CN105289036A - Novel method for performing vacuum crystallization on ferrous sulfate from titanium liquid in titanium dioxide production process - Google Patents
Novel method for performing vacuum crystallization on ferrous sulfate from titanium liquid in titanium dioxide production process Download PDFInfo
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- CN105289036A CN105289036A CN201510724436.XA CN201510724436A CN105289036A CN 105289036 A CN105289036 A CN 105289036A CN 201510724436 A CN201510724436 A CN 201510724436A CN 105289036 A CN105289036 A CN 105289036A
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Abstract
The invention discloses a novel method for performing vacuum crystallization on ferrous sulfate from titanium liquid in titanium dioxide production. According to the method, the conventional ferrous sulfate vacuum crystallization process and equipment are innovated. The process innovation refers to the operation of replacing the conventional method for generating vacuum by virtue of steam jet by a method for condensing water vapor above titanium liquid in a crystallization kettle so as to generate vacuum by virtue of cryogenic refrigeration. The equipment innovation refers to the operation of replacing the conventional secondary steam jet equipment and circulating cooling water equipment for cooling high-temperature acid containing liquid by the complete refrigerating equipment generating a certain low temperature. According to the method disclosed by the invention, ferrous sulfate is separated from the titanium liquid in the crystallization kettle, lots of high-temperature high-pressure steam can be saved, and the production cost of titanium dioxide by sulfuric acid method is greatly reduced. In addition, the acidic condensate extracted from the crystallization kettle by vacuum can return to be used for an ilmenite powder sulfuric acid dissolving process, so that the amount of sulfuric acid in the process of generating titanium dioxide by a sulfuric acid method is reduced, the emission amount of acid waste liquid is greatly reduced, and clean production is realized.
Description
Technical field:
The invention belongs to Chemical Engineering and field of chemical equipment, be specifically related to a kind of method obtaining condition of high vacuum degree in Chemical Manufacture, particularly in a kind of Titanium White Production By Sulfuric Acid Process technique by byproduct ferrous sulfate from titanium liquid vacuum crystallization separate out new method and relevant chemical industry equipment.
Background technology:
The formal name used at school of titanium dioxide is titanium dioxide, its stable chemical nature, nontoxic, it is the best Chinese white of the performance of generally acknowledging in the world at present, be widely used in the industries such as coating, plastics, rubber, ink, paper, chemical fibre, pottery, daily use chemicals, medicine, food, wherein coating, plastics and papermaking are the maximum three large industries of titanium dioxide consumption, almost account for more than 80% of the total consumption of titanium dioxide; Compared with other Chinese whites, titanium dioxide has superior whiteness, tinting strength, tinting power, covering power, weatherability, heat resistance and chemical stability, does not particularly have toxicity, and therefore, the market demand of titanium dioxide is huge and in the trend that increases year by year.
According to the statistics display of Chinese Titanium white powder employer's organization in 2014, current China titanium white production is mainly based on sulfuric acid process, the output of sulfuric acid method titanium pigment is 246.63 ten thousand tons/year, and the output of Titanium Dioxide Produced by Chloride Procedure, less than 50,000 tons/year, only accounts for 1.78% of national total output.Nearly 100 of existing titanium white production enterprise of China, wherein most employing sulfuric acid process, adopts the enterprise of chloridising to only have two or three.In the enterprise of the Titanium White Production By Sulfuric Acid Process that the current whole nation is all, byproduct ferrous sulfate vacuum crystallization all adopts the steam two-stage injection of certain pressure (0.5 ~ 0.8MPa) to add the vacuum technique of water ring vacuum pump, this technique can make the end vacuum pressure in ferrous sulfate crystallization system reach 1000Pa (absolute pressure), operation pressure can maintain 1800 ~ 5000Pa, can make the moisture explosive evaporation at a lower temperature in titanium liquid; Along with moisture evaporation and constantly taken away by vacuum, the ferrous sulfate concentration in titanium liquid to become after supersaturation crystallization from titanium liquid from unsaturated.Although this technique can obtain the vacuum required for ferrous sulfate crystallization and substantially meet production requirement, there are following three large problems:
1, bring into wherein by the acid water steam in ferrous sulfate crystallization system in pressurized vapor course of injection, this steam generates a large amount of acid waste liquids after cooling water system condensation, adds the burden of environmental protection pressure and wastewater treatment.
2, ferrous sulfate crystallization system adopts pressurized vapor to spray and produces the kinetic energy that vacuum with only steam, and the saturated-steam temperature that pressure is 0.5 ~ 0.8MPa just reaches 152 ~ 170 DEG C, although such steam still has higher waste heat energy after spraying, but because there is acid water steam to be mixed into, sour corrosion problem and safety problem need be solved to its UTILIZATION OF VESIDUAL HEAT IN, this part of waste heat is not utilized effectively substantially at present, causes the serious waste of steam thermal energy; According to statistics, current sulfuric acid method titanium pigment is produced product per ton and is always consumed steam about 1.3 ~ 1.5 tons, consume steam the overwhelming majority be used for ferrous sulfate vacuum crystallization workshop section, current present situation is, the steam that this workshop section uses forms acid vapors after spraying, its heat energy contained and remaining kinetic energy not only fail to be utilized, and need to set up another set of recirculating cooling water system on the contrary and cool and emission treatment it, therefore make sulfuric acid method titanium pigment production cost remain high.
3, existing high steam two-stage injection adds the vacuum technique of water ring vacuum pump and is difficult to for a long time the operation lengthy pressure of system be maintained 1500Pa (absolute pressure) in ferrous sulfate crystallization system, because this technique to external world variations in temperature is more responsive, when ambient air temperature is higher, because the water temperature of recirculated cooling water raises, cooling water declines to the steam cooling effect after injection, system vacuum is decreased, moisture evaporation in titanium liquid reduces, and causes production efficiency to produce fluctuation.
In order to overcome problem existing in existing ferrous sulfate vacuum crystallization technique, although existing titanium white production enterprise and research institution have carried out correlation technique research and development, but these development activities lay particular emphasis on the improvement of steam injection equipment as steam two-stage injection changed into three grades of injections more, or pay attention to improve recirculating cooling water system to the cooling effect spraying rear steam, or pay attention to the improvement to water ring vacuum pump water seal cooling system.And of the present invention by steam-condensation for the combination of liquid+vavuum pump produces the method for the condition of high vacuum degree required for ferrous sulfate crystallization and relevant complete set of equipments, and to the method for acid condensate water recycling so far there are no open report.
Summary of the invention:
Goal of the invention: deficiency existing in ferrous sulfate vacuum crystallization technique in producing for existing sulfuric acid method titanium pigment, the invention discloses the byproduct ferrous sulfate new method that vacuum crystallization is separated out from titanium liquid in a kind of Titanium White Production By Sulfuric Acid Process technique.Mentality of designing of the present invention is novel, Method And Principle science, and process route is simple, and scrap build is easy.
Technical scheme:
In Titanium White Production By Sulfuric Acid Process technique of the present invention, the byproduct ferrous sulfate new method that vacuum crystallization is separated out from titanium liquid is achieved through the following technical solutions:
1, utilize material from vapor state for volume during liquid acutely shrinks vacuum principle, the steam of evaporation side on titanium liquid in ferrous sulfate crystallization still is introduced condenser, and the chilled water through coming from refrigeration unit is condensed into liquid and obtains certain vacuum.
2, steam-condensation is adopted to be the condition of high vacuum degree that the mode of liquid+vavuum pump combination produces required for ferrous sulfate vacuum crystallization.
3, corrosion-resistant condensate liquid receiving slit is adopted to eliminate to the method that acid condensate liquid carries out recycling the acid waste water produced in ferrous sulfate crystallization process.
Beneficial effect:
In producing with existing sulfuric acid method titanium pigment compared with ferrous sulfate vacuum crystallization technique, present invention process route is reasonable, and equipment operating is simple.Adopt new method of the present invention can obtain four large beneficial effects, one is remove from using high temperature, high steam, significantly decreases the consumption of steam energy, reduces the production cost of titanium dioxide; Two be a cancellation in former technique because of steam spray take acid vapors out of after a large amount of acid waste waters of producing, alleviate the burden of environmental pressure and acid waste water process; Three is produce vacuum to be cryogenic condensation steam be that liquid produces vacuum because infantile feverish perspiration vapour sprays, eliminate the variation of ambient temperature that causes because of seasonal variations to the impact of former technique vacuum, the production efficiency of ferrous sulfate crystallization operation can be made to keep stable throughout the year; Four is that acid condensate liquid can all recycle in the acid dissolve operation to ilmenite powder by the inventive method, accomplishes twice laid, energy-saving and cost-reducing, realizes the cleaner production of sulfuric acid method titanium pigment.
Accompanying drawing explanation
Fig. 1 is existing sulfuric acid method titanium pigment ferrous sulfate vacuum crystallization process route view;
Fig. 2 is sulfuric acid method titanium pigment ferrous sulfate vacuum crystallization process route view of the present invention.
detailed description of the invention:
Embodiment 1: the pre-cooled system in complete set of equipments of the present invention is connected with the top steam (vapor) outlet of ferrous sulfate crystallization still according to Fig. 2, again condenser system is connected with pre-cooled system, vacuum equipment Roots vaccum pump is exported upper pipe by Fig. 2 mode with condenser condenses liquid in condenser system with water ring vacuum pump be connected, valve-off 1 and valve 3, form the ferrous sulfate vacuum crystallization integrated system equipment that steam-condensation of the present invention is liquid+mono-vavuum pump combination thus.
Open valve 4, by the titanium liquid 35M that sulfuric acid dissolution ilmenite powder generates
3squeeze into valve-off 4 after the ferrous sulfate crystallization still of suitable volume.When titanium liquid temp reaches 54 ~ 56 DEG C in crystallization kettle, start water ring vacuum pump and vacuumize, when the vacuum pressure in crystallization kettle is lower than 2000Pa, open pre-cooled system, carry out pre-cooled to the vapours coming from crystallization kettle; When in crystallization kettle, titanium liquid temp reaches 41 ~ 43 DEG C, open refrigeration system, the water vapour through condenser is condensed into aqueous water and falls into condensate liquid receiving slit; When titanium liquid temp reaches 25 ~ 27 DEG C in crystallization kettle, close the operation of pre-cooled system equipment; When titanium liquid temp reaches 15 ~ 17 DEG C in crystallization kettle, first close refrigeration system equipment, it is out of service after 10 minutes that water ring vacuum pump continues operation.Open valve 4 emptying on crystallization kettle, open valve 5 blowing, ferrous sulfate crystallization terminates, whole crystallization operation process about 2.5 hours.
Embodiment 2: the pre-cooled system in complete set of equipments of the present invention is connected with the top steam (vapor) outlet of ferrous sulfate crystallization still according to Fig. 2, again condenser system is connected with pre-cooled system, vacuum equipment Roots vaccum pump is exported upper pipe by Fig. 2 mode with condenser condenses liquid in condenser system with water ring vacuum pump be connected, valve-off 2, open valve 1 and valve 3, form the ferrous sulfate vacuum crystallization integrated system equipment that steam-condensation of the present invention is liquid+bis-vavuum pump combination thus.
Open valve 4, by the titanium liquid 35M that sulfuric acid dissolution ilmenite generates
3squeeze into valve-off 4 after the ferrous sulfate crystallization still of suitable volume, when titanium liquid temp reaches 56 ~ 58 DEG C in still, start Roots vaccum pump and water ring vacuum pump vacuumizes; When the vacuum pressure in crystallization kettle is lower than 1800Pa, open pre-cooled system, carry out pre-cooled to the vapours coming from crystallization kettle; When in crystallization kettle, titanium liquid temp reaches 39 ~ 41 DEG C, open refrigeration system, the water vapour through condenser is condensed into aqueous water and falls into condensate liquid receiving slit; When titanium liquid temp reaches 25 ~ 27 DEG C in crystallization kettle, close the operation of pre-cooled system equipment; When in crystallization kettle, titanium liquid temp reaches 15 ~ 17 DEG C, first close refrigeration system equipment, it is out of service after 10 minutes that Roots vaccum pump and water ring vacuum pump continue operation.Open valve 4 emptying on crystallization kettle, open valve 5 blowing, ferrous sulfate crystallization terminates, whole crystallization operation process about 2 hours.
By above-mentioned two embodiments, the present invention may be better understood, but, to one skilled in the art, content described by embodiment is only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet, in the technology of the present invention field, anyly exceed the present embodiment but the behavior fallen within the scope of the claims in the present invention all should be regarded as the claims in the present invention infringement.
Claims (7)
1. in a kind of sulfuric acid method titanium pigment production technology of the present invention by byproduct ferrous sulfate from titanium liquid vacuum crystallization separate out new method, it is characterized in that the method comprises two parts, one is the new technology producing condition of high vacuum degree in crystallization kettle and pipe-line system, two be acid water steam is cooled, the complete set of equipments of condensation.
2., according to claim 1, the described new technology producing condition of high vacuum degree in crystallization kettle and pipe-line system, is characterized in that have employed the technique that following water vapour is condensed into liquid+vavuum pump combination:
(1) steam adopting condensation at low temperature to make to stem from evaporation side on titanium liquid in crystallization kettle is condensed into liquid in the condenser of condenser system, when saturated steam is condensed into liquid state from steam state, its volume occupied acutely is contracted to more than 1200 of original volume doubly, produces higher vacuum thus;
(2) adopt one or two vavuum pump+steam-condensation combinations, the air intake of vavuum pump is connected with the outlet of condenser; When employing vavuum pump+steam-condensation combination, the preferred vavuum pump of the present invention is water ring pump; When employing two vavuum pumps+steam-condensation combination, the preferred vavuum pump of the present invention is that a lobe pump is contacted mutually with a water ring pump.
3. according to claim 2, described steam-condensation is the technique of liquid+vavuum pump combination, it is characterized in that this technique can make the limiting pressure in ferrous sulfate vacuum crystallization system be less than or equal to 350Pa (absolute pressure), when in crystallization kettle, titanium liquid temp is 15 DEG C, this technique can make the operating pressure in ferrous sulfate crystallization system maintain all the time lower than 1400Pa (absolute pressure) below.
4. according to claim 1, described acid water steam to be cooled, the complete set of equipments of condensation, it is characterized by this complete set of equipments and comprise a set of refrigeration unit, the pre-cooled system of a set of steam and a set of steam and condensate system.
5. according to claim 4, described a set of refrigeration unit, is characterized in that a set of refrigeration machine producing 4 ~ 6 DEG C of cryogenic freezing water, and this refrigeration machine can be ammonia machine, freon refrigerator and lithium bromide refrigerator, the preferred lithium-bromide absorption-type refrigerating machine of the present invention.
6. according to claim 4, described a set of pre-cooled system, it is characterized in that the tubular heat exchanger that this system is corroded by acid resistance and open type circulating cooling wetting system form, wherein acid water steam walks tube side, recirculated cooling water walks shell side, and the temperature of steam after this pre-cooled system reduces to 8 ~ 12 DEG C.
7. according to claim 4, described a set of steam and condensate system, it is characterized in that the vertical condensation liquid receiving slit of the horizontal shell and tube stram condenser that this condenser system is corroded by an acid resistance and an acid resistance corrosion forms, condensate liquid receiving slit is positioned at the below of stram condenser, and its import is connected with the outlet end socket of tubulation stram condenser; In horizontal shell and tube stram condenser, acid water steam walks tube side, and the water at low temperature coming from refrigeration machine walks shell side.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106390507A (en) * | 2016-11-23 | 2017-02-15 | 重庆鹏越科技发展有限公司 | Continuous vacuum crystallization system of titanium black liquor and application method of continuous vacuum crystallization system |
| CN107670321A (en) * | 2017-10-17 | 2018-02-09 | 南京圆点环境清洁技术有限公司 | A kind of processing system for being used for ferrous sulfate vacuum crystallization in titanium liquid |
| CN107935029A (en) * | 2017-11-23 | 2018-04-20 | 河北麦森钛白粉有限公司 | A kind of purification method of decorating base paper titanium white production raw material |
| CN108635902A (en) * | 2018-05-09 | 2018-10-12 | 杭州安永环保科技有限公司 | Titanium liquid ferrous iron crystal system and method |
| CN108992964A (en) * | 2018-07-20 | 2018-12-14 | 杭州安永环保科技有限公司 | A kind of vacuum crystallization system and method |
| CN109091905A (en) * | 2018-09-13 | 2018-12-28 | 四川龙蟒钛业股份有限公司 | Sulfuric acid method titanium pigment vacuum crystallization system and method |
| CN109650462A (en) * | 2019-01-07 | 2019-04-19 | 天津乐科节能科技有限公司 | A kind of system and method for titanium liquid pumping compression separation ferrous sulfate |
| CN109850954A (en) * | 2019-04-15 | 2019-06-07 | 卢星 | A kind of sulfate process titanium dioxide ferrous sulfate crystallization device |
| CN113044880A (en) * | 2021-03-23 | 2021-06-29 | 江苏勃仑化学有限公司 | Production process for increasing whiteness of titanium dioxide |
| WO2022094780A1 (en) * | 2020-11-04 | 2022-05-12 | 成都千砺金科技创新有限公司 | Method for crystallizing ferrous sulfate heptahydrate during sulfuric-acid-method-based titanium dioxide production process |
| CN115818727A (en) * | 2022-10-26 | 2023-03-21 | 浙江鑫隆达真空设备股份有限公司 | Freezing and crystallizing process and production system of ferrous sulfate in titanium dioxide production |
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| JP2002284509A (en) * | 2001-03-28 | 2002-10-03 | Osaka Gas Co Ltd | Treatment method of spent sulfuric acid and the treatment equipment |
| CN203816265U (en) * | 2014-03-27 | 2014-09-10 | 江阴市江中设备制造有限公司 | Inorganic salt continuous crystallization device |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106390507A (en) * | 2016-11-23 | 2017-02-15 | 重庆鹏越科技发展有限公司 | Continuous vacuum crystallization system of titanium black liquor and application method of continuous vacuum crystallization system |
| CN107670321A (en) * | 2017-10-17 | 2018-02-09 | 南京圆点环境清洁技术有限公司 | A kind of processing system for being used for ferrous sulfate vacuum crystallization in titanium liquid |
| CN107935029A (en) * | 2017-11-23 | 2018-04-20 | 河北麦森钛白粉有限公司 | A kind of purification method of decorating base paper titanium white production raw material |
| CN108635902A (en) * | 2018-05-09 | 2018-10-12 | 杭州安永环保科技有限公司 | Titanium liquid ferrous iron crystal system and method |
| CN108992964B (en) * | 2018-07-20 | 2020-12-29 | 杭州安永环保科技有限公司 | Vacuum crystallization system and method thereof |
| CN108992964A (en) * | 2018-07-20 | 2018-12-14 | 杭州安永环保科技有限公司 | A kind of vacuum crystallization system and method |
| CN109091905B (en) * | 2018-09-13 | 2021-02-23 | 龙佰四川钛业有限公司 | Sulfuric acid method titanium dioxide vacuum crystallization system and method |
| CN109091905A (en) * | 2018-09-13 | 2018-12-28 | 四川龙蟒钛业股份有限公司 | Sulfuric acid method titanium pigment vacuum crystallization system and method |
| CN109650462A (en) * | 2019-01-07 | 2019-04-19 | 天津乐科节能科技有限公司 | A kind of system and method for titanium liquid pumping compression separation ferrous sulfate |
| CN109850954A (en) * | 2019-04-15 | 2019-06-07 | 卢星 | A kind of sulfate process titanium dioxide ferrous sulfate crystallization device |
| CN109850954B (en) * | 2019-04-15 | 2023-11-24 | 卢星 | Sulfuric acid process titanium white ferrous sulfate crystallization device |
| WO2022094780A1 (en) * | 2020-11-04 | 2022-05-12 | 成都千砺金科技创新有限公司 | Method for crystallizing ferrous sulfate heptahydrate during sulfuric-acid-method-based titanium dioxide production process |
| CN113044880A (en) * | 2021-03-23 | 2021-06-29 | 江苏勃仑化学有限公司 | Production process for increasing whiteness of titanium dioxide |
| CN113044880B (en) * | 2021-03-23 | 2023-01-10 | 江苏勃仑化学有限公司 | Production process for increasing whiteness of titanium dioxide |
| CN115818727A (en) * | 2022-10-26 | 2023-03-21 | 浙江鑫隆达真空设备股份有限公司 | Freezing and crystallizing process and production system of ferrous sulfate in titanium dioxide production |
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