Beruflich Dokumente
Kultur Dokumente
YTSJ/CZ 0120-2014
Project Name:
2014-02-20 Publish
2014-00-00 Implement
YTSJ/CZ0120-2014
Purified Brine Operation Manual
Editor: Xu Feng
Proofreader: Xu Feng
Auditor: Gu Junlin
Approver: Li Yi
YTSJ/CZ0120-2014
Purified Brine Operation Manual
Contents
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Asia Chemical Engineering CO., LTD.
Caustic Soda Technology Department
YTSJ/CZ0120-2014
Purified Brine Operation Manual
CaCO3
In order to purge out Ca2+,the quantity of sodium carbonate added must exceed the response
equation's demand in theory, excess of caustic soda of sodium carbonate in this technology is
300~500mg/l.
1.3 Removing magnesium ions with sodium hydroxide
TO add NaOH solution to brine, it reacts with Mg2+ in brine and generates the insoluble Mg(OH)2
precipitation, the response equation is as the following:
Mg2+ + 2OH-
Mg(OH)2
In order to purge out Mg2+,the quantity of NaOH added must exceed the response equation's demand
in theory, excess of caustic soda of sodium hydroxide in this technology is 100~300mg/l.
1.4 Brine filtration and purification
To add refining agent to the solution, crude brine after refining action passes through primary filter
and mechanical impurities particle size 1mm are separated, and then it enters inorganic membrane brine
filter. Inorganic membrane brine filter adopts inorganic membrane tube(the membrane pore size standard
is 50nm, pore size ranges between 3050nm, average pore size is 40nm)as the filter component,
"cross-flow" filtration as the way to filtrate suspended particles after refining action, insuring the brine
reach the technological requirements of SS content less than 0.5ppm, Mg2+ content less than 0.5ppm.
The control of clear liquid flow in inorganic membrane brine filter when filtrating is by adopting
artificially setting required flow valve, then control system automatically detects actual flow valves of
filter first, second and third-level components; by changing each level 's clear liquid regulating valve's
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YTSJ/CZ0120-2014
Purified Brine Operation Manual
opening to realize the control of each level's clear liquid flow value meeting the specified value, thus
realizing automatic control of clear liquid flow, i.e., electromagnetic flowmeter transmitter's signals at
inorganic membrane brine filter primary, second and third-level components' outlets are connected into
controller, according to the change between the specified flow and detected flow, the controller
respectively control the opening of first, second and third-level components' outlet regulating valves, then
change the outlet backpressure of each level's component, by changing the permeate side backpressure to
realize flow change of inorganic membrane brine filter outlet, thus reaching the purpose of stabilizing the
filtering flow of inorganic membrane brine filter.
The backflushing of inorganic membrane brine filter is proceeded by PLC automatic control.
Chemical cleaning is manually operated after machine halt.
2Position Tasks
Production tasks of this position are: After the refining action, mechanical impurities in brine
separated by brine primary filter are filtrated by inorganic membrane brine filter, ridding Mg(OH)2
CaCO3 SS and other substances, thus to obtain purified brine meeting the requirements.
YTSJ/CZ0120-2014
Purified Brine Operation Manual
mud pool, and the rest returns to membrane filtration circulating pump inlet, mixed with crude brine sent
by feed pump(P0102ab) to adjust feed liquid's solid-to-liquid ratio, realizing the purpose of stabilizing
system circulating feed liquid solid content and guaranteeing membrane surface flow rate. Crude brine
after mixture passes filtration circulating pump(P0103) returns to inorganic membrane brine filter(N0102)
to circulate and filtrate. Refined brine filtrated by each level's filtration component is sent out by inorganic
membrane brine filter(N0102) each level's clear liquid outlet to refined brine buffer tank outside battery
limit.
After long-time operation, inorganic membrane brine filter(N01020's flux will change and filtering
ability will decline because of pollution on membrane surface, and then regeneration should be proceeded
on membrane surface to recover membrane flux, making its filtering ability reach the initial state. Ways to
regenerate include physical backflushing and chemical cleaning. Physical backflushing adopts refined
brine after filtration to instantaneously back flush membrane surface in backflushing tank(V0107) after
being pressurized by compressed air, thus pollutant attached on membrane surface is cleared away and
filtering ability is recovered; chemical cleaning adopts 10%~15% hydrochloric to chemically clean the
membrane, making the membrane surface thoroughly clear and completely recover filtering flux.
Technological process is shown in flow charts one and two.
300310
Na2CO3(g/L)
0.30.5
NaOH(g/L)
0.10.3
Temperature
5060
Flowm3/h
23
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Purified Brine Operation Manual
5.
Serial
Control
Control index
number
point
Person in
Control times
method
charge
I. Temperature
1
55-65
Operator
5060
Operator
0.6
Operator
0.3
Pressure gage
1 time/hour
Operator
0.4
Pressure gage
1 time/hour
Operator
0.35
Pressure gage
1 time/hour
Operator
1 time/hour
Operator
II. PressureMPa
Air duct pressure entering
1
this process
Inorganic
membrane
pressure
Inorganic
membrane
outlet pressure
Inorganic membrane brine
filter
first-level
inlet
pressure
Inorganic membrane brine
filter
third-level
outlet
pressure
0.16
Pressure gage
0.6
Operator
Concentration
1Intermediate pool outlet liquid
NaCl
300310g/l
Titration
1 time/2 hours
Analyst
NaOH
0.10.3g/l
Titration
1 time/4 hours
Analyst
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YTSJ/CZ0120-2014
Purified Brine Operation Manual
Serial
Control
Control index
number
point
Person in
Control times
method
charge
Na2CO3
0.30.5g/l
Titration
1 time/4 hours
Analyst
NaClO
25-40ppm
Titration
1 time/4 hours
Analyst
300310g/l
Titration
1 time/8 hours
Analyst
0.5mg/l
Titration
1 time/8 hours
Analyst
NaOH
0.10.3g/l
Titration
1 time/8 hours
Analyst
Na2CO3
0.30.5g/l
Titration
1 time/8 hours
Analyst
NaClO
2540ppm
Titration
1 time/4 hours
Analyst
0.5mg/l
Gravimetry
1 time/day
Analyst
Frequently
Operator
SS
Concentrated solution solid
Specific
5~10%wt
content
gravity
10-15%
Titration
Analyst
washing
12%
5%
5%
Liquid level
Intermediate
pool
level
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1/2
Frequently
Operator
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Purified Brine Operation Manual
6Operational approach
6.1
6.1.1. To check linkage test record and rectification record, to prepare to start up only when it is ensured
that actual situation and technological process are correct.
6.1.2. To prepare refining agent according to specification.
6.1.3 To transport qualified light brine to salt dissolving pool, after salt dissolving saturated, add refining
agent when it passes through baffling tank, and then it overflows to intermediate pool. To normally add
sodium hydroxide when crude brine enters intermediate pool.
6.1.4
When the intermediate pool liquid level reaches 1/2, to analyze sodium carbonate and sodium
hydroxide's excess of caustic soda quantity, free chlorine content in crude brine.
6.1.5 When crude brine enters brine primary filter, notice and frequently discharge the mechanical
impurities and salty mud in brine primary filter, to keep the filter interior clean and tunnels unblocked.
6.1.6 When controlling each index to reach technological requirement, it needs to open filter venting valve
KV107, filter exhaust valve GV111, filter feed valve GV101, concentrated solution return valve GV102,
and open membrane filtration circulating pump's terminal valve, start membrane filtration feed pump to
feed inorganic membrane brine filter liquid; when inorganic membrane brine filter is filled with feed
liquid(after no gas discharge in venting pipe sight glass),close filter venting valve KV107, filter exhaust
valve GV111,close membrane filtration circulating pump's outlet valve, start membrane filtration
circulating pump, and slowly open membrane filtration circulating pump's outlet valve.
6.1.7 To check filter operational state, according to technological requirements to adjust filter inlet, outlet
pressure and temperature, set each level component's clear liquid flow value, open clear liquid discharge
valves GV106, GV108, take samples to detect refined brine's index, discharge disqualified filtered brine to
salty mud pool, after the filtered brine is qualified, close clear liquid discharge valves GV106, GV108,
click on PLC automatic operation and fine tune each operating parameter, send qualified brine to refined
brine buffer tank.
6.1.8 To control the solid concentration ( solid-to-liquid ratio ) of concentrated liquid in inorganic
membrane brine filter, it requires solid volume ratio to lie between 30% ~ 40%, control methods are to
adjust concentrated solution discharge valve( FIT103) to control concentrated brine flow to salty mud tank,
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Purified Brine Operation Manual
to increase concentrated solution discharge flow (FIC103) when solid content is high, and to reduce
concentrated solution discharge flow when solid content is low.
6.1.9 To adjust refining agent quantity added, and to take samples to analyze, making it under the control
of specified index.
6.1.10 Adjustment is operated under the specified clear liquid flow.
6.2 Start-up after Shut-off
Procedures of restart-up after shut-off are the same as 6.1.36.1.46.1.56.1.66.1.76.1.86.1.9
6.1.10.
6.3
Normal operation
To proceed operation control according to technological operation index, to proceed inspection tour
with fixed time, to find out and handle various abnormal conditions and problems in time.
6.4 Shut-off
6.4.1 Normal shut-off is proceeded according to the following procedures:
To adjust crude brine flow sent to intermediate pool, to click on PLC stop operation, to entirely open
concentrated solution discharge valve(FIT103) for 5 minutes and then to close membrane filtration
feed pump, after stabilization of inorganic membrane brine filter's each-level pressure, to shut off
membrane filtration feed pump.
1) To close inorganic membrane brine filter's filter feed valve GV101, concentrated solution return
valve GV102,to open inorganic membrane brine filter's discharge valves GV105, GV106,
GV107, GV108, component lower permeate side valve GV110a~1, filter venting valves GV112,
KV107, to slowly open clear liquid side venting valves GV113,GV114 and later to discharge to
salty mud pool valve, to completely discharge the brine in inorganic membrane brine filter to
salty mud pool.
2) Brine is to be drained in pipelines, brine primary filter.
3) To close all the valves of inorganic membrane brine filter except first-level liquid collecting
chamber discharge valve GV105, filter exhaust valve GV111, filter venting valve KV107, to
slowly open refining brine liquid inlet valve GV104, to send refined brine to inorganic
membrane brine filter to wash, and to discharge from first-level liquid collecting chamber
discharge valve GV105 to salty mud pool, to close filter venting valve KV107, filter exhaust
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Purified Brine Operation Manual
valve GV111 after the equipment is filled with feed liquid, after washing over the salty mud in
equipment( the measurement of inorganic membrane brine filter's PH value is refined brine's PH
value or discharge header pipe sight glass brine is clear), to close refined brine liquid inlet valve
GV104, to open filter venting valve KV107, filter venting valves GV112, Kv107, second and
third-level liquid collecting chamber discharge valve GV107, discharge brine in inorganic
membrane brine filter outside the system.
6.4.2.
Emergent shut-off
If electricity suddenly shuts down, it needs to immediately close each pump's inlet and outlet valves.
Other procedures are operated as 2),3) of normal shut-off procedures.
6.5
Cleaning operation
Cleaning process is divided in primary washing, acid washing and secondary washing these three
steps. After inorganic membrane brine filter in operation for a period of time, membrane pollution causes
membrane components filtration pressure increase, filtering flux decrease, at this time filtration ability can
rapidly recover by cleaning. The cleaning cycle interval is 14~15 days.
6.5.1 Primary washing
Primary washing is usually operated immediately after shut-off of inorganic membrane brine filter,
specific washing procedures are to be seen in 2), 3) of normal shut-off procedures.
6.5.2
6.5.2.1
Acid washing
To detect acid washing solution concentration in acid washing solution tank, to control
YTSJ/CZ0120-2014
Purified Brine Operation Manual
GV107, GV108 to discharge acid washing solution to acid washing solution tank, and then acid washing is
finished.
6.5.3
Secondary washing
6.5.3.1 To open filter venting valve KV107, exhaust valve GV111, first-level liquid collecting chamber
discharge valve GV105 and relative valves from discharge header pipe to salty mud pool, to slowly open
refined brine inlet valve GV104 to send refined brine to inorganic membrane brine filter to wash. After the
equipment is filled with feed liquid, to close filter venting valve KV107, exhaust valve GV111, from
first-level liquid collecting chamber discharge valve (GV105) to discharge to salty mud pool, after the
exhaust of washing brine in equipment, to close refined brine inlet valve, to open filter venting valves
GV112, KV107, discharge valves GV105, GV106, GV107, GV108, to discharge washing brine outside the
system.
6.5.3.2 According to actual situation to adopt different medium ( industrial water or light brine) to fill filter
to prevent freezing phenomena. Before start-up, to discharge medium filled in filter, to close all the valves,
keeping inorganic membrane brine filter in start-up standby state.
Notes: Valve codes to be seen in Figure Three
6.7
Serial
Reasons
Treating methods
Number
1
Low NaCl concentration in 1. Too low salt bed in salt dissolving tank
crude brine
height
2-
3. To clean in time
2+
High Ca Mg
2+
content in 1.Too low excess of caustic soda in brine, especially Na2CO3 content 1.To properly increase excess of
refined brine
is too low
caustic soda
2.
temperature around 55
To
carefully
3. To control flow
3
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1. To contact to dispose
control
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Purified Brine Operation Manual
Serial
Phenomenon
Reasons
Treating methods
Number
4
1. Bad heat perseveration, salt crystallization when temperature is 1. Good heat perseveration work
low
2.To
properly
reduce
concentration
brine
according
to
actual situation
3. To reduce chlorate, SO42content in brine
Too high pressure at inorganic 1. Primary filter leak causes inorganic membrane channel clogging 1.
inlet
channels
2.
to
increase
backflushing frequency
6
excess of standard
7.2
YTSJ/CZ0120-2014
Purified Brine Operation Manual
It adopts concentrated solution's solid content comes out of inorganic membrane brine
filter to adjust inorganic membrane brine filter concentrated solution discharge flow, then
to control filter concentrated solution's solid content, i.e., according to concentrated
brine's solid content (manually measured) to intervene concentrated solution's discharge
flow. To connect inorganic membrane concentrated brine electromagnetic flow meter
transmitter's signal into controller, then controller controls former concentrated solution
discharge's automatic regulating valves' opening according to flow value has been set,
then change concentrated brine flow to be discharged, thus achieve the purpose of stably
control inorganic membrane brine filter circulating brine's solid content.
7.5 Inorganic membrane brine filter's backflushing automatic control
Join up inorganic membrane brine filter's inlet pressure signal up to controller, to
control backflush valve and out-coming liquid's opening, closing and switching, thus to
realize the automatic backflushing and automatic control in operation of inorganic
membrane brine filter.
Inorganic membrane brine filter's backflushing automatic control adopts special PLC
controller to control.
7.6
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Standard
Type
Quantity
Function
Status
KV101
DN80
Ball valve
Backflush
FIC101
DN80
Ball valve
Disconnect
On when filtering
KV102
DN80
Ball valve
Backflush
FIC102
DN80
Ball valve
Disconnect
On when filtering
KV107
DN50
Ball valve
Vent
KV108
DN40
Ball valve
Exhaust
KV109
DN40
Ball valve
Exhaust
FIC103
DN25
Globe valve
Simple description
On when
backflushing
Off when
backflushing
On when
backflushing
Off when
backflushing
On when
equipments start,
stop
Off when in high
liquid level
On when in high
liquid level
Feed temperature
Temperature of crude brine entering inorganic membrane brine filter to be controlled
between 5060
SSCa2+ Mg2+ control in inorganic membrane brine filter's clear liquid (refined
8.2
brine)
After filter be in operation by rule, adjust process control parameters and frequently
check to make it operate under the best condition, if you find SSCa2+ + Mg2+ content exceed
the standard, the you should judge according to the specific situation of clear liquid(refined
brine):
1Turbid, to immediately stop inorganic membrane brine filter's automatic operation,
singly open component low permeate side discharge valve GV110, clear liquid discharge
valve GV105, GV108 valve for sampling inspection, after detecting disqualified components,
shut off according to the procedures in 6.4.1, then replace the disqualified components.
2 Brine is not turbid, to immediately check whether refining agent added and
intermediate pool's excess of caustic soda, temperature and other process parameters satisfy
process requirements:
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Purified Brine Operation Manual
brine filter concentrated solution's solid content change, to strictly control solid content
between 5~10%wt, no more than 12%, to prevent density increase which leads to poor
liquidity and then causes clogging of filter channels, if you find solid content is high, you can
properly increase concentrated solution discharge flow to shorten the reaction period; on the
contrary, you can properly reduce concentrated solution discharge flow.
8.4
about 0.35 MPa, it can be realized by regulating inorganic membrane filter feed pump's
frequency converting control, meanwhile, pay attention to observing front and back backflush
valves' opening change, valves' opening change under same condition but different time as
well as flow change curve.
After system operation is normal, observe first-level inlet pressure, observe whether
pressure change is normal, and stabilize in the range of <0.35MPa, if pressure continues to
rise, to analyze reasons: 1)detect whether concentrated solution's solid content >10%,
if >10%, increase concentrated solution discharge until concentrated solution solid content is
about 5%; 2)observe pressure change before and after backflushing, if there is no change,
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Purified Brine Operation Manual
then you can properly shorten the reaction period; 3) observe valve's opening change in the
same backflush cycle of operation process, whether it can keep stable, if valve opening
continues to increase, then shorten the backflush cycle.
If methods mentioned above still cannot reduce first-level inlet valve pressure(operating
under the consistent pressure >0.4MPa is not allowed), then you should shut off to clean.
After system operation is normal, observe first and second, third-level valve opening's
cycle change tendency, with increase of time, if backflush front valve's opening continues to
rapidly increase in same time periods of different backflush cycles, then shorten backflush
time interval until valve's opening keep almost the same in same time periods of different
backflush cycles.
8.5
opening and already set outlet flow change of each level component, to set backflush cycle to
realize stable operation of inorganic membrane brine filter.
8.6
Shut-off procedures
To open vent valve and discharge valve after shutting off, drain all the feed liquid in
inorganic membrane brine filter, then to proceed primary washing, acid washing, secondary
washing, if not started up for a long time, it needs to immerse inorganic membrane with clear
water or light brine, then unload feed liquid in pipelines, circulating tank, primary filter.
8.7
Data recording
Pay attention to observing and recording inorganic membrane brine filter's temperature,
each level's pressure and already set outlet flow of each level's components, regulating valves'
opening, concentrated solution's solid content change.
3055
Ca2++Mg2+(mg/L)
SS(mg/L)
SO42-(g/L)
Fe2++Fe3+(mg/L)
0.1
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Purified Brine Operation Manual
10Safety production
10.1 Safety production and matters need attention
10.1.1 Strictly observe labor discipline and operation instruction, no operation against rules,
no matters nothing to do with production.
10.1.2 Staff on duty should wear labor protection appliances before entering positions, wear
rubber gloves and protective glasses when batching.
10.1.3 When dismounting sight glass and valve, you must drain residual material in inorganic
membrane brine filter, pipelines; crystal substance on sight glass is not allowed to be cleared
away by knocking.
10.1.4 When entering equipment to overhaul, you should obey chemical entering tank
criterion; first you should cut off all the inlet and outlet pipelines of equipment, clear residual
material, and wear essential labor protection appliance.
10.1.5 When working high above the ground, you must fasten the safety belt, and be guarded
with specially-assigned person, throwing objects from the high altitude is not allowed.
10.1.6 Electrical equipment should be frequently checked, to keep good insulation, put out
fire with carbon tetrachloride, stacking sundries in power distribution cabinet is not allowed.
10.1.7In the procedure of pump and conveyor maintenance, it needs specially-assigned
person to guard; pressure gage should be frequently inspected to keep sensitive state.
10.1.8 To frequently check whether liquid level alarm is out of order, if fault occurs, you
should notice instrument technician in time to overhaul, to ensure instrument be in good
condition.
10.1.9 After accident occurs, unauthorized leave is not allowed, you should report to monitor,
dispatcher in time, accident analysis should achieve "three not let off", and report to superior
department.
10.2 Labor protection
10.2.1 It is essential to wear labor protection appliance by rule strictly when in operation.
10.2.2
This procedure adopts steam heat method to dissolve salt, be careful to prevent burn;
there is caustic soda in refining agent, please wash with clear water in time when skin
accidentally touches it.
10.2.3
When working high above the ground, you must fasten the safety belt, be careful to
prevent fall.
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Purified Brine Operation Manual
Sanitation in equipment area should be divided to all the staff, each person must clean
YTSJ/CZ0120-2014
Purified Brine Operation Manual
Appendix
Attached drawing 1:Technological process diagrammatic drawing
Attached drawing 2:Technological process diagrammatic drawing
Attached drawing 3: Inorganic membrane brine filter valve bit number drawing
Attached table 1: Inorganic membrane brine filter valve bit number table
Attached table 2: Inorganic membrane brine filter valve state table
Attached table 3: Inorganic membrane brine filter operational data record table
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