CN107805828A - Press from both sides the post-processing approach of salt titanium valve crude product - Google Patents
Press from both sides the post-processing approach of salt titanium valve crude product Download PDFInfo
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- CN107805828A CN107805828A CN201710996065.XA CN201710996065A CN107805828A CN 107805828 A CN107805828 A CN 107805828A CN 201710996065 A CN201710996065 A CN 201710996065A CN 107805828 A CN107805828 A CN 107805828A
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- titanium valve
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/04—Electrolytic production, recovery or refining of metal powders or porous metal masses from melts
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1295—Refining, melting, remelting, working up of titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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Abstract
The present invention relates to titanium valve recovery method field, especially a kind of post-processing approach for the folder salt titanium valve crude product that wastewater rate is greatly lowered and improves organic efficiency, comprise the following steps：A, folder salt titanium valve crude product obtained by molten-salt electrolysis is positioned in vacuum distillation furnace, the vacuum system for opening vacuum distillation furnace carries out system pump down；B, open heating system to be heated up, after temperature to be distilled rises to target temperature, carry out constant temperature distillation；C, heating system is disconnected after distillation terminates makes system carry out natural cooling, after in-furnace temperature is reduced to room temperature, disconnects retort vacuum system；D, wash, finally obtain titanium valve finished product.The present invention effectively reduces the contaminated wastewater that traditional washing is brought with pickling aftertreatment technology, drastically reduce the area the growing amount of waste water in titanium valve preparation process by the inventive improvements to recovery process.Among the recovery of titanium valve in folder salt titanium valve crude product.
Description
Technical field
The present invention relates to titanium valve recovery method field, especially a kind of post-processing approach for pressing from both sides salt titanium valve crude product.
Background technology
Titanium valve is (high-melting-point, low close except possessing the property of Titanium in itself as one of staple product in titanium industry chain
Degree, corrosion resistant candle, nonmagnetic etc.) beyond, also have the characteristics that low intensity, plasticity are good.It is widely used in electronics industry, aviation boat
My god, 3D printing, medical treatment, the field such as automobile；At present, the process equipment of a variety of preparation high quality titanium valves, such as electricity are developed both at home and abroad
Arc rotary electrode method, plasma rotating electrode process, electron beam rotating pan, electric arc rotation crucible method and recent development without crucible
High-frequency induction melting gas atomization etc..
Deng outer titanium fused salt electrolysis process because that can prepare the porous titanium valve of high-quality, its technology developed recently is rapid, but with
The further expansion of electrolysis installation and yield, the aftertreatment technology of electrolysis gained metallic titanium powder, which turns into, restricts fused salt electrolysis process preparation
The key technology bottleneck of high-quality titanium valve；It is slow that electrolysate folder salt titanium valve crude product post processing speed is progressively highlighted in production process
The problems such as efficiency is low, wastewater flow rate greatly pollutes environment.Using current pickling --- washing process often produces 1t titanium valves and about produced
15~20t brine wastes, and also it is difficult to even if by means such as evaporation, condensing crystallizings the synthesis of sodium salt in waste water, sylvite
Recycle.Although using etc. outer titanium fused salt electrolysis process prepare high-quality titanium valve and possess good commercial application prospect, and accord with
Titanium valve industry development demand is closed, if but wanting its real industrialization production need to urgently seek a low cost, high efficiency, green ring
The aftertreatment technology of the metallic titanium powder of guarantor substitutes current pickling --- washing process.
The Patents and document that draff processing method is refined to titanium tetrachloride have：Patent CN104511595A reports one
The preparation method of the high-purity titanium valve of kind.Domestic Central South University, Zunyi Titanium Industry Co. Ltd. report titanium sponge in NaCl-KCl-
The high-purity titanium valve process of electrolytic preparation in TiClx fused salt mixt systems, but aftertreatment technology and method are not reported.Pan Gangji
Group Co., Ltd of research institute Zhu Fuxing et al. is using the dissolution of absolute ethyl alcohol selectivity, the hot dissolving of insoluble solids product --- cold conditions
The method of crystallization realizes the recovery of KCl in electrolysate and obtains titanium valve；Filtrate through chlorination, distillation realize metatitanic acid second fat prepare and
The recovery of ethanol, but the method complex process, wastewater flow rate are big, less efficient.
The content of the invention
The technical problems to be solved by the invention, which are to provide, a kind of to be greatly lowered wastewater rate and improves organic efficiency
Press from both sides the post-processing approach of salt titanium valve crude product.
The technical solution adopted for the present invention to solve the technical problems is：The post-processing approach of salt titanium valve crude product is pressed from both sides, including
Following steps：
A, folder salt titanium valve crude product obtained by molten-salt electrolysis is positioned in the molybdenum crucible in vacuum distillation furnace, opens vacuum and steam
The vacuum system of furnace carries out system pump down；
B, after system pressure is reduced to 50Pa, open heating system and heated up, temperature to be distilled rises to target temperature
Afterwards, constant temperature distillation is carried out；
C, heating system is disconnected after distillation terminates makes system carry out natural cooling, after in-furnace temperature is reduced to room temperature, breaks
Retort vacuum system is opened, obtains the titanium valve containing very small amount impurity salt；
D, the titanium valve containing very small amount impurity salt is washed, finally obtains titanium valve finished product.
It is further that in the step b, vacuum distillation furnace is cooled down by retort condenser condensed water.
It is further that in vacuum distillation process, vapo(u)rizing temperature scope is 720~750 DEG C.
It is further that the distillation time scope is 1.5h~5h.
It is further that when constant temperature distills, the scope of system pressure is 0.5~10Pa.
It is further that the folder salt titanium valve is mainly made up of titanium valve, NaCl and KCl.
It is further that secondary vacuum distillation, purification are carried out to the sodium salt of gained, sylvite volatile matter after the vacuum distillation
NaCl, the KCl obtained afterwards is returned in molten-salt electrolysis step as new salt and reused.
The beneficial effects of the invention are as follows：The present invention effectively reduces tradition by the inventive improvements to recovery process
The contaminated wastewater that brings of washing and pickling aftertreatment technology, drastically reduce the area the growing amount of waste water in titanium valve preparation process；
The efficiency of recovery is greatly improved simultaneously, reduces the cost that fused salt electrolysis process prepares high-quality titanium valve, lifting process and production
The added value of product.Among the recovery of titanium valve in folder salt titanium valve crude product.
Brief description of the drawings
Fig. 1 is the flow chart of the present invention.
Embodiment
The present invention is further described with reference to the accompanying drawings and examples.
Such as the post-processing approach of Fig. 1 folder salt titanium valve crude product, comprise the following steps：A, by folder salt titanium valve obtained by molten-salt electrolysis
Crude product is positioned in the molybdenum crucible in vacuum distillation furnace, and the vacuum system for opening vacuum distillation furnace carries out system pump down；B, treat
After system pressure is reduced to 50Pa, opens heating system and heated up, after temperature to be distilled rises to target temperature, carry out constant temperature steaming
Evaporate；C, heating system is disconnected after distillation terminates makes system carry out natural cooling, after in-furnace temperature is reduced to room temperature, disconnects distillation
Stove vacuum system, obtain the titanium valve containing very small amount impurity salt；D, the titanium valve containing very small amount impurity salt is washed,
Finally obtain titanium valve finished product.
In the step b of practical operation, in order to ensure that vacuum distillation furnace can not destroyed while distillation by high temperature
The stability of equipment, vacuum distillation furnace can be selected to be cooled down by retort condenser condensed water, so as to ensure that vacuum is steamed
Furnace realizes stable operation on the premise of vapo(u)rizing temperature is ensured.In general, in vacuum distillation process, vapo(u)rizing temperature scope
Preferably 720~750 DEG C, distillation time ranges preferably from 1.5h~5h.In addition, when constant temperature distills, the scope of system pressure is excellent
Elect 0.5~10Pa as.
In general, folder salt titanium valve are mainly made up of titanium valve, NaCl and KCl.As shown in figure 1, for gained after vacuum distillation
Sodium salt, sylvite volatile matter can carry out secondary vacuum distillation, NaCl, the KCl obtained after purification returns to fused salt electricity as new salt
Reused in solution step.
Embodiment
Embodiment 1
When being tested using medium-sized vertical type vacuum distillation furnace, load sample 1000g to be distilled, it is 750 DEG C to control vapo(u)rizing temperature,
During to fix distillation time be 2.5h, system vacuum can reach the vacuum 0.5Pa of actual maximum, and experiment process is actual
System pressure is controlled between 1~10Pa, is evaporated in vacuo, and distillation continues to vacuumize after terminating and cooling down is to room temperature,
Blow-on is collected with volatile matter to distillation leftover, weighed, and product of distillation is entered using detection means such as XRD, SEM, EDS
Row analysis.The a small amount of folder salt titanium valve EDS analysis results of gained are shown in Table 1 after distillation：
The a small amount of folder salt titanium valve of gained after table 1 distills
Above-mentioned as shown by data, the present invention can all take off NaCl in titanium valve crude product, and by most of KCl salt and titanium valve
Separation is realized, substantially reduces the difficulty of titanium valve post processing.
Claims (7)
1. press from both sides the post-processing approach of salt titanium valve crude product, it is characterised in that comprise the following steps：
A, folder salt titanium valve crude product obtained by molten-salt electrolysis is positioned in the molybdenum crucible in vacuum distillation furnace, opens vacuum distillation furnace
Vacuum system carry out system pump down；
B, after system pressure is reduced to 50Pa, open heating system and heated up, after temperature to be distilled rises to target temperature, entered
Row constant temperature distills；
C, heating system is disconnected after distillation terminates makes system carry out natural cooling, after in-furnace temperature is reduced to room temperature, disconnects and steaming
Furnace vacuum system, obtain the titanium valve containing very small amount impurity salt；
D, the folder salt titanium valve containing very small amount fused salt impurity is washed, finally obtains titanium valve finished product.
2. the post-processing approach of folder salt titanium valve crude product as claimed in claim 1, it is characterised in that：In the step b, vacuum is steamed
Furnace is cooled down by retort condenser condensed water.
3. the post-processing approach of folder salt titanium valve crude product as claimed in claim 1, it is characterised in that：In vacuum distillation process, steam
Temperature range is evaporated for 720~750 DEG C.
4. the post-processing approach of folder salt titanium valve crude product as claimed in claim 1, it is characterised in that：The distillation time scope is
1.5h~5h.
5. the post-processing approach of folder salt titanium valve crude product as claimed in claim 1, it is characterised in that：When constant temperature distills, system pressure
The scope of power is 0.5~10Pa.
6. the post-processing approach of folder salt titanium valve crude product as claimed in claim 1, it is characterised in that：The folder salt titanium valve mainly by
Titanium valve, NaCl and KCl are formed.
7. the post-processing approach of folder salt titanium valve crude product as claimed in claim 6, it is characterised in that：To institute after the vacuum distillation
Sodium salt, the sylvite volatile matter obtained carries out secondary vacuum distillation, and NaCl, the KCl obtained after purification returns to molten-salt electrolysis as new salt
Reused in step.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710996065.XA CN107805828A (en) | 2017-10-23 | 2017-10-23 | Press from both sides the post-processing approach of salt titanium valve crude product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710996065.XA CN107805828A (en) | 2017-10-23 | 2017-10-23 | Press from both sides the post-processing approach of salt titanium valve crude product |
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| Publication Number | Publication Date |
|---|---|
| CN107805828A true CN107805828A (en) | 2018-03-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710996065.XA Pending CN107805828A (en) | 2017-10-23 | 2017-10-23 | Press from both sides the post-processing approach of salt titanium valve crude product |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108690916A (en) * | 2018-08-02 | 2018-10-23 | 绵阳力洋英伦科技有限公司 | High temperature distillation separation equipment and separation method applied to titanium sponge fused salt |
| CN110093515A (en) * | 2019-04-16 | 2019-08-06 | 北京科技大学 | A method of the brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948958A (en) * | 2009-12-30 | 2011-01-19 | 陈静 | Non-ferrous metal vacuum electromagnetic suspension distillatory refining method and equipment |
-
2017
- 2017-10-23 CN CN201710996065.XA patent/CN107805828A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948958A (en) * | 2009-12-30 | 2011-01-19 | 陈静 | Non-ferrous metal vacuum electromagnetic suspension distillatory refining method and equipment |
Non-Patent Citations (2)
| Title |
|---|
| 陆爱美 等: "简议海绵钛生产真空蒸馏过程中的质量控制", 《有色金属设计》 * |
| 魏剑: "粗锂脱钠的真空蒸馏研究", 《中国优秀硕士学位论文全文数据库》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108690916A (en) * | 2018-08-02 | 2018-10-23 | 绵阳力洋英伦科技有限公司 | High temperature distillation separation equipment and separation method applied to titanium sponge fused salt |
| CN110093515A (en) * | 2019-04-16 | 2019-08-06 | 北京科技大学 | A method of the brilliant directly distillation-melting of folder salt titanium prepares hypoxemia high purity titanium ingot |
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Application publication date: 20180316 |