CN104745822A - Method for extracting titanium ions from titanium alloy chemical-milling waste liquid - Google Patents
Method for extracting titanium ions from titanium alloy chemical-milling waste liquid Download PDFInfo
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- CN104745822A CN104745822A CN201510107958.5A CN201510107958A CN104745822A CN 104745822 A CN104745822 A CN 104745822A CN 201510107958 A CN201510107958 A CN 201510107958A CN 104745822 A CN104745822 A CN 104745822A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for extracting titanium ions from titanium alloy chemical-milling waste liquid, which comprises the following typical steps: taking 200mL of titanium alloy chemical-milling waste liquid, putting the waste liquid into a plastic beaker, adding 40-55g of potassium fluoride, and fully mixing for completely dissolving the potassium fluoride, thus obtaining a solution A; reducing the solution A to 0 DEG C, holding the temperature for 30-55min so as to fully precipitate out precipitate potassium fluotitanate, and filtering to obtain clear filtrate B; and determining titanium ions in chemical-milling waste liquid and the clear filtrate B in the same batch by using an ultraviolet spectrometry, wherein the results show that the extraction ratio of the titanium ions in the waste liquid is as high as 90%. For solving the problem that metal ions in titanium alloy chemical-milling waste liquid are difficult to handle, the invention discloses a method for efficiently extracting titanium ions so that titanium alloy chemical-milling liquid can be recycled, thereby reducing the production cost and avoiding the environment pollution. A byproduct produced by using the method is potassium fluotitanate which has a certain industrial application value.
Description
Technical field
The invention belongs to chemical field, be specifically related to the extracting method of titanium ion in a kind of Chemical milling technology for titanium alloy waste liquid.
Background technology
Potassium fluotitanate, has another name called for titanium potassium fluoride, is white flaky crystals, is dissolved in hot water, be slightly soluble in cold water and mineral acid, be insoluble to ammoniacal liquor under normal temperature.Fusing point is 780 DEG C.Poisonous, irritant.Industrial being commonly used to makes metatitanic acid and metal titanium.The preparation method of potassium fluotitanate is, after hydrofluoric acid and metatitanic acid effect, obtains with potassium hydroxide neutralization.
The chemistry milling of titanium alloy is that titanium alloy is placed in chemical milling solution, titanium alloy workpiece is made to need the part of processing controlledly uniform dissolution in chemical milling solution, thus the shape and size needed for obtaining: choose the milling waste liquid of TA15 as experimental study object, composition, the working conditions of TA15 titanium alloy chemistry milling liquid are: hydrofluoric acid 44-45g/L, nitric acid 185-230g/L, additive Tween-20 0.2-0.3g/L.
Bath life is the maximum titanium content that 1L corrosion processing solution can dissolve, after chemical milling solution processes certain part, titanium ion content in corrosion processing liquid increases, process velocity can significantly decline, surfaceness first reduces rear rising, and the viscosity of solution strengthens, and corrosion processing depth difference increases, when in solution, titanium ion content reaches certain value, chemical milling solution is scrapped.
In solution, titanium ion is measured by ultraviolet spectrometry, utilize diantipyrylmethane as developer, in acid condition with titanium ion generation color reaction, reaction product has maximum absorption band at 420nm wavelength place, the depth of reaction product color is directly proportional to titanium ion content in mensuration liquid, therefore utilizes light absorption value that determined by ultraviolet spectrophotometry reaction soln goes out at 420nm to determine the titanium ion content in solution.
The waste liquid that titanium alloy chemistry milling processing produces is the acid waste water being rich in heavy metal, emission treatment is improper, easily cause water body pollution in wide area, directly threaten vegeto-animal health, the recycling of the heavy metal titanium be therefore rich in milling waste liquid just seems significant.Milling waste liquid after extracting titanium ion, can realize recycling by adding a certain amount of acid.
Summary of the invention
The object of the invention is the treatment process proposing titanium ion in a kind of Chemical milling technology for titanium alloy waste liquid, this method is for the reluctant problem of existing Chemical milling technology for titanium alloy waste liquid, propose one and can alleviate environmental pollution, be convenient to the method for simple process waste liquid, the milling waste liquid simultaneously extracting titanium ion can realize recycling by adding a certain amount of acid, and the potassium fluotitanate that milling waste liquid extracts also has certain using value.
The present invention is achieved in that its characterization step is:
(1) the Chemical milling technology for titanium alloy waste liquid getting 200mL is placed in plastic beaker, adds the sylvite of 40 ~ 55g, and fully stir potassium to be fluorinated and dissolve completely, potassium ion can be combined with hydrofluotitanic acid radical ion and generate potassium fluotitanate, obtains mixed liquor A, for subsequent use; Separately get the Chemical milling technology for titanium alloy waste liquid C with batch 200mL;
(2) mixed liquor A is placed in refrigerator 30 ~ 55min that temperature is 0 DEG C, for subsequent use;
(3) mixed liquor A is filtered, obtain cleaner liquid B, at 85 DEG C, much filtrate is dried, obtain potassium fluotitanate, and weigh;
(4) titanium ion in cleaner liquid B and solution C is measured by ultraviolet spectrometry, draw titanium ion utilization ratio in waste liquid.
Further, the described sylvite added in waste liquid comprises Potassium monofluoride, Repone K, one or more in saltpetre.
Further, the described potassium fluotitanate generated in waste liquid, utilizes it to be slightly soluble in cold water and mineral acid, makes it separate out in waste liquid by the mode reducing temperature.
Further, described Chemical milling technology for titanium alloy liquid component type comprises hydrofluoric acid base, hydrofluoric acid-nitric acid type, hydrofluoric acid-nitric acid-hydrochloric acid type.
The invention has the advantages that: a kind of method providing high efficiency extraction titanium ion in milling waste liquid, the medicine required for the method is sylvite, common on the market, and the requirement of the method to equipment is low, easy handling.The efficiency that the method extracts titanium ion is very high, is about 90%, and the milling waste liquid after this method extraction can realize recycling by adding a certain amount of acid, reduces production cost, avoids environmental pollution.The by product of this method is potassium fluotitanate, can be used for preparing metatitanic acid and metal titanium, be conducive to the sustainable use of resource, have certain industrial application value.
Embodiment
Example one
A method for high efficiency extraction titanium ion from Chemical milling technology for titanium alloy waste liquid, comprises following processing step:
Get Chemical milling technology for titanium alloy liquid 200mL in plastic beaker, add 40g Potassium monofluoride, fully be stirred to till all dissolving, plastic beaker is placed in the refrigerating chamber 30min of 0 DEG C, and filter in refrigerating chamber, at 85 DEG C, much filtrate is dried, obtain white powder potassium fluotitanate and small part impurity, be weighed as 52g.Contrasted by ultraviolet spectrometry before and after chemical milling solution, chemical milling solution originally titanium ion content is 55g/L, and cleaner liquid titanium ion content is 5.3g/L, and titanium ion extraction yield is about 90.3%.
Example two
A method for high efficiency extraction titanium ion from Chemical milling technology for titanium alloy waste liquid, comprises following processing step:
Get Chemical milling technology for titanium alloy liquid 200mL in plastic beaker, add 45g Potassium monofluoride, fully be stirred to till all dissolving, plastic beaker is placed in the refrigerating chamber 30min of 0 DEG C, and filter in refrigerating chamber, at 85 DEG C, much filtrate is dried, obtain white powder potassium fluotitanate and small part impurity, be weighed as 55g.Contrasted by ultraviolet spectrometry before and after chemical milling solution, chemical milling solution originally titanium ion content is 55g/L, and cleaner liquid titanium ion content is 4.9g/L, and titanium ion extraction yield is about 91%.
Example three
A method for high efficiency extraction titanium ion from Chemical milling technology for titanium alloy waste liquid, comprises following processing step:
Get Chemical milling technology for titanium alloy liquid 200mL in plastic beaker, add 50g Potassium monofluoride, fully be stirred to till all dissolving, plastic beaker is placed in the refrigerating chamber 30min of 0 DEG C, and filter in refrigerating chamber, at 85 DEG C, much filtrate is dried, obtain white powder potassium fluotitanate and small part impurity, be weighed as 59g.Contrasted by ultraviolet spectrometry before and after chemical milling solution, chemical milling solution originally titanium ion content is 62g/L, and cleaner liquid titanium ion content is 6g/L, and titanium ion extraction yield is about 90.3%.
Example four
A method for high efficiency extraction titanium ion from Chemical milling technology for titanium alloy waste liquid, comprises following processing step:
Get Chemical milling technology for titanium alloy liquid 200mL in plastic beaker, add 45g Potassium monofluoride, fully be stirred to till all dissolving, plastic beaker is placed in the refrigerating chamber 30min of 0 DEG C, and filter in refrigerating chamber, at 85 DEG C, much filtrate is dried, obtain white powder potassium fluotitanate and small part impurity, be weighed as 57g.Contrasted by ultraviolet spectrometry before and after chemical milling solution, chemical milling solution originally titanium ion content is 62g/L, and cleaner liquid titanium ion content is 6.1g/L, and titanium ion extraction yield is about 90.1%.
Claims (4)
1. from Chemical milling technology for titanium alloy waste liquid, extract a method for titanium ion, it is characterized in that, comprise following Exemplary process steps:
(1) the Chemical milling technology for titanium alloy waste liquid getting 200mL is placed in plastic beaker, adds the sylvite of 40 ~ 55g, fully stirs potassium to be fluorinated and dissolves completely, and potassium ion can be combined generation potassium fluotitanate by hydrofluotitanic acid radical ion in solution, obtains mixed liquor A, for subsequent use; Separately get the Chemical milling technology for titanium alloy waste liquid C with batch 200mL;
(2) mixed liquor A is placed in refrigerator 30 ~ 55min that temperature is 0 DEG C, for subsequent use;
(3) mixed liquor A is filtered, obtain cleaner liquid B, at 85 DEG C, much filtrate is dried, obtain potassium fluotitanate, and weigh;
(4) titanium ion in cleaner liquid B and solution C is measured by ultraviolet spectrometry, draw titanium ion utilization ratio in waste liquid.
2. according to a kind of method extracting titanium ion from Chemical milling technology for titanium alloy liquid according to claim 1, it is characterized in that, the described sylvite added in waste liquid comprises Potassium monofluoride, Repone K, one or more in saltpetre.
3. according to a kind of method extracting titanium ion from Chemical milling technology for titanium alloy liquid according to claim 1, it is characterized in that, the described potassium fluotitanate generated in waste liquid, utilize it to be slightly soluble in cold water and mineral acid, make it separate out in waste liquid by the mode reducing temperature.
4. according to a kind of method extracting titanium ion from Chemical milling technology for titanium alloy liquid according to claim 1, it is characterized in that, described Chemical milling technology for titanium alloy liquid component type comprises hydrofluoric acid base, hydrofluoric acid-nitric acid type, hydrofluoric acid-nitric acid-hydrochloric acid type.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510107958.5A CN104745822A (en) | 2015-03-12 | 2015-03-12 | Method for extracting titanium ions from titanium alloy chemical-milling waste liquid |
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| CN201510107958.5A CN104745822A (en) | 2015-03-12 | 2015-03-12 | Method for extracting titanium ions from titanium alloy chemical-milling waste liquid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668621A (en) * | 2016-01-15 | 2016-06-15 | 江苏新泰材料科技股份有限公司 | Method for preparing potassium fluotitanate from fluorine-containing wastewater |
| CN110455793A (en) * | 2019-08-29 | 2019-11-15 | 佛山市安齿生物科技有限公司 | Method for distinguishing pure titanium and titanium alloy |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1044025A (en) * | 1962-04-22 | 1966-09-28 | Chem & Phosphates Ltd | Process for the production of fluotitanic acid and of fluotitanates |
| CN86104454A (en) * | 1986-06-24 | 1988-01-06 | 宝鸡稀有金属加工研究所 | The recovery method of titanium and titanium alloy spent pickle liquor thereof |
| CN1143048A (en) * | 1996-05-20 | 1997-02-19 | 陈既明 | Method for producing potassium fluotitanate from tantalum and niobium extracting waste liquid containing titanium |
| CN1702179A (en) * | 2005-03-21 | 2005-11-30 | 南昌大学 | Method for extracting titanium from tantalum and niobium raffinate |
| CN102786081A (en) * | 2012-08-01 | 2012-11-21 | 沈阳理工大学 | Method for preparing potassium fluotitanate from titanium alloy chemical milling waste liquid |
-
2015
- 2015-03-12 CN CN201510107958.5A patent/CN104745822A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1044025A (en) * | 1962-04-22 | 1966-09-28 | Chem & Phosphates Ltd | Process for the production of fluotitanic acid and of fluotitanates |
| CN86104454A (en) * | 1986-06-24 | 1988-01-06 | 宝鸡稀有金属加工研究所 | The recovery method of titanium and titanium alloy spent pickle liquor thereof |
| CN1143048A (en) * | 1996-05-20 | 1997-02-19 | 陈既明 | Method for producing potassium fluotitanate from tantalum and niobium extracting waste liquid containing titanium |
| CN1702179A (en) * | 2005-03-21 | 2005-11-30 | 南昌大学 | Method for extracting titanium from tantalum and niobium raffinate |
| CN102786081A (en) * | 2012-08-01 | 2012-11-21 | 沈阳理工大学 | Method for preparing potassium fluotitanate from titanium alloy chemical milling waste liquid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668621A (en) * | 2016-01-15 | 2016-06-15 | 江苏新泰材料科技股份有限公司 | Method for preparing potassium fluotitanate from fluorine-containing wastewater |
| CN110455793A (en) * | 2019-08-29 | 2019-11-15 | 佛山市安齿生物科技有限公司 | Method for distinguishing pure titanium and titanium alloy |
| CN110455793B (en) * | 2019-08-29 | 2021-12-14 | 佛山市安齿生物科技有限公司 | Method for distinguishing pure titanium and titanium alloy |
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Application publication date: 20150701 |