CN104261468B - A kind of manufacture method of low alkali catalysis titanium white - Google Patents
A kind of manufacture method of low alkali catalysis titanium white Download PDFInfo
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- CN104261468B CN104261468B CN201410480446.9A CN201410480446A CN104261468B CN 104261468 B CN104261468 B CN 104261468B CN 201410480446 A CN201410480446 A CN 201410480446A CN 104261468 B CN104261468 B CN 104261468B
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Abstract
nullThe invention discloses the manufacture method of a kind of low alkali catalysis titanium white，It comprises the following steps: acidolysis、Crystallization、Concentration、Hydrolysis、One washes、Bleaching、Two wash、Salt treatment、Calcining and pulverizing，After salt treatment completes, before calcining, wash qualified metatitanic acid sucking filtration pull an oar two to 320-380g/l，Take 1000ml after stirring evenly and put into continuation stirring in clean beaker，It is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs，Beaker is heated up as the thermostat water bath of 85-95 °，The mixed solution temperature that intensification limit, limit is stirred to beaker reaches 80-90 °，Take out beaker after insulation 1h and be cooled to 35-50 DEG C，Add with metatitanic acid volume ratio 1:(5-10) the alcoholic solution that mass fraction is 75%，Sucking filtration after stirring 25-60min，Take filter cake drying and grind rear tabletting；The invention has the beneficial effects as follows that product alkali metal containing is few, particle diameter is little, need not crush and classification.
Description
Technical field
The present invention relates to denitration catalyst titanium white production technical field, particularly relate to the manufacture method of a kind of low alkali catalysis titanium white.
Background technology
TiO2As a kind of new function material, with its make the active height of catalyst of carrier, selectivity toxic good, anti-is strong, low temperature active good, surface acidity is adjustable and the advantage such as high temperature reducibility, although the research of each side is ripe all not enough at present, but its shown huge applications potentiality can not be ignored, many scholars think, TiO2The SiO that continues will be become2,Al2O3Third generation catalyst carrier afterwards.The primary raw material of the titanium dioxide sold on market is exactly TiO2The production technology of sulfuric acid method titanium pigment generally comprises acidolysis, crystallization, concentration, hydrolysis, one washes, bleaches, two wash, salt treatment, calcining and pulverizing, its technological process described in detail in " sulfuric acid method titanium pigment production " literary composition, at present, the alkali metal salt and K, Na ion that contain in the catalysis titanium white finished product prepared in this way are typically in about 100ppm.Catalyst poisoning will be made to lose efficacy it is known that the alkali metal content such as potassium, sodium is slightly higher in catalysis titanium white.And the existing most of factory of technique all adopts negative and positive leaving office exchanger resin or semi-transparent embrane method etc. to remove most of alkali metal ion in the demineralized water of washing, the alkali metal salt content that the result of this technique is in final products is almost consistent with the content of demineralized water, it is impossible to accomplish the purpose further reduced.
Summary of the invention
The technical problem to be solved in the present invention is that existing titanium white production technique can not effectively remove alkali metal, provides the manufacture method of a kind of low alkali catalysis titanium white for this.
nullThe technical scheme is that the manufacture method of a kind of low alkali catalysis titanium white，It comprises the following steps: acidolysis、Crystallization、Concentration、Hydrolysis、One washes、Bleaching、Two wash、Salt treatment、Calcining and pulverizing，It is characterized in that wash qualified metatitanic acid sucking filtration after salt treatment completes before calcining pulls an oar two to 320-380g/l，Take 1000ml after stirring evenly and put into continuation stirring in clean beaker，It is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs，Beaker is heated up as the thermostat water bath of 85-95 °，The mixed solution temperature that intensification limit, limit is stirred to beaker reaches 80-90 °，Take out beaker after insulation 1h and be cooled to 35-50 DEG C，Add with metatitanic acid volume ratio 1:(5-10) the alcoholic solution that mass fraction is 75%，Sucking filtration after stirring 25-60min，Take filter cake drying and grind rear tabletting.
Described in such scheme, two wash the making beating of qualified metatitanic acid sucking filtration to 360g/l.
Take out after the insulation 1h of beaker described in such scheme and be cooled to 40 DEG C.
The alcoholic solution added described in such scheme and metatitanic acid volume ratio 1:10, mass fraction is 75%.
Processing through brittle before pulverizing after calcining described in such scheme, described brittle process includes the material hard X ray obtained after calcining is irradiated 10-30min, more suddenly freezes 3-7min under-5-0 °.
The invention has the beneficial effects as follows and in salt treatment operation, be proportionally added into 75% alcoholic solution in order to absorb the alkali metal salt in inclined material once again.Alcoholic solution itself without alkali metal ion and can arbitrary proportion be dissolved in water, therefore can accomplish again to dissolve the effect of alkali metal salt.And alcoholic solution is removed by filter pressing in squeezing process later, remain in material ethanol then rotary kiln calcining process in volatilization or burning and remove, to ensure the pure of product, below 40ppm can be down to the product caustic soda metal salt concentration that this technology obtains.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1: wash qualified metatitanic acid sucking filtration after salt treatment completes before calcining by two and pull an oar to 320g/l, take 1000ml after stirring evenly and put into continuation stirring in clean beaker, it is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs, surveying PH afterwards is 10.7, beaker is heated up as the thermostat water bath of 85 °, the mixed solution temperature that intensification limit, limit is stirred to beaker reaches 80 °, recording PH after insulation 1h is 10.4, take out beaker and be cooled to 35 DEG C, add the alcoholic solution that mass fraction is 75% of 50ml, sucking filtration after stirring 25min, take filter cake drying and grind rear tabletting.
Embodiment 2: wash qualified metatitanic acid sucking filtration after salt treatment completes before calcining by two and pull an oar to 360g/l, take 1000ml after stirring evenly and put into continuation stirring in clean beaker, it is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs, surveying PH afterwards is 11, beaker is heated up as the thermostat water bath of 95 °, the mixed solution temperature that intensification limit, limit is stirred to beaker reaches 90 °, recording PH after insulation 1h is 10.5, take out beaker and be cooled to 50 DEG C, add the alcoholic solution that mass fraction is 75% of 67ml, sucking filtration after stirring 40min, take filter cake drying and grind rear tabletting.
Embodiment 3: wash qualified metatitanic acid sucking filtration after salt treatment completes before calcining by two and pull an oar to 380g/l, take 1000ml after stirring evenly and put into continuation stirring in clean beaker, it is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs, surveying PH afterwards is 10.8, beaker is heated up as the thermostat water bath of 90 °, the mixed solution temperature that intensification limit, limit is stirred to beaker reaches 85 °, recording PH after insulation 1h is 11.7, take out beaker and be cooled to 40 DEG C, add the alcoholic solution that mass fraction is 75% of 100ml, sucking filtration after stirring 30min, take filter cake drying and grind rear tabletting.
Embodiment 4: wash qualified metatitanic acid sucking filtration after salt treatment completes before calcining by two and pull an oar to 360g/l, take 1000ml after stirring evenly and put into continuation stirring in clean beaker, it is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs, surveying PH afterwards is 10.7, beaker is heated up as the thermostat water bath of 90 °, the mixed solution temperature that intensification limit, limit is stirred to beaker reaches 85 °, recording PH after insulation 1h is 10.3, take out beaker and be cooled to 40 DEG C, add the alcoholic solution that mass fraction is 75% of 200ml, sucking filtration after stirring 30min, take filter cake drying and grind rear tabletting.
Embodiment 5: wash qualified metatitanic acid sucking filtration after salt treatment completes before calcining by two and pull an oar to 360g/l, take 1000ml after stirring evenly and put into continuation stirring in clean beaker, it is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs, surveying PH afterwards is 11.2, beaker is heated up as the thermostat water bath of 90 °, the mixed solution temperature that intensification limit, limit is stirred to beaker reaches 85 °, recording PH after insulation 1h is 10.5, take out beaker and be cooled to 50 DEG C, add the alcoholic solution that mass fraction is 75% of 100ml, sucking filtration after stirring 30min, take filter cake drying and grind rear tabletting.
Embodiment 6: wash qualified metatitanic acid sucking filtration after salt treatment completes before calcining by two and pull an oar to 360g/l, take 1000ml after stirring evenly and put into continuation stirring in clean beaker, it is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs, surveying PH afterwards is 10.9, beaker is heated up as the thermostat water bath of 90 °, the mixed solution temperature that intensification limit, limit is stirred to beaker reaches 85 °, recording PH after insulation 1h is 10.6, take out beaker and be cooled to 45 DEG C, add the alcoholic solution that mass fraction is 75% of 100ml, sucking filtration after stirring 30min, take filter cake drying and grind rear tabletting.
Embodiment 7: wash qualified metatitanic acid sucking filtration after salt treatment completes before calcining by two and pull an oar to 360g/l, take 1000ml after stirring evenly and put into continuation stirring in clean beaker, it is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs, surveying PH afterwards is 11.1, beaker is heated up as the thermostat water bath of 90 °, the mixed solution temperature that intensification limit, limit is stirred to beaker reaches 85 °, recording PH after insulation 1h is 10.7, take out beaker and be cooled to 40 DEG C, add the alcoholic solution that mass fraction is 75% of 100ml, sucking filtration after stirring 30min, take filter cake drying and grind rear tabletting.
Embodiment 8: wash qualified metatitanic acid sucking filtration after salt treatment completes before calcining by two and pull an oar to 360g/l, take 1000ml after stirring evenly and put into continuation stirring in clean beaker, it is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs, surveying PH afterwards is 11.1, beaker is heated up as the thermostat water bath of 90 °, the mixed solution temperature that intensification limit, limit is stirred to beaker reaches 85 °, recording PH after insulation 1h is 10.2, take out beaker and be cooled to 35 DEG C, add the alcoholic solution that mass fraction is 75% of 100ml, sucking filtration after stirring 30min, take filter cake drying and grind rear tabletting.
It is designated as embodiment 9 without the tabletting of the Ethanol Treatment that mass fraction is 75%, after salt treatment completes, before calcining, wash qualified metatitanic acid sucking filtration pull an oar two to 360g/l, take 1000ml after stirring evenly and put into continuation stirring in clean beaker, it is simultaneously introduced ammonia spirit 115ml that mass fraction is 20% and stirs, surveying PH afterwards is 10.5, beaker is heated up as the thermostat water bath of 90 °, the mixed solution temperature that intensification limit, limit is stirred to beaker reaches 85 °, recording PH after insulation 1h is 10.2, sucking filtration after stirring 30min, takes filter cake drying and grinds rear tabletting.
Na ion concentration, K ion concentration diffractometer contained by the tabletting of embodiment 1-10 gained being detected, correction data is as shown in the table:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | |
| Na+ | 85ppm | 77ppm | 39ppm | 30ppm | 98ppm | 68ppm | 39ppm | 33ppm | 130ppm |
| K+ | 85ppm | 70ppm | 32ppm | 27ppm | 92ppm | 58ppm | 32ppm | 29ppm | 125ppm |
As can be seen from the above table, adding mass fraction 75% alcoholic solution and can effectively absorb K, Na ion in material, in finished product, alkali metal salt content can effectively reduce；Material should control at 10:1 with adding volumes of aqueous ethanol ratio.Ethanol added K, Na ionic absorption DeGrain at least, and the while that time too much, assimilation effect promoting inconspicuous, production cost is high；During the interpolation of alcoholic solution, temperature of charge optimum is at 40 degree.Temperature too high ethanol volatilization is serious, and assimilation effect is poor；Then length consuming time, energy resource consumption are big in process of production for too low material.
In filter pressing operation, alcoholic solution is filtered is separated with squeezing, and part residual is then volatilized in the process of rotary kiln calcining or burns and remove.Filtrate portion need to collect, and uses fractionating column again to separate, purifying ethanol and ammonia, to reach the recycling of alcoholic solution, reduces production cost.
The present invention is the ethanol that the material obtained on the basis of above-described embodiment 1-9 eliminates residual after firing, obtain pure titanium dioxide granule, if directly titanium dioxide granule is crushed, due to some bonding of the material after calcining, special equipment such as Raymond machine is needed to crush, classification then through classifying turbine, material feeding feed screw after pulverizing is delivered to finished product bin, complex steps, use Raymond machine and classifying turbine energy consumption higher, preference for this present invention is to add a brittle step processed between calcining and pulverizing, some bonding dry materials can be separated refinement, save broken and classification step, shorten technological process, improve work efficiency.
Specifically, preferred embodiment 10: the material hard X ray obtained after calcining is irradiated 10min, suddenly 3min is frozen again under-5 °, after hard X ray is irradiated, material can dry, will not be bonding between material particles, freezes process then through too urgent, material can be quickly brittle, it is refined into evengranular particulate, it is not necessary to through broken and classification, it is possible to directly as finished product.
Preferred embodiment 11: the material hard X ray obtained after calcining is irradiated 30min, more suddenly freezes 7min at 0.
Hard X ray irradiation time can not be too short, does not otherwise have the effect of dried material, also can not be long, and long meeting causes the unstable chemcial property of material, the temperature suddenly frozen can not too low also can not be too high, otherwise material particular diameter will not produce brittle reaction.Data Comparison is shown in following table:
| Condition | Size |
| Hard X ray irradiates 8min, and-7 ° of urgency freeze 1min | 200nmn |
| Hard X ray irradiates 10min, and-5 ° of urgency freeze 3min | 100nmn |
| Hard X ray irradiates 20min, and-2 ° of urgency freeze 5min | 96nmn |
| Hard X ray irradiates 30min, and 0 ° of urgency freezes 7min | 97nmn |
| Hard X ray irradiates 35min, and 0 ° of urgency freezes 8min | 204nmn |
Claims (5)
- null1. the manufacture method of a low alkali catalysis titanium white，It comprises the following steps: acidolysis、Crystallization、Concentration、Hydrolysis、One washes、Bleaching、Two wash、Salt treatment、Calcining and pulverizing，It is characterized in that wash qualified metatitanic acid sucking filtration after salt treatment completes before calcining pulls an oar two to 320-380g/L，Take 1000mL after stirring evenly and put into continuation stirring in clean beaker，It is simultaneously introduced ammonia spirit 115mL that mass fraction is 20% and stirs，Beaker is heated up as the thermostat water bath of 85-95 DEG C，The mixed solution temperature that intensification limit, limit is stirred to beaker reaches 80-90 DEG C，Take out beaker after insulation 1h and be cooled to 35-50 DEG C，Add with metatitanic acid volume ratio 1:(5-10) the alcoholic solution that mass fraction is 75%，Sucking filtration after stirring 25-60min，Take filter cake drying and grind rear tabletting.
- 2. the manufacture method of a kind of low alkali catalysis titanium white as claimed in claim 1, is characterized in that described two wash the making beating of qualified metatitanic acid sucking filtration to 360g/L.
- 3. the manufacture method of a kind of low alkali catalysis titanium white as claimed in claim 2, takes out after it is characterized in that described beaker insulation 1h and is cooled to 40 DEG C.
- 4. the manufacture method of a kind of low alkali catalysis titanium white as claimed in claim 3, is characterized in that the alcoholic solution of described addition and metatitanic acid volume ratio 1:10, and mass fraction is 75%.
- 5. the manufacture method of a kind of low alkali catalysis titanium white as described in as arbitrary in claim 1-4, process through embrittlement before pulverizing after it is characterized in that described calcining, described brittle process includes the material hard X ray obtained after calcining is irradiated 10-30min, more suddenly freezes 3-7min at-5-0 DEG C.
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| CN107298460B (en) * | 2017-05-22 | 2020-01-07 | 超彩环保新材料科技有限公司 | Low-sulfur titanium dioxide with ultrahigh specific surface area, and preparation method and application thereof |
| CN112473640A (en) * | 2020-12-09 | 2021-03-12 | 安徽迪诺环保新材料科技有限公司 | Method for micro-adjusting pore volume and pore diameter of nano titanium dioxide for flue gas denitration catalyst |
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