CN105692950B - A kind of processing method of Intermatallic Ti-Al compound chemistry milling waste liquid - Google Patents
A kind of processing method of Intermatallic Ti-Al compound chemistry milling waste liquid Download PDFInfo
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- 238000003801 milling Methods 0.000 title claims abstract description 87
- 239000007788 liquid Substances 0.000 title claims abstract description 58
- 239000002699 waste material Substances 0.000 title claims abstract description 58
- 229910004349 Ti-Al Inorganic materials 0.000 title claims abstract description 17
- 229910004692 Ti—Al Inorganic materials 0.000 title claims abstract description 17
- 150000001875 compounds Chemical class 0.000 title claims abstract description 17
- 238000003672 processing method Methods 0.000 title claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 23
- 239000002667 nucleating agent Substances 0.000 claims abstract description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000008929 regeneration Effects 0.000 claims abstract description 8
- 238000011069 regeneration method Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 6
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 6
- 239000011591 potassium Substances 0.000 claims abstract description 6
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 6
- 239000001103 potassium chloride Substances 0.000 claims abstract description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004458 analytical method Methods 0.000 claims abstract description 5
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 5
- 239000011737 fluorine Substances 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 22
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 5
- 239000004480 active ingredient Substances 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 239000012047 saturated solution Substances 0.000 claims description 5
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical group FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims description 3
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 3
- 235000003270 potassium fluoride Nutrition 0.000 claims description 3
- 239000011698 potassium fluoride Substances 0.000 claims description 3
- 229910001414 potassium ion Inorganic materials 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 239000013589 supplement Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 230000007547 defect Effects 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910000601 superalloy Inorganic materials 0.000 description 3
- 229910003708 H2TiF6 Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910017111 AlOF Inorganic materials 0.000 description 1
- 241000406668 Loxodonta cyclotis Species 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- UOBPHQJGWSVXFS-UHFFFAOYSA-N [O].[F] Chemical compound [O].[F] UOBPHQJGWSVXFS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 208000020442 loss of weight Diseases 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
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Abstract
The present invention relates to field of waste liquid treatment, especially a kind of processing method of Intermatallic Ti-Al compound chemistry milling waste liquid, the detailed process of processing is：(1) it filters：Solid impurity in chemistry milling waste liquid is filtered into removal；(2) nucleating agent is added after chemistry milling waste liquid is cooled to 20 DEG C or less, fluorine alumina is made to be precipitated out from solution；(3) sylvite is added in waste liquid, so that titanium ion is precipitated out from solution as potassium fluotitanate, and focused in residue by centrifugal separator；(4) waste liquid that centrifugal separator comes out carries out analysis of effective component calibration, can be used as regeneration chemical milling solution.The present invention can be such that the chemistry milling waste liquid of failure is regenerated, it is recycled, effectively reduce chemical milling solution cost, reduce the discharge costs of chemistry milling waste liquid, factory can be made to see apparent economic benefit, and chemistry milling discharging of waste liquid pollution on the environment is reduced, there is apparent social benefit.
Description
Technical field
The present invention relates to field of waste liquid treatment, especially a kind of processing side of Intermatallic Ti-Al compound chemistry milling waste liquid
Method.
Background technology
Intermatallic Ti-Al compound material is a kind of lightweight high-temperature material to attract attention at present, and density is less than Ni-based height
The half of temperature alloy, high-temperature behavior, creep resistance and nickel base superalloy are close, can fill up titanium alloy and nickel base superalloy
Use blank, the larger nickel base superalloy of density is substituted in certain temperature range, the loss of weight of parts is effectively realized, can use
In aerospace, the shell etc. of the high temperature resistant parts of automobile and other industries or super speed vehicle, it is considered to be most there is application
The lightening fire resistant structural material of new generation of potentiality.
Chemistry milling also makes corrosion process, and is to generate chemical reaction to metal using chemical solutions such as acid, alkali, salt, makes gold
Belong to dissolving, changes a kind of processing method of workpiece size and shape (or surface property).Currently, milling processing has become aviation
The reliable processing method of space flight parts forming.The main corrosion ingredient of Intermatallic Ti-Al compound chemical milling solution be hydrofluoric acid and
The chemical reactions of many complexity vied each other can occur for nitric acid, when milling, and several possible key reactions are as follows：
2Al+6HF=2AlF3+3H2
Al+HNO3+H2O=H3AlO3+NO
2H3AlO3+AlF3=3AlOF+3H2O
6HF+Ti=H2TiF6+2H2
Ti+6HF+4HNO3=H2TiF6+4NO2+4H2O
Chemical milling solution is after use after a period of time, and with the progress of reaction, the metal ion in solution gradually increases,
Chemical milling solution active ingredient gradually decreases, and milling rate can be caused to reduce, and part quality declines after milling, when milling rate reduces
After to a certain extent, chemical milling solution is declared to scrap, and cannot reuse.
Chemical milling solution is directly scrapped or is scrapped after simple process and not only bring white elephant to environmental protection,
And waste of resources is caused, increases production cost.
Invention content
The purpose of the present invention is to provide a kind of processing method of Intermatallic Ti-Al compound materials chemistry milling waste liquid, profits
Above-mentioned failure chemistry milling waste liquid is handled with this method, chemistry milling waste liquid can be made to be regenerated, the band of discharging of waste liquid is reduced
The environmental pollution come, and reduce production cost.
The technical scheme is that：
A kind of processing method of Intermatallic Ti-Al compound chemistry milling waste liquid, comprises the steps of：
(1) it filters：Solid impurity in chemistry milling waste liquid is filtered into removal, the chemistry milling for obtaining no suspended substance is useless
Liquid；
(2) nucleating agent is added after chemistry milling waste liquid is cooled to 20 DEG C or less, obtains fluorine alumina and is settled out from solution
Come；
(3) saturation potassium salt soln is added in chemistry milling waste liquid, titanium ion is made to become potassium fluotitanate precipitation chemically
It filters out in milling waste liquid, and is further detached by centrifugal separator, focused in residue；
(4) the chemistry milling waste liquid for coming out centrifugal separator carries out analysis of effective component calibration, by chemistry milling solution
After standard requires supplement active ingredient, as regeneration chemistry milling solution.
The processing method of the Intermatallic Ti-Al compound chemistry milling waste liquid, in step (2), nucleating agent is fluorination
One or both of aluminium, aluminium oxide.
The processing method of the Intermatallic Ti-Al compound chemistry milling waste liquid, in step (3), sylvite be potassium fluoride,
One or both of potassium nitrate, and it is configured to saturated solution use.
The advantages of the present invention are：
The processing method of chemistry milling waste liquid of the present invention can be such that the chemistry milling waste liquid (milling waste liquid) of failure obtains again
It is raw, it is recycled, effectively reduces chemical milling solution cost, reduced the discharge costs of milling waste liquid, factory can be made to see
Apparent economic benefit, and milling discharging of waste liquid pollution on the environment is reduced, there is apparent social benefit.
Specific implementation mode
In the present invention, different chemical milling solution formulas and milling technique can make chemical milling solution in failure with different
Ion component and concentration, therefore need first to carry out constituent analysis to milling waste liquid when chemical milling solution failure, according in milling waste liquid
Various ion concentration concrete numerical values, determine the addition of various substances, further determine that and how many nucleating agent and potassium ion is added,
In obtained regeneration chemical milling solution concentration of metal ions in 30g/L hereinafter, and the active ingredients such as hydrofluoric acid, nitric acid are supplemented to conjunction
Suitable concentration range, specific range is referring to related Chinese invention patent：1. publication number CN 103590042A；2. publication number CN
103556151A；3. publication number CN104073802A；4. publication number CN 104073801A.
Embodiment
In the present embodiment, the main component of Intermatallic Ti-Al compound chemistry milling waste liquid is：Titanium ion 96g/L, aluminium
Ion 38g/L, nitrate ion 120g/L, fluorine ion 32g/L, the processing side of Intermatallic Ti-Al compound chemistry milling waste liquid
Method is as follows：
(1) it filters：Solid impurity in chemistry milling waste liquid is removed by way of filtering, obtains the change of no suspended substance
Learn milling waste liquid；
(2) when milling waste liquid is cooled to 20 DEG C or less, nucleating agent is added, the aluminium ion in chemistry milling waste liquid is made to form fluorine
Aluminium oxide (AlOF) solid precipitates, and precipitates in chemically milling waste liquid solid by filtering and separates；Wherein, nucleating agent is
One or both of aluminum fluoride, aluminium hydroxide.
In the present embodiment, nucleating agent is aluminum fluoride, and nucleating agent addition is 5~8g/L, and nucleating agent, which is added, can make fluorine oxygen
Change aluminum precipitation to be more readily formed.
(3) saturation potassium salt soln is added in chemistry milling waste liquid, titanium ion is made to become potassium fluotitanate precipitation chemically
It filters out in milling waste liquid, and is further detached by centrifugal separator, focused in residue；
In the present embodiment, chemistry milling waste liquid is used as regeneration chemical milling solution after processing, not introduce foreign ion,
Sylvite selects one or both of potassium fluoride, potassium nitrate, and is configured to saturated solution use, and being configured to saturated solution can make
Reaction is uniform, while not introducing too many water, and sylvite addition is 220~280g/L.Potassium ion, which is added, so that titanium ion is given birth to
It is precipitated out at potassium fluotitanate, if milling waste liquid direct emission, most of soluble potassium salts after processing is qualified can be used.
(4) the chemistry milling waste liquid for coming out centrifugal separator carries out analysis of effective component, supplement nitric acid and hydrofluoric acid and
Other active ingredients can be used as regeneration chemistry milling solution.
In the present embodiment, the final active constituent content for obtaining chemical milling solution and technical indicator are as follows：
120~150g/L of hydrofluoric acid, 500~600g/L of nitric acid, 50~80g/L of urea, 40~60g/L of vanadic anhydride,
20~30g/L of metal ion, remaining is water.
Using above-mentioned regeneration chemical milling solution handle Intermatallic Ti-Al compound, after milling product surface do not have any pit-hole,
The defects of spine, intercrystalline corrosion, 0.010~0.030mm/min of milling rate, hydrogen content increases by 8~15ppm after milling.
Embodiment the result shows that, the present invention milling waste liquid of failure can be made to be regenerated, recycled, effectively drop
Low corrosive agent cost, reduces the discharge costs of milling waste liquid.
Claims (1)
1. a kind of processing method of Intermatallic Ti-Al compound chemistry milling waste liquid, which is characterized in that Intermatallic Ti-Al compound
The main component of chemistry milling waste liquid is：Titanium ion 96g/L, aluminium ion 38g/L, nitrate ion 120g/L, fluorine ion 32g/
L, the processing method of Intermatallic Ti-Al compound chemistry milling waste liquid, is as follows：
(1) it filters：Solid impurity in chemistry milling waste liquid is removed by way of filtering, obtains the chemical milling of no suspended substance
Cut waste liquid；
(2) when milling waste liquid is cooled to 20 DEG C or less, nucleating agent is added, the aluminium ion in chemistry milling waste liquid is made to form fluorine oxidation
Aluminium solid precipitates, and precipitates in chemically milling waste liquid solid by filtering and separates；Wherein, nucleating agent is aluminum fluoride, shape
Core agent addition is 5~8g/L, and nucleating agent, which is added, makes fluorine alumina precipitation be more readily formed；
(3) saturation potassium salt soln is added in chemistry milling waste liquid, so that titanium ion is become potassium fluotitanate and precipitates chemically milling
It filters out in waste liquid, and is further detached by centrifugal separator, focused in residue；
Sylvite selects one or both of potassium fluoride, potassium nitrate, and is configured to saturated solution use, and being configured to saturated solution makes
Reaction is uniform, and sylvite addition is 220~280g/L, and potassium ion, which is added, makes titanium ion generation potassium fluotitanate be precipitated out；
(4) the chemistry milling waste liquid for coming out centrifugal separator carries out analysis of effective component, supplement nitric acid and hydrofluoric acid and other
Active ingredient, as regeneration chemistry milling solution；
The final active constituent content for obtaining chemical milling solution and technical indicator are as follows：
120~150g/L of hydrofluoric acid, 500~600g/L of nitric acid, 50~80g/L of urea, 40~60g/L of vanadic anhydride, metal
20~30g/L of ion, remaining is water；
Using above-mentioned regeneration chemical milling solution handle Intermatallic Ti-Al compound, after milling product surface do not have any pit-hole, spine,
Intercrystalline corrosion defect, 0.010~0.030mm/min of milling rate, hydrogen content increases by 8~15ppm after milling.
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| CN110820028B (en) * | 2018-08-09 | 2021-07-30 | 湖北工业大学 | Treatment method for recycling waste acid of aluminum profile anodic oxidation tank |
| CN110127801A (en) * | 2019-05-16 | 2019-08-16 | 沈阳飞机工业（集团）有限公司 | A method of aluminum alloy chemical milling waste water is pre-processed by modified activated carbon particle |
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|---|---|---|---|---|
| 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 |
| CN101899666A (en) * | 2010-07-09 | 2010-12-01 | 成都飞机工业（集团）有限责任公司 | Stabilization and regeneration method of aluminum and aluminum alloy chemical milling solution |
| JP2013133506A (en) * | 2011-12-27 | 2013-07-08 | Panasonic Corp | Apparatus for regenerating etching solution |
| CN103572294A (en) * | 2012-07-27 | 2014-02-12 | 王润强 | Treating method, technology and system for waste aluminum alloy chemical milling solution |
-
2014
- 2014-11-28 CN CN201410714220.0A patent/CN105692950B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101899666A (en) * | 2010-07-09 | 2010-12-01 | 成都飞机工业（集团）有限责任公司 | Stabilization and regeneration method of aluminum and aluminum alloy chemical milling solution |
| JP2013133506A (en) * | 2011-12-27 | 2013-07-08 | Panasonic Corp | Apparatus for regenerating etching solution |
| CN103572294A (en) * | 2012-07-27 | 2014-02-12 | 王润强 | Treating method, technology and system for waste aluminum alloy chemical milling solution |
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| Title |
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