CN101654274A - Barium chloride production technology - Google Patents
Barium chloride production technology Download PDFInfo
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- CN101654274A CN101654274A CN200910307050A CN200910307050A CN101654274A CN 101654274 A CN101654274 A CN 101654274A CN 200910307050 A CN200910307050 A CN 200910307050A CN 200910307050 A CN200910307050 A CN 200910307050A CN 101654274 A CN101654274 A CN 101654274A
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- barium chloride
- crystallization kettle
- barium
- vacuum
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Abstract
The invention discloses a technology for producing barium chloride by the witherite containing barium carbonate, which mainly comprises steps as follows: sulfur iron impurities are decomposed and oxidated to remove and the hydrated barium salt raw material liquid is prepared; the raw material liquid is electrically heated and concentrated in vacuum, which is driven by an axial flow pump, the solute is thermally crystallized to form the hydrated barium chloride dihydrate saturated crystalline; the crystallized hydrate is cooled to produce the serial barium salt products, wherein the vacuum heating condensation crystallization is a continuous production process; the whole technological process is implemented in the closed state; the by-products could be recycled; the crystallisation processis completed at one time and the production process is continuous. The products manufactured in the technological process has low impurity content, saves energy, is adaptive to the large-scale industrialization production and reduces the pollution and resource waste to a large extent.
Description
Technical field
The present invention relates to chemical field, relate in particular to a kind of production technique of producing bariumchloride by barium carbonate.
Background technology
The method of producing bariumchloride at present is a lot, mainly is to be raw material with the barite, after fusing with barite and coal dust reduction, make bariumchloride with hydrochloric acid reaction again, be to be raw material with the barite in addition, reduce with coal dust and calcium water fuse, through the leaching, make bariumchloride after the processing such as desulfurization.The method of above-mentioned production bariumchloride, not only energy consumption is big, labour intensity is big, and the processing of the three wastes is not easy very much, pollutes to environment.
Another kind method is to be the raw material production bariumchloride with the witherite.The main component of witherite is a barium carbonate, and witherite and hydrochloric acid reaction are generated bariumchloride, need through repeatedly more than 4 times spontaneous nucleation make bariumchloride.The shortcoming of this method is:
1, impurity is difficult to eliminate fully.Because its production process is wide-open, impurity enters easily and carries secretly, and recrystallization also is difficult to eliminate fully repeatedly.
2, power consumption is high.Because its production process is to need 4 crystallizations, its 4 crystallization process of cooling are to carry out under state of nature, cause energy loss.
3, can not continuous production, the incompatibility large-scale industrial needs.
4, pollute waste seriously.Steam, carbonic acid gas discharge fully and can't reclaim in this method production process, pollute the waste with resource.
Summary of the invention
The production technique that the purpose of this invention is to provide a kind of bariumchloride, it has overcome above-mentioned shortcoming.The present invention realizes by following method.
1, decomposing oxidation sulphur removal iron contamination, preparation hydration barium salt stock liquid.
Contain barium carbonate 65% weight percent meter by witherite, with witherite: hydrochloric acid: water: hydrogen peroxide was in 1: 0.37: 1: 0.1 ratio is at the uniform velocity imported in the reactor, and chemical reaction takes place:
BaCO
3+2HCl+nH
2O→BaCl
2·nH
2O+CO
2↑......(1)
Free sulphur (S), iron (Fe) are with hydrogen peroxide generation oxidizing reaction and generation precipitation;
HS+4H
2O
2+OH→5H
2O+SO
4 2
SO
4 2-+Ba
2+→BaSO
4↓
2Fe
2++3H
2O
2→2Fe(OH)
3↓
Fo
3++3OH
-→Fe(OH)
3↓
Question response does not remove filter residue after having carbonic acid gas release, and filtrate is hydration bariumchloride stock liquid.
Wherein the concentration expressed in percentage by weight of hydrochloric acid is 30～32%, and the concentration expressed in percentage by weight of hydrogen peroxide is 〉=29%.
The carbonic acid gas that this step (1) discharges is used to produce barium carbonate, filter residue making cement additive through reclaiming purifying.
2, the electrically heated of stock liquid vacuum concentrates, and the solute thermal crystalline forms hydration barium chloride saturated crystallization body.
Crystallization kettle is provided with the electrically heated temperature regulating device, and crystallization kettle and vacuum condensation retrieving arrangement are by pipe connection, and the crystallization kettle internal upper part is provided with propeller pump, and the crystallization kettle bottom is the centrum shape, and the centrum top connects the crystallization kettle bottom valve.
Hydration bariumchloride stock liquid continues send into crystallization kettle by feedstock pump by pipeline through adjusting PH=4～6.When stock liquid enters crystallization kettle, the heating temperature control is at 100 ℃～113 ℃, preferred 103 ℃, continue vacuum 10～30Kpa suction filtration, along with moisture evaporation, concentration of raw material progressively increases, its time-continuing process solute is by nucleus one brilliant clock (adding crystal seed for the first time brings out) thermal crystalline, when concentration is thickened to that 32 Baumes are critical spends, barium chloride crystal in the supersaturated solution because of gravity settling in crystallization kettle bottom, continue initiate stock liquid under propeller pump drives and in the crystallization kettle solution mix to be incorporated in and form the still center in the crystallization kettle and upwards flow, arrive the still top again along downward the circulating of still wall, the adding speed of control stock liquid makes the crystallization output reach balance, and the bariumchloride crystalline hydrate continues to discharge along with crystalline produces through the crystallization kettle bottom valve.
This step evaporation condensed water reclaims for preparation hydration barium salt stock liquid and uses.
3, serial barium salt product is produced in crystalline hydrate cooling.
Saturated barium chloride crystalline hydrate enters cooling pool, filters, and its a small amount of filtrate is returned evaporative crystallization, and the white crystal solid substance is barium chloride, and further the processing dehydration can be produced a water bariumchloride, anhydrous barium chloride and other barium products.
All commercially available chemical industry equipments such as aforesaid reaction vessel, feedstock pump, pipeline, crystallization kettle, electrically heated temperature regulating device, vacuum condensation retrieving arrangement, propeller pump.Wherein propeller pump is vertically mounted on the middle part of crystallization kettle, pump impeller should be greater than high by 1/3rd in the whole crystallization kettle apart from crystallization kettle bottom, reactive force to stock liquid during pump impeller work should make progress, riser pipe is installed around pump shaft and pump impeller, the riser pipe upper and lower opening, be fixed on the crystallization kettle top cover, pump impeller is in the riser pipe lower opening, riser pipe makes up and down, and flowing fluid separates, because pump impeller has certain distance apart from the crystallization kettle bottom, the crystalline particle that grows up to is no longer stirred by pump impeller because of gravity sinks to greatly in the crystallization kettle centrum, and nucleus and mother liquor continue circulation by propeller pump; The electrically heated temperature regulating device is installed in the crystallization kettle inner height and locates more than 1/2nd, be looped around the crystallization kettle periphery of inner wall, electrically heated is common quartz heater, temperature regulating device is the usual procedure temperature regulating device, it has overcome the heating jacket type of heating makes whole crystallization kettle temperature identical, makes crystallization kettle upper and lower temperature different and help evaporation and crystallization; The vacuum condensation retrieving arrangement can be compositions such as formations such as vacuum pump, condenser, preferably water odd test jet vacuum pump and condenser, and water odd test jet vacuum pump is simple in structure, and water of condensation and the merging of evaporation reuse water are re-used.
Compared with prior art, the beneficial effect that the present invention has is: this technological process is produced in enclosed environment, and by product all obtains recycling, and crystallisation process is once finished, and reduces evaporation concentration equipment quantity, and production process is continuous.Therefore, low, the save energy of the product foreign matter content produced of this technological process, adaptation large-scale industrial production needs, reduced the waste of pollution and resource to greatest extent.
Description of drawings
Fig. 1 is apparatus of the present invention structural representations.
Embodiment
Embodiment 1: contain barium carbonate 65% weight percent meter by witherite, with witherite: hydrochloric acid: water: hydrogen peroxide was by 1: 0.37: 1: 0.1 mixed thing 1 is at the uniform velocity imported in the reactor 2, chemical reaction takes place, wherein the concentration expressed in percentage by weight of hydrochloric acid is 30～32%, the concentration expressed in percentage by weight of hydrogen peroxide is 〉=29%, free sulphur (S), iron (Fe) is with hydrogen peroxide generation oxidizing reaction and generate precipitation, after question response does not have carbonic acid gas release, centrifugal 4 remove filter residue, filtrate is hydration bariumchloride stock liquid, the carbonic acid gas that discharges is used to produce barium carbonate, filter residue making cement additive through exporting 3 recovery purifying; Stock liquid is through feedstock pump 5 input crystallization kettles 21, electrically heated temperature regulating device 13 heating temperature controls make crystallization kettle 21 interior temperature remain on 100 ℃～113 ℃, preferred 103 ℃, vacuum condensation retrieving arrangement 10 pump up water steam and condensation reuse, vacuum keeps 10～30Kpa, stock liquid is at propeller pump 6,7,8 drive down in crystallization kettle 21 forms the still centers and upwards flows, arrive the still top again along downward the circulating of still wall, concentration of raw material progressively increases, its time-continuing process solute is by nucleus one brilliant clock (adding crystal seed for the first time brings out) thermal crystalline, when concentration is thickened to that 32 Baumes are critical spends, barium chloride crystal in the supersaturated solution because of gravity settling in crystallization kettle bottom 22, crystallization kettle bottom 22 is the centrum shape, and the centrum top connects crystallization kettle bottom valve 14, and the bariumchloride crystalline hydrate continues to discharge along with crystalline produces through crystallization kettle bottom valve 14; Stock liquid continue to mend goes into and mixes with stock liquid in the crystallization kettle under propeller pump 6,7,8 drives production is carried out continuously, and the adding speed of controlling stock liquid makes crystallization reach balance; Saturated barium chloride liquid and crystal grain enter cooling pool 15, filter, and its a small amount of filtrate is returned evaporative crystallization, and the white crystal solid substance is barium chloride, and further the processing dehydration can be produced a water bariumchloride, anhydrous barium chloride and other barium products.
Barium chloride microscopy branch crystallographic system detects BaCl
22H
2O molecular weight=244.10, content 〉=99.56%, density 3.10, in 100ml water, solubleness 35.5 grams (20 ℃), 58.45 grams (100 ℃).
The transformation temperature barium chloride generates a water bariumchloride, anhydrous barium chloride series barium salt product
BaCl
22H
2O → BaCl
2113 ℃ of Heating temperatures
BaCl
22H
2O → BaCl
2H
2113 ℃＞Heating temperature of O 〉=105 ℃
The colourless tabular monocline strain of anhydrous barium chloride, BaCl
2Molecular weight=218.14, relative density 3.887,961.5 ℃ of fusing points, 1560 ℃ of boiling points.
Above-mentioned crystallization kettle centrum bottom 22 helps crystalline gravity settling, collection, discharge; Electrically heated temperature regulating device 13 is installed in the crystallization kettle inner height and locates more than 1/2nd, be looped around the crystallization kettle periphery of inner wall, the interior solution of stock liquid that new benefit is gone into and crystallization kettle mixes and obtains heating, the mixing solutions of heating flows downward and helps crystalline and separate out sedimentation, and electrically heated temperature regulating device 13 makes crystallization kettle upper and lower temperature different and help evaporation and crystallization; Propeller pump 6,7,8 makes the mixed interior still center that forms of crystallization kettle that is incorporated in of the interior solution of crystallization kettle make progress mobile in the middle part of being vertically mounted on crystallization kettle, arrive the still top again along downward the circulating of still wall, it makes, and solution has afterflow moving in the crystallization kettle, crystal is separated out the sedimentation continous-stable, because pump impeller 6 has certain distance apart from the crystallization kettle bottom, the crystalline particle that grows up to is no longer stirred by pump impeller because of gravity sinks to greatly in the crystallization kettle centrum, and nucleus and mother liquor continue circulation by propeller pump.
In crystallization kettle 21, around propeller pump pump shaft 8 and the pump impeller 6 riser pipe 7 is installed also, riser pipe 7 upper and lower openings 9,11, riser pipe 7 is fixed on crystallization kettle 21 top covers, pump impeller 6 is in riser pipe 7 lower openings 11, riser pipe 7 upwards flows stock liquid from riser pipe 7 under the effect of pump impeller 6, arrive crystallization kettle 21 tops and flow downward along crystallization kettle 21 walls from the outside of riser pipe 7 again, raw material liq separately flows up and down and makes heating efficiency improve crystallization-stable.
Extract steam out in conjunction with vacuum condensation withdrawer 10, whole process realizes once heating up, consecutive evaporation, concentrated, and continuous crystallisation goes out product.
To produce 1.5 ten thousand tons of bariumchlorides per year is example: 1.4～1.8 meters of crystallization kettle diameters, preferred 1.4 meters; High 5～6 meters, preferred 5 meters; The centrum height is 1/2nd of a crystallization kettle diameter; In the normal productive process, the stock liquid input speed is per hour 11 cubic metres, 600～700 kilowatts of electrical heating powers, 500-550 rev/min of control axial flow revolution speed, then can reach in 0.5 ℃ of heating part, crystallization kettle top and the bottom subsidence part temperature head, this helps crystal grain grows up and sedimentation, and is no longer stirred by the propeller pump pump impeller, the continuation circulation of nucleus and mother liquor; This moment, 8 cubic metres/hour of the water yields were reclaimed in the whole process of production evaporation, discharged 3 cubic metres/hour in mother liquor, barium chloride 2000kg/ hour, realized continuous production.
Embodiment 3: repeat embodiment 1 by described same steps as, but witherite contains barium carbonate with 50% weight percent meter, with witherite: hydrochloric acid: water: hydrogen peroxide is by 1.3: 0.37: 1: 0.1 mixed 1 is at the uniform velocity imported in the reactor 2, the generation chemical reaction.The products obtained therefrom bariumchloride is identical with embodiment 1.
Embodiment 4: repeat embodiment 1 by described same steps as, but witherite contains barium carbonate with 70% weight percent meter, with witherite: hydrochloric acid: water: hydrogen peroxide is by 0.93: 0.37: 1: 0.1 mixed 1 is at the uniform velocity imported in the reactor 2, the generation chemical reaction.The products obtained therefrom bariumchloride is identical with embodiment 1.
Claims (6)
1, a kind of barium chloride production technology is characterized in that comprising the following steps:
1) raw material that will contain barium carbonate mixes with hydrochloric acid, water, hydrogen peroxide, reacts in the input reactor, and decomposing oxidation sulphur removal iron contamination reclaims the carbonic acid gas that produces, and removes filter residue after reaction is finished;
2) with 1) stock liquid that obtains adjusts PH=4～6, heating under vacuum condensing crystal in the continuous crystallisation still, the barium chloride crystallization is discharged;
3) with 2) obtain the crystalline hydrate cooling, send follow-up deep processing operation.
2. barium chloride production technology according to claim 1, it is characterized in that described Concentrated and crystallized in vacuum is to continue to add stock liquid in crystallization kettle, electrically heated, propeller pump drives stock liquid center in crystallization kettle and makes progress, circulates downwards along the crystallization kettle wall, vacuum is extracted water vapor and condensation reuse out, barium chloride crystal in the supersaturated solution because of gravity settling in crystallization kettle bottom, continue to be interrupted through the crystallization kettle bottom and discharge.
3. barium chloride production technology according to claim 2, it is characterized in that it is to be 100% barium carbonate in conversion that the described raw material that will contain barium carbonate mixes with hydrochloric acid, water, hydrogen peroxide, weight ratio is a barium carbonate: hydrochloric acid: water: hydrogen peroxide is 0.65: 0.37: 1: 0.1, wherein the concentration expressed in percentage by weight of hydrochloric acid is 30～32%, and the concentration expressed in percentage by weight of hydrogen peroxide is 〉=29%.
4. barium chloride production technology according to claim 3 is characterized in that the temperature when described heating under vacuum concentrates is 100 ℃～113 ℃, preferred 103 ℃.
5. barium chloride production technology according to claim 3, the vacuum tightness when it is characterized in that described vacuum concentration is 10～30Kpa.
6. according to each described barium chloride production technology of claim 1 to 5, it is characterized in that Concentrated and crystallized in vacuum carries out continuously.
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| CN102583488A (en) * | 2012-03-30 | 2012-07-18 | 贵州红星发展股份有限公司 | Method for producing low-strontium high-purity barium chloride and low-strontium high-purity barium chloride |
| CN102616823A (en) * | 2012-03-30 | 2012-08-01 | 贵州红星发展股份有限公司 | Titanium plant tail gas treatment method as well as barium chloride produced by using titanium plant tail gas treatment method and production method of barium chloride |
| CN102745732A (en) * | 2011-04-22 | 2012-10-24 | 山东众诚钡盐股份有限公司 | Barium chloride reactor |
| CN102961881A (en) * | 2012-11-16 | 2013-03-13 | 福州东星生物技术有限公司 | Heater structure in vacuum concentrator set |
| CN105967216A (en) * | 2016-07-01 | 2016-09-28 | 丁淑暖 | Production method of barium chloride |
| CN106145174A (en) * | 2016-07-04 | 2016-11-23 | 深州嘉信化工有限责任公司 | A kind of barium sulfate barium slag produces the method for industrial chlorinating titanate |
| CN106186025A (en) * | 2016-07-01 | 2016-12-07 | 丁淑暖 | Method for producing barium chloride |
| CN109336158A (en) * | 2018-12-11 | 2019-02-15 | 宜昌华昊新材料科技有限公司 | The method that high calcium witherite mineral produces barium chloride |
| CN110451548A (en) * | 2019-09-23 | 2019-11-15 | 山西北化关铝化工有限公司 | Spherical narrow granularity barium nitrate of one kind and preparation method thereof |
| CN112624172A (en) * | 2020-12-30 | 2021-04-09 | 宜昌华昊新材料科技有限公司 | Production process of barium carbonate |
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| CN101190797A (en) * | 2006-11-29 | 2008-06-04 | 天津渤天化工有限责任公司 | Method for producing barium chloride |
| CN101302028B (en) * | 2008-06-11 | 2010-10-27 | 黄其兵 | Method for producing barium chloride by heterogeneous co-heating method |
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| CN102745732A (en) * | 2011-04-22 | 2012-10-24 | 山东众诚钡盐股份有限公司 | Barium chloride reactor |
| CN102745732B (en) * | 2011-04-22 | 2015-07-15 | 山东众诚钡盐股份有限公司 | Barium chloride reactor |
| CN102583488A (en) * | 2012-03-30 | 2012-07-18 | 贵州红星发展股份有限公司 | Method for producing low-strontium high-purity barium chloride and low-strontium high-purity barium chloride |
| CN102616823A (en) * | 2012-03-30 | 2012-08-01 | 贵州红星发展股份有限公司 | Titanium plant tail gas treatment method as well as barium chloride produced by using titanium plant tail gas treatment method and production method of barium chloride |
| CN102961881A (en) * | 2012-11-16 | 2013-03-13 | 福州东星生物技术有限公司 | Heater structure in vacuum concentrator set |
| CN105967216A (en) * | 2016-07-01 | 2016-09-28 | 丁淑暖 | Production method of barium chloride |
| CN106186025A (en) * | 2016-07-01 | 2016-12-07 | 丁淑暖 | Method for producing barium chloride |
| CN106186025B (en) * | 2016-07-01 | 2018-02-09 | 嵊州明智科技服务有限公司 | Utilize the method for barium sulfate barium slag production barium chloride |
| CN106145174A (en) * | 2016-07-04 | 2016-11-23 | 深州嘉信化工有限责任公司 | A kind of barium sulfate barium slag produces the method for industrial chlorinating titanate |
| CN109336158A (en) * | 2018-12-11 | 2019-02-15 | 宜昌华昊新材料科技有限公司 | The method that high calcium witherite mineral produces barium chloride |
| CN110451548A (en) * | 2019-09-23 | 2019-11-15 | 山西北化关铝化工有限公司 | Spherical narrow granularity barium nitrate of one kind and preparation method thereof |
| CN112624172A (en) * | 2020-12-30 | 2021-04-09 | 宜昌华昊新材料科技有限公司 | Production process of barium carbonate |
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| CN101654274B (en) | 2011-01-26 |
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Effective date of registration: 20180412 Address after: 401121 Yubei District, Chongqing, Longxi street, Hong Jin Avenue 500, sun rising Phoenix 13 2-1-1 Patentee after: Chongqing Yangming chemical products Co.,Ltd. Address before: 610300 19 12 Qinghua East Road, Qingbaijiang District, Chengdu, Sichuan, China 108 Patentee before: Lai Chengwen |
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