CN1102600A - Process and unit for separating sulfate from sodium chloride in high temp. salt - Google Patents

Process and unit for separating sulfate from sodium chloride in high temp. salt Download PDF

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CN1102600A
CN1102600A CN 94108026 CN94108026A CN1102600A CN 1102600 A CN1102600 A CN 1102600A CN 94108026 CN94108026 CN 94108026 CN 94108026 A CN94108026 A CN 94108026A CN 1102600 A CN1102600 A CN 1102600A
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salt
separation chamber
temp
sodium chloride
conically shaped
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CN1041510C (en
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牛自得
王宗玉
李臻
田哲
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Engineering And Tech Research Academy China Petroleum And Gas Corp
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Engineering And Tech Research Academy China Petroleum And Gas Corp
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Abstract

High-temp. salt is processed into suspension by use of a solution containing potassium chloride, magnesium chloride, sodium chloride and magnesium sulfate and the suspension is separated via separator into magnesium milk and salt slurry. The magnesium milk may be used to prepare potassium or magnesium sulfate and the salt slurry is centrifugally dried to obtain industrial salt. Said separator is composed of inlet and top pipes, separation chamber and conic cylinder. It features high efficiency and low energy consumption.

Description

Process and unit for separating sulfate from sodium chloride in high temp. salt
The present invention relates to a kind of chemical separating technology and device, the technology and the device of sulfate and sodium chloride in particularly a kind of separating high-temp salt.
The discarded object that the bittern evaporation is produced behind the potassium chloride is a sulfur-bearing hydrochlorate in the high temp. salt (comprising the magnesium sulfate, kainite, the langbeinite that contain the different crystallizations water) about 30%, sodium chloride about 30%, and contain small amount of impurities such as potassium chloride, magnesium chloride and bromine, 10 tons of high temp. salts of the about by-product of 1 ton of potassium chloride of every production.Past domestic most of producer all high temp. salt is discarded need not, existing at present part producer adopts distinct methods that high temp. salt is recycled, but all not too proves effective.As " natural freezing method " is in the winter time high temperature salinization halogen to be frozen the system sal glauberi, is reprocessed into anhydrous sodium sulfate (claiming glauber salt again), and this method investment is many, cost height, energy consumption are big, its sulfate radical rate of recovery has only about 40%, because glauber salt is often unsalable, some producer has to stop production; " hot melt soaks method " is at first thin up high temp. salt of the principle utilizing common-ion effect and increase the total ionic strength adjustment buffer degree, heating then, leach with magnesium chloride solution, remove the suspension naturally frozen or freeze the system epsom salt again behind the sodium chloride with the mechanical refrigeration method, this method equipment is many, and energy consumption is big, and the magnesium sulfate rate of recovery has only about 45%, the sodium chloride rate of recovery has only about 30%, not fine as yet applying in actual production process; " succusion " is to utilize that sodium chloride varies in size with sulphate particle, proportion is different, thereby the different principle of sinking speed, adopt vibration separation of produced epsom salt, but this method can not effectively be separated magnesium sulfate with sodium chloride, the rate of recovery of magnesium sulfate has only 30~40%, and sodium chloride still can not be recycled; " press over system ", Chinese patent CN 1035096A proposes overflow separation method according to the static vertical-overflow device control of overflow size separation principle utilization certain flow rate and is applied to separating of sulfate and sodium chloride in the high temp. salt, though this method can be separated the two, but because the magnesia magma that overflows is very rare, it is very slow that sedimentation concentrates speed, and suitability for industrialized production hardly may; " floatation " utilized can optionally adsorb the foaming agent that catching of magnesium sulfate monohydrate crystal grain got agent and can be bubbled, high temp. salt is made slurry to be separated in flotation washer, because a large amount of foams are arranged, magnesium sulfate monohydrate is difficult to sedimentation separation, and the easy polluted product of the introducing of medicament, so method is difficult to promote.
The objective of the invention is to provide the technology and the device thereof of sulfate and sodium chloride in a kind of separating high-temp salt, it can be with the sulfate in the similar seawer system bittern chemical waste residue high temp. salt and sodium chloride separately, to reach comprehensive utilization.
The object of the present invention is achieved like this: in view of sulfate in the high temp. salt and sodium chloride crystalline characteristics there are differences, promptly proportion and granularity have than big-difference, utilize fluid rotary principle that the two is separated.One water and epsom salt are the magnesia magma shape, and epsom salt proportion is 1.68; Sodium chloride proportion is 2.16, and granularity is bigger, analyzes by screen analysis and finds that account for the following magnesium salts of 87.20%, 200 order at the above sodium chloride of 200 orders and account for 95.88%, the two has tangible separability.Based on this separability, the invention provides the two technology of separating and device.
This device is made up of feed pipe, push pipe, separation chamber, conically shaped, the separation chamber of this separator is a cylindrical shape working chamber, the conically shaped of it and bottom adopts flange coupling (also can weld), feed pipe and separation chamber are tangent, and feed pipe can be circular when access to plant, also can become rectangle by circle.Push pipe is the pipe concentric with the separation chamber, and some stretches into inside, separation chamber.The conically shaped cone angle is 5~50 °, plays a kind of guide functions, and the bottom is outlet.Feed pipe import, push pipe outlet, conically shaped outlet all connect with valve, liner sealing (not drawing among the figure).
The technology of separating high-temp salt of the present invention and sodium chloride is: with high temp. salt with a kind of MgCl that contains 25~25%(is heavy), KC10.1~10%(is heavy), NaCl0.1~10%, (weight), MgSO 40.1~15%(is heavy) solution mix by 1: 0.1~10 ratio (volume ratio) and be made into the high temp. salt mass suspension, 20~90 ℃ of temperature, usefulness has the separator that is pumped into of certain lift.Because the pressure of pump, particle in the suspension has certain speed, begin to do circular motion after tangentially entering the separation chamber, under the suitable condition of suspension flow velocity, because the difference of particle diameter and quality, particle diameter is big and sodium chloride particle that quality is heavy is made downward spiral circular motion in the separation chamber, is discharged by outlet through the conically shaped water conservancy diversion.Little and the sulphate particle of light weight of particle diameter is assembled to the center because of providing enough centripetal force, is carried under one's arms by fluid and discharges from the push pipe outlet.What discharge from push pipe outlet like this is the magnesia magma of sulfur-bearing hydrochlorate, and what discharge from the conically shaped lower part outlet is the salt slurry of sodium chloride-containing, the salt slurry after centrifuge dries, Nacl, get rid of back liquid and incorporate suspension into.Realized the separation of high temp. salt like this.
The present invention is because be the separator that utilizes fluid rotary principle to be designed to dexterously, so technology is simple, and the separative efficiency height, processing ease is saved energy consumption, thereby has solved many drawbacks that the flotation of traditional salt chemical industry or overflow mechanism are introduced.Utilize technology of the present invention and device effectively sulfate in the similar seawer system bittern chemical waste residue high temp. salt and sodium chloride to be separated, reach the purpose of comprehensive utilization.
The present invention is provided in detail by following embodiment and accompanying drawing thereof.
Fig. 1 is the side view of the high temp. salt separator of proposition according to the present invention.
Fig. 2 is the vertical view of the high temp. salt separator of proposition according to the present invention.
Fig. 3 is a n level separating technology flow chart of using apparatus of the present invention, M-magnesia magma among the figure, G-high temp. salt slurry, Y-Nacl.
Fig. 4 is 2 grades of separating technology flow charts using apparatus of the present invention, M-magnesia magma among the figure, G-high temp. salt slurry, Y-Nacl.
Describe the details and the working condition of the concrete device that proposes according to the present invention in detail below in conjunction with accompanying drawing 1-4.
Referring to Fig. 1 and 2, this device is by feed pipe (3), push pipe (1), separation chamber (2), conically shaped (5) is formed, and the separation chamber of this device (2) are cylindrical shape working chambers, the conically shaped (5) of it and bottom adopts flange (4) to connect (also can weld), feed pipe (3) and separation chamber (2) are tangent, and feed pipe (3) can be circular when access to plant, also can be become square by circle.Push pipe (1) is and the concentric pipe in separation chamber (2), and some stretches into inside, separation chamber (2), and conically shaped (5) cone angle is 5~50 °, plays a kind of guide functions, and its underpart is outlet.The feed pipe import, the push pipe outlet, the conically shaped outlet all connects with valve, liner sealing (for outstanding principal character of the present invention, not drawing valve among the figure).This device each several part size is preferably as follows: feed pipe (3) diameter is 20~200 millimeters, push pipe (1) diameter is 20~200 millimeters, the conically shaped outlet diameter is 20~200 millimeters, separation chamber (2) diameter is 50~500 millimeters, separation chamber (2) highly is 50~500 millimeters, 200~2000 millimeters of conically shaped (5) height, cone angle is 5~50 °.
During separating high-temp salt, with high temp. salt with a kind of MgCl that contains 25~25%(is heavy), NaCl0.1~10%(is heavy), KC10.1~10%(is heavy), MgSO 40.1~15%(is heavy) solution mix in 1: 0.1~10 ratio (volume ratio) and be made into the high temp. salt mass suspension, 20~90 ℃ of temperature of charge, the charging operating pressure is 2~60 meters the separator that is pumped into lift between 0.02~2.0MPa.Because the pressure of pump, particle in the suspension has the speed of 1~50 meter per second in import department, begin to do circular motion after tangentially entering the separation chamber, under the suitable condition of charging rate, because the difference of particle diameter and quality, particle diameter is big and sodium chloride particle that quality is heavy is made downward spiral circular motion in the separation chamber, through the conically shaped water conservancy diversion, is discharged by end mouth.Little and the sulphate particle of light weight of particle diameter is assembled to the center because of providing enough centripetal force, is carried under one's arms from the top by fluid and mouthful discharges.Be the magnesia magma of sulfur-bearing hydrochlorate from what push up mouthful discharge like this, the concentration of the magnesia magma of arranging can be used for preparing magnesium sulfate and potassium sulfate at 20~60Be '.What discharge from end mouth is the salt slurry of sodium chloride-containing, the salt slurry after centrifuge dries Nacl, get rid of back liquid and incorporate high temp. salt suspension into, realized the separation of high temp. salt like this.
In the actual production,, the multistage combination of apparatus of the present invention can be realized separating more completely in order to realize separating fully of sodium chloride and sulfate, as the n level separate (n is the integer more than or equal to 1, as n=1,2,3 ...).The separation of n level is combined by 2n-1 apparatus of the present invention, and every increase one-level is separated, and just increases right two devices of a first from left.The process flow of constructing in fact following (accompanying drawing 3), the top that one-level is separated flow to into parting on the left side from device that secondary separates, and underflow enters parting on the right side from device of secondary separation.Secondary parts on the left side from the top of device and flows to into next stage (third level) and part on the left side from device, and underflow is got back to upper level (first order) separator.The underflow that secondary parts on the right side from device enters next stage (third level) and parts on the right side from device, and the top flow back into upper level (first order) separator.And the like, it is qualified magnesia magma that the n level parts on the left side from what install top mouthful discharge, underflow is got back to the n-1 level and is parted on the left side from device.It is qualified salt slurry that the n level parts on the right side from the device underflow, the salt slurry after centrifuge dries, Nacl and get rid of back liquid, get rid of back liquid and get back to the n-1 level with n level top stream and part on the right side from device.The n value is looked technological requirement and is determined.
Referring to accompanying drawing 4, utilize the application examples of technology of the present invention and device separating high-temp salt as follows: to adopt the combination of 2 stage arrangements that high temp. salt is separated, soon high temp. salt carries out just revolving, essence is revolved and tailspin, process conditions see Table 1, used separator size is listed in table 2, and corresponding separating resulting is listed in the table 3.
Table 1
Figure 941080269_IMG2
Annotate: the suspension proportioning is that high temp. salt is with a kind of MgCl that contains in the table 1 214.86% NaCl4.13% Kcl5.94% MgSO 4The ratio that 7.40% solution mixes mutually (volume ratio).
Table 2
Table 3
Figure 941080269_IMG4

Claims (4)

1, the device of sulfate and sodium chloride in a kind of separating high-temp salt, the separation chamber (2) that it is characterized in that this device is a cylindrical shape working chamber, the conically shaped (5) of separation chamber (2) and bottom, adopt flange (4) to connect (also can directly weld), feed pipe (3) is tangent with separation chamber (2), and feed pipe (3) can be circular when access to plant, also can become rectangle by circle, push pipe (1) is and the concentric pipe in separation chamber (2), and some stretches into inside, separation chamber (2), and the cone angle of conically shaped (5) is 5~50 °.
2, by the described device of claim 1, it is characterized in that feed tube diameter 20~200mm, top tube diameter 20~200mm, conically shaped outlet diameter 20~200mm, diameter 50~the 500mm of separation chamber, the height 50~500mm of separation chamber, conically shaped height 200~2000mm.
3, the technology of sulfate and sodium chloride in a kind of separating high-temp salt, when it is characterized in that separating high-temp salt, earlier with high temp. salt with a kind of MgCl that contains 25~25%, NaCl0.1~10%, KC10.1~10%, MgSO 40.1~15% solution mixes in 1: 0.1~10 ratio (volume ratio), be made into the high temp. salt mass suspension, 20~90 ℃ of temperature of charge, with the pressure of 0.02~2.0MPa suspension is sent into claim 1 then, 2 described devices separate, and the concentration of magnesia magma that push pipe is arranged can be used for preparing magnesium sulfate and potassium sulfate at 20~60Be ', the salt slurry that the conically shaped outlet is discharged becomes Nacl after centrifuge dries, get rid of back liquid and incorporate in the high temp. salt suspension.
4, by the described technology of claim 3, it is characterized in that can adopting in the actual production one-level and/or n(n is integer more than or equal to 1) the stage arrangement combination separates.
CN94108026A 1994-08-04 1994-08-04 Process and unit for separating sulfate from sodium chloride in high temp. salt Expired - Fee Related CN1041510C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100588614C (en) * 2008-08-21 2010-02-10 天津科技大学 Method for preparing sodium chloride and magnesium sulphate heptahydrate with brine
CN102762499A (en) * 2009-05-29 2012-10-31 嘉吉公司 Method of producing naturally purified salt products
CN106276976A (en) * 2015-06-12 2017-01-04 金達行有限公司 A kind of recovery method of magnesium sulfate monohydrate cleaning mixture
CN111762803A (en) * 2020-06-17 2020-10-13 天津长芦汉沽盐场有限责任公司 Method for producing magnesium sulfate fertilizer by using high-temperature salt

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE406713B (en) * 1977-07-18 1979-02-26 Celleco Ab HYDROCYCLOSE SEPARATOR WITH SLIDES IN THE CIRCULAR CYLINDRICAL PART OF THE SEPARATION CHAMBER
CN1020272C (en) * 1988-02-12 1993-04-14 轻工业部制盐工业科学研究所 Preparation method of magnesium sulphate and sodium chloride from high temp. salt

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100588614C (en) * 2008-08-21 2010-02-10 天津科技大学 Method for preparing sodium chloride and magnesium sulphate heptahydrate with brine
CN102762499A (en) * 2009-05-29 2012-10-31 嘉吉公司 Method of producing naturally purified salt products
US8951305B2 (en) 2009-05-29 2015-02-10 Cargill, Incorporated Method of producing naturally purified salt products
CN102762499B (en) * 2009-05-29 2015-11-25 嘉吉公司 Produce the method through the salt product of natural purifying
CN106276976A (en) * 2015-06-12 2017-01-04 金達行有限公司 A kind of recovery method of magnesium sulfate monohydrate cleaning mixture
CN106276976B (en) * 2015-06-12 2018-07-06 金達行有限公司 A kind of recovery method of magnesium sulfate monohydrate cleaning solution
CN111762803A (en) * 2020-06-17 2020-10-13 天津长芦汉沽盐场有限责任公司 Method for producing magnesium sulfate fertilizer by using high-temperature salt

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