan).Reactor 11 is divided into conversion zone 1101 and gas collecting segment 1102.Be provided with 4 openings on reactor 11, respectively for adding the first opening 111 of raw material Calcium Fluoride (Fluorspan), for entering the second opening 112 of overheated steam, for the 3rd opening 113 of exporting hydrogen fluoride gas with for discharging, take four opening 114 of calcium oxide as main solid materials.Wherein the first opening, the second opening and the 4th opening are positioned on conversion zone 1101, the first opening 114 is arranged on the middle and upper part of conversion zone 1101, the second opening is arranged on the bottom of conversion zone 1101, and the 4th opening is positioned at the bottom of conversion zone 1101 and on the top of the second opening.The inside of conversion zone 1101 also is provided with is with foraminate grid distributor 115, grid distributor 115 to be positioned at the top of the second opening and the bottom of the 4th opening, for by overheated steam and prevent that material is directly from the bottom landing.Cross for delivery of the device for cleaning pipeline of calcium oxide the conversion zone 1101 that the first opening 111 enters reactor 11, heating unit 13 is pipeline heater (for commercially available prod).Overheating steam generator 12(is commercially available prod) be used for water is become to overheated steam, enter the conversion zone 1101 of reactor 11 by the second opening, aperture on grid distributor 115 wherein is the passage passed through for overheated steam, simultaneously, reaction raw materials Calcium Fluoride (Fluorspan) is fluidized state in conversion zone 1101, can not fall down by the aperture on grid distributor 115.Conversion zone 1101 of the present utility model is similar with the principle of fluidized-bed reactor.The hydrogen fluoride gas generated after reaction is discharged by the 3rd opening 113.
As shown in Figure 2, for the preparation of hydrofluoric device 2, this device is compared with the device that accompanying drawing 1 shows, has increased washing tower 21, condensing equipment 22 and storage tank 23.The 3rd opening 113, washing tower 21, condensing equipment 22, storage tank 23 communicate and are tightly connected by pipeline successively.Enter from the hydrogen fluoride gas of the 3rd opening 113 outputs the dehydration washing tower 21 that contains the vitriol oil, use the vitriol oil to clean, remove moisture and solid dust, enter afterwards condensing works 22, be condensed into hydrogen fluoride liquid, be stored in storage tank 23 after making with extra care.
As shown in Figure 3, for the preparation of hydrofluoric device 3, this device is compared with the device that accompanying drawing 1 shows, has increased absorption tower 31 and storage tank 32.The 3rd opening 113, absorption tower 31, storage tank 32 communicate and are tightly connected by pipeline successively.Entered water hydrofluoric acid absorption tower 31 from the hydrogen fluoride gas of the 3rd opening 113 outputs, obtained hydrofluoric acid liquid, be stored in afterwards in storage tank 32.
The apparatus structure that accompanying drawing 1 shows is basic structure of the present utility model, can be according to the requirement difference that makes product, and increase equipment, such as increasing absorption tower, or increase washing tower etc.
Application examples 1:
Raw material: Fluorspar Powder (CaF 2content is 97.1%) be 1500g, the water (H that high-temperature steam is used 2o) 900g.
Preparation process is as follows: the preparation facilities of use is participated in shown in accompanying drawing 1.
Fluorspar Powder is put into to pipeline and be heated to 950 ℃, then add in reactor 11 by the first opening 111.The high-temperature steam water is added in overheating steam generator 12, be heated to 1100 ℃, vapour pressure is 0.1MPa.Overheated steam out in overheating steam generator 12 is passed in reactor 11 by the pipeline be connected with the second opening 112.In reaction process, Fluorspar Powder is fluidized state, overheated steam makes progress away by the aperture on grid distributor 115, hydrogen fluoride gas (HF) 718g generated after reaction draws by the 3rd opening 113 of reactor 11, the particle wherein risen along with gas is because reactor 11 gas collecting segments 1102 are inverted cone-shaped structure, lift velocity is slack-off, and natural landing is proceeded reaction to the conversion zone 1101 of reactor.What reaction generated take calcium oxide (CaO) as main solid materials 1069g, by the 4th opening 14, discharges.
Application examples 2:
Raw material: Fluorspar Powder (CaF 2content is 97.1%) be 1500g, the water (H that high-temperature steam is used 2o) 900g, the sulfuric acid 12kg that mass percent is 98%.
Preparation process is as follows: the preparation facilities of use is participated in shown in accompanying drawing 2.
Fluorspar Powder is put into to pipeline and be heated to 550 ℃, then add in reactor 11 by the first opening 111.The high-temperature steam water is added in overheating steam generator 12, be heated to 950 ℃, vapour pressure is 1.0MPa.Overheated steam out in overheating steam generator 12 is passed in reactor 11 by the pipeline be connected with the second opening 112.In reaction process, Fluorspar Powder is fluidized state, overheated steam makes progress away by the aperture on grid distributor 115, the hydrogen fluoride gas (HF) generated after reaction is drawn by the 3rd opening 113 of reactor 11, the particle wherein risen along with gas is because reactor 11 gas collecting segments 1102 are inverted cone-shaped structure, lift velocity is slack-off, and natural landing is proceeded reaction to the conversion zone 1101 of reactor.The hydrogen fluoride gas that reaction obtains enters washing tower 21 by the 3rd opening 113, uses the vitriol oil to clean, and removes moisture and solid dust, enters afterwards condensing works 22, is condensed into hydrogen fluoride liquid, after making with extra care, obtains hydrogen fluoride liquid 610g, is stored in storage tank 23.
What reaction generated take calcium oxide (CaO) as main solid materials 1102g, by the 4th opening 14, discharges.
Application examples 3:
Raw material: Fluorspar Powder (CaF 2content is 97.1%) be 1500g, the water (H that high-temperature steam is used 2o) 900g.Absorb the water 2000g of use.
Preparation process is as follows: the preparation facilities of use is participated in shown in accompanying drawing 3.
Fluorspar Powder is put into to pipeline and be heated to 950 ℃, then add in reactor 11 by the first opening 111.The high-temperature steam water is added in overheating steam generator 12, be heated to 950 ℃, vapour pressure is 0.5MPa.Overheated steam out in overheating steam generator 12 is passed in reactor 11 by the pipeline be connected with the second opening 112.In reaction process, Fluorspar Powder is fluidized state, overheated steam makes progress away by the aperture on grid distributor 115, the hydrogen fluoride gas (HF) generated after reaction enters absorption tower 31 by the 3rd opening 113 of reactor 11, the hydrogen fluoride gas water obtained obtains the hydrofluoric acid 2719g of content 26.2% after absorbing, what reaction generated take calcium oxide (CaO) as main solid materials 1066g, by the 4th opening 14, discharges.
These are only preferred embodiment of the present utility model, not in order to limit the utility model, all within spirit of the present utility model and principle, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection domain of the present utility model.

Claims (6)

1. one kind for the preparation of hydrofluoric device, comprise,
Reactor, overheating steam generator and be used for heating the heating unit of Calcium Fluoride (Fluorspan);
Described reactor comprises conversion zone and gas collecting segment, and described gas collecting segment is arranged on the top of described conversion zone;
Described reactor comprises at least the first opening, the second opening and the 3rd opening, and described the first opening is positioned at the middle and upper part of described conversion zone, and described the second opening is positioned at the bottom of described conversion zone, and described the 3rd opening is positioned at the top of described gas collecting segment; Described the first opening communicates and is tightly connected with the pipeline of delivery of fluorinated calcium; Described the second opening communicates and is tightly connected with the superheated vapo(u)r hair device by pipeline; The delivery port that described the 3rd opening is hydrogen fluoride gas;
The bottom of described conversion zone is provided with is with foraminate grid distributor.
2. device according to claim 1, is characterized in that, the gas collecting segment of described reactor is inverted cone-shaped structure.
3. device according to claim 1, is characterized in that, the conversion zone of described reactor is cylindrical structural.
4. device according to claim 1, is characterized in that, the bottom of described reactor, the top of grid distributor are provided with for discharging the 4th opening of calcium oxide.
5. according to the described device of the arbitrary claim of claim 1-4, it is characterized in that, described device also comprises washing tower and condensing equipment, and described the 3rd opening, washing tower, condensing equipment communicate and are tightly connected by pipeline successively.
6. according to the described device of the arbitrary claim of claim 1-4, it is characterized in that, described device also comprises absorption tower, and described absorption tower communicates and is tightly connected by pipeline with described the 3rd opening.
CN 201320407180 2013-07-09 2013-07-09 Device for preparing hydrogen fluoride Withdrawn - After Issue CN203359979U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103332655A (en) * 2013-07-09 2013-10-02 衢州市鼎盛化工科技有限公司 Hydrogen fluoride preparation method and apparatus thereof
CN106829867A (en) * 2017-04-14 2017-06-13 衢州市鼎盛化工科技有限公司 The method and apparatus of fluorine-containing mixing spent acid comprehensive reutilization

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103332655A (en) * 2013-07-09 2013-10-02 衢州市鼎盛化工科技有限公司 Hydrogen fluoride preparation method and apparatus thereof
CN103332655B (en) * 2013-07-09 2015-06-17 衢州市鼎盛化工科技有限公司 Hydrogen fluoride preparation method and apparatus thereof
CN106829867A (en) * 2017-04-14 2017-06-13 衢州市鼎盛化工科技有限公司 The method and apparatus of fluorine-containing mixing spent acid comprehensive reutilization

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Granted publication date: 20131225

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