CN205973775U - Device by fluosilicic acid preparation hydrogen fluoride - Google Patents

Device by fluosilicic acid preparation hydrogen fluoride Download PDF

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CN205973775U
CN205973775U CN201620195245.9U CN201620195245U CN205973775U CN 205973775 U CN205973775 U CN 205973775U CN 201620195245 U CN201620195245 U CN 201620195245U CN 205973775 U CN205973775 U CN 205973775U
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delivery outlet
import
solid
bed
rectifying column
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应盛荣
姜战
应悦
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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 discloses a device by fluosilicic acid preparation hydrogen fluoride, include ammoniation reaction cauldron, filter, synthetic reation kettle, separation solid -liquid apparatus, rectifying column, drying -machine, forge burning furnace and fluidization reaction bed, the ammoniation reaction cauldron with the filter is connected, the filter with synthetic reation kettle connects, synthetic reation kettle with separation solid -liquid apparatus connects, separation solid -liquid apparatus still is connected with the rectifying column with the drying -machine, the rectifying column with the ammoniation reaction cauldron is connected, the drying -machine with it connects to forge burning furnace, forge burning furnace with the fluidization reaction bed is connected, the fluidization reaction bed still with synthetic reation kettle connects. The device has realized the calcium oxide cyclic utilization that preparation hydrogen fluoride in -process produced to make the purity of final hydrogen fluoride product reach more than 99.9999%.

Description

A kind of device being prepared fluohydric acid gas by hexafluosilicic acid
Technical field
This utility model belongs to fluohydric acid gas preparing technical field and in particular to one kind prepares fluohydric acid gas by hexafluosilicic acid Device.
Background technology
Fluohydric acid gas (Hydrogen Fluoride), chemical molecular formula is HF, molecular weight 20.01, soluble in water, Ethanol.It is colourless transparent liquid under anhydrous hydrogen fluoride (abbreviation AHF) low temperature or pressure, 19.4 DEG C of boiling point, - 83.37 DEG C of fusing point, density 1.008g/cm3(water=1).Under room temperature with room temperature, highly volatile becomes white smoke. Its chemical property is extremely active, can react with alkali, metal, oxide and silicate etc..Fluohydric acid gas is existing Generation fluorination work basis, be produce element fluorine, various fluorine refrigerant, fluorine-containing new material, inorganic fluorine salt dissolving, The most basic raw material of various organic fluorides etc..
China mainly adopts fluorite and sulfuric acid reaction preparation to produce AHF, although the hydrogen fluoride production technology of China It is in world lead level, but the problems of " fluorite sulfuric acid process " production technology, such as:The energy Utilization rate is low, and production cost is higher, and dust pollution is serious etc., still can not be ignored.Advocate energy-conservation in the whole world Consumption reduction, the epoch of development low-carbon economy, explore new production technology and technique has become the common recognition of insider. Along with fluorite is the non-renewable grand strategy resource that national requirements controls, in recent years, government is to fluorite The control of ore deposit yield is more and more tighter, and policy is also received tighter and tighter, and the fluorine resource price of fluorite must more and more higher. So, how to develop the fluorine efficient low-consume from by-product fluosilicic acid, produce fluohydric acid gas technology to environmental protection Increasingly draw attention.
Chinese patent application Publication No. CN103754824A discloses one kind and utilizes phosphate fertilizer by-product hexafluosilicic acid system The method of standby fluohydric acid gas, mainly comprises the following steps and prepares fluohydric acid gas ammonia solid with hexafluosilicic acid for raw material, then will with dense Sulfuric acid reaction prepares Fluohydric acid..Although the method protects fluorite and fluorine resource, need in its preparation process Will be with concentrated sulphuric acid as raw material, not only severe reaction conditions, and also effect on environment is big, and reaction finally gives Fluorination hydrogen purity is lower.Further, this reaction uses ammonia and prepares ammonium fluoride, and such ammonium fluoride is molten Liquid concentration is too low, needs to concentrate, increases thermal energy consumption.In order that silicon dioxide becomes white carbon, just The form making silicon dioxide form white carbon can only be only possible at low concentrations.Liao Jing China in 2014 and Wang Li Fine jade exists《Environmental science guide》33rd phase delivered in " ammonium fluoride prepares the research of calcium fluoride optimal conditionss " and has carried To calcium fluoride mainly for the production of Fluohydric acid., with lime cream and ammonium fluoride solution preparation fluorination calcium product, it is anti- The calcium fluoride purity that should produce is only 89.17%, this is because the impurity content of pulverized limestone is high, its calcium fluoride Product purity is relatively low.
Utility model content
For solution is existing, the harshness of preparation process condition present in fluohydric acid gas and product are prepared for raw material with hexafluosilicic acid The low problem of product purity, the utility model proposes a kind of device being prepared fluohydric acid gas by hexafluosilicic acid, this device is in fact Show the calcium oxide producing during preparing fluohydric acid gas to recycle, and make the pure of final fluorination hydrogen production Degree reaches more than 99.9999%.
The technical solution of the utility model is realized in:
A kind of by hexafluosilicic acid prepare fluohydric acid gas device it is characterised in that include aminating reaction kettle, filter, Synthesis reaction vessel, solid-liquid separating equipment, rectifying column, dehydrator, calcining furnace and fluidized reaction bed, described ammonia Change reactor to be connected with described filter, described filter is connected with described synthesis reaction vessel, described synthesis is anti- Answer kettle to be connected with described solid-liquid separating equipment, described solid-liquid separating equipment be also associated with described rectifying column with described Dehydrator, described rectifying column is connected with described aminating reaction kettle, and described dehydrator is connected with described calcining furnace, Described calcining furnace is connected with described fluidized reaction bed, and described fluidized reaction bed is also connected with described synthesis reaction vessel.
Further, described synthesis reaction vessel is provided with ammonium fluoride solution import, calcium oxide import and synthesis and produces Thing delivery outlet, described solid-liquid separating equipment is provided with material inlet, weak ammonia delivery outlet and calcium fluoride output Mouthful, described fluidized reaction bed is provided with calcium fluoride import, superheated steam import, fluohydric acid gas delivery outlet and oxygen Change calcium delivery outlet, the calcium oxide delivery outlet of the calcium oxide import of described synthesis reaction vessel and described fluidized reaction bed Connect, the material inlet that described synthetic product delivery outlet is arranged with described solid-liquid separation is connected, described weak ammonia Delivery outlet is connected with described rectifying column, and the calcium fluoride delivery outlet of described solid-liquid separating equipment is with described dehydrator even Connect, the calcium fluoride import of described fluidized reaction bed is connected with described calcining furnace.
The beneficial effects of the utility model are,
The present inventor is surprised to find with calcium fluoride in R&D process (Chinese patent 201310288043X) During preparing fluohydric acid gas for raw material, its produce calcium oxide purity can reach 99% and more than;And incite somebody to action If this by-product-calcium oxide and ammonium fluoride solution are reacted, its not only can obtain purity reach 99 and with On calcium fluoride, thus purity is obtained reach more than 99.9999% fluorination hydrogen production, and achieve following of calcium Ring utilizes.
Brief description
In order to be illustrated more clearly that this utility model embodiment or technical scheme of the prior art, below will be right In embodiment or description of the prior art the accompanying drawing of required use be briefly described it should be apparent that, below Accompanying drawing in description is only some embodiments of the present utility model, for those of ordinary skill in the art, On the premise of not paying creative work, can also obtain other accompanying drawings according to these accompanying drawings.
Fig. 1 is prepared the structural representation of the device of fluohydric acid gas for this utility model by hexafluosilicic acid.
Accompanying drawing indicates:1st, aminating reaction kettle, 2, filter, 3, synthesis reaction vessel, 4, solid-liquid separation sets Standby, 5, rectifying column, 6, dehydrator, 7, calcining furnace, 8, fluidized reaction bed, 31, ammonium fluoride solution enters Mouthful, 32, calcium oxide import, 33, synthetic product delivery outlet, 41, material inlet, 42, weak ammonia output Mouthful, 43, calcium oxide delivery outlet, 81, calcium fluoride import, 82, superheated steam import, 83, fluohydric acid gas defeated Outlet, 84, calcium oxide delivery outlet.
Specific embodiment
Below in conjunction with the accompanying drawing in this utility model embodiment, to the technical side in this utility model embodiment Case is clearly and completely described it is clear that described embodiment is only this utility model part reality Apply example, rather than whole embodiments.Based on the embodiment in this utility model, ordinary skill people The every other embodiment that member is obtained under the premise of not making creative work, broadly falls into this utility model The scope of protection.
With reference to Fig. 1, a kind of device being prepared fluohydric acid gas by hexafluosilicic acid, including aminating reaction kettle 1, filter 2, Synthesis reaction vessel 3, solid-liquid separating equipment 4, rectifying column 5, dehydrator 6, calcining furnace 7 and fluidized reaction bed 8. Aminating reaction kettle 1 is connected with filter 2, and filter 2 is connected with synthesis reaction vessel 3, synthesis reaction vessel 3 It is connected with solid-liquid separating equipment 4, solid-liquid separating equipment 4 is also associated with rectifying column 5 and dehydrator 6, rectifying column 5 are connected with aminating reaction kettle 1, and dehydrator 6 is connected with calcining furnace 7, and calcining furnace 7 is with fluidized reaction bed 8 even Connect, fluidized reaction bed 8 is also connected with synthesis reaction vessel 3.
Further, synthesis reaction vessel 3 is provided with ammonium fluoride solution import 31, calcium oxide import 32 and synthesis Product delivery outlet 33.Solid-liquid separating equipment 4 is provided with material inlet 41, weak ammonia delivery outlet 42 and fluorine Change calcium delivery outlet 43.Fluidized reaction bed 8 is provided with calcium fluoride import 81, superheated steam import 82, fluohydric acid gas Delivery outlet 83 and calcium oxide delivery outlet 84.Calcium oxide import 32 and the fluidized reaction bed of synthesis reaction vessel 3 8 calcium oxide delivery outlet 84 connects, and synthetic product delivery outlet 33 arranges 4 material inlet with solid-liquid separation 41 connections, weak ammonia delivery outlet 42 is connected with rectifying column 5, the calcium fluoride delivery outlet of solid-liquid separating equipment 4 43 are connected with dehydrator 6, and the calcium fluoride import 81 of fluidized reaction bed 8 is connected with calcining furnace 7.
The foregoing is only preferred embodiment of the present utility model, not in order to limit this utility model, All of the present utility model spirit and principle within, any modification, equivalent substitution and improvement made etc., all Should be included within protection domain of the present utility model.

Claims (2)

1. a kind of by hexafluosilicic acid prepare fluohydric acid gas device it is characterised in that include aminating reaction kettle, filtration Device, synthesis reaction vessel, solid-liquid separating equipment, rectifying column, dehydrator, calcining furnace and fluidized reaction bed, institute State aminating reaction kettle to be connected with described filter, described filter is connected with described synthesis reaction vessel, described conjunction Become reactor be connected with described solid-liquid separating equipment, described solid-liquid separating equipment be also associated with described rectifying column and Described dehydrator, described rectifying column is connected with described aminating reaction kettle, and described dehydrator is with described calcining furnace even Connect, described calcining furnace is connected with described fluidized reaction bed, described fluidized reaction bed also with described synthesis reaction vessel Connect.
2. according to claim 1 the device of fluohydric acid gas is prepared by hexafluosilicic acid it is characterised in that described Synthesis reaction vessel is provided with ammonium fluoride solution import, calcium oxide import and synthetic product delivery outlet, described solid Liquid separation equipment is provided with material inlet, weak ammonia delivery outlet and calcium fluoride delivery outlet, described fluidized reaction Bed is provided with calcium fluoride import, superheated steam import, fluohydric acid gas delivery outlet and calcium oxide delivery outlet, described The calcium oxide import of synthesis reaction vessel is connected with the calcium oxide delivery outlet of described fluidized reaction bed, and described synthesis is produced The material inlet that thing delivery outlet is arranged with described solid-liquid separation is connected, described weak ammonia delivery outlet and described rectification Tower connects, and the calcium fluoride delivery outlet of described solid-liquid separating equipment is connected with described dehydrator, described fluidized reaction The calcium fluoride import of bed is connected with described calcining furnace.
CN201620195245.9U 2016-03-14 2016-03-14 Device by fluosilicic acid preparation hydrogen fluoride Active CN205973775U (en)

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