CN101837998A - Method for evaporating, concentrating and crystallizing solution of aluminum chloride - Google Patents

Method for evaporating, concentrating and crystallizing solution of aluminum chloride Download PDF

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Publication number
CN101837998A
CN101837998A CN 201010161829 CN201010161829A CN101837998A CN 101837998 A CN101837998 A CN 101837998A CN 201010161829 CN201010161829 CN 201010161829 CN 201010161829 A CN201010161829 A CN 201010161829A CN 101837998 A CN101837998 A CN 101837998A
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evaporating
aluminum chloride
filter
concentrating
crystallization
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CN101837998B (en
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郭昭华
刘希全
周正明
陈德
王永旺
张文广
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China Shenhua Energy Co Ltd
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China Shenhua Energy Co Ltd
Shenhua Zhungeer Energy Co Ltd
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Abstract

The invention relates to a method for evaporating, concentrating and crystallizing the solution of aluminum chloride. The method comprises the following steps of: a, performing circulating evaporation: performing circulating evaporation concentration on the solution of aluminum chloride stage by stage by using a multi-effect forced circulation evaporator; b, performing settlement separation: in at least a part of a separation room of the forced circulation evaporator, performing settlement separation on solid crystals of aluminum chloride hexahydrate (AlCl3.6H2O); c, performing flash evaporation crystallization: sending the solution containing solid crystals of aluminum chloride obtained by the settlement separation step to a flash evaporation crystallization tank and performing vacuum flash evaporation on the solution under the condition that the temperature is between 60 and 75 DEG C and the vacuum degree is 0.095 to 0.08MPa; and d, performing crystallization filtration: conveying the discharged materials obtained by the flash evaporation crystallization step to a filter for filtrating. In the method, the aluminum chloride in the solution is completely crystallized into the crystals of aluminum chloride hexahydrate in a concentration process by adopting the mode of combining the three-effect complete counter-current forced circulation evaporator group and the one-effect flash evaporation.

Description

A kind of method for evaporating, concentrating and crystallizing of liquor alumini chloridi
Technical field
The present invention relates to a kind of method for evaporating, concentrating and crystallizing of saline solns, particularly relate to the method for evaporating, concentrating and crystallizing that a kind of salt acid system flyash is produced liquor alumini chloridi in the alumina technology.
Background technology
It is the of paramount importance a kind of mode of total utilization of PCA that flyash extracts aluminum oxide, and this not only can administer plant residue, can also bring economic benefit, environmental benefit and social benefit simultaneously, therefore is subjected to paying close attention to widely.
Flyash production method of alumina mainly concentrates on sintering process (lime sinter process, soda-lime sintering process), alkaline leaching (sodium hydroxide solution molten silicon is earlier carried aluminium again) and acid system (salt acid system, sulfuric acid process) at present.Salt acid system flyash is produced alumina technology and exactly hydrochloric acid and flyash is mixed by certain proportioning in simple terms, stripping under the pressurized conditions of heating then, and slip is through the acid sludge separating, washing after the stripping, and slag is further handled as the raw material of carrying silicon.And parting liquid is sent to the condensing crystal operation after reducing seston content, and the Aluminum Chloride Hexahydrate crystallization that obtains obtains metallurgical-grade aluminum oxide after roasting, the hydrogen chloride gas that the roasting decomposition course is emitted relieving haperacidity after reclaiming.By above-mentioned situation as can be seen liquor alumini chloridi evaporating, concentrating and crystallizing technology be that salt acid system flyash is produced an important ring in the alumina technology.
The evaporation of liquor alumini chloridi evaporating, concentrating and crystallizing and alumina producer has some similar part, but different.Mainly show: 1, the liquor alumini chloridi elevation of boiling point is bigger, nearly 20 ℃; 2, liquor alumini chloridi has very strong corrodibility, and equipment material is had higher requirement; 3, the saturation concentration of liquor alumini chloridi is little with variation of temperature, and it is less to the crystallization content influence therefore to improve its degree of supersaturation by cooling; 4, evaporative process itself is to be purpose to obtain xln.Because the above-mentioned characteristic that liquor alumini chloridi itself is had has determined the evaporative process of its evaporating concentration process and alumina producer sodium aluminate solution to have than big-difference.
Summary of the invention
The objective of the invention is to, solve the prior art problem and a kind of simple and reliable process is provided, energy consumption is lower and the method for evaporating, concentrating and crystallizing of the liquor alumini chloridi that facility investment economizes.
For achieving the above object, the present invention takes following design:
A kind of method for evaporating, concentrating and crystallizing of liquor alumini chloridi, described method comprises the steps: a, circulating and evaporating: step by step liquor alumini chloridi is carried out circulating and evaporating by the multiple-effect pump feed evaporator that comprises heating chamber and separate chamber respectively and concentrate; B, settlement separate: to the separate chamber of the described pump feed evaporator of small part, settlement separate Aluminum Chloride Hexahydrate solid crystal thing; C, flash crystallization: the aluminum chloride solids crystallisate that obtains in the described settlement separate step is sent into the flash crystallization groove, and be that 60~75 ℃, vacuum tightness are to carry out vacuum flashing under the condition of 0.095~0.08Mpa in temperature; D, crystallization are filtered: the discharging in the described flash crystallization step is delivered to filter filters.
Preferably, described circulating and evaporating step comprises triple effect heating chamber and the triple effect separate chamber that links to each other at interval step by step, imitates in the heating chamber at I liquor alumini chloridi is heated to 60~75 ℃, imitates the separate chamber through I then and carry out flash distillation under vacuum tightness 0.095~0.08Mpa; In II effect heating chamber, liquor alumini chloridi is heated to 90~110 ℃, imitates the separate chamber through II then and under vacuum tightness 0.07~0.03Mpa, carry out flash distillation; In III effect heating chamber, liquor alumini chloridi is heated to 125~145 ℃, imitates the separate chamber through III then and carry out flash distillation at 0.12~0.23Mpa.
Preferably, in described settlement separate step, in the bottom of described I effect and II effect separate chamber be set the awl end, 40 °~70 ° of cone angles make Aluminum Chloride Hexahydrate solid crystal thing obtain settlement separate.
Preferably, in described flash crystallization step, it is 40 °~70 ° pointed cone type bottom land that the bottom of described flash crystallization groove is provided with cone angle.
Preferably, attached liquid rate<5% of described six water crystallization aluminum chloride filter cakes.
Advantage of the present invention is: the present invention adopts the full adverse current pump feed evaporator of triple effect group to add the mode of an effect flash distillation, making the aluminum chloride composition complete crystallization in concentration process in the solution is the Aluminum Chloride Hexahydrate crystal, crystal solution uses filter to filter, and makes Aluminum Chloride Hexahydrate filter cake attached liquid rate less than 5%.Simple and reliable process of the present invention, energy consumption is lower, and facility investment economizes.
Description of drawings
Fig. 1 is the structural representation of an embodiment of the present invention.
Among the figure: 1-I is imitated heating chamber; 2-I is imitated the separate chamber; 3-II is imitated heating chamber; 4-II is imitated the separate chamber; 5-III is imitated heating chamber; 6-III is imitated the separate chamber; The 7-condenser; 8-1# condensation water pot; 9-2# condensation water pot; 10-3# condensation water pot; 11-flash crystallization groove; The 12-filtrate receiver; The 13-centrifugal filter; The 14-rubber conveyer; The 15-condensate pump; 16-I is imitated recycle pump; 17-II is imitated the punishment in advance pump; 18-II is imitated recycle pump; 19-III is imitated the punishment in advance pump; 20-III is imitated recycle pump; 21-flash crystallization discharging pump; The 22-filtrate pump.
Embodiment
Referring to Fig. 1, the preferred embodiment of the method for evaporating, concentrating and crystallizing of a kind of liquor alumini chloridi of the present invention shown in it, in the present embodiment, liquor alumini chloridi (about 80 ℃) from a last operation enters filtrate receiver 12, imitate recycle pump 20 by filtrate pump 22 and III and enter III effect heating chamber 5, liquor alumini chloridi and II are imitated secondary steam (about 76 ℃) and enter III effect separate chamber 6 after III are imitated heating chamber 5 heat exchange, (vacuum tightness is 0.095~0.08Mpa to high vacuum in III effect separate chamber 6, be preferably 0.088Mpa in the present embodiment) effect under, present " explosion type " flash distillation, steam the water yield and be about 33% of total steaming water yield, secondary vapour is inhaled into direct condenser 7 and discharges with cooling backwater.
III is imitated the discharging solution temperature and is about 60~75 ℃, is preferably 65 ℃, and wherein the part liquor alumini chloridi is imitated recycle pump 20 by III and imitated the forced circulation evaporation internal recycling at III.Another part liquor alumini chloridi imitates punishment in advance pump 19 by III and II effect recycle pump 18 enters II effect heating chamber 3, (vacuum tightness is 0.07~0.03Mpa) to enter separate chamber's 4 flash distillations of II effect with I effect secondary steam (about 113 ℃) after II is imitated heating chamber 3 heat exchange, II is imitated the steaming water yield and is about 25% of total steaming water yield, and II is imitated secondary vapour and entered III effect pump circulation heating chamber 5.Consider solution under the condition that II is imitated (saturation solubility about 32%), (AlCl that separates out is separated out in existing suitable solid salt crystallization 36H 2The granularity of O solid crystal thing is 0.3~0.5mm, because thicker, the settlement separate better performances of particle), imitate 4 bottoms, separate chamber at II the awl end is set, the solution that contains solid salt separated at the awl end, and cone angle design is 40~70 °, be preferably 45 ° of pointed cone types, help AlCl 36H 2O solid crystal thing settlement separate.This part solution that contains solid salt will be discharged in the flash crystallization groove 11 by pipeline.
II is imitated the discharging solution temperature and is about 90~110 ℃, is preferably 97 ℃, and wherein part solution is imitated recycle pump 18 by II and imitated the pump feed evaporator internal recycling at II.Another part solution imitates punishment in advance pump 17 by II and I effect recycle pump 16 enters I effect heating chamber 1, (vacuum tightness is 0.12~0.23Mpa), and I is imitated the steaming water yield and is about 34% of total steaming water yield to enter separate chamber's 2 flash distillations of I effect with live steam (155~160 ℃ of temperature) after I is imitated heating chamber 1 heat exchange.Solution is under the condition that I is imitated (saturation solubility about 33%), and the solid salt mass crystallization is separated out, and I is imitated 2 bottoms, separate chamber the awl end is set, and cone angle design is 40~70 °, is preferably 45 ° of pointed cone types, helps AlCl 36H 2O solid crystal thing settlement separate.This part solution that contains solid salt will be discharged in the flash crystallization groove 11 by pipeline.Remain saturated liquor alumini chloridi and imitate the forced circulation evaporation internal recycling at I.
I is imitated (about 125~145 ℃ of dischargings, preferably be about 137 ℃ in the present embodiment) and II imitate (about 90~110 ℃ of dischargings, be preferably 99 ℃) the solution that contains solid salt (vacuum tightness is 0.095~0.08Mpa) flash distillation dehydration once more in flash crystallization groove 11, crystallization content further strengthens, and flash distillation is steamed the water yield and is about 7% of total steaming water yield.Flash crystallization groove 11 dischargings (about 60~75 ℃ of drop temperature, be preferably 65 ℃) then deliver to centrifugation in the centrifugal filter 13 (rotating speed 3000rpm) by flash crystallization discharging pump 21, obtain six water crystallization aluminum chloride and saturated aluminum chloride filtrate, (the attached liquid rate is less than 5% for six water crystallization aluminum chloride filter cakes, present embodiment is 2%~5% attached liquid rate) be sent to calcining process through rubber conveyer 14, filtrate enters filtrate receiver 12.
In the evaporating, concentrating and crystallizing process, respectively imitate the vacuum flashing step by step in 1#, 2#, 3# condensation water pot 8,9,10 of heating steam water of condensation, be pooled to finally that 3# condensation water pot delivers to by condensate pump 15 that full factory circulation water station is handled or the acid sludge separation circuit as bath water.
Obviously, those of ordinary skill in the art can constitute various types of method for evaporating, concentrating and crystallizing with the method for evaporating, concentrating and crystallizing of a kind of liquor alumini chloridi of the present invention.
The foregoing description is only for the usefulness that the present invention is described; and be not to be limitation of the present invention; the those of ordinary skill in relevant technologies field; without departing from the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.

Claims (6)

1. the method for evaporating, concentrating and crystallizing of a liquor alumini chloridi, it is characterized in that: described method comprises the steps:
A, circulating and evaporating: step by step liquor alumini chloridi is carried out circulating and evaporating by the multiple-effect pump feed evaporator that comprises heating chamber and separate chamber respectively and concentrate;
B, settlement separate: to the separate chamber of the described pump feed evaporator of small part, settlement separate Aluminum Chloride Hexahydrate solid crystal thing;
C, flash crystallization: the solution that contains aluminum chloride solid crystal thing that obtains in the described settlement separate step is sent into the flash crystallization groove, and be that 60~75 ℃, vacuum tightness are to carry out vacuum flashing under the condition of 0.095~0.08Mpa in temperature;
D, crystallization are filtered: the discharging in the described flash crystallization step is delivered to filter filters.
2. method for evaporating, concentrating and crystallizing according to claim 1, it is characterized in that: described circulating and evaporating step comprises triple effect pump feed evaporator group, in the heating chamber of III effect pump feed evaporator liquor alumini chloridi is heated to 60~75 ℃, the separate chamber through III effect pump feed evaporator carries out flash distillation under vacuum tightness 0.095~0.08Mpa then; In the heating chamber of II effect pump feed evaporator liquor alumini chloridi is heated to 90~110 ℃, the separate chamber through II effect pump feed evaporator carries out flash distillation under vacuum tightness 0.07~0.03Mpa then; In the heating chamber of I effect pump feed evaporator liquor alumini chloridi is heated to 125~145 ℃, the separate chamber through I effect pump feed evaporator carries out flash distillation at 0.12~0.23Mpa then.
3. method for evaporating, concentrating and crystallizing according to claim 1 is characterized in that: in described settlement separate step, in the bottom of described I effect and II effect separate chamber be set the awl end, 40 °~70 ° of cone angles make Aluminum Chloride Hexahydrate solid crystal thing obtain settlement separate.
4. method for evaporating, concentrating and crystallizing according to claim 1 is characterized in that: in described flash crystallization step, it is 40 °~70 ° pointed cone type bottom land that the bottom of described flash crystallization groove is provided with cone angle.
5. method for evaporating, concentrating and crystallizing according to claim 1, it is characterized in that: in described filtration step, filter can be a centrifugal filter, any in vacuum-type drum filter, vacuum band-type filter machine, horizontal table filter, vertical-disk filter, pressure filter and the ceramic filter.
6. method for evaporating, concentrating and crystallizing according to claim 5 is characterized in that: attached liquid rate<5% of described six water crystallization aluminum chloride filter cakes.
CN2010101618291A 2010-04-27 2010-04-27 Method for evaporating, concentrating and crystallizing solution of aluminum chloride Active CN101837998B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103657136A (en) * 2012-09-13 2014-03-26 石家庄工大化工设备有限公司 Method and equipment for evaporative crystallization of aluminium chloride
CN103803617A (en) * 2013-12-30 2014-05-21 中国神华能源股份有限公司 Method for producing aluminum oxide from coal ash through acid process
CN104671570A (en) * 2014-12-24 2015-06-03 江苏同禾药业有限公司 Method for treating aluminum-containing wastewater in preparation process of 6-oxo-8-chloro ethyl caprylate
CN105692713A (en) * 2016-02-24 2016-06-22 石家庄工大化工设备有限公司 Treatment process and equipment adopting hydrochloric acid method to produce deironing eluent in alumina
CN107324364A (en) * 2017-08-31 2017-11-07 宿迁科思化学有限公司 A kind of technique for preparing crystal aluminum chloride
CN109336153A (en) * 2018-12-26 2019-02-15 河南省福可思环保科技有限公司 The method for producing polyaluminium chloride from water treatment agent polyaluminium chloride waste residue dechlorination treatment fluid

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Publication number Priority date Publication date Assignee Title
US4371503A (en) * 1979-06-17 1983-02-01 Dietmar Aichelmann Apparatus for the vaporization of aluminum trichloride
US4548795A (en) * 1981-04-29 1985-10-22 Comalco Aluminum Limited Treatment of aluminous materials
CN1436730A (en) * 2002-02-09 2003-08-20 黄建林 Prepn of high-purity aluminium chloride
CN101311118A (en) * 2007-05-21 2008-11-26 杨风春 Aluminum trichloride (anhydrous) sublimation purification and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4371503A (en) * 1979-06-17 1983-02-01 Dietmar Aichelmann Apparatus for the vaporization of aluminum trichloride
US4548795A (en) * 1981-04-29 1985-10-22 Comalco Aluminum Limited Treatment of aluminous materials
CN1436730A (en) * 2002-02-09 2003-08-20 黄建林 Prepn of high-purity aluminium chloride
CN101311118A (en) * 2007-05-21 2008-11-26 杨风春 Aluminum trichloride (anhydrous) sublimation purification and preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《长春光学精密机械学院学报》 19990331 候福春等 利用煤矸石制备结晶氯化铝、聚合氯化铝 第65-67页 1-6 第22卷, 第1期 2 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103657136A (en) * 2012-09-13 2014-03-26 石家庄工大化工设备有限公司 Method and equipment for evaporative crystallization of aluminium chloride
CN103657136B (en) * 2012-09-13 2015-07-22 石家庄工大化工设备有限公司 Method and equipment for evaporative crystallization of aluminium chloride
CN103803617A (en) * 2013-12-30 2014-05-21 中国神华能源股份有限公司 Method for producing aluminum oxide from coal ash through acid process
CN103803617B (en) * 2013-12-30 2016-03-16 中国神华能源股份有限公司 A kind of flyash acid system produces the method for aluminum oxide
CN104671570A (en) * 2014-12-24 2015-06-03 江苏同禾药业有限公司 Method for treating aluminum-containing wastewater in preparation process of 6-oxo-8-chloro ethyl caprylate
CN105692713A (en) * 2016-02-24 2016-06-22 石家庄工大化工设备有限公司 Treatment process and equipment adopting hydrochloric acid method to produce deironing eluent in alumina
CN107324364A (en) * 2017-08-31 2017-11-07 宿迁科思化学有限公司 A kind of technique for preparing crystal aluminum chloride
CN109336153A (en) * 2018-12-26 2019-02-15 河南省福可思环保科技有限公司 The method for producing polyaluminium chloride from water treatment agent polyaluminium chloride waste residue dechlorination treatment fluid
CN109336153B (en) * 2018-12-26 2021-01-08 河南省福可思环保科技有限公司 Method for preparing polyaluminium chloride from dechlorination treatment liquid of polyaluminium chloride waste residue of water treatment agent

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