CN110372012A - A kind of embrane method total halogenated caustic production method of no solid waste discharge - Google Patents

A kind of embrane method total halogenated caustic production method of no solid waste discharge Download PDF

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CN110372012A
CN110372012A CN201910591512.2A CN201910591512A CN110372012A CN 110372012 A CN110372012 A CN 110372012A CN 201910591512 A CN201910591512 A CN 201910591512A CN 110372012 A CN110372012 A CN 110372012A
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brine
salt
sodium chloride
comparatively high
earth containing
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石风强
尹燕亓
庆珺
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Ma'anshan Xingqida New Material Technology Co Ltd
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Ma'anshan Xingqida New Material Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00—Halides of sodium, potassium or alkali metals in general
    • C01D3/04—Chlorides
    • C01D3/06—Preparation by working up brines; seawater or spent lyes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00—Halides of sodium, potassium or alkali metals in general
    • C01D3/14—Purification
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
    • C25B1/46—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in diaphragm cells

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The present invention relates to a kind of embrane method total halogenated caustic production methods of no solid waste discharge, it includes the following steps: that brine is sent into organic tubular type membranous system after refining reaction and is filtered, filtered permeate is divided into two parts, and a portion permeate obtains low salt made from earth containing a comparatively high percentage of sodium chloride water and high salt made from earth containing a comparatively high percentage of sodium chloride water after denitration process；Another part permeate is mixed with the resulting low salt made from earth containing a comparatively high percentage of sodium chloride water of step S1, obtains primary brine；Caustic soda and light salt brine is made after adsorbing, then through ionic membrane alkaline system in primary brine.The application directly carries out denitration to saturated bittern using alkali resistant nanofiltration membrane, compared with tradition is first diluted with water again salt dissolving to the technique being saturated, has saved salt consumption, the steam consumption, water consume, has substantially reduced denitration cost；And by high salt made from earth containing a comparatively high percentage of sodium chloride water and Mg (OH)2、CaCO3Mud infuses well processing, solves high salt made from earth containing a comparatively high percentage of sodium chloride water problem of outlet, also thoroughly solves the problems, such as that salt slurry is subsequent intractable.

Description

A kind of embrane method total halogenated caustic production method of no solid waste discharge
Technical field
The invention belongs to salt refining technical fields, and in particular to a kind of embrane method total halogenated caustic production method of no solid waste discharge.
Background technique
Currently, domestic chlor-alkali industry mainly uses ionic membrane method alkaline, using saturated brine as raw material, electrolysis generates hydroxide The products such as sodium, if containing the impurity such as a large amount of calcium, magnesium in salt water, calcium and magnesium ion can in electrolytic process with the OH on anode-Instead Insoluble matter should be generated to be deposited on ionic membrane, seriously affect service life of ion-exchange membrane, therefore, salt refining is produced in ionic membrane method alkaline It is particularly important in the process.
Traditional primary refined brine work of the country based on " barrel type reactor+dongle settling tank+sand filter " process route Skill is eliminated substantially, currently, domestic chlor-alkali enterprises are mainly used to there is following two membrane filtration process: gore film, HVM film is generations The organic microfiltration membrane process and ceramic membrane crossflow filtration technique of table.
New varieties of organic tubular membrane as membrane separation technique, the runner for having both tubular membrane is wide, cross-flow filtration and organic film Mature preparation process the advantages that, since the advent of the world is concerned, be widely used at present juice clarification, external MBR, processing, the reuse of spent acid lye and sewage treatment project of oil field reinjection water etc..Organic tubular membrane refined brine technique is one Kind makes full use of tubular membrane to carry out the salt water electric process for refining of high efficient solid and liquid separation effect, is by being added in salt water first Sodium hydroxide, sodium carbonate refining agent make the calcium ions and magnesium ions in salt water generate precipitating, then efficiently separating by tubular membrane component Effect make sediment and water quickly, be completely separated, effluent quality is strengthened.
Country's salt water, which removes nitre conventional method, at present barium chloride method, calcium method, freezing, embrane method.Wherein embrane method denitration conduct A kind of emerging denitration technology removes the sulfate ion in salt water, tool using nanofiltration membrane to divalent ion crown_interception There is the advantages that operation energy consumption is low, occupied area is small, does not introduce third component, cleanliness without any pollution.Currently, domestic chlor-alkali enterprises only will Embrane method is used for light salt brine denitration, and cannot be used for high concentration salt water (NaCl > 260g/L) denitration process.Therefore, de- for brine Nitre, this requires must first add water from the saturated bittern of underground mining out to reduce wherein NaCl content, again through salt dissolving after denitration Technique increases NaCl content, low efficiency.In addition, calcium ions and magnesium ions content is higher in brine, domestic chlor-alkali enterprises mainly use two alkali Method removal, by the way that NaOH, Na are added into brine2CO3, reaction generation Mg (OH) 2、CaCO3Then solid matter is cut by film Concentrate is stayed in, then salt slurry is extruded by filter press, salt slurry send to the external world and handles, but salt slurry subsequent processing is also more and more difficult.
Summary of the invention
The purpose of the present invention is to provide a kind of embrane method total halogenated caustic production methods of no solid waste discharge, and organic tubular membrane is gone Removing calcium and magnesium and nanofiltration membrane denitration combine the total Halogenated Caustic Production for carrying out salt refining, which is directly used in nanofiltration full With the denitration of brine, and thoroughly solve the problems, such as that salt slurry is intractable.
Specific technical solution is as follows:
A kind of embrane method total halogenated caustic production method of no solid waste discharge, includes the following steps:
S1, brine are sent into organic tubular type membranous system after refining reaction and are filtered, and filtered permeate is divided into two parts, Middle a part of permeate obtains low salt made from earth containing a comparatively high percentage of sodium chloride water and high salt made from earth containing a comparatively high percentage of sodium chloride water after denitration process；
S2, another part permeate are mixed with the resulting low salt made from earth containing a comparatively high percentage of sodium chloride water of step S1, obtain primary brine；
Caustic soda and light salt brine is made after adsorbing, then through ionic membrane alkaline system in S3, primary brine.
Further scheme is sent into subsider, sedimentation through the filtered concentrate of organic tubular type membranous system in the step S1 After 0.5-2h, subsider middle and upper part clear liquid returns to organic tubular type membranous system reprocessing.
Further scheme, the mud of the sedimentation trench bottom infuse well after mixing with the high salt made from earth containing a comparatively high percentage of sodium chloride water, light salt brine.
Further scheme, NaCl content is 290~310g/L in brine described in step S1.
Further scheme, refining reaction described in step S1 is that brine to be processed is first sent into baffling slot, in baffling slot In metered refining agent and degradation agent, when being then introduced into reaction container row react.
Further scheme, the refining agent are NaOH and Na2CO3, the degradation agent be NaClO, wherein NaClO plus Entering amount is 10-50mg/L.
Specifically, NaOH, Na is added into the brine that NaCl content is 290~310g/L2CO3Refining agent, NaOH additional amount For with Mg2+Excessive 0.1~0.3g/L, Na after reaction2CO3Additional amount is and Ca2+Excessive 0.3~0.5g/L after reaction；Degradation agent The additional amount of NaClO is 10-50mg/L.
Further scheme, denitration process described in step S1 be first will transmit through liquid be adjusted to pH value be 7-9, ORP < 0mV, Then the alkali resistant nanofiltration membrane that pH value is 7-9 is re-fed into be handled.
HCl, Na are added in the permeate for further scheme2SO3To adjust its pH value and ORP.
Further scheme, the content of sulfate radical reaches 5g/L in primary brine described in step S2.
Two parts will be divided into through organic filtered permeate of tubular type membranous system in the application, be due to after denitration process Low glass gall sulfate radical content is low (generally less than 5g/L), and sulfate radical content height (generally higher than 5g/L) in permeate, and mixes Primary brine will carry out resin adsorption afterwards, it requires that wherein sulfate radical content is 5-7g/L, so organic tubular type membranous system mistake Permeate after filter will be divided into two parts and be blended.
Denitration process is using alkali resistant nanofiltration membrane, and operation pH range is 7-9, so will transmit through liquid is adjusted to pH value It for 7-9, ORP < 0mV, is then re-fed into alkali resistant nanofiltration membrane and is handled, to meet into film requirement.
The present invention directly filters the salt water after refining reaction using organic tubular type membranous system, the Mg that reaction is generated (OH)2Colloid, CaCO3The impurity such as the suspended matter carried in precipitating and salt water removal, through the refined brine of organic tubular type membranous system Middle Ca2+、Mg2+Total content < 1mg/L, SS < 0.5mg/L.
Organic tubular membrane system structure in the application is made of as disclosed in CN109133112A 1~10 group of membrane stack, Every group of membrane stack series connection 3-8 props up organic tubular membrane component, and filter type is interior press filtration, 0.1 ~ 0.6MPa of operating pressure, film surface stream Fast 1m/s-3m/s.Membrane module diameter is 6 inches, 8 inches or 10 inches, and membrane module length is 3m or 4m.Organic tubular membrane component It is encapsulated in putamina sealant and is formed by more organic tubular type membrane tube both ends, membrane channels diameter is 5mm or 8mm, membrane aperture 10- 50nm, membrane material are Kynoar, polyether sulfone, polysulfones or polyacrylonitrile.
Organic tubular membrane is applied to salt refining field as a kind of novel technology, has the advantages that filtering accuracy Height, pore-size distribution are narrow, and obtained brine quality is higher, quality is more stable；Membrane tube is not broken, good airproof performance；It is logical with broader film Road, channel will not block；Stronger contamination resistance, the chemical cleaning period is long, easy cleaning；
The application directly carries out denitration to saturated bittern using alkali resistant nanofiltration membrane, is first diluted with water again salt dissolving to saturation with tradition Technique compare, saved salt consumption, the steam consumption, water consume, brine denitration cost substantially reduces；
Traditional nanofiltration denitrating system uses acid-resistant disintegration, needs that salt water pH is first adjusted to acidity, salt water pH is adjusted to alkali again after denitration Property, to meet the requirement of resin adsorption condition, cause acid, alkali consumption big.And the application nanofiltration system uses alkali resistant nanofiltration membrane, fortune Row pH range is 7-9, to save acid adding plus alkali expense.
By high salt made from earth containing a comparatively high percentage of sodium chloride water and Mg (OH) in the application 2、CaCO3Mud infuses well processing, solves high salt made from earth containing a comparatively high percentage of sodium chloride water problem of outlet, Also thoroughly solve the problems, such as that salt slurry is subsequent intractable.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention Limitation.
Embodiment 1
NaCl content 300g/L, SO from the brine that Jing Kuang is produced4 2-Content 12g/L, Ca2+Content 0.65g/L, Mg2+Content 0.07g/L is pumped directly into baffling slot, the metered sodium carbonate 2.1g/L, sodium hydroxide 0.35g/L, secondary in baffling slot Then sodium chlorate 20mg/L flows into reaction container and carries out refining reaction；Wherein, the Mg in salt dissolving2+、Ca2+Respectively with NaOH, Na2CO3 Reaction generates Mg (OH)2、CaCO3Solid matter, the crude brine after refining reaction are sent into organic tubular type membranous system, organic tubular membrane System is made of 2 groups of membrane stacks, organic tubular membrane component of 5 10 inches of diameters of every group of membrane stack series connection, length 4m, organic tubular membrane Channel 5mm, aperture 30nm, membrane material are Kynoar；It controls operating pressure 0.3MPa, crossflow velocity 1.5m/s, instead The Mg (OH) that should be generated2Colloid, CaCO3The impurity such as the suspended matter carried in precipitating and salt water are trapped, through organic tubular membrane Ca in the refined brine of system2+、Mg2+Total content 0.65mg/L, SS=0.36mg/L；
HCl, Na is added in a part of permeate2SO3It adjusts pH=9, be sent into alkali resistant nanofiltration membrane system after ORP < 0mV, through receiving SO in the low salt made from earth containing a comparatively high percentage of sodium chloride water of filter membrane4 2-Content 1.5g/L, SO in the high salt made from earth containing a comparatively high percentage of sodium chloride water being trapped4 2-Content 42g/L, low salt made from earth containing a comparatively high percentage of sodium chloride water and remainder Permeate mixing after obtain primary brine, make wherein SO4 2-Content 7g/L adsorbs to obtain secondary brine using chelate resin, It is sent into ionic membrane alkaline system, caustic soda and light salt brine is made；
The concentrate of organic tubular membrane retention is sent into subsider, residence time 1h, and upper part clear liquid returns to organic tubular type membranous system Reprocessing, bottom mud (solid content 5%) infuse well after mixing with high salt made from earth containing a comparatively high percentage of sodium chloride water, light salt brine.
Embodiment 2
NaCl content 295g/L, SO from the brine that Jing Kuang is produced4 2-Content 18g/L, Ca2+Content 1.32g/L, Mg2+Content 0.18g/L is pumped directly into baffling slot, metered sodium carbonate 4g/L, sodium hydroxide 0.9g/L, sodium hypochlorite in baffling slot Then 30mg/L flows into reaction container and carries out refining reaction；Wherein, the Mg in salt dissolving2+、Ca2+Respectively with NaOH, Na2CO3Reaction life At Mg (OH)2、CaCO3Solid matter, the crude brine after refining reaction are sent into organic tubular type membranous system, and organic tubular type membranous system is by 4 Group membrane stack composition, organic tubular membrane component of 6 10 inches of diameters of every group of membrane stack series connection, length 4m, organic tubular type membrane channels 8mm, aperture 50nm, membrane material are Kynoar.Organic tubular membrane controls operating pressure 0.35MPa, crossflow velocity 2m/s, React the Mg (OH) generated2Colloid, CaCO3The impurity such as the suspended matter carried in precipitating and salt water are trapped, through organic tubular type Ca in the refined brine of membranous system2+、Mg2+Total content 0.65 mg/L, SS=0.43mg/L；
HCl, Na is added in a part of permeate2SO3It is sent into alkali resistant nanofiltration membrane system after adjusting pH=8.5, ORP < 0mV, is penetrated SO in the low salt made from earth containing a comparatively high percentage of sodium chloride water of nanofiltration membrane4 2-Content 2g/L, SO in the high salt made from earth containing a comparatively high percentage of sodium chloride water being trapped4 2-Content 45g/L, low salt made from earth containing a comparatively high percentage of sodium chloride water and remainder Permeate mixing after obtain primary brine, make wherein SO4 2-Content 5g/L adsorbs to obtain secondary brine using chelate resin, It is sent into ionic membrane alkaline system, caustic soda and light salt brine is made；
The concentrate of organic tubular membrane retention is sent into subsider, residence time 0.5h, and upper clear supernate returns to organic tubular type membranous system Reprocessing, bottom mud (solid content 6%) infuse well after mixing with high salt made from earth containing a comparatively high percentage of sodium chloride water, light salt brine.
Embodiment 3
NaCl content 295g/L, SO from the brine that Jing Kuang is produced4 2-Content 13g/L, Ca2+Content 0.86g/L, Mg2+Content 0.1g/L is pumped directly into baffling slot, metered sodium carbonate 2.7g/L, sodium hydroxide 0.53g/L, sodium hypochlorite in baffling slot Then 20mg/L flows into reaction container and carries out refining reaction；Wherein, the Mg in salt dissolving2+、Ca2+Respectively with NaOH, Na2CO3Reaction life At Mg (OH)2、CaCO3Solid matter, the crude brine after refining reaction are sent into organic tubular type membranous system, and organic tubular type membranous system is by 1 Group membrane stack composition, organic tubular membrane component of 48 inches of diameters of every group of membrane stack series connection, length 3m, organic tubular type membrane channels 5mm, Aperture is 30nm, and membrane material is Kynoar.Operating pressure 0.3MPa is controlled, crossflow velocity 1.8m/s reacts the Mg of generation (OH)2Colloid, CaCO3The impurity such as the suspended matter carried in precipitating and salt water are trapped, through the refined salt of organic tubular type membranous system Ca in water2+、Mg2+Total content 0.74 mg/L, SS=0.38mg/L；
HCl, Na are added in a part of permeate2SO3It is sent into alkali resistant nanofiltration membrane system after adjusting pH=9, ORP < 0mV, thoroughly Cross SO in the low salt made from earth containing a comparatively high percentage of sodium chloride water of nanofiltration membrane4 2-Content 1g/L, SO in the high salt made from earth containing a comparatively high percentage of sodium chloride water being trapped4 2-Content 40g/L, low salt made from earth containing a comparatively high percentage of sodium chloride water with it is remaining Under permeate mixing after obtain primary brine, make wherein SO4 2-Content 5g/L adsorbs to obtain secondary salt using chelate resin Water is sent into ionic membrane alkaline system, and caustic soda and light salt brine is made；
The concentrate of organic tubular membrane retention is sent into subsider, residence time 0.5h, and upper clear supernate returns to organic tubular type membranous system Reprocessing, bottom mud (solid content 5%) infuse well after mixing with high salt made from earth containing a comparatively high percentage of sodium chloride water, light salt brine.
Comparative example
Former halogen NaCl content 300g/L, SO produced from Jing Kuang4 2-Content 12g/L, Ca2+Content 1.30g/L, Mg2+Content 0.32g/L is pumped directly into baffling slot, metered sodium carbonate 4g/L, sodium hydroxide 1.3g/L, sodium hypochlorite in baffling slot Then 20mg/L flows into reaction container, wherein the Mg in salt dissolving2+、Ca2+Respectively with NaOH, Na2CO3Reaction generates Mg (OH)2、 CaCO3Solid matter, the crude brine after refining reaction are sent into ceramic membranous system, react the Mg (OH) of generation2Colloid, CaCO3Precipitating And the impurity such as suspended matter carried in salt water are trapped, Ca in the refined brine of permeation ceramic membrane system2+、Mg2+Total content 1.24mg/L,SS=0.96mg/L；
Soft water is added in wherein a part of permeate, NaCl content is diluted to 260g/L and then plus HCl, Na2SO3Adjust pH =6, it is sent into nanofiltration membrane system after ORP < 0mV, through SO in the low salt made from earth containing a comparatively high percentage of sodium chloride water of nanofiltration membrane4 2-Content 2g/L, the high salt made from earth containing a comparatively high percentage of sodium chloride being trapped SO in water4 2-Content 40g/L, low glass gall is using being steam heated to 60 DEG C, then salt dissolving is to NaCl content 300g/L, salt dissolving water with it is remaining Primary brine is obtained after lower transmission mixing, makes wherein SO4 2-Content 5g/L is adsorbed to obtain secondary brine using chelate resin, be sent Enter ionic membrane alkaline system, caustic soda and light salt brine is made；
Ceramic membranous system concentrate carries out filters pressing processing, and salt slurry outward transport is used as fixed-end forces, and pressing filtering liquid returns to preamble workshop section and locates again Reason.Well is infused after high salt made from earth containing a comparatively high percentage of sodium chloride water, light salt brine mixing.
Acid-resistant disintegration is used in comparative example, needs that salt water pH is first adjusted to acidity, salt water pH is adjusted to alkalinity again after denitration, with Meet the requirement of resin adsorption condition, causes acid, alkali consumption big.The embodiment of the present application 1-3 is using alkali resistant nanofiltration membrane directly to full Denitration is carried out with brine, compared with tradition is first diluted with water again salt dissolving to the technique being saturated, has saved salt consumption, the steam consumption, water consume, salt Water denitration cost substantially reduces；In addition, the application simple process, and be by high salt made from earth containing a comparatively high percentage of sodium chloride water and Mg (OH) 2、CaCO3Mud note Well processing, solves high salt made from earth containing a comparatively high percentage of sodium chloride water problem of outlet, also thoroughly solves the problems, such as that salt slurry is subsequent intractable.

Claims (9)

1. a kind of embrane method total halogenated caustic production method of no solid waste discharge, characterized by the following steps:
S1, brine are sent into organic tubular type membranous system after refining reaction and are filtered, and filtered permeate is divided into two parts, Middle a part of permeate obtains low salt made from earth containing a comparatively high percentage of sodium chloride water and high salt made from earth containing a comparatively high percentage of sodium chloride water after denitration process；
S2, another part permeate are mixed with the resulting low salt made from earth containing a comparatively high percentage of sodium chloride water of step S1, obtain primary brine；
Caustic soda and light salt brine is made after adsorbing, then through ionic membrane alkaline system in S3, primary brine.
2. embrane method total halogenated caustic production method according to claim 1, it is characterised in that: through organic tubular membrane in the step S1 The filtered concentrate of system is sent into subsider, and after settling 0.5-2h, subsider middle and upper part clear liquid returns to organic tubular type membranous system Reprocessing.
3. embrane method total halogenated caustic production method according to claim 2, it is characterised in that: the mud of the sedimentation trench bottom and institute High salt made from earth containing a comparatively high percentage of sodium chloride water, the light salt brine stated infuse well after mixing.
4. embrane method total halogenated caustic production method according to claim 1, it is characterised in that: NaCl contains in brine described in step S1 Amount is 290~310g/L.
5. embrane method total halogenated caustic production method according to claim 1, it is characterised in that: refining reaction described in step S1 be by Brine to be processed is first sent into baffling slot, metered refining agent and degradation agent in baffling slot, when being then introduced into reaction container Row reaction.
6. embrane method total halogenated caustic production method according to claim 5, it is characterised in that: the refining agent is NaOH and Na2CO3, The degradation agent is NaClO, and wherein the additional amount of NaClO is 10-50mg/L.
7. embrane method total halogenated caustic production method according to claim 1, it is characterised in that: denitration process described in step S1 is first Will transmit through liquid and be adjusted to pH value is 7-9, ORP < 0mV, is then re-fed into the alkali resistant nanofiltration membrane that pH value is 7-9 and is handled.
8. embrane method total halogenated caustic production method according to claim 7, it is characterised in that: in the permeate be added HCl, Na2SO3To adjust its pH value and ORP.
9. embrane method total halogenated caustic production method according to claim 1, it is characterised in that: in primary brine described in step S2 The content of sulfate radical reaches 5g/L.
CN201910591512.2A 2019-07-02 2019-07-02 A kind of embrane method total halogenated caustic production method of no solid waste discharge Pending CN110372012A (en)

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Application publication date: 20191025