Summary of the invention
For the problems of the prior art, the object of the invention is to provide the preparation method of a kind of denitrating catalyst titanium tungsten composite powder
Technical scheme of the present invention is: the preparation method of titanium tungsten composite powder for a kind of denitrating catalyst, in the concentrated titanium liquid of Titanium White Production By Sulfuric Acid Process, add hydrolysis crystal seed and ammonium metatungstate solution, after hydrolysis, pulverize and obtain this titanium tungsten composite powder through detergent bleach calcining.
Further, described concentrated titanium concentration is with TiO
2count 180 ~ 220 g/L.
Further, the concentration of described ammonium metatungstate solution is 800-1200 g/L.
Further, the preparation method of described hydrolysis crystal seed is: by concentration with TiO
2the concentrated titanium liquid of counting 180 ~ 220 g/L is added in the soda bath of 6 ~ 10wt%, and the volume ratio of concentrated titanium liquid and soda bath is 3.0 ~ 3.2:1, controls reaction temperature and is not less than 85 DEG C, when being stirred to its stability and reaching 70-110mL.
The method comprises the following steps:
1) the concentrated titanium liquid of Titanium White Production By Sulfuric Acid Process is heated to 96 DEG C and insulation, concentrated titanium concentration is with TiO
2meter 180 ~ 220 g/L;
2) hydrolysis crystal seed is added to concentrated titanium liquid, addition is the concentrated long-pending 2.5-3.0% of titanium liquid;
3) ammonium metatungstate solution is heated to 90 ~ 100 DEG C, is then added in concentrated titanium liquid, addition is with mass ratio WO
3/ TiO
2meter 5-10:95-90;
4) will concentrate after titanium liquid is incubated 15 ~ 20min and be warming up to 112 DEG C, after it becomes steel grey, be warming up to 114 DEG C, after reaction 1h, start moisturizing, make TiO
2concentration is 150-170 g/L.
5) hydrolyzation material steps d being obtained washs, bleaches, two washings, and the filter cake after press filtration is at 450-550 DEG C of temperature lower calcination 2-5 h; Then pulverize.
Further, the ammonium metatungstate solution and step 2 of step 3)) crystal seed together be added in titanium liquid.
Further, when the ammonium metatungstate solution of step 3) is warming up to 112 DEG C in step 4), be added in titanium liquid.
Further, when the ammonium metatungstate solution of step 3) becomes steel grey in step 4), be added in titanium liquid.
The present invention is taking the concentrated titanium liquid of Production By Sulfuric Acid Process as raw material, in the process of the hydrolysis of titanium liquid, adds tungsten solution, in the process of hydrolysis, make like this tungsten and titanium evenly, combine closely, and after hydrolysis, the content of tungsten can and not bleached and reduce along with washing.For the factory that has whole Production By Sulfuric Acid Process technique, the method has reduced the follow-up step that adds tungsten, has shortened production technology.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
Step 1: get concentrated titanium liquid 500 L that measure, titanium concentration is (with TiO
2meter) 180 g/L, be heated to 96 DEG C of heat preservation for standby use;
Step 2: the preparation of hydrolysis crystal seed: by the titanium liquid phase that is heated to the titanium liquid 4.5L(of 85 DEG C and step 1 with) join in the soda bath that 85 DEG C of 1.5L mass fractions are 6%, be incubated in 85 DEG C of whipping process and survey its stability, until stability stops while reaching 70-110mL;
Step 3: compound concentration is 800g/L ammonium metatungstate solution;
Step 4: the crystal seed that 5.04L step 2 is prepared joins in the ready titanium liquid of step 1;
Step 5: the ammonium metatungstate solution that 6.78L step 3 is prepared and step 4 join in the ready titanium liquid of step 1 simultaneously;
Step 6: be warming up to 112 DEG C after step 5 being added to the titanium liquid insulation 15min of crystal seed and tungsten solution, wait after becoming steel grey and be warming up to 114 DEG C, start moisturizing 92.7L after 1h, 2h has mended, and hydrolysis finishes;
Step 7: the hydrolyzation material that step 6 is obtained carries out washing, bleaches, two washes according to the technique of Production By Sulfuric Acid Process, then by the filter cake after press filtration at 450 DEG C of temperature lower calcination 5h;
Step 8: the calcining material that step 7 is obtained is pulverized, and obtains TiO
2/ WO
3the denitrating catalyst of=95:5 titanium tungsten composite powder.
Embodiment 2:
Step 1: get concentrated titanium liquid 500 L that measure, titanium concentration is (with TiO
2meter) 195 g/L, be heated to 96 DEG C of heat preservation for standby use;
Step 2: the preparation of hydrolysis crystal seed: by the titanium liquid phase that is heated to the titanium liquid 4.65L(of 85 DEG C and step 1 with) join in the soda bath that 85 DEG C of 1.5L mass fractions are 8%, be incubated in 85 DEG C of whipping process and survey its stability, until stability stops while reaching 70-110mL;
Step 3: compound concentration is 1100g/L ammonium metatungstate solution;
Step 4: the crystal seed that 5.56L step 2 is prepared joins in the ready titanium liquid of step 1;
Step 5: the ammonium metatungstate solution that 5.36L step 3 is prepared and step 4 join in the ready titanium liquid of step 1 simultaneously;
Step 6: be warming up to 112 DEG C after step 5 being added to the titanium liquid insulation 15min of crystal seed and tungsten solution, wait after becoming steel grey and be warming up to 114 DEG C, start moisturizing 103.6L after 1h, 2h has mended, and hydrolysis finishes;
Step 7: the hydrolyzation material that step 6 is obtained carries out washing, bleaches, two washes according to the technique of Production By Sulfuric Acid Process, then by the filter cake after press filtration at 450 DEG C of temperature lower calcination 3h;
Step 8: the calcining material that step 7 is obtained is pulverized, and obtains TiO
2/ WO
3the denitrating catalyst of=94:6 titanium tungsten composite powder.
Embodiment 3:
Step 1: get concentrated titanium liquid 500 L that measure, titanium concentration is (with TiO
2meter) 200 g/L, be heated to 96 DEG C of heat preservation for standby use;
Step 2: the preparation of hydrolysis crystal seed: by the titanium liquid phase that is heated to the titanium liquid 4.73L(of 85 DEG C and step 1 with) join in the soda bath that 85 DEG C of 1.5L mass fractions are 8%, be incubated in 85 DEG C of whipping process and survey its stability, until stability stops while reaching 70-110mL;
Step 3: compound concentration is 1200g/L ammonium metatungstate solution;
Step 4: the crystal seed that 5.6L step 2 is prepared joins in the ready titanium liquid of step 1;
Step 5: be warming up to 112 DEG C after step 4 being added to the titanium liquid insulation 15min of crystal seed, wait after becoming steel grey and be warming up to 114 DEG C, start moisturizing 82.6L after 1h, 2h has mended, and hydrolysis finishes;
Step 6: the ammonium metatungstate solution that 5.04L step 3 is prepared joins in the titanium liquid that step 5 has just been warming up to 112 DEG C;
Step 7: the hydrolyzation material that step 5 is obtained carries out washing, bleaches, two washes according to the technique of Production By Sulfuric Acid Process, then by the filter cake after press filtration at 500 DEG C of temperature lower calcination 3h;
Step 8: the calcining material that step 7 is obtained is pulverized, and obtains TiO
2/ WO
3the denitrating catalyst of=93:7 titanium tungsten composite powder.
Embodiment 4:
Step 1: get concentrated titanium liquid 500 L that measure, titanium concentration is (with TiO
2meter) 200 g/L, be heated to 96 DEG C of heat preservation for standby use;
Step 2: the preparation of hydrolysis crystal seed: by the titanium liquid phase that is heated to the titanium liquid 4.73L(of 85 DEG C and step 1 with) join in the soda bath that 85 DEG C of 1.5L mass fractions are 8%, be incubated in 85 DEG C of whipping process and survey its stability, until stability stops while reaching 70-110mL;
Step 3: compound concentration is 1000g/L ammonium metatungstate solution;
Step 4: the crystal seed that 5.7L step 2 is prepared joins in the ready titanium liquid of step 1;
Step 5: the ammonium metatungstate solution that 6.05L step 3 is prepared joins in the ready titanium liquid of step 1;
Step 6: be warming up to 112 DEG C after step 5 being added to the titanium liquid insulation 20min of crystal seed and tungsten solution, wait after becoming steel grey and be warming up to 114 DEG C, start moisturizing 161L after 1h, 2h has mended, and hydrolysis finishes;
Step 7: the hydrolyzation material that step 6 is obtained carries out washing, bleaches, two washes according to the technique of Production By Sulfuric Acid Process, then by the filter cake after press filtration at 450 DEG C of temperature lower calcination 4h;
Step 8: the calcining material that step 7 is obtained is pulverized, and obtains TiO
2/ WO
3the denitrating catalyst of=95:5 titanium tungsten composite powder.
Embodiment 5:
Step 1: get concentrated titanium liquid 500 L that measure, titanium concentration is (with TiO
2meter) 205 g/L, be heated to 96 DEG C of heat preservation for standby use;
Step 2: the preparation of hydrolysis crystal seed: by the titanium liquid phase that is heated to the titanium liquid 4.65L(of 85 DEG C and step 1 with) join in the soda bath that 85 DEG C of 1.5L mass fractions are 8%, be incubated in 85 DEG C of whipping process and survey its stability, until stability stops while reaching 70-110mL;
Step 3: compound concentration is 1100g/L ammonium metatungstate solution;
Step 4: the crystal seed that 5.74L step 2 is prepared joins in the ready titanium liquid of step 1;
Step 5: be warming up to 112 DEG C after step 5 being added to the titanium liquid insulation 20min of crystal seed and tungsten solution, wait after becoming steel grey and be warming up to 114 DEG C, start moisturizing 144L after 1h, 2h has mended, and hydrolysis finishes;
Step 6: the ammonium metatungstate solution that 5.63L step 3 is prepared adds when titanium liquid has just become steel grey in step 5;
Step 7: the hydrolyzation material that step 5 is obtained carries out washing, bleaches, two washes according to the technique of Production By Sulfuric Acid Process, then by the filter cake after press filtration at 550 DEG C of temperature lower calcination 2h;
Step 8: the calcining material that step 7 is obtained is pulverized, and obtains TiO
2/ WO
3the denitrating catalyst of=94:6 titanium tungsten composite powder.
Embodiment 6:
Step 1: get concentrated titanium liquid 500 L that measure, titanium concentration is (with TiO
2meter) 220g/L, be heated to 96 DEG C of heat preservation for standby use;
Step 2: the preparation of hydrolysis crystal seed: by the titanium liquid phase that is heated to the titanium liquid 4.8L(of 85 DEG C and step 1 with) join in the soda bath that 85 DEG C of 1.5L mass fractions are 10%, be incubated in 85 DEG C of whipping process and survey its stability, until stability stops while reaching 70-110mL;
Step 3: compound concentration is 1200g/L ammonium metatungstate solution;
Step 4: the crystal seed that 6.27 L steps 2 are prepared joins in the ready titanium liquid of step 1;
Step 5: the ammonium metatungstate solution that 5.53L step 3 is prepared joins in the ready titanium liquid of step 1;
Step 6: be warming up to 112 DEG C after step 5 being added to the titanium liquid insulation 30min of crystal seed and tungsten solution, wait after becoming steel grey and be warming up to 114 DEG C, start moisturizing 141.44L after 1h, 2h has mended, and hydrolysis finishes;
Step 7: the hydrolyzation material that step 6 is obtained carries out washing, bleaches, two washes according to the technique of Production By Sulfuric Acid Process, then by the filter cake after press filtration at 550 DEG C of temperature lower calcination 2h;
Step 8: the calcining material that step 7 is obtained is pulverized, and obtains TiO
2/ WO
3the denitrating catalyst of=90:10 titanium tungsten composite powder.
Above embodiment is only that the technical scheme that the present invention is recorded illustrates, and all simple distortion of making in the situation that not departing from core of the present invention or amendment all fall into protection scope of the present invention.