CN102830200A - Method for detecting titanium-containing mineral acidolysis rate - Google Patents
Method for detecting titanium-containing mineral acidolysis rate Download PDFInfo
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- CN102830200A CN102830200A CN2012102974659A CN201210297465A CN102830200A CN 102830200 A CN102830200 A CN 102830200A CN 2012102974659 A CN2012102974659 A CN 2012102974659A CN 201210297465 A CN201210297465 A CN 201210297465A CN 102830200 A CN102830200 A CN 102830200A
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Abstract
The invention provides a method for detecting a titanium-containing mineral acidolysis rate. The method comprises the following steps of analyzing chemical components of titanium-containing mineral, determining an acid-mineral ratio of an acidolysis reaction, mixing a preset amount of the titanium-containing mineral and a preset amount of concentrated sulfuric acid according to the acid-mineral ratio to obtain a mixture, adding water into the mixture so that a mass concentration of the concentrated sulfuric acid is reduced to 80-92%, carrying out an acidolysis reaction process, after the acidolysis reaction process, curing to obtain reaction products, carrying out an extraction process on the reaction products in a water bath, filtering to separate extract so that a titanium liquid and residues are obtained, calcining the residues, and calculating an acidolysis rate according to an equation 1, wherein the equation 1 shows that an acidolysis rate is equal to mA/(mA+mB)*100%; mA represents mass of TiO2 in the titanium liquid; and mB represents mass of TiO2 in the residues. The method can produce an accurate detection result, objectively evaluate ilmenite acidolysis performances of different factories and mines, and provides a basis for ilmenite purchase carried out by titanium white production manufacturers.
Description
Technical field
The present invention relates to titaniferous ore acidolysis rate detection technique field, more particularly, relate to a kind of accurately method of the acidolysis rate of titaniferous ore.
Background technology
In the prior art; Titaniferous ore (for example, ilmenite) is the important source material of Producing Titanium Dioxide, and the acidolysis rate of titaniferous ore can reflect the utilization factor of Producing Titanium Dioxide technology to titanium resource; Therefore, upright the connecing of the acid hydrolysis of titaniferous ore is related to the titanium white production cost of products.
Present domestic titanium white powder is a lot, and the employed titaniferous ore mineral resources of each producer also is not quite similar.Buy titaniferous ore at present and all calculate, buy titaniferous ore like this and just must be noted that its acidolysis performance quality according to content of titanium dioxide in the titaniferous ore.For the acidolysis performance of the titaniferous ore of estimating different mineral resources just needs a unified acidolysis rate assay method.
The document (" steel vanadium titanium " the 30th volume the 2nd phase 6-11 page or leaf, Wang Bin etc.) that in April, 2009, disclosed name was called acid-dissolved titanium slag acidolysis performance study discloses a kind of acidolysis rate computing method, yet the document does not relate to how specifically the acidolysis parameter is set.
In addition, the titanium liquid after the leaching is normally directly got to the detection of acidolysis rate in the Producing Titanium Dioxide scene from acidolysis pot top, detect the titanium in filtrating and the residue after filtering respectively, calculates acidolysis rate then.The shortcoming of this method is owing to take a sample on acidolysis pot top, and top does not have the solid phase residue basically, thereby the acidolysis rate that this testing result is often measured is more higher than actual acidolysis rate.
In addition, the people is also arranged when detecting acidolysis rate, directly calculate acidolysis rate with titania in the titanium liquid and the titania ratio in the titanium ore; Yet this method error is bigger, and repeatability is poor.
Summary of the invention
To one in the above-mentioned deficiency that exists in the prior art or multinomial, the invention provides a kind of method that can accurately record the acidolysis rate of titaniferous ore.
To achieve these goals, the invention provides a kind of method that detects the titaniferous ore acidolysis rate, said method comprising the steps of: analyze the titaniferous ore chemical constitution, confirm the sour ore deposit ratio of acidolysis reaction then; Mix than the titaniferous ore and the concentrated sulphuric acid according to sour ore deposit, form potpourri scheduled volume; In said potpourri, adding water, is 80%～92% with the mass concentration dilution with the concentrated sulphuric acid; Carry out acidolysis reaction; After treating that acidolysis reaction finishes, slaking is to obtain reaction product; Under water bath condition, leach said reaction product; Isolated by filtration leaching gains obtain titanium liquid and residue, and calcine said residue; Calculate acidolysis rate according to formula 1, formula 1 is: acidolysis rate=m
A/ (m
A+ m
B) * 100%, wherein, m
ATiO in the expression titanium liquid
2Quality, m
BTiO in the expression residue
2Quality.
In one exemplary embodiment of the present invention, said method also can be included in before the step that said titaniferous ore and the concentrated sulphuric acid with scheduled volume mix, and titaniferous ore is carried out ball milling.
In one exemplary embodiment of the present invention, the step of the sour ore deposit ratio of said definite acidolysis reaction can be carried out according to formula 2, and formula 2 is: sour ore deposit ratio=(F * m
TiO2+ N)/M, wherein, m
TiO2TiO in the expression titaniferous ore
2Quality, N representes non-TiO in the titaniferous ore
2The acid consumption of composition, M are represented the quality of titaniferous ore, and F is controlled between 1.75～2.1.
In one exemplary embodiment of the present invention; Said method also can be included in after the said step that in potpourri, adds water; Liberated heat is not enough to cause under the situation of acidolysis reaction in diluting concentrated sulfuric acid institute; Said potpourri is heated with the initiation acidolysis reaction, and after acidolysis reaction takes place, stop heating.
In one exemplary embodiment of the present invention, the control of the temperature of said water-bath can be 65 ℃～75 ℃.
In one exemplary embodiment of the present invention, the control of the temperature of said calcining can be for more than 200 ℃.
In one exemplary embodiment of the present invention, the step service property (quality) concentration of said leaching reaction product is that 10～30% dilute sulfuric acid aqueous solution is as leaching liquid.
In one exemplary embodiment of the present invention, said method also can be included in the step that said titaniferous ore and the concentrated sulphuric acid with scheduled volume mix, and potpourri is stirred.
By compared with prior art; The present invention can provide a kind of method of accurate detection ilmenite acidolysis rate; And can compare the ilmenite acidolysis performance of the different factories and miness of objective appraisal through method of the present invention, foundation is provided for Producing Titanium Dioxide producer buys ilmenite.
Embodiment
Hereinafter, with combining concrete example to specify the method for detection titaniferous ore acidolysis rate of the present invention.
According to one exemplary embodiment of the present invention, the method that detects the titaniferous ore acidolysis rate may further comprise the steps: analyze the titaniferous ore chemical constitution, confirm the sour ore deposit ratio of acidolysis reaction then; Mix than the titaniferous ore and the concentrated sulphuric acid according to sour ore deposit, form potpourri scheduled volume; In said potpourri, adding water, is 80%～92% with the mass concentration dilution with the concentrated sulphuric acid; Carry out acidolysis reaction; After treating that acidolysis reaction finishes, slaking is to obtain reaction product; Under water bath condition, leach said reaction product; Isolated by filtration leaching gains obtain titanium liquid and residue, and calcine said residue; Calculate acidolysis rate according to formula 1, formula 1 is: acidolysis rate=m
A/ (m
A+ m
B) * 100%, wherein, m
ATiO in the expression titanium liquid
2Quality, m
BTiO in the expression residue
2Quality.Here; With the mass concentration dilution of the concentrated sulphuric acid is 80%～92%, in order to guarantee suitable acidolysis reaction speed and acidolysis rate; Generally speaking; The reaction velocity of the high more then acidolysis reaction of the acid concentration during acidolysis reaction is faster, maximum temperature is high more, and is too high like fruit acid concentration, then occurs rapid expansion of volume easily and causes the fryer accident; Concentration is crossed to hang down and then can be caused the acidolysis reaction time long, and acidolysis rate also possibly reduce.
Preferably; In one exemplary embodiment of the present invention, said method also can be included in before the step that said titaniferous ore and the concentrated sulphuric acid with scheduled volume mix, and titaniferous ore is carried out ball milling; Thereby reduce the granularity of titaniferous ore, so that carry out acidolysis and constituent analysis.Ball milling can reduce the granularity of titaniferous ore, if granularity is excessive, acidolysis rate is obviously reduced.Carry out after being diffused into titanium ore because the acidolysis reaction process is a sulfuric acid, particle is big, and sulfuric acid is difficult to diffuse into granule interior.
Preferably, in one exemplary embodiment of the present invention, the step of the sour ore deposit ratio of said definite acidolysis reaction is carried out according to formula 2, and formula 2 is: sour ore deposit ratio=(F * m
TiO2+ N)/M, wherein, m
TiO2TiO in the expression titaniferous ore
2Quality, N representes non-TiO in the titaniferous ore
2The acid consumption of composition, M are represented the quality of titaniferous ore, and F is controlled between 1.75～2.1.Here; The F value is controlled at 1.75～2.1st, has advantages of higher stability in order to make titanium liquid, thereby can store the long period, satisfies the requirement of later stage hydrolyzing process simultaneously; The too high then hydrolysis rate of F value is slow, and the low excessively then hydrolysis rate of F value is fast, the hydrolysis metatitanic acid is of poor quality.Yet, the invention is not restricted to this, those of ordinary skills also can confirm sour ore deposit ratio according to other common method.Here,,, consumed more sulfuric acid like this, increased production cost though can improve acidolysis rate to a certain extent if the acid amount that adds surpasses the upper limit of the sour ore deposit ratio that formula 2 draws; If the acid amount that adds is lower than the lower limit of the sour ore deposit ratio that formula 2 draws, then acidolysis reaction is incomplete, and acidolysis rate reduces.
Preferably; In one exemplary embodiment of the present invention; Said method also is included in after the said step that in potpourri, adds water; Be not enough to cause under the situation of acidolysis reaction at diluting concentrated sulfuric acid institute liberated heat, said potpourri is heated with the initiation acidolysis reaction, and after acidolysis reaction takes place, stop heating immediately.Acidolysis reaction is themopositive reaction, and initiation back id reaction liberated heat is enough to keep reaction velocity to carry out reaction fully, need not in heating after therefore causing.If do not stop heating, the excessive reaction of heat is too violent, might cause the system volume sharply to expand, even the danger that fryer takes place is arranged.
Preferably, in one exemplary embodiment of the present invention, the temperature of said water-bath is controlled to be 65 ℃～75 ℃.
Preferably, in one exemplary embodiment of the present invention, the temperature of said calcining is controlled to be more than 500 ℃.
Preferably, in one exemplary embodiment of the present invention, the step service property (quality) concentration of said leaching reaction product is that 10～30% dilute sulfuric acid aqueous solution is as leaching liquid.Add the appropriate amount of acid leaching and improved titanium liquid F value, can increase the stability of titanium liquid, the early stage hydrolysis that the local temperature height causes when can prevent just to have added water.In addition, also can use the sulfur waste acid of suitable concentration.Add sulfur waste acid and can reduce sulfur waste acid discharging and reduce production costs, reduce environmental pollution.
Preferably, in one exemplary embodiment of the present invention, said method also can be included in the step that said titaniferous ore and the concentrated sulphuric acid with scheduled volume mix, and potpourri is stirred, thereby add the carrying out of fast response.Here,, then can make some titanium ores of solid formation parcel that reaction earlier generates in inside if stir inhomogeneously, sulfuric acid can't be diffused into that these are wrapped the titanium ore surface, thereby influence acidolysis rate.
In one exemplary embodiment of the present invention, detect the method for titaniferous ore (is example with the ilmenite) acidolysis rate and also can implement through following steps:
1) chemical constitution of analysis ilmenite, for example, the chemical constitution of ilmenite can mainly comprise TiO
2, FeO, Fe
2O
3, MgO, CaO, SiO
2, Al
2O
3, V
2O
5, Cr
2O
3Deng; The titanium ore ball milling is crossed 320 mesh sieves later.
2) confirm the sour ore deposit ratio of acidolysis reaction.For example, can confirm the sour ore deposit ratio of acidolysis reaction based on the chemical composition of ilmenite, here, said sour ore deposit ratio is bright sulfur acid and ilmenite mass ratio.Preferably, can confirm the sour ore deposit ratio of acidolysis reaction according to formula 2, formula 2 is: sour ore deposit ratio=(F * m
TiO2+ N)/M, wherein, m
TiO2TiO in the expression titaniferous ore (being ilmenite here)
2Quality, N representes non-TiO in the titaniferous ore (being ilmenite here)
2The acid consumption of composition, M are represented the quality of titaniferous ore (, being ilmenite here), and the F value is controlled between 1.75～2.1.In addition, those of ordinary skills also can confirm sour ore deposit ratio based on other common method.
3) a certain amount of ilmenite of weighing and calculate the required concentrated sulphuric acid by sour ore deposit ratio fully stirs sulfuric acid and ilmenite.Here, the mixing time of sour ore deposit mixing can be 10～30min.
4) add dilution water concentrated sulphuric acid concentration dilution is arrived reaction acid concentration, add heat if the dilution heat that dilution water produces can not cause main reaction with electric jacket and after causing main reaction, stop heating at once.Here, the acid concentration of acidolysis reaction can just get 80%～92% according to content of titanium dioxide.
5) after acidolysis reaction (also can be described as main reaction) finished, slaking was to obtain reaction product.For example; After acidolysis reaction finishes with solid formation (promptly; Reaction product) transfers to and be incubated the schedule time in the baking oven of predetermined temperature (for example, temperature can be 150 ℃～170 ℃) (for example, 60～120min) to carry out slaking; Yet the mode and the temperature of slaking are not limited thereto, and those of ordinary skills also can adopt alternate manner and temperature to carry out slaking.
6) naturally cool to back below 70 ℃ after insulation finishes and add leaching water, in 65 ℃～75 ℃ water-baths, stir leaching 60～90min.Here; Preferably; When leaching, can add 10%～30% dilute sulfuric acid or mass concentration is the sulfur waste acid (spent acid that this sulfur waste acid is recycled for the titanium powder plant hydrolysis process) of 10-30%, and addition is 2～4 times of titanium ore quality; The concrete concentration control for preparing titanium liquid as required, general control leaching titanium concentration is in 120g/l～180g/l scope.Add the appropriate amount of acid leaching and improved titanium liquid F value, can increase the stability of titanium liquid, the early stage hydrolysis that the local temperature height causes when can prevent just to have added water.The industrial spent acid that adds can reduce spent acid discharging and reduces production costs, and reduces environmental pollution.
7) isolated by filtration obtains titanium liquid and residue, and the long-pending V (L) of record titanium liquid is with residue weighing residue quality m (g) after calcining 10～20min more than 500 ℃.
8) detect TiO in the titanium liquid
2Be C
1(g/L) (C1 is the TiO in the titanium liquid of unit volume
2Quality) TiO and in the residue
2Mass percent be C
2(%);
9) calculate acidolysis rate according to following formula 1;
Formula 1 is: acidolysis rate=m
A/ (m
A+ m
B) * 100%, wherein, m
A=C
1V, m
B=C
2M.
Further describe exemplary embodiment of the present invention below in conjunction with concrete example.
Example 1 is climbed the monitoring of titanium ilmenite concentrate acidolysis rate
1) the titanium ore ball milling is crossed 320 mesh sieves later, the analytical chemistry composition, its chemical constitution is as shown in table 1:
Table 1 ilmenite chemical composition analysis/%
2) calculate sour ore deposit ratio
The F value is got 1.9 sour ore deposit ratios
Used 98% acid in 100g ore deposit is 1.535 * 100 ÷ 98%=156.63g
Reaction acid concentration gets 85%, needs dilution water 1.535 * 100 ÷ 85%-156.63=23.96g
3) weighing 100g ilmenite joins in the 1000ml beaker that contains 156.63g 98% concentrated sulphuric acid, fully stirs 15min;
4) add the 23.96g dilution water and in beaker, cause main reaction, add heat if the dilution heat that dilution water produces can not cause main reaction with electric jacket and after causing main reaction, stop heating at once.
5) main reaction is transferred to solid formation more than the baking oven slaking 60min after finishing;
6) naturally cool to the adding of back below 70 ℃ 300ml water after insulation finishes, in 65 ℃～75 ℃ water-baths, stir leaching 60～90min.
7) isolated by filtration obtains titanium liquid and residue, and the long-pending 390ml of record titanium liquid is with residue weighing residue quality 14.16g after calcining 10～20min more than 500 ℃;
8) detect TiO in the titanium liquid
2Content is 114.36g/L, TiO in the residue
2Be 10.7/%;
9) calculate acidolysis rate;
Peaceful 10 acidolysis rate of example 2 Panzhihuas detect
1) the titanium ore ball milling is crossed 320 mesh sieves later.The analytical chemistry composition, its chemical constitution is as shown in table 2:
The peaceful 10 ore deposit composition/% of table 2 Panzhihua
2) calculate sour ore deposit ratio
The F value is got 1.9 sour ore deposit ratios
Used 98% acid in 100g ore deposit is 1.57 * 100 ÷ 98%=160.2g
Reaction acid concentration gets 84%, needs dilution water 1.57 * 100 ÷ 84%-160.2=26.7g
3) weighing 100g ilmenite joins in the 1000ml beaker that contains 160.2g 98% concentrated sulphuric acid, fully stirs 15min;
4) add the 26.7g dilution water and in beaker, cause main reaction, add heat if the dilution heat that dilution water produces can not cause main reaction with electric jacket and after causing main reaction, stop heating at once.
5) main reaction is transferred to baking oven matured 120min with solid formation after finishing;
6) naturally cool to the adding of back below 70 ℃ 250ml water after insulation finishes, in 65 ℃～75 ℃ water-baths, stir leaching 60～90min.
7) isolated by filtration obtains titanium liquid and residue, and the long-pending 380ml of record titanium liquid is with residue weighing residue quality 16.6g after calcining 10～20min more than 500 ℃;
8) detect TiO in the titanium liquid
2Content is 108.55g/L, TiO in the residue
2Be 11.8/%;
9) calculate acidolysis rate;
Example 3 is climbed steel titanium slag acidolysis rate and is detected
1) titanium ore slag ball milling is crossed 320 mesh sieves later.The titanium slag chemical composition analysis is as shown in table 3:
Table 3 titanium slag chemical composition analysis/%
2) sour ore deposit is than calculating
The F value is got 1.9 sour ore deposit ratios
Used 98% acid in 100g ore deposit is 1.71 * 100 ÷ 98%=174.49g
Reaction acid concentration gets 91%, needs dilution water 1.71 * 100 ÷ 91%-174.49=13.42g
3) weighing 100g ilmenite joins in the 1000ml beaker that contains 174.49g 98% concentrated sulphuric acid, fully stirs 15min;
4) add the 13.42g dilution water and in beaker, cause main reaction, add heat if the dilution heat that dilution water produces can not cause main reaction with electric jacket and after causing main reaction, stop heating at once.
5) main reaction is transferred to solid formation more than the baking oven matured 80min after finishing;
6) naturally cool to the adding of back below 70 ℃ 300ml water after insulation finishes, in 65 ℃～75 ℃ water-baths, stir leaching 60～90min.
7) isolated by filtration obtains titanium liquid and residue, and titanium liquid amasss 380ml, with residue weighing residue quality 9.7g after calcining 10～20min more than 500 ℃;
8) detect TiO in the titanium liquid
2Content is 175.75g/L, TiO in the residue
2Be 35.03/%;
9) calculate acidolysis rate;
In sum, the invention provides a kind of method that can accurately detect the ilmenite acidolysis rate.Can compare the ilmenite acidolysis performance of the different factories and miness of objective appraisal through method of the present invention, foundation is provided for Producing Titanium Dioxide producer buys ilmenite.
Although combined exemplary embodiment to describe the present invention above, those of ordinary skills should be clear, under the situation of spirit that does not break away from claim and scope, can carry out various modifications to the foregoing description.
Claims (8)
1. a method that detects the titaniferous ore acidolysis rate is characterized in that, said method comprising the steps of:
Analyze the titaniferous ore chemical constitution, confirm the sour ore deposit ratio of acidolysis reaction then;
Mix than the titaniferous ore and the concentrated sulphuric acid according to sour ore deposit, form potpourri scheduled volume;
In said potpourri, adding water, is 80%～92% with the mass concentration dilution with the concentrated sulphuric acid;
Carry out acidolysis reaction;
After treating that acidolysis reaction finishes, slaking is to obtain reaction product;
Under water bath condition, leach said reaction product;
Isolated by filtration leaching gains obtain titanium liquid and residue, and calcine said residue;
Calculate acidolysis rate according to formula 1, formula 1 is: acidolysis rate=m
A/ (m
A+ m
B) * 100%, wherein, m
ATiO in the expression titanium liquid
2Quality, m
BTiO in the expression residue
2Quality.
2. the method for detection titaniferous ore acidolysis rate according to claim 1 is characterized in that, said method also is included in before the step that said titaniferous ore and the concentrated sulphuric acid with scheduled volume mix, and titaniferous ore is carried out ball milling.
3. the method for detection titaniferous ore acidolysis rate according to claim 1 is characterized in that, the step of the sour ore deposit ratio of said definite acidolysis reaction is carried out according to formula 2, and formula 2 is: sour ore deposit ratio=(F * m
TiO2+ N)/M, wherein, m
TiO2TiO in the expression titaniferous ore
2Quality, N representes non-TiO in the titaniferous ore
2The acid consumption of composition, M are represented the quality of titaniferous ore, and F is controlled between 1.75～2.1.
4. the method for detection titaniferous ore acidolysis rate according to claim 1; It is characterized in that; Said method also is included in after the said step that in potpourri, adds water; Be not enough to cause under the situation of acidolysis reaction at diluting concentrated sulfuric acid institute liberated heat, said potpourri is heated with the initiation acidolysis reaction, and after acidolysis reaction takes place, stop heating.
5. the method for detection titaniferous ore acidolysis rate according to claim 1 is characterized in that, the temperature of said water-bath is controlled to be 65 ℃～75 ℃.
6. the method for detection titaniferous ore acidolysis rate according to claim 1 is characterized in that the temperature of said calcining is controlled to be more than 200 ℃.
7. the method for detection titaniferous ore acidolysis rate according to claim 1 is characterized in that, the step service property (quality) concentration of said leaching reaction product is that 10～30% dilute sulfuric acid aqueous solution is as leaching liquid.
8. the method for detection titaniferous ore acidolysis rate according to claim 1 is characterized in that, said method also is included in the step that said titaniferous ore and the concentrated sulphuric acid with scheduled volume mix, and potpourri is stirred.
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| CN113607670B (en) * | 2021-08-05 | 2024-04-02 | 攀枝花学院 | Method for measuring hydrolysis rate of industrial titanium liquid before hydrolysis ash-turning point |
| CN113740479A (en) * | 2021-08-18 | 2021-12-03 | 安徽迪诺环保新材料科技有限公司 | Method for qualitatively determining acidolysis rate degree of acid-ore mixture |
| CN113702570A (en) * | 2021-08-24 | 2021-11-26 | 广西蓝星大华化工有限责任公司 | Analysis method for hydrolysis rate of titanium liquid |
| CN115308079A (en) * | 2022-08-26 | 2022-11-08 | 攀钢集团重庆钒钛科技有限公司 | Characterization method for acidolysis rate of titanium concentrate in laboratory |
| CN115308079B (en) * | 2022-08-26 | 2024-03-29 | 攀钢集团重庆钒钛科技有限公司 | Characterization method of acidolysis rate of titanium concentrate in laboratory |
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