CN105293439A - Method for recycling hydrochloric acid from titanium slag leaching waste fluid - Google Patents
Method for recycling hydrochloric acid from titanium slag leaching waste fluid Download PDFInfo
- Publication number
- CN105293439A CN105293439A CN201510708429.0A CN201510708429A CN105293439A CN 105293439 A CN105293439 A CN 105293439A CN 201510708429 A CN201510708429 A CN 201510708429A CN 105293439 A CN105293439 A CN 105293439A
- Authority
- CN
- China
- Prior art keywords
- hydrochloric acid
- titanium slag
- waste
- recycling
- leaching
- Prior art date
- 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.)
- Pending
Links
Abstract
The invention belongs to the field of chemical waste liquid recycling treatment, and particularly relates to a method for recycling hydrochloric acid from titanium slag leaching waste fluid. The technical problems that for the industry at present, the technology energy consumption of recycling waste diluted hydrochloric acid is large, the cost is high, and recycled hydrochloric acid concentration is low are solved. According to the technical scheme, the invention provides the method for recycling the hydrochloric acid in the titanium slag leaching waste fluid, and the method comprises that following steps that 1, dried mixed salt is added to waste hydrochloric acid of hydrochloric acid leaching fluid of titanium slags; 2, distilling is conducted for 20-30 min under 110+/-5 DEG C, and recycled hydrochloric acid is obtained. According to the method for recycling the hydrochloric acid from the titanium slag leaching waste fluid, operation is easy, energy consumption can be greatly reduced, the problems of large roasting energy consumption, high leaching cost and the like are solved, and meanwhile high pure hydrochloric acid with higher concentration is obtained through recycling.
Description
Technical field
The invention belongs to chemical waste liquid recycling field, be specifically related to the method reclaiming hydrochloric acid in titanium slag leaching waste liquid.
Background technology
At present, along with natural GOOD TASTE rutile ore is fewer and feweri, the artificial rutile prepared by titanium slag or rich titanium material have become the main production raw material of titanium dioxide.Titanium slag is through a series of oxidation or reduction pretreatment, and need to carry out leaching by hydrochloric acid to it afterwards and prepare artificial rutile, the solid after leaching is artificial rutile, and impurity is stayed in hydrochloric acid.Leaching process is the most important link realizing magazins' layout, the content of titanium dioxide in artificial rutile can be made to reach or close to 90%, if the waste and old dilute hydrochloric acid that can reclaim leaching process generation will realize material and circulate in technological process, reduce costs and raise the efficiency.
The technique of the waste and old dilute hydrochloric acid of current industrial recovery is mostly realized by fluiddized-bed roasting or spray roasting, but energy expenditure is large, and cost is higher, and concentration of hydrochloric acid after reclaiming is lower.
Summary of the invention
The technical problem to be solved in the present invention is that the process energy consumption of the waste and old dilute hydrochloric acid of current industrial recovery is large, and cost is higher, and concentration of hydrochloric acid after reclaiming is lower.
The scheme that the present invention solves the problems of the technologies described above is to provide a kind of method reclaiming hydrochloric acid in hydrochloric acid leachate of titanium slag.
Reclaim the method for hydrochloric acid in above-mentioned titanium slag leaching waste liquid, comprise the following steps:
A, the mixing salt of drying is joined in waste hydrochloric acid;
B, then distillation 20 ~ 30min at 110 ± 5 DEG C, collect steam condensate, be recycled hydrochloric acid.
Reclaim in the method for hydrochloric acid in above-mentioned titanium slag leaching waste liquid, the waste hydrochloric acid described in step a is the waste hydrochloric acid of titanium slag hydrochloric acid leachate.
Reclaim in the method for hydrochloric acid in above-mentioned titanium slag leaching waste liquid, the mixing salt described in step a is MgCl
2and CaCl
2mix with mass ratio 1 ︰ 3 and obtain.
Reclaim in the method for hydrochloric acid in above-mentioned titanium slag leaching waste liquid, mixing salt described in step a add-on be: in the waste hydrochloric acid of the hydrochloric acid leachate of titanium slag during hydrogen ion concentration≤2mol/L, mixing salt add-on be 75 ~ 80Kg/ ton acid; In the waste hydrochloric acid of the hydrochloric acid leachate of titanium slag during hydrogen ion concentration > 2mol/L, mixing salt add-on be 35 ~ 40Kg/ ton acid.
Reclaim in the method for hydrochloric acid in above-mentioned titanium slag leaching waste liquid, in the still-process described in step b, regulate the flow of water coolant that leaving water temperature(LWT) is controlled below 45 DEG C.
The method of hydrochloric acid is reclaimed in titanium slag leaching waste liquid provided by the invention, simple to operate, significantly can reduce energy consumption, solve roasting energy consumption large, leach high in cost of production problem, reclaim the high purity hydrochloric acid obtaining concentration higher (22 ~ 24%) simultaneously.
Embodiment
Reclaim the method for hydrochloric acid in titanium slag leaching waste liquid, comprise the following steps:
A, the mixing salt of drying is joined in waste hydrochloric acid; Described mixing salt is MgCl
2and CaCl
2mix with mass ratio 1 ︰ 3 and obtain;
B, then distillation 20 ~ 30min at 110 ± 5 DEG C, collect steam condensate, be recycled hydrochloric acid.
Reclaim in the method for hydrochloric acid in above-mentioned titanium slag leaching waste liquid, the waste hydrochloric acid described in step a is the waste hydrochloric acid of titanium slag hydrochloric acid leachate.
Reclaim in the method for hydrochloric acid in above-mentioned titanium slag leaching waste liquid, mixing salt described in step a add-on be: in the waste hydrochloric acid of the hydrochloric acid leachate of titanium slag during hydrogen ion concentration≤2mol/L, mixing salt add-on be 75 ~ 80Kg/ ton acid; In the waste hydrochloric acid of the hydrochloric acid leachate of titanium slag during hydrogen ion concentration > 2mol/L, mixing salt add-on be 35 ~ 40Kg/ ton acid.
Reclaim in the method for hydrochloric acid in above-mentioned titanium slag leaching waste liquid, in the still-process described in step b, regulate the flow of water coolant that leaving water temperature(LWT) is controlled below 45 DEG C.
Wherein, the selection of distillation temperature is mainly determined the impact of system boiling point according to after salt adding, considers the violent situation of boiling simultaneously.If temperature is lower than 105 DEG C, distillation is carried out slowly, and the time is longer; If temperature can cause evaporation of water amount to increase substantially more than 115 DEG C, the concentration of hydrochloric acid of recovery gained is reduced.
The present invention adds mixing salt in waste hydrochloric acid, its role is to the elevation of boiling point making water, reduces evaporation of water amount, is acted on by salt effect, realizes salt acid high concentration and reclaims.The blending ratio of salt considers the factor of cost and effect two aspect, and the effect of magnesium chloride is better, but cost is higher, and calcium chloride effect is slightly poor, but price is lower.After becoming mixing salt with the proportions of 1:3, the effect of salt effect is all better than effect during single use, is also that in mixing salt, effect is best simultaneously.
In still-process, if the water outlet water temperature of water coolant is more than 45 DEG C, fouling in prolong can be caused, in addition, the recovery condensation number of hydrochloric acid also can be caused to reduce.
Embodiment 1
Collect the waste and old dilute hydrochloric acid that certain leaches titanium slag gained, the hydrogen ion concentration detected in spent acid is 1.5mol/L, the distillation waste acid getting 100mL adds in distilling flask, take 8g mixing salt in proportion afterwards, and join in flask and mix with spent acid, heating is started at 110 DEG C, start to carry out condensation to steam adding after thermal distillation has steam to emerge, collect steam condensate, regulate water coolant flow velocity, make the outlet temperature of water coolant be 40 DEG C, distillation is stopped after distillation 20min, detect the concentration of the steam condensate of gained, concentration of hydrochloric acid is 22.3%, removing H
2outside O and HCl, foreign matter content is lower than 0.01%.
Embodiment 2
Collect the waste and old dilute hydrochloric acid that certain leaches titanium slag gained, the hydrogen ion concentration detected in spent acid is 2.1mol/L, the distillation waste acid getting 200mL adds in distilling flask, take 8g mixing salt in proportion afterwards, and join in flask and mix with spent acid, heating is started at 105 DEG C, start to carry out condensation to steam adding after thermal distillation has steam to emerge, collect steam condensate, regulate water coolant flow velocity, make the outlet temperature of water coolant be 42 DEG C, distillation is stopped after distillation 25min, detect the concentration of the steam condensate of gained, concentration of hydrochloric acid is 22.6%, removing H
2outside O and HCl, foreign matter content is lower than 0.01%.
Embodiment 3
Collect the waste and old dilute hydrochloric acid that certain leaches titanium slag gained, the hydrogen ion concentration detected in spent acid is 2.5mol/L, the distillation waste acid getting 500mL adds in distilling flask, take 20g mixing salt in proportion afterwards, and join in flask and mix with spent acid, heating is started at 108 DEG C, to start after thermal distillation has steam to emerge that condensation is carried out to steam and collect steam condensate adding, regulate water coolant flow velocity, make the outlet temperature of water coolant be 45 DEG C, stop distillation after distillation 23min, detect the concentration of the steam condensate of gained, concentration of hydrochloric acid is 22.8%, removing H
2outside O and HCl, foreign matter content is lower than 0.01%.
Embodiment 4
Collect the waste and old dilute hydrochloric acid that certain leaches titanium slag gained, the hydrogen ion concentration detected in spent acid is 2.3mol/L, the spent acid getting 500mL adds in distilling flask, start distillation after being heated to 110 DEG C, regulate the flow velocity of water of condensation, the water speed that goes out controlling water of condensation is 43 DEG C, stop after distillation 30min, carry out Rong Yang detection to the distillate collected, wherein concentration of hydrochloric acid is 12.5%, goes out H
2outside O and HCl, foreign matter content <0.04%.
Do not add mixing salt in the spent acid of the present embodiment, the concentration reclaiming hydrochloric acid is only 12.5%, is starkly lower than embodiment 1,2 and 3.
The method of hydrochloric acid is reclaimed in titanium slag leaching waste liquid provided by the invention, simple to operate, significantly can reduce energy consumption, reclaim the high purity hydrochloric acid obtaining concentration higher (22 ~ 24%) simultaneously.
Claims (4)
1. reclaim the method for hydrochloric acid in titanium slag leaching waste liquid, comprise the following steps:
A, the mixing salt of drying is joined in waste hydrochloric acid;
B, then distillation 20 ~ 30min at 110 ± 5 DEG C, collect steam condensate, be recycled hydrochloric acid.
2. reclaim the method for hydrochloric acid according to claim 1 in titanium slag leaching waste liquid, it is characterized in that: the mixing salt described in step a is MgCl
2and CaCl
2mix with mass ratio 1 ︰ 3 and obtain.
3. reclaim the method for hydrochloric acid according to claim 1 in titanium slag leaching waste liquid, it is characterized in that: mixing salt described in step a add-on be: in the waste hydrochloric acid of the hydrochloric acid leachate of titanium slag during hydrogen ion concentration≤2mol/L, mixing salt add-on be 75 ~ 80Kg/ ton acid; In the waste hydrochloric acid of the hydrochloric acid leachate of titanium slag during hydrogen ion concentration > 2mol/L, mixing salt add-on be 35 ~ 40Kg/ ton acid.
4. reclaim the method for hydrochloric acid according to claim 1 in titanium slag leaching waste liquid, it is characterized in that: in the still-process described in step b, regulate the flow of water coolant that leaving water temperature(LWT) is controlled below 45 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510708429.0A CN105293439A (en) | 2015-10-27 | 2015-10-27 | Method for recycling hydrochloric acid from titanium slag leaching waste fluid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510708429.0A CN105293439A (en) | 2015-10-27 | 2015-10-27 | Method for recycling hydrochloric acid from titanium slag leaching waste fluid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105293439A true CN105293439A (en) | 2016-02-03 |
Family
ID=55191386
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510708429.0A Pending CN105293439A (en) | 2015-10-27 | 2015-10-27 | Method for recycling hydrochloric acid from titanium slag leaching waste fluid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105293439A (en) |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088544A (en) * | 1992-12-18 | 1994-06-29 | 技术信息有限公司 | Regeneration of hydrochloric acid |
| CN1295969A (en) * | 1999-11-10 | 2001-05-23 | 住友化学工业株式会社 | Process for separation and recovery hydrogen chloride from water |
| CN1562732A (en) * | 2004-04-01 | 2005-01-12 | 上海交通大学 | Method for preparing strong hydrochloric acid through extracting and distilling deposed dilute hydrochloric acid semi continuously |
| CN101219974A (en) * | 2008-01-22 | 2008-07-16 | 浙江海虹控股集团有限公司 | Method for recovery utilization of mother solution hydrochloric acid for ADC foaming agent production |
| CN102040196A (en) * | 2009-10-15 | 2011-05-04 | 盐城师范学院 | Method for reclaiming hydrochloric acid and ferrous sulfate from steel hydrochloric acid washing waste liquid |
| CN102102149A (en) * | 2009-12-21 | 2011-06-22 | 陈树忠 | Leaching solution for leaching ilmenite, hydrochloric acid leaching method and application of leaching residues |
| CN102275970A (en) * | 2011-05-20 | 2011-12-14 | 攀枝花市微创科技开发有限公司 | Comprehensive utilization method of titanium white waste acid and wastewater |
| CN102417162A (en) * | 2011-08-29 | 2012-04-18 | 浙江金壳生物化学有限公司 | Recycling method of hydrochloric acid-acetic acid waste liquid |
| CN102502500A (en) * | 2011-11-07 | 2012-06-20 | 韩扶军 | Device for producing hydrogen chloride by resolving hydrochloric acid |
| CN102627321A (en) * | 2012-04-01 | 2012-08-08 | 沙立林 | Method for preparing titanium pigment by using titanium residues obtained by directly reducing titanium-iron oxide |
| CN103288232A (en) * | 2013-04-17 | 2013-09-11 | 浙江大学 | Resourceful treatment apparatus and method for waste liquid of chlorohydric acid pickling of steel |
| CN104150444A (en) * | 2014-08-20 | 2014-11-19 | 来宾华锡冶炼有限公司 | Method for recovering hydrochloric acid in anti-molten iron during indium extraction process |
| CN104986736A (en) * | 2015-07-16 | 2015-10-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering waste hydrochloric acid solution in hydrochloric acid method rutile preparation technology |
-
2015
- 2015-10-27 CN CN201510708429.0A patent/CN105293439A/en active Pending
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088544A (en) * | 1992-12-18 | 1994-06-29 | 技术信息有限公司 | Regeneration of hydrochloric acid |
| CN1295969A (en) * | 1999-11-10 | 2001-05-23 | 住友化学工业株式会社 | Process for separation and recovery hydrogen chloride from water |
| CN1562732A (en) * | 2004-04-01 | 2005-01-12 | 上海交通大学 | Method for preparing strong hydrochloric acid through extracting and distilling deposed dilute hydrochloric acid semi continuously |
| CN101219974A (en) * | 2008-01-22 | 2008-07-16 | 浙江海虹控股集团有限公司 | Method for recovery utilization of mother solution hydrochloric acid for ADC foaming agent production |
| CN102040196A (en) * | 2009-10-15 | 2011-05-04 | 盐城师范学院 | Method for reclaiming hydrochloric acid and ferrous sulfate from steel hydrochloric acid washing waste liquid |
| CN102102149A (en) * | 2009-12-21 | 2011-06-22 | 陈树忠 | Leaching solution for leaching ilmenite, hydrochloric acid leaching method and application of leaching residues |
| CN102275970A (en) * | 2011-05-20 | 2011-12-14 | 攀枝花市微创科技开发有限公司 | Comprehensive utilization method of titanium white waste acid and wastewater |
| CN102417162A (en) * | 2011-08-29 | 2012-04-18 | 浙江金壳生物化学有限公司 | Recycling method of hydrochloric acid-acetic acid waste liquid |
| CN102502500A (en) * | 2011-11-07 | 2012-06-20 | 韩扶军 | Device for producing hydrogen chloride by resolving hydrochloric acid |
| CN102627321A (en) * | 2012-04-01 | 2012-08-08 | 沙立林 | Method for preparing titanium pigment by using titanium residues obtained by directly reducing titanium-iron oxide |
| CN103288232A (en) * | 2013-04-17 | 2013-09-11 | 浙江大学 | Resourceful treatment apparatus and method for waste liquid of chlorohydric acid pickling of steel |
| CN104150444A (en) * | 2014-08-20 | 2014-11-19 | 来宾华锡冶炼有限公司 | Method for recovering hydrochloric acid in anti-molten iron during indium extraction process |
| CN104986736A (en) * | 2015-07-16 | 2015-10-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering waste hydrochloric acid solution in hydrochloric acid method rutile preparation technology |
Non-Patent Citations (3)
| Title |
|---|
| 张荣臻: "加盐蒸馏回收盐酸和混凝剂制备技术资源化利用盐酸酸洗废液", 《环境工程学报》 * |
| 张颖等: "盐对盐酸一水体系气液平衡的影响", 《精细化工》 * |
| 陆春宏: "加盐精馏和加盐解吸回收稀盐酸的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101691239B (en) | Comprehensive utilization method for bittern | |
| CN103723765B (en) | Method for preparing titanium dioxide through sulfuric acid method | |
| CN103924096B (en) | Reclaim the method for vanadium chromium resource | |
| CN103952560B (en) | A kind of method of Leaching of Vanadium from Vanadium slag | |
| CN103276227B (en) | Method for extracting vanadium from vanadium-titanium magnetite concentrates | |
| CN102352437A (en) | Method for treating hydrochloric acid leachate of ferrotitanium materials | |
| CN102337411A (en) | Method for recycling vanadium and chromium from high-chromium low-vanadium vanadium precipitation wastewater | |
| CN102745743A (en) | Method for preparing artificial rutile by titanium slags | |
| CN106755967A (en) | A kind of sulfuric acid calcination processing lepidolite and the method for producing lithium carbonate | |
| CN102745742B (en) | Method for producing titanium-rich material by processing vanadium-titanium-containing blast furnace slag with titanium white waste acid | |
| CN108946772A (en) | A method of pure Lithium Carbonate is prepared by lithium ore | |
| CN106337135A (en) | Novel method for producing vanadium pentoxide through ammonium-free vanadium precipitation | |
| CN104724753A (en) | Method for preparing rutile type titanium dioxide by using ilmenite as raw material | |
| CN102260801B (en) | Clean conversion method of stone coal | |
| CN103936063A (en) | Method and system for recycling vanadium-containing mud generated in vanadium removal process of crude titanium tetrachloride | |
| CN101585553A (en) | Method for producing vanadium pentoxide by ore containing vanadium and intermediate material containing vanadium | |
| CN109835951A (en) | A kind of system and method for chloridising production powder vanadium | |
| CN106636615B (en) | The mica treatment process of lithium carbonate is prepared using lepidolite | |
| CN101935755B (en) | Two-stage leaching method for vanadium in vanadium-containing ore | |
| CN103936047A (en) | Preparation method of anhydrous aluminum chloride | |
| CN103014316A (en) | Novel method for processing lepidolite material | |
| CN102732727A (en) | Method for extracting vanadium from high vanadium-sodium-aluminum-silicon slag | |
| CN109467239A (en) | A kind of method of iron and steel pickling waste liquid recovery acid | |
| CN104294033A (en) | Vanadium extracting process for silicate type vanadium ore | |
| CN104555948A (en) | Concentration technology for waste acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160203 |
|
| RJ01 | Rejection of invention patent application after publication |