CN102764601A - Device and process for preparing titanium tetrachloride aqueous solution - Google Patents
Device and process for preparing titanium tetrachloride aqueous solution Download PDFInfo
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- CN102764601A CN102764601A CN201210283783XA CN201210283783A CN102764601A CN 102764601 A CN102764601 A CN 102764601A CN 201210283783X A CN201210283783X A CN 201210283783XA CN 201210283783 A CN201210283783 A CN 201210283783A CN 102764601 A CN102764601 A CN 102764601A
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- titanium tetrachloride
- aqueous solution
- acid fog
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Abstract
The invention relates to a process for preparing a titanium tetrachloride aqueous solution. The process is characterized by using an ejector vacuum pump for extracting titanium tetrachloride. The invention further relates to a device for preparing the titanium tetrachloride aqueous solution. The device is characterized by further comprising the ejector vacuum pump for extracting titanium tetrachloride. The ejector vacuum pump is connected in series between a number one anticorrosive centrifugal pump and a graphite heat exchanger. Compared with the prior art, the device and the method for preparing the titanium tetrachloride aqueous solution have the advantages of reducing risks and environment pollution of the titanium tetrachloride in the preparing process and energy consumption, such as ice cakes used for cooling.
Description
Technical field
The present invention relates to a kind of titanium tetrachloride aqueous solution preparing process; This technology is used to prepare titanium tetrachloride aqueous solution; The invention still further relates to a kind of titanium tetrachloride aqueous solution device for formulating; This device is used for the titanium tetrachloride water is diluted, and the titanium tetrachloride solution after the dilution is as the raw material of products such as titanium dioxide.
Background technology
Existing titanium tetrachloride process for preparation technology does, titanium tetrachloride pressurizes in to packing container with oxygen when preparation, from the barreled container, extrudes titanium tetrachloride through pressure, flows in the titanium liquid mixing channel, in titanium liquid mixing channel, carries out mixed diluting.Because of producing huge heat, hydrochloric acid and acid mist in the mixed process of titanium tetrachloride and water, control bad titanium tetrachloride and directly hydrolysis can occur and produce titanium white powder and cause titanium tetrachloride can not produce pearl essence.Generally in the process for preparation, need each preparation one barrel (closing 250KG) need lower the temperature, not allow titanium tetrachloride generation hydrolysis as far as possible and titanium white powder occurs toward adding ice cube in the titanium liquid mixing channel.
Because of titanium tetrachloride runs into air or water can produce huge heat, hydrochloric acid and acid mist; So above-mentioned defective workmanship is many; At first pressurization is difficult to control in the barreled titanium tetrachloride; Because of unicom pipeline easy blocking sometimes, internal pressure is too high spills titanium tetrachloride after causing rubber stopper to produce and produce the concentrated acid fog dust and influence environment for bucket, the operative employee is prone to produce injures.Be exactly to need to add ice cube in addition at every turn, can produce acid mist when in the mixed with titanium liquid bath, adding ice cube in the operation, human body is had damage.
Publication number is in the utility model specification of CN2923668Y; Disclose a kind of titanium tetrachloride and be diluted to covering device; Heat exchanger is not set in this device, makes titanium tetrachloride easily hydrolysis heat release in dilution, and produce titanium white powder; Not only waste raw material, also may cause security incident.
Though this titanium tetrachloride is diluted to covering device and is provided with the vacuum unit; But because titanium tetrachloride hydrolysis produces the cause of hydrogen chloride; Make the vacuum unit discharge toxic and harmful, and hydrogen chloride gas also can corrode the vacuum unit, increase substantially the maintenance cost of vacuum unit.
Summary of the invention
The objective of the invention is to overcome the above-mentioned deficiency that exists in the prior art, and provide a kind of processing step few, can realize the continuous drawing titanium tetrachloride; Extraction and mixing are carried out simultaneously; Good mixing effect, percent hydrolysis is low, the titanium tetrachloride aqueous solution preparing process of environmental protection.
The present invention addresses the above problem the technical scheme that is adopted: this titanium tetrachloride aqueous solution preparing process is characterized in that: use ejector vacuum pump to extract titanium tetrachloride.
Among the present invention, the titanium tetrachloride of water and extraction is mixed into titanium tetrachloride aqueous solution, mixes the back cooling.
The present invention also provides a kind of reasonable in design that realizes above-mentioned technology, energy savings, and the vacuum drawn titanium tetrachloride can effectively be protected environment, reduces the titanium tetrachloride hydrolysis rate significantly, realizes the titanium tetrachloride aqueous solution device for formulating of non-pollution discharge.
This titanium tetrachloride aqueous solution device for formulating comprises graphite heat exchanger, anticorrosion centrifugal pump, titanium tetrachloride mixing channel, No. two anticorrosion centrifugal pumps, a spray equipment and an acid fog absorption tower; A described anticorrosion centrifugal pump links to each other with the titanium tetrachloride mixing channel, and a described anticorrosion centrifugal pump is connected with graphite heat exchanger, and described graphite heat exchanger is connected with the titanium tetrachloride mixing channel; Described titanium tetrachloride mixing channel is connected with No. two anticorrosion centrifugal pumps; These No. two anticorrosion centrifugal pumps are connected with a spray equipment; A described spray equipment is installed in acid fog absorption tower; This acid fog absorption tower is connected with the titanium tetrachloride mixing channel, it is characterized in that: also comprise the ejector vacuum pump that is used to extract titanium tetrachloride, described ejector vacuum pump is connected between anticorrosion centrifugal pump and the graphite heat exchanger.
Through the graphite heat exchanger cooling, can guarantee temperature, reduce the titanium tetrachloride hydrolysis rate.Draw titanium tetrachloride through ejector vacuum pump, easy to operate, can stop pernicious gas and overflow; Ejector vacuum pump can effectively mix the liquid in titanium tetrachloride and the titanium tetrachloride mixing channel, and mixing efficiency is high.An acid fog absorption tower absorbing hydrogen chloride gas can effective inhibition titanium tetrachloride hydrolysis, but also can reduce the discharge rate of hydrogen chloride gas.The whole system sealing can prevent effectively that toxic and harmful is excessive, the protection environment.
The present invention also comprises clear water absorption cell, No. two acid fog absorption towers, No. three anticorrosion centrifugal pumps and No. two spray equipments; The inlet of described No. three anticorrosion centrifugal pumps links to each other with the clear water absorption cell; These No. three anticorrosion centrifugal delivery side of pump links to each other with No. two spray equipments; Described No. two spray equipments are installed in No. two acid fog absorption towers, and these No. two acid fog absorption towers link to each other with the clear water absorption cell, and the gaseous phase outlet of a said clear water absorption cell and an acid fog absorption tower is connected.
Can absorb most of hydrogen chloride gas through No. two acid fog absorption towers, by-product hydrochloric acid still is one of important raw material of industry, can realize twice laid, energy savings, protection environment.
The present invention also comprises alkali absorption cell, No. four anticorrosion centrifugal pumps, No. three acid fog absorption towers, No. three spray equipments and centrifugal blower; The inlet of described No. four anticorrosion centrifugal pumps is connected with the alkali absorption cell; These No. four anticorrosion centrifugal delivery side of pump is connected with No. three spray equipments; Described No. three spray equipments are installed in No. three acid fog absorption towers; These No. three acid fog absorption towers link to each other with the alkali absorption cell, and the gaseous phase outlet of described alkali absorption cell and No. two acid fog absorption towers links to each other, and the gaseous phase outlet of described No. three acid fog absorption towers links to each other with centrifugal blower.
Alkali lye is absorbing hydrogen chloride gas thoroughly, makes the gas of emptying nontoxic, and centrifugal blower can be drawn gas, improves vent gas treatment efficient.
The liquid pumping hole diameter of ejector vacuum pump according to the invention is 5-13mm.Make take out as the titanium tetrachloride flow can be controlled, prevent that flow is too big and sharply hydrolysis heat release causes temperature uncontrollable.
All be provided with filler in an acid fog absorption tower of the present invention, No. two acid fog absorption towers and No. three acid fog absorption towers.Increase absorption efficiency.
Ejector vacuum pump of the present invention comprises nozzle and liquid pumping hole, and this liquid pumping hole is made up of a straight tube and an inclined tube, and said inclined tube is connected with straight tube, and the axis of said inclined tube is parallel with the bus of nozzle.Improve mixed effect.
The liquid pumping hole diameter of ejector vacuum pump according to the invention is 8-10mm.Suction effect is good.Among the present invention, the liquid pumping hole diameter is that 9mm has optimum efficiency.
The present invention compared with prior art has the following advantages and effect: reduce the danger in the titanium tetrachloride process for preparation; Reduce the environmental pollution of titanium tetrachloride at process for preparation; Reduce the consumption of the energy, as the employed ice cube of lowering the temperature.
Description of drawings
Fig. 1 is the structural representation of titanium tetrachloride aqueous solution device for formulating in the embodiment of the invention.
Fig. 2 is the structural representation of ejector vacuum pump among the present invention.
Label declaration: graphite heat exchanger 1,2, numbers anticorrosion centrifugal pumps 3 of ejector vacuum pump, 4, No. two anticorrosion centrifugal pumps 5 of titanium tetrachloride mixing channel; 6, numbers acid fog absorption towers 7 of a spray equipment, 9, No. three anticorrosion centrifugal pumps 10 of 8, No. two acid fog absorption towers of clear water absorption cell; No. two spray equipments 11,14, No. three spray equipments 15 of alkali absorption cell 13, No. three acid fog absorption towers of 12, No. four anticorrosion centrifugal pumps; Centrifugal blower 16, filler 17, nozzle 18, straight tube 19, inclined tube 20.
The specific embodiment
Below in conjunction with accompanying drawing and through embodiment the present invention is done further detailed description, following examples are to explanation of the present invention and the present invention is not limited to following examples.
Embodiment 1.
Among the present invention, the titanium tetrachloride aqueous solution preparing process may further comprise the steps: use ejector vacuum pump 2 to extract titanium tetrachloride, the titanium tetrachloride and the water of extraction mix, and are mixed into titanium tetrachloride aqueous solution, mix the back cooling.
Referring to Fig. 1 and Fig. 2; Realize the titanium tetrachloride aqueous solution device for formulating of titanium tetrachloride aqueous solution preparing process among the embodiment 1, comprise graphite heat exchanger 1, ejector vacuum pump 2, anticorrosion centrifugal pump 3, titanium tetrachloride mixing channel 4, No. two anticorrosion centrifugal pumps 5, a spray equipment 6 and an acid fog absorption tower 7.
The inlet of an anticorrosion centrifugal pump 3 is connected with titanium tetrachloride mixing channel 4; Anticorrosion centrifugal pump 3 outlets are connected with the inlet of ejector vacuum pump 2; Ejector vacuum pump 2 outlets are connected with the inlet of graphite heat exchanger 1, and the outlet of graphite heat exchanger 1 is connected on the titanium tetrachloride mixing channel 4.
In the present embodiment, the heat exchange area of graphite heat exchanger 1 is 100 square metres.Can effectively remove heat, guarantee that the temperature of the mixed liquor in the titanium tetrachloride mixing channel 4 is unlikely to too high.
During the operation of titanium tetrachloride aqueous solution device for formulating, No. one anticorrosion centrifugal pump 3 is worked, and the liquid in the titanium tetrachloride mixing channel 4 is pumped into the inlet of ejector vacuum pump 2.In running, the liquid pumping hole of ejector vacuum pump 2 forms certain vacuum, titanium tetrachloride is sucked in the ejector vacuum pump 2, and with ejector vacuum pump 2 in liquid mixing.After the mixing, mixing material is admitted to heat exchange cooling in the graphite heat exchanger 1, uses the water quench mixing material usually.Mixing material after the cooling gets in the titanium tetrachloride mixing channel 4 from the outlet of graphite heat exchanger 1.
In this process; Ejector vacuum pump 2 constantly extract titanium tetrachlorides and with titanium tetrachloride mixing channel 4 in liquid mixing, then through graphite heat exchanger 1 cooling, keep fluid temperature in the titanium tetrachloride mixing channel 4 below 20 ℃; Reduce the percent hydrolysis of titanium tetrachloride, increase economic efficiency.
When the titanium tetrachloride content of liquid in the titanium tetrachloride mixing channel 4 arrives 320g/L, 2/3rds of the liquid in the titanium tetrachloride mixing channel 4 is pumped in the holding vessel, stay 1/3rd as mother liquor.In titanium tetrachloride mixing channel 4, replenish suitable quantity of water again, restart to suck titanium tetrachloride then and dilute.Stay mother liquor and can suppress titanium tetrachloride hydrolysis.
The liquid phase outlet and the titanium tetrachloride mixing channel 4 of an acid fog absorption tower 7 are connected, and the inlet of No. two anticorrosion centrifugal pumps 5 links to each other with titanium tetrachloride mixing channel 4, and the outlet of No. two anticorrosion centrifugal pumps 5 is connected with a spray equipment 6.Be provided with 17, numbers spray equipments 6 of filler in the acid fog absorption tower 7 and be installed in acid fog absorption tower 7, outlet of the liquid phase of an acid fog absorption tower 7 and 4 connections of titanium tetrachloride mixing channel.An acid fog absorption tower 7 is installed in the top of titanium tetrachloride mixing channel 4.
During the operation of titanium tetrachloride aqueous solution device for formulating, No. two anticorrosion centrifugal pump 5 operations with the liquid lifting of titanium tetrachloride mixing channel 4, and make this liquid spray from a spray equipment 6 downwards.Air-flow gets into from ejector vacuum pump 2, and in acid fog absorption tower 7 of titanium tetrachloride mixing channel 4 entering, spray the liquid countercurrent that comes out with a spray equipment 6 and contact, the liquid absorbing member hydrogen chloride gas, the liquid-absorbent hydrogen chloride gas helps suppressing hydrolysis.
In the present embodiment, the titanium tetrachloride aqueous solution device for formulating also comprises clear water absorption cell 8, No. two acid fog absorption towers 9, No. three anticorrosion centrifugal pumps 10 and No. two spray equipments 11.
The inlet of No. three anticorrosion centrifugal pumps 10 links to each other with clear water absorption cell 8, and the outlet of No. three anticorrosion centrifugal pumps 10 links to each other with No. two spray equipments 11.No. two spray equipments 11 are installed in No. two acid fog absorption towers 9; No. two acid fog absorption tower 9 links to each other with clear water absorption cell 8, and the liquid phase outlet and the clear water absorption cell 8 of No. two acid fog absorption towers 9 are communicated with, and No. two acid fog absorption tower 9 is fixed on the clear water absorption cell 8; Clear water absorption cell 8 is connected with the gaseous phase outlet of an acid fog absorption tower 7.Be provided with filler 17 in No. two acid fog absorption towers 9.
Before the operation of titanium tetrachloride aqueous solution device for formulating, in clear water absorption cell 8, inject a certain amount of clear water earlier.
During the operation of titanium tetrachloride aqueous solution device for formulating, No. three anticorrosion centrifugal pump 10 actions suck 10, No. three anticorrosion centrifugal pumps 10 of No. three anticorrosion centrifugal pumps with liquid in the clear water absorption cell 8 this liquid are pumped into spray equipment 11 No. two.The gas that comes out from the gaseous phase outlet of an acid fog absorption tower 7 gets into No. two acid fog absorption towers 9 through clear water absorption cell 8; The liquid of No. two spray equipment 11 ejections contacts with the back flow of gas that gets into from No. two acid fog absorption tower 9 liquid phases outlets, makes that wherein the hydrogen chloride composition is partially absorbed.Wherein, increase filler 17 and can increase gas phase and liquid phase contact area, improve absorption rate.
In the present embodiment, the titanium tetrachloride aqueous solution device for formulating also comprises the anticorrosion centrifugal pump of alkali absorption cell 12, No. four 13, No. three acid fog absorption towers 14, No. three spray equipments 15 and centrifugal blowers 16.
The inlet of No. four anticorrosion centrifugal pumps 13 is connected with alkali absorption cell 12; The outlet of No. four anticorrosion centrifugal pumps 13 is connected with No. three spray equipments 15; No. three spray equipments 15 are installed in No. three acid fog absorption towers 14; No. three acid fog absorption tower 14 links to each other with alkali absorption cell 12, and alkali absorption cell 12 links to each other with the gaseous phase outlet of No. two acid fog absorption towers 9.
The gaseous phase outlet of No. three acid fog absorption towers 14 links to each other with centrifugal blower 16.
Be provided with filler 17 in No. three acid fog absorption towers 14.Increase filler 17 and can increase gas phase and liquid phase contact area, improve absorption rate.
Before the operation of titanium tetrachloride aqueous solution device for formulating, in alkali absorption cell 12, inject a certain amount of alkali lye.
During the operation of titanium tetrachloride aqueous solution device for formulating, No. four anticorrosion centrifugal pump 13 work promote the alkali lye in the alkali absorption cell 12, and make alkali lye from No. three spray equipment 15 interior ejections.The back flow of gas that the alkali lye of ejection and the gaseous phase outlet of No. two acid fog absorption towers 9 come out contacts, and alkali lye absorbs hydrogen chloride in gas, and remaining gas is drawn and emptying by centrifugal blower 16, and the gas of emptying is nontoxic, compliance with environmental protection requirements.
Among the present invention, gaseous phase outlet is positioned at the upper end of acid fog absorption tower, and the liquid phase outlet is positioned at the lower end of acid fog absorption tower.
Above content described in this specification only is illustrating that the present invention is done.Person of ordinary skill in the field of the present invention can make various modifications or replenishes or adopt similar mode to substitute described specific embodiment; Only otherwise depart from the content of specification of the present invention or surmount the defined scope of these claims, all should belong to protection scope of the present invention.
Claims (9)
1. a titanium tetrachloride aqueous solution preparing process is characterized in that: use ejector vacuum pump to extract titanium tetrachloride.
2. titanium tetrachloride aqueous solution preparing process according to claim 1 is characterized in that: the titanium tetrachloride of water and extraction is mixed into titanium tetrachloride aqueous solution, mixes the back cooling.
3. realize the titanium tetrachloride aqueous solution device for formulating of the described titanium tetrachloride aqueous solution preparing process of claim 1, it is characterized in that: comprise graphite heat exchanger, anticorrosion centrifugal pump, titanium tetrachloride mixing channel, No. two anticorrosion centrifugal pumps, a spray equipment and an acid fog absorption tower; A described anticorrosion centrifugal pump links to each other with the titanium tetrachloride mixing channel, and a described anticorrosion centrifugal pump is connected with graphite heat exchanger, and described graphite heat exchanger is connected with the titanium tetrachloride mixing channel; Described titanium tetrachloride mixing channel is connected with No. two anticorrosion centrifugal pumps; These No. two anticorrosion centrifugal pumps are connected with a spray equipment; A described spray equipment is installed in acid fog absorption tower; This acid fog absorption tower is connected with the titanium tetrachloride mixing channel, it is characterized in that: also comprise the ejector vacuum pump that is used to extract titanium tetrachloride, described ejector vacuum pump is connected between anticorrosion centrifugal pump and the graphite heat exchanger.
4. titanium tetrachloride aqueous solution device for formulating according to claim 3; It is characterized in that: also comprise clear water absorption cell, No. two acid fog absorption towers, No. three anticorrosion centrifugal pumps and No. two spray equipments; The inlet of described No. three anticorrosion centrifugal pumps links to each other with the clear water absorption cell; These No. three anticorrosion centrifugal delivery side of pump links to each other with No. two spray equipments; Described No. two spray equipments are installed in No. two acid fog absorption towers, and these No. two acid fog absorption towers link to each other with the clear water absorption cell, and the gaseous phase outlet of a said clear water absorption cell and an acid fog absorption tower is connected.
5. titanium tetrachloride aqueous solution device for formulating according to claim 4; It is characterized in that: also comprise alkali absorption cell, No. four anticorrosion centrifugal pumps, No. three acid fog absorption towers, No. three spray equipments and centrifugal blower; The inlet of described No. four anticorrosion centrifugal pumps is connected with the alkali absorption cell; These No. four anticorrosion centrifugal delivery side of pump is connected with No. three spray equipments, and described No. three spray equipments are installed in No. three acid fog absorption towers, and these No. three acid fog absorption towers link to each other with the alkali absorption cell; The gaseous phase outlet of described alkali absorption cell and No. two acid fog absorption towers links to each other, and the gaseous phase outlet of described No. three acid fog absorption towers links to each other with centrifugal blower.
6. according to claim 3,4 or 5 described titanium tetrachloride aqueous solution device for formulating, it is characterized in that: the liquid pumping hole diameter of said ejector vacuum pump is 5-13mm.
7. titanium tetrachloride aqueous solution device for formulating according to claim 5 is characterized in that: all be provided with filler in a described acid fog absorption tower, No. two acid fog absorption towers and No. three acid fog absorption towers.
8. according to claim 3,4 or 5 described titanium tetrachloride aqueous solution device for formulating; It is characterized in that: described ejector vacuum pump comprises nozzle and liquid pumping hole; This liquid pumping hole is made up of a straight tube and an inclined tube, and said inclined tube is connected with straight tube, and the axis of said inclined tube is parallel with the bus of nozzle.
9. titanium tetrachloride aqueous solution device for formulating according to claim 6 is characterized in that: the liquid pumping hole diameter of said ejector vacuum pump is 8-10mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210283783XA CN102764601A (en) | 2012-08-10 | 2012-08-10 | Device and process for preparing titanium tetrachloride aqueous solution |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210283783XA CN102764601A (en) | 2012-08-10 | 2012-08-10 | Device and process for preparing titanium tetrachloride aqueous solution |
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| CN102764601A true CN102764601A (en) | 2012-11-07 |
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| CN201210283783XA Pending CN102764601A (en) | 2012-08-10 | 2012-08-10 | Device and process for preparing titanium tetrachloride aqueous solution |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104459019A (en) * | 2014-12-12 | 2015-03-25 | 国家纳米科学中心 | Method for detecting content of free hydrochloric acid content in titanium tetrachloride water solution |
| CN108854617A (en) * | 2018-06-06 | 2018-11-23 | 杭州弗沃德精细化工有限公司 | A kind of titanium tetrachloride aqueous solution device for formulating and method |
| CN112250117A (en) * | 2020-10-16 | 2021-01-22 | 河南佰利联新材料有限公司 | Method for improving quality of waste and side-product titanium oxychloride |
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| CN2923668Y (en) * | 2006-03-31 | 2007-07-18 | 建德市大洋化工有限公司 | Complete apparatus for diluting titanic chloride |
| CN201940202U (en) * | 2011-01-19 | 2011-08-24 | 南京清海环保设备有限公司 | Device for preparing ammonia water with liquid ammonia |
| CN202741021U (en) * | 2012-08-10 | 2013-02-20 | 杭州弗沃德精细化工有限公司 | Preparing device for aqueous solution of titanium tetrachloride |
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2012
- 2012-08-10 CN CN201210283783XA patent/CN102764601A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2923668Y (en) * | 2006-03-31 | 2007-07-18 | 建德市大洋化工有限公司 | Complete apparatus for diluting titanic chloride |
| CN201940202U (en) * | 2011-01-19 | 2011-08-24 | 南京清海环保设备有限公司 | Device for preparing ammonia water with liquid ammonia |
| CN202741021U (en) * | 2012-08-10 | 2013-02-20 | 杭州弗沃德精细化工有限公司 | Preparing device for aqueous solution of titanium tetrachloride |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104459019A (en) * | 2014-12-12 | 2015-03-25 | 国家纳米科学中心 | Method for detecting content of free hydrochloric acid content in titanium tetrachloride water solution |
| CN104459019B (en) * | 2014-12-12 | 2016-05-11 | 国家纳米科学中心 | A kind of method that detects free content of hydrochloric acid in titanium tetrachloride aqueous solution |
| CN108854617A (en) * | 2018-06-06 | 2018-11-23 | 杭州弗沃德精细化工有限公司 | A kind of titanium tetrachloride aqueous solution device for formulating and method |
| CN112250117A (en) * | 2020-10-16 | 2021-01-22 | 河南佰利联新材料有限公司 | Method for improving quality of waste and side-product titanium oxychloride |
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Application publication date: 20121107 |