Friday, August 7, 2020

BRINE PURIFICATION BY I.E.M

Brine Purification for I.E.M

 

I.E.M brine unit provides feed of brine solution to ion exchange membrane Cell room. The brine solution feed must be ultra pure. The ideal concentration Of brine is 300g/l. Following are the main components of I.E.M brine unit.

1. Saturator

2. Purifier

3. Settler

4. Primary and Secondary Filters

5. Ion Exchange Unit

Saturator

Saturator consists of large storage of rock salt. At the rock salt, depleted and de chlorinated brine having 220 g/l concentration which exist from the anode of iem cells called anolite is showered in order to concentrate it through a 10 inch dia pipe line. From saturator saturated brine goes to pits. There are three primary and two secondary pits. From secondary pits saturated solution at 300g/l concentration and 60-650C temp. is pumped via centrifugal pump having 60 hp and 2900 rpm into purification section.

 

Purifiers

There are two purifiers both have capacity 70 m3. In first purifier solution of barium carbonate has been added to remove sulphate ions. Excess carbonates are maintained in the solution to insure removal of sulphate ions. Sludge formed is periodically remove from bottom of the first purifier and is send to the recovery pits. Overflow from first purifier goes to second purifier where caustic solution is added into it. This will settle Mg as Mg (OH) 2. Purpose of adding caustic in purifier 2 is of dual purpose:

·         Maintaining conc. Of Na+ ions in brine feed.

·         To convert Mg+ to Mg(OH)2.

One important thing is that If we don’t add BaCO3 in first purifier then we add calcium chloride in CaCl2 pits and also add Na2CO3 in first purifier.From purifier the brine is transferred to settler prior to the introduction of Brine into the settler, a flocculent named “Accofloc” is added which solution is prepared into accofloc storage tank. Purifier is made of mild steel and lined with fiber glass. Following are the reactions involved in purifiers

 

Ba2co3+Na2so4     -----------à                  Baso4+Na2co3

 

Na2co3+Cacl2    ----------à                      Caco3+2Nacl

 

       Mgcl2+2NaoH    ----------à                 Mg (OH) 2+2Nacl


Settler


Settler has capacity of 1000m3, brine overflows from settler after settling. A Scraper is also installed in the center; it takes 8 min and 53 sec to complete one revolution or 6.75 rev/hr near the bottom of the settler to push the sludge settled, towards the bottom of the tank where an automatic pneumatic control valve is opens for 30 sec after every 45 mint. The sludge from the settler is send to the recovery pits and from the recovery pit brine is send to the purifier one. From settler, the brine moves to a clarified tank. Settler is made of mild steel and coated with a type of resin which is corrosion resistant.

Primary and Secondary Filters

From settler, the brine moves to a series of filters where 5 different layers of Pebbles are used to filter the brine solution. The layer at the top is of Anthracite and remaining layer are of pebbles whose size increases from top to bottom. Here further purification from any sort of suspended impurity takes place. Backwash of these Primary filters takes place once in 24 hours. 

Steps for Backwashing of Primary Filters:

To backwash a primary filter following steps should b followed:

·         Close inlet and outlet valves simultaneously

·         Open the vent valve

·         Open the valve of the line going to the backwash from the top

·         Open the drain valve for 5-10min and drain it to recovery pit

·         Close the drain and recovery pit valve

·         Open the water valve connected to the drain line

·         Backwashing will start in a while and water will start coming out of the backwash pipe at the top

·         When water becomes clear it means filter is clean now close the water inlet valve and open the drain valve and drain the water into drain line

·         Now close the drain valve and backwash valve

·         Open the inlet valve

·         When brine starts coming out the vent then open the outlet valve and close the vent valve the filter will into the circuit again

. After primary filter brine is passing in to 2 storage tanks. Now it is pumped to secondary FILTERS (for suspended / insoluble impurities), containing tubes in it 137 in no. with 10 openings for each tube, and above flanged portion (that is hollow) brine is accumulated. Alfa cellulose solution is prepared in agitated tank and pumped to secondary filter to form a coating, in order to remove suspended impurities. There are three secondary filters 2 in circuit at a time and 1 under coat layer formation for 30 mins. One of the circuited filters is made to be refreshed when its coating is chocked resisting further flow and developing pressure which is then drained with great pressure and newly coated filter is in circuited.Following are the steps involving in the backwashing of the secondary filters.

Steps for backwashing of Secondary Filters:

·         Close the inlet and outlet valves simultaneously

·         Open the vent valve for the removal of air

·         Open the drain valve and drain the filter into the pit

·         Brine will drain at a high rate because of the compressed air entrap inside the filter

·         Close the drain valve

·         Open the backwash water valve the water will start coming out from the top of the filter

 from the watch glass line and close the vent valve

·         When the filter become clear close the water valve

·         Open the drain valve and drain the water and then close darin valve

·          pump the arbocell in the filter it comes out from the top and will move to the arbocell tank

·         Watch glass will show milky liquid coming out of the filter when it becomes clear the coating will complete close the arbocell coating

·         Close the arbocell coating valve

 After passing through it, feed is sending to feed to ionizer tank. By pump brine is send to feed to ionizer.

Ion Exchange Unit

Freshly regenerated resin of sodium zeolite is called as a polisher since it provide final touch to remove any dissolved impurity if any, and when it contains enough amount of soluble impurities it is called ionizer since it actually removes solubility’s. Ionizer contains cations and zeolite, which when acting as a ionizer removes Ca+2 and Mg+ by converting to calcuim zeolite and magnesium zeolite. Two out of three ionizers/polishers are in circuit at a time one as ionizer and other as polisher, and third one under regeneration. Then this regenerated one is made as ionizer and polisher as ionizer. This transition depends on feed quality.

Regeneration of Resin

To regenerate resin HCl along with NaOH is used. Sodium sulphide is added in order to remove chlorine gas. S-2 are also present in small extent. For regeneration first caustic is drained, followed by the displacement ( water wash) and backwashing with water. Acid HCl (dechlorinated with sodiumsuphite) is showered after diluting it 4% from 30% else it will damage resin. Once again it is displaced with water. Ca+2 and Mg+ adsorbed on resin will remove using HCl and HCl is displaced by water. NaOH is injected in order to add Na+2 and OH-1ions in resin. All of the ions are removed and converted into respective compounds. Temperature of the feed to ion exchange is maintained via heat exchanger.

Steps for Regeneration of Resin: 

Ø Brine Drain:

Drain the brine before regeneration.Open Drain valve and also open manual and automatic valves so that brine could drain easily.

Ø Brine displacement:

After the brine is completely drained, open water inlet valve as the drain valve is already open. Check if drain is complete. If so close the water inlet valve and drain valve. Backwash it

Ø Back Washing:

This procedure takes place from bottom to top. Open the backwash valve and outlet valve. Adjust the water manual valve so that resin does come out of the vessel.  And all the suspended particles go out through it. Close the back wash valves.

Ø Water Drain:

To drain water after backwash, open drain valve and vent valve so that water can be drained easily and early. After drain is complete, prepare acid injection.

Ø HCL Injection

To remove 32% free chlorine from acid tank, inject sodium sulphite and check from the laboratory that chlorine is completely removed. After the removal of free chlorine, open chemical valve and to reduce 32% acid to 4%, adjust the water manual valve and start 32% acid pump. Open the suction and delivery valves. Adjust the pump stroke to 78%. Check the concentration of acid from sample point. It should be 4%. After 1 hour, check the acid concentration from the drain valve and if this concentration is equal to the inlet concentration, acid injection is complete. If this concentration is not equal to 4% then continue acid injection.

Ø Acid Displacement:

To remove the excess acid from ion exchanger, open the water inlet valve and check the pH of water coming out of drain valve. Continue this process until pH is normal and when the excess acid is completely removed. Close the water inlet valve and completely drain the water.

Ø Caustic Injection:

After complete water drain, start caustic injection. Open chemical valve and adjust the water manual valve so that the concentration of caustic is 4%. Start the caustic injection pump and open its suction and delivery valves. Keep the pump strokes to 66%. Check the caustic

Material Balance of IEM Brine:

Basis: - 150ton/day

Brine required/salt requirement

2Nacl+2H2 O       --------à    2NaOH+H2 +Cl2

NaOH            :               Nacl

2                     :                              2

1                            :                       1

1*40       :                       1*58.5

40g                :                 58.5g

40g caustic required Nacl=58.5g

1g caustic required Nacl=58.5/40

150,000,000g caustic required Nacl=585/40*150,000,000

                                =219375000g

                        =219 ton

Nacl required=219

 

Salt Composition:-


Nacl           =94%

Sulphate   =2.2%

Ca               =0.35%

Mg             =0.35%

Others       =3%

Fe               =0.002%

Rock Salt Required to be charge:-

94 ton Nacl is present in rock salt= 100 ton

1 ton Nacl is present in rock salt = 100/94

219 ton Nacl is present in rock salt= 100/94*219

                                                              = 233 ton

So rock salt required= 233 ton

Rock salt required= 233 ton


Sulphate in rock salt= 233*2.2/100= 5.126 ton

Ca in rock salt           = 233*0.35/100= 0.8 ton

Mg in rock salt         = 233*0.35/100= 0.8 ton

Others in rock salt   = 233*3/100     = 7 ton

Fe in rock salt           = 233*0.002/100= 0.005 ton

BaCo3  Required:-

BaCo3+Na2 So4     -------à               BaSo4+Na2 Co3         

Mass of Na2 So4 = 5.126 ton

Molar mass of Na2 So4 = 118 ton

Moles                             = 5.126/118= 0.043

BaCo3                   :                              Na2 So4

1                            :                    1

0.043                   :                   0.043

BaCo3  Required=            0.043*137

BaCo3  Required=            5.891

BaCo3  Required=          5.8 ton

BaCo3  Required=          5.8 ton

 

Na2Co3 Produced:-


Na2 Co3             :                   Na2 So4

1                    :             1

0.043            :            0.043

Na2 Co3 Produced= 0.043*94= 4

Na2 Co3 Produced= 4 ton 

 

Na2 Co3   REQUIRED

Na2 Co3+CaCl2      --------à               CaCo3+2NaCL

Mass of CaCl2 =            0.8 ton

Molar Mass of CaCl2 = 40

Moles                         = 0.8/111 = 0.007

                                    = 0.07

Na2 Co3                   :            CaCl2

  1                             :             1

0.07                 =             0.07   

Na2 Co3 required = 94*0.07 = 6.6 ton

Amount of Na2 Co3 required= 6.6 ton

Amount of Na2 Co3 required= 6.6 to


NaOH Required:-

MgCl2+2NaOH   ------à      Mg (OH) 2+2NaCl

Mass of MgCl2   = 0.8

Molar Mass      = 90

Moles                = 0.8/90 = 0.01

NaOH        :        MgCl2

  2              :           1

0.02          :          0.01

NaOH Required to remove MgCl2 =0.02*40    = 0.8 ton

NaOH required to remove MgCl2 = 0.8 ton

NaOH required to remove MgCl2 = 0.8 ton


FeCl2+2NaOH         ---------à             Fe (OH) 2+2NaCl

Mass of FeCl2   = 0.005 ton

Molar Mass      = 55.8g/mole+70 = 125.8

Moles                = 0.005/125.8 = 3.9*10-5

FeCl2          :        NaOH

1                 :           2

3.9*10-5   :    2*3.9*10-5

                   :     7.9*10-5

                   :     7.9*10-5 *40

                        0.03 ton

NaOH required to remove FeCl2 = 0.03 ton

NaOH required to remove FeCl2 = 0.03 ton


NaOH required= 0.8+0.03

                           = 0.83 ton

NaOH required= 1 ton

NaOH required= 1 ton

 

Results:

Nacl required=219

Rock salt required= 233 ton

BaCo3 required=   5.8 ton

Na2 Co3 required= 1 ton

Na2 Co3 Produced= 4 ton

NaOH required to remove MgCl2 = 0.8 ton

NaOH required to remove FeCl2 = 0.03 ton

NaOH required= 1 ton

Material Injections:

Baco3=  5.8 tons

NaOH= 1 ton

  Flow Rates

All pumps have volumetric flow rate 110 m3/hr and working on 80% effienency and maximum 2900 rpm.

 

Pump

Max RPM

    (a)

Given RPM

      (b)

88/2900 *b

Flow rates

  (m3/hr)

Crude Brine

2900

1050

.0303*1050

31.86

I.E

2900

1650

.0303*1650

49.99

Secondary Storage Tank

2900

2150

.0303*2150

65.154

Clarifier

2900

2700

.0303*2700

81.81


IEM Brine Block diagram








Brine Purification for D.S.A

DSA brine unit provides brine to DSA cell rooms. The purity level of brine solution required here is not that mush high as that for I.E.M cell room. That’s why lesser purifiers is installed into this unit. Another distinguishing feature of the unit is that brine is dechlorinated in this unit as oppose to I.E.M brine unit where dechlorinated brine is received from cell room. The unit consist of following sub units.

1. DeChlorination Unit

2. Saturator

3. Purifier    

4. Settler

5. Sand Filters

De- Chlorination Unit

Depleted brine from DSA is sent to storage tank(2D10) behind DSA , with storage temp. 800C, with such a low level that on addition of HCl Cl2 gas covers maximum volume available, extracted and sent via suction of blowers to HCl plant or else. There are two storage tanks and two pumps to pump depleted brine. 31% caustic is imported into storage tank via pump and lift upward to provide flow under gravity since it is more well controlled, and fast way. From overhead this brine is injected into depleted brine line coming by passing through air strippers installed in series in which brine is entered from middle and air is blown through it to DE chlorinate brine. This chlorinated air is sent to calcium hypo chlorite unit. Chlorine is reduced to 7.1-21.3 g/l.After injection of caustic through over head arrangment,it is stored into DE chlorinated brine tank(2D13 A,B). Here its pH is 8.5-9.5. The dechlorinated brine is sent to saturator in dechlorination unit, the chlorine contents in brine solution is reduced to 7.1 ppm

Saturator

The declorinated brine then pumped to the saturators where it showered on the rock salt and becomes saturated. Saturated brine (320 – 325gpl ) is difficult to handle due to the variation in temperature, causing crystallization of the salt in pipe lines and equipments. In order to control the concentration of NaCl to the desired 300gpl a bypass line of depleted brine is mixed with saturated brine in pits. Here in pits insoluble fractions are settle down and then after required time of settlement brine is pumped to the purifiers for further.

Purifiers

There are two purifiers both have capacity 70 m3. In first purifier solution of barium carbonate has been added to remove sulphate ions. Excess carbonates are maintained in the solution to insure removal of sulphate ions. Sludge formed is periodically remove from bottom of the first purifier and is send to the recovery pits. Overflow from first purifier goes to second purifier. where caustic solution is added into it. This will settle Mg as Mg (OH) 2. Purpose of adding caustic in purifier 2 is of dual purpose:

Maintaining conc. Of Na+ ions in brine feed.

To convert Mg+ to Mg(OH)2.

From purifier the brine is transferred to settler prior to the introduction of Brine into the settler, a flocculent named “Accofloc” is added which solution is prepared into accofloc storage tank. Purifier is made of mild steel and lined with fiber glass. Following are the reactions involved in purifiers

 

Ba2co3+Na2so4      -----------à                   Baso4+Na2co3

   Na2co3+Cacl2               -----------à                           Caco3+2Nacl

   Mgcl2+2NaoH             --------à                  Mg (oH) 2+2Nacl

Settler

Settler has capacity of 2300m3, brine overflows from settler after settling. A Scraper is also installed in the center, near the bottom of the settler to push the sludge settled, towards the bottom of the tank where an automatic pneumatic control valve is opens for 15 sec after every 30 mint. The sludge from the settler is send to the recovery pits and from the recovery pit brine is send to the purifier one. From settler, the brine moves to a clarified tank. Settler is made of mild steel and coated with a type of resin which is corrosion resistant.

 Primary Filters

From settler, the brine moves to a series of filters where 5 different layers of Pebbles are used to filter the brine solution. Internals of primary filters, 8 in no. and 6 in circuit, consists of rocky pebbles leading from smaller size to larger one supported via rod support at bottom that do not allow them to flow out. At the top there is a layer of small particles enough small that it looks like a layer of sand. Fluid is entered from bottom of filters. Here further purification from any sort of suspended impurity takes place. Backwash of these Primary filters takes place once in 24 hours.

Purified brine with small amount of chlorine is pumped to 2D6 tank. After 2D6 tank HCl is added to adjust pH to 4-5, while its temperature is maintained by passing it through heat exchanger rising it to 700C. after heat exchanger brine is sent to overhead storage tank 2D7 where further from here it is sent to DSA cell rom.

Material Balance of IEM Brine:

Basis: - 90 ton/day

Brine required/salt requirement

2Nacl+2H2 O    --------à       2NaOH+H2 +Cl2

NaOH            :               Nacl

2                     :                 2

1                     :                  1

1*40              :                1*58.5

40g                :                 58.5g

40g caustic required Nacl=58.5g

1g caustic required Nacl=58.5/40

150,000,000g caustic required Nacl=58.5/40*90,000,000

                                =131625000g

                        =131 ton

Nacl required=131

 

Salt Composition:-


Nacl           =94%

Sulphate   =2.2%

Ca               =0.35%

Mg             =0.35%

Others       =3%

Fe               =0.002%

Rock Salt Required to be charge:-

94 ton Nacl is present in rock salt= 100 ton

1 ton Nacl is present in rock salt = 100/94

131 ton Nacl is present in rock salt= 100/94*131

                                                              = 139 ton

So rock salt required= 139 ton

Rock salt required= 139 ton

 

Sulphate in rock salt= 139*2.2/100= 3.058 ton

Ca in rock salt           = 139*0.35/100= 0.5 ton

Mg in rock salt         = 139*0.35/100= 0.5 ton

Others in rock salt   = 139*3/100     = 4 ton

Fe in rock salt           = 139*0.002/100= 0.003 ton

BaCo3  Required:-

 BaCo3+Na2 So4   ----------à                     BaSo4+Na2 Co3         

Mass of Na2 So4 = 3.058 ton

Molar mass of Na2 So4 = 118 ton

Moles                             = 3.058/118= 0.03

 

BaCo3                   :                              Na2 So4

1                           :                    1

0.03                     :                   0.03

BaCo3  Required=            0.03*137

BaCo3  Required=            4.11

BaCo3  Required=          4.11 ton

BaCo3  Required= 4.11 ton

 

Na2Co3 Produced:-

Na2 Co3             :                   Na2 So4

1                         :             1

0.03                   :            0.03

Na2 Co3 Produced= 0.03*94= 3 ton

Na2 Co3 Produced= 3 ton

Na2 Co3 Required:-

Na2 Co3+CaCl2  --------à    CaCo3+2NaCL

Mass of CaCl2 =            0.5 ton

Molar Mass of CaCl2 = 40

Moles                         = 0.5/111 = 0.005

                                    = 0.01

Na2 Co3                   :            CaCl2

  1                             :             1

0.05                 =             0.05   

Na2 Co3 required = 94*0.05 = 5 ton

Amount of Na2 Co3 required= 5 ton

Amount of Na2 Co3 required= 5 ton

 

NaOH Required:-

MgCl2+2NaOH      ---------à        Mg (OH) 2+2NaCl

Mass of MgCl2   = 0.5

Molar Mass      = 90

Moles                = 0.5/90 = 0.005

NaOH        :        MgCl2

  2              :           1

0.01          :          0.005

NaOH   Required to remove MgCl2 =0.01*40    = 0.4 ton

NaOH  required to remove MgCl2 = 0.4 ton

NaOH required to remove MgCl2 = 0.4 ton

 

FeCl2+2NaOH       -------------à               Fe (OH) 2+2NaCl

Mass of FeCl2   = 0.003 ton

Molar Mass      = 55.8g/mole+70 = 125.8

Moles                = 0.003/125.8 = 2.4*10-4

FeCl2          :        NaOH

1                 :           2

2.4*10-4       :    2*2.4*10-4

                   :     4.8*10-4

                   :     4.8*10-4 *40

                        0.02 ton

NaOH required to remove FeCl2 = 0.02 ton

NaOH required to remove FeCl2 = 0.02 ton

 

NaOH required= 0.4+0.02


                          
= 0.42 ton

NaOH required= 0.42 ton

NaOH required= 0.42 ton

 


Results:

Nacl required=131

Rock salt required= 139 ton

BaCo3 required=   4.11 ton

Na2 Co3 required= 5 ton

Na2 Co3 Produced= 3 ton

NaOH required to remove MgCl2 = 0.4 ton

NaOH required to remove FeCl2 = 0.02 ton

NaOH required= 0.42 ton

 

Material Injections

Baco3= 4.11 tons

NaOH= 0.42 tons

DSA Block diagram:



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