CN204768725U - Closed niobium oxide apparatus for producing - Google Patents

Closed niobium oxide apparatus for producing Download PDF

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Publication number
CN204768725U
CN204768725U CN201520508898.3U CN201520508898U CN204768725U CN 204768725 U CN204768725 U CN 204768725U CN 201520508898 U CN201520508898 U CN 201520508898U CN 204768725 U CN204768725 U CN 204768725U
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CN
China
Prior art keywords
closed
ammonia
layer
tank body
niobium oxide
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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.)
Expired - Fee Related
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CN201520508898.3U
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Chinese (zh)
Inventor
王常清
易艳萍
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Yichun Jinyang New Meterials Co Ltd
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Yichun Jinyang New Meterials Co Ltd
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Priority to CN201520508898.3U priority Critical patent/CN204768725U/en
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Expired - Fee Related legal-status Critical Current
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Abstract

The utility model provides a closed niobium oxide apparatus for producing, it includes reaction unit, reaction unit includes the retort body, is equipped with feed inlet, discharge gate, intake pipe, agitating unit on the retort is personally experienced sth. Part of the body, the retort body is the withstand voltage device of closed, the withstand voltage device of closed includes voltage resistance, delays presses the layer to reach outer wall layer, it is internal that voltage resistance locates the jar, presses the layer for delaying between voltage resistance and the outer wall layer. The device has broken through at present and led to the neutralizing way of ammonia under the system of opening wide, adopts to let in the ammonia in the presence of the pressure certain in airtight system, has both accelerated the reaction rate, and the control to the volume of letting in the ammonia can be realized again to the while, furthest has practiced thrift manufacturing cost, can realize the zero release of ammonia, has solved in the production process pollution problem to the environment.

Description

Closed niobium oxide process units
technical field:
The utility model relates to prepares niobium oxide process units field, particularly a kind of closed niobium oxide process units.
background technology:
Niobium is important rare metal, is widely used in the industrial circles such as space flight and aviation, atomic energy, metallurgy, telecommunications, petrochemical industry, glass ceramics, and countries in the world government pays much attention to the development of the strategic material of niobium industry.
Niobium oxide is a kind of important niobium product, is arranged in the source of niobium industrial chain, the other products of nearly all niobium, is all be that raw material obtains with niobium oxide.In recent years, the consumption of niobium oxide is very active, and world's niobium demand annual amplification is stabilized in more than 10%, and China is niobium consumption big country, and average annual amplification is close to 30%.Along with the application of niobium deepens constantly, estimate that the demand of following niobium oxide keeps higher growth rate by continuing.
Preparation facilities and the method for current niobium oxide generally adopt HF-H 2sO 4-MIBK hydrometallurgical processes, its technological process is, after tantalum-niobium concentrate grinds, use HF-H 2sO 4nitration mixture decomposes, decomposed solution organic solvent extraction, after tantalum niobium organic phase purification and impurity removal, strips obtain the fluorine niobic acid aqueous solution, fluorine niobic acid aqueous solution alkali neutralization precipitation with anti-niobium liquid, then can produce Nb through filtration, oven dry, calcining 2o 5.Wherein neutralization precipitation one step of fluorine niobic acid, the normally used alkali of industrial production is precipitate after liquefied ammonia is converted into ammonia.The advantage of ammonia is relative inexpensiveness, and impurity is easily removed, and is conducive to large-scale production, so in the preparation of niobium oxide, ammonia is the most frequently used precipitating reagent of industrial production.The process units of existing normal employing is generally an open reaction vessel, under the condition that ammonia outlet opens wide, fluorine niobic acid system ammonia being passed into acidity is translated into niobium hydroxide and carries out neutralization precipitation, can inevitably there is escaping in a large number of ammonia in this device, cause the increase of production cost, bring larger pressure to environment protection treating simultaneously.
The Chinese patent being CN1203567A as Chinese publication number discloses kind of the method producing niobium oxide powder, wherein, in in the stirred reactor of niobium liquid more than 2 or 2 and, by the niobium oxide powder controlling temperature in each reactor, pH value, sediment time of staying in each reactor produce different-grain diameter and shape.But this apparatus structure is relatively more complicated, and reaction process is longer, thus increases production cost accordingly.And the reaction unit one of existing employing opened type causes waste to raw material ammonia, and to environment; The reaction unit of existing opened type, not withstand voltage on the other hand, and namely cannot react under pressure exists, so just need the reaction time more grown, this equally also can increase the production cost of product.
utility model content:
The purpose of this utility model is the deficiency for existing process units, a kind of closed niobium oxide process units is provided, this device breach at present under unlimited system in logical ammonia and way, ammonia is passed under adopting pressure certain in enclosed system to exist, both accelerated reaction speed, and the control to passing into ammonia amount can being realized again simultaneously, having saved production cost to greatest extent, the zero-emission of ammonia can be realized, solve the pollution problem to environment in production process.
For achieving the above object, the utility model is by the following technical solutions:
oneplant closed niobium oxide process units, comprise reaction unit, described reaction unit comprises reacting tank body, reacting tank body is provided with charging aperture, discharging opening, air inlet pipe, agitating device, described reacting tank body is closed pressure-resistant apparatus, described closed pressure-resistant apparatus comprises Withstand voltage layer, slow pressure layer and outer wall layer, and described Withstand voltage layer is located in tank body, is slow pressure layer between Withstand voltage layer and outer wall layer.
The top of described reacting tank body is provided with blast pipe, and blast pipe is provided with safety device.
Described reacting tank body is hydrostatic column, and the diameter controlling hydrostatic column is 1.2-3.5 rice, is highly 1.5-3.5 rice.
The body border tube wall that described air inlet pipe is positioned at reacting tank body is provided with some breeder tubes.
The utility model has following beneficial effect:
Use the niobium hydroxide that the utility model closed reaction unit obtains, then obtained niobium oxide powder, has less particle diameter, distribution of particles also evenly, logical ammonia N-process ammonia utilization rate is high, and environmental pollution is little to be specially:
(1), that the utility model prepares niobium oxide powder ammonia utilization rate is high, and almost can arrive the zero-emission of ammonia, environmental pollution is little;
(2) the niobium oxide powder particle diameter little (0.1um-1.0um), through the utility model device prepared, particle size distribution is little;
(3), the utility model equipment is simple, easily operates; Adopt under pressure existent condition, pass into ammonia, improve the speed preparing niobium oxide greatly, comparatively opened type reaction unit, react safer, more secure to operator, and can not pollute production environment, prepare niobium oxide powder efficiency high.
Accompanying drawing explanation
fig. 1for the structural representation of the utility model process units;
In figure: 1, reacting tank body, 2, Withstand voltage layer, 3 slow pressure layers, 4, outer wall layer, 5, floss hole, 6, breeder tube, 7, charging aperture, 8 agitators, 9 stirring motors, 10 discharging openings, 11, safety device, air inlet pipe 12.
detailed description of the invention:the utility model is described in further detail below.
embodiment 1,
First by containing tantalum, niobium ore through broken, be milled to-300 orders, through H 2s0 4-HF system is decomposed, and the acid solution organic solvent containing tantalum niobium extracts.Obtain highly purified fluorotantalic acid solution and fluooxycolumbic acid solution.Niobium liquid utilizes ammoniacal liquor as follows as precipitating reagent precipitation reaction:
H 2NbF 7+7NH 3H 20→Nb(OH) 5↓+7NH 4F+H 2O
The feed postition of the utility model precipitating reagent is passed into by ammonia in niobium liquid; In niobium hydroxide chemical precipitation process, the growth of particle experienced by nucleation, growth, coalescent and aggregation procedure, in each tiny area, degree of supersaturation minor variations will cause nucleus number to change in a large number, thus make nucleus not of uniform size, namely mutually merge the larger particle of formation between nucleus, between nucleus and particulate or between particulate, thus inhibit secondary nucleation and nucleus growth.Airtight logical ammonia neutralising arrangement of the present utility model, under strong stirring, ammonia is passed into niobium liquid surface through ammonia import under air-tight state, significantly increase the contact surface of ammonia and niobium liquid, can effectively increase instantaneous nucleation number, prevent the degree of supersaturation of local in niobium liquid from reducing rapidly, thus prevent particle agglomeration, growth.The utility model closed niobium oxide process units, its reacting tank body is a billy, and controlling diameter is 1.2 meters-3.5 meters, and height is for being 1.5 meters-3.5 meters, and material can be the anticorrosives such as stainless steel, irony, liner rubber; Be circular arc bottom billy, and have discharging opening.
As shown in Figure 1, closed niobium oxide process units described in the utility model, comprise a reaction unit, described reaction unit comprises reacting tank body 1, reacting tank body 1 is provided with charging aperture 7, discharging opening 10, air inlet pipe 12, floss hole 5, agitator 8, and described reacting tank body 1 is pressure-resistant apparatus, and described pressure-resistant apparatus comprises Withstand voltage layer 2, slow pressure layer 3, outer wall layer 4, Withstand voltage layer 2 is located at inner tank wall, is set to delay to press layer 3 between Withstand voltage layer 2 and outer wall layer 4; Stirring motor 9 is connected with on agitator 8 top, a safety device 11 is provided with on air inlet pipe 12 top, described safety device 11 can be pressure controller valve, or induction installation is as Inductance valve, as when the reaction pressure of reacting tank body 1 inner chamber is excessive, adding of ammonia is controlled, to ensure the safety in production in reaction unit and course of reaction by safety device 11.A discharging opening 10 is provided with in the bottom of reacting tank body 1.
As preferably, reacting tank body 1 of the present utility model is set to billy, and its diameter is 1.2 meters, is highly 2 meters, when using the utility model to prepare superfine niobium oxide, get fluooxycolumbic acid solution 1000 liters, prepare liquefied ammonia and gasification installation, conveyance conduit, niobium liquid is transported in reactor of the present utility model, add deionized water and regulate niobium liquid concentration, controlling agitator speed is about 25 revs/min, ammonia is passed into niobium liquid surface reacting tank body 1 from air inlet pipe 12 mouthfuls, also can adopt in niobium liquid air inlet pipe 12 is inserted in reacting tank body 1, the outside wall surface border being positioned at reacting tank body 1 in reaction air inlet pipe 12 is provided with breeder tube 6, such ammonia and niobium liquid react, until pH is 9.5, precipitation is transferred to ceramic filter from the discharging opening 10 of bottom, utilizes 1-5% ammoniacal liquor and deionized water washing, dry, dry, the niobium hydroxide after drying is pulverized, then uses incinerator calcination, obtain Nb 2o 5through grinding, the obtained finished product niobium oxide of screening.Using the utility model device can prepare particle diameter is superfine niobium oxide powder O.1-1.Oum.
The foregoing is only the preferred embodiment of the utility model and oneself; not limit practical range of the present utility model with this; all persons that is familiar with technique; use principle of the present utility model and technical characteristic; the various change done and decoration, all should be covered by within protection category that these claims define.

Claims (4)

1. a closed niobium oxide process units, comprise reaction unit, described reaction unit comprises reacting tank body, reacting tank body is provided with charging aperture, discharging opening, air inlet pipe, agitating device, it is characterized in that, described reacting tank body is closed pressure-resistant apparatus, and described closed pressure-resistant apparatus comprises Withstand voltage layer, slow pressure layer and outer wall layer, described Withstand voltage layer is located in tank body, is slow pressure layer between Withstand voltage layer and outer wall layer.
2. a kind of closed niobium oxide process units as claimed in claim 1, it is characterized in that being provided with blast pipe in the top of described reacting tank body, blast pipe is provided with safety device.
3. a kind of closed niobium oxide process units as claimed in claim 1, is characterized in that described reacting tank body is hydrostatic column, and the diameter controlling hydrostatic column is 1.2-3.5 rice, is highly 1.5-3.5 rice.
4. a kind of closed niobium oxide process units as claimed in claim 1, is characterized in that the body border tube wall that described air inlet pipe is positioned at reacting tank body is provided with some breeder tubes.
CN201520508898.3U 2015-07-14 2015-07-14 Closed niobium oxide apparatus for producing Expired - Fee Related CN204768725U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201520508898.3U CN204768725U (en) 2015-07-14 2015-07-14 Closed niobium oxide apparatus for producing

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201520508898.3U CN204768725U (en) 2015-07-14 2015-07-14 Closed niobium oxide apparatus for producing

Publications (1)

Publication Number Publication Date
CN204768725U true CN204768725U (en) 2015-11-18

Family

ID=54508856

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201520508898.3U Expired - Fee Related CN204768725U (en) 2015-07-14 2015-07-14 Closed niobium oxide apparatus for producing

Country Status (1)

Country Link
CN (1) CN204768725U (en)

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C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20151118

Termination date: 20170714