CN109455685A - A kind of method that the purification of crude product sodium pyrophosphate produces sodium dihydrogen phosphate and sodium chloride - Google Patents
A kind of method that the purification of crude product sodium pyrophosphate produces sodium dihydrogen phosphate and sodium chloride Download PDFInfo
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- CN109455685A CN109455685A CN201811618894.5A CN201811618894A CN109455685A CN 109455685 A CN109455685 A CN 109455685A CN 201811618894 A CN201811618894 A CN 201811618894A CN 109455685 A CN109455685 A CN 109455685A
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- sodium
- crude product
- sodium chloride
- dihydrogen phosphate
- pyrophosphate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
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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
Abstract
The invention discloses the methods of a kind of phosphorous brine waste by-product crude product sodium pyrophosphate purification production sodium dihydrogen phosphate such as glyphosate mother solution and sodium chloride product.The Special use method that crude product sodium pyrophosphate mixed solution dispersibility and process water are improved using oxidisability auxiliary agent is improved phosphoric acid, improves crystallization effect.Orthophosphoric acid sodium salt and sodium chloride are extracted using the dissolubility difference of sodium pyrophosphate in crude product sodium pyrophosphate and its hydrolysate, sodium chloride under different temperatures, pH value condition and promoter effect.Production process solution rate is fast, and product quality is excellent, and wastewater flow rate is small, and environmental protection treatment cost declines to a great extent, and has reaction advantage, environment-friendly advantage, quality-advantage, cost advantage.
Description
Technical field
The invention belongs to three-protection design production technical field, the high sodium chloride such as specially a kind of glyphosate mother solution is phosphorous useless
The refining methd for the crude product sodium pyrophosphate that water is obtained in burning or high-temperature oxydation, is particularly suitable for glycine method or IDA method grass is sweet
Phosphine mother liquor burns or the purification of high-temperature oxydation gained crude product sodium pyrophosphate.
Background technique
Glyphosate mother solution processing is professional problem, either glycine method or IDA method production glyphosate, mother liquor
All has the characteristics that high COD, high TP, with high salt, complicated component, difficult to degrade, processing difficulty is very big, at high cost.Mainstream mother liquor at present
Treatment process be using oxidizing process degradation mother liquor and recycling P elements, mainly have incineration method, high-temperature oxidation, medium temperature oxidizing process,
Low-temperature oxidation method etc. also passes through membrane separation technique or evaporation and concentration recycling sodium chloride and phosphate during mother liquid disposal.
Such as: UF membrane recycles sodium chloride and glyphosate and other substances, is concentrated by evaporation recycling glyphosate and sodium chloride, and concentration is female
Liquid orientation conversion recycling sodium pyrophosphate, mother liquor catalytic oxidation recycle phosphate, etc..Every kind of method has superiority and inferiority, and several grass are sweet
Mainly different treatment process is respectively adopted in big producer to phosphine, and above-mentioned several techniques are combined processing by most enterprises
Glyphosate mother solution.Currently, Xingfa Group, new Anhua work, Shandong Run Fengdeng company have concentrated mother liquor orientation conversion production burnt
The device of sodium phosphate, the obtained main content 40-85% of burnt sodium crude product, sodium chloride content is according to the difference of each business processes technique
In 3-35% range, the also impurity such as containing sodium carbonate, sodium bicarbonate, sodium sulfite, sodium hydrogensulfite, organic phosphorus.For the road
Line, either film process desalination are still concentrated by evaporation desalination process, contain higher chlorination in final gained sodium pyrophosphate crude product
Sodium, product impurity is more, colour-difference, has peculiar smell, main content low, of poor quality, and the market price is low, and application is also restrained,
It needs further to purify, improves main content and quality.
Glyphosate mother solution processing is industry problems, to carry out glyphosate mother solution environmental protection treatment, National Industrial and information conscientiously
Change portion is organized in 2014-2017 and makes thorough investigation and study establishment " glyphosate by-product Nacl part 1: sodium chloride ", " glyphosate
By-product Nacl part 2: crude product sodium pyrophosphate ", " the 3rd part of glyphosate by-product Nacl: disodium hydrogen phosphate " professional standard
Exposure draft.And currently, the mark is not achieved in the crude product sodium pyrophosphate crude product product of most producer's prior art productions
Standard, therefore sodium pyrophosphate crude product outlet is urgently to be resolved, purification is trend of the times.
Crude product sodium pyrophosphate is refining to obtain sodium pyrophosphate by part company, but in production process, there are crude product pyrophosphoric acids
The problem of sodium dissolution is slow, dissolution fluid viscosity is big, processing capacity is small and wastewater flow rate is big, at high cost and poor product quality, phosphoric acid
Sodium chloride, organophosphorus residue amount are big in product salt, of poor quality.Such as a kind of pair of glyphosate mother solution advanced treating of CN206915770U
The system that phosphor resource afterwards is purified.A kind of method for preparing sodium pyrophosphate using crude product sodium pyrophosphate of CNIO68098llA
And a kind of crude product sodium pyrophosphate purification of CN106882781A produces the method decolourized when sodium pyrophosphate product and directly refines extraction
Sodium pyrophosphate, equally there is also the dissolutions of crude product sodium pyrophosphate during handling crude product sodium pyrophosphate slowly, dissolution fluid viscosity is big,
Device processing capacity is small and sodium pyrophosphate product in the high problem of sodium chloride content.Therefore it needs to combine material feature exploitation new
Process.
Summary of the invention
The method of crude product sodium pyrophosphate purification production orthophosphoric acid sodium salt and sodium chloride provided by the present invention, in crude product coke
In sodium phosphate subtractive process,
Using each component in crude product sodium pyrophosphate and hydrolysate under different temperatures, pH value condition and promoter effect
The characteristics of dissolving sex differernce separates orthophosphates, sodium chloride.According to market sale needs, the orthophosphates can be produced specifically
For the mixture or phosphoric acid hydrogen two of sodium dihydrogen phosphate, disodium hydrogen phosphate, tertiary sodium phosphate or sodium dihydrogen phosphate and disodium hydrogen phosphate
The mixture of sodium and tertiary sodium phosphate, the hydrated product of the specially described sodium ascorbyl phosphate can be realized by adjusting temperature, pH value etc..
It is handled using phosphoric acid and with oxidizing substance as auxiliary agent, promotes the dissolution of by-product crude product sodium pyrophosphate, hydrolysis and crystallization,
Raising crystallization effect is realized by changing phosphoric acid while removing impurity, improves the sodium matter of orthophosphoric acid sodium salt and chlorination
Amount.First sodium chloride is extracted in filtering from the mixed slurry after the dissolution of crude product sodium pyrophosphate, hydrolysis, then positive phosphorus is extracted from filtrate
Hydrochlorate.Then the sodium chloride crude product and orthophosphates crude product that extract are refined respectively.Filter device B is separating positive phosphorus
Liquor B obtained in hydrochlorate process returns to hydrolysis kettle and carries out recycled.
In traditional glyphosate mother solution treatment process, the mother liquor generated in crude product sodium pyrophosphate subtractive process usually covers past
The devices such as glyphosate mother solution mvr evaporation, multiple-effect evaporation are evaporated concentration desalination, and the mother liquor after desalination burns again, form one
Systemic circulation, the technique have the characteristics that long flow path, processing cost are high, wastewater flow rate is big.In this method production process, due to that will mention
Recycling Mother Solution set after pure phosphoric acid salt is for dissolving crude product sodium pyrophosphate, into the water in system finally with sodium orthophosphate salt water
The form for closing object is taken out of, and the enriched crystallization of the sodium chloride in crude product is also constantly precipitated, rather than reuses evaporating and concentrating process
Desalination, water removal reduce at steam consumption, cost and environmental protection so significantly reducing the consumption and waste water yield of fresh water
Manage pressure.
A kind of method that the purification of crude product sodium pyrophosphate produces sodium dihydrogen phosphate and sodium chloride product, includes the following steps:
(1) ingredient and analysis salt: crude product sodium pyrophosphate and water are mixed in hydrolysis kettle, phosphoric acid is added dropwise and controls mixed material pH value
In 0.5-4.5 range, the at a temperature of stirring 5-60min after oxidisability auxiliary agent at 70-120 DEG C, which is added, keeps crude product sodium pyrophosphate molten
Solution and hydrolysis；
Preferably, the pH value is in 4.0-4.5 range.
(2) sodium chloride Product recycling: slurry in hydrolysis kettle described in step (1) is discharged filtering while hot, obtains chlorination
Sodium product and filtrate；Hydrolysis kettle slurry is discharged filtering while hot, obtains sodium chloride product and filtrate, the filtrate main component
For water, sodium dihydrogen phosphate and sodium chloride, the filtrate sodium dihydrogen phosphate, sodium chloride, which have been satisfied, to be reached and state.
Filter residue A (i.e. sodium chloride) is washed using the liquor B 2 of the heat after heat exchanger preheating and heater are heated
Material, gained cleaning solution A are back to use hydrolysis kettle recycled.Gained sodium chloride product reaches " glyphosate by-product Nacl: chlorination
Sodium " standard.
Aforementioned sodium chloride product produces as product or further goes to sodium chloride deep refining device and further purifies.
Preferably, cleaning solution or filtrate of the sodium chloride deep refining device in purification sodium chloride product process return to hydrolysis kettle and carry out
It applies.
It is further preferred that making leaching extraction agent to obtained sodium chloride using the alcoholic solution of hydrochloric acid or alcoholic solution or hydrogen chloride
Product carries out leaching extraction purification, and the sodium chloride product through refining adjusts pH value to neutrality, sodium chloride product quality using a small amount of liquid alkaline
Better than " glyphosate by-product Nacl: sodium chloride " standard, residue of glyphosate is reduced within 0.02% (mass ratio), total phosphorus
It is reduced within 0.08%.
Preferably, the hydrochloric acid after leaching extraction is back to glyphosate mother solution postprocessing working procedures, for adjusting mother liquor pH value, simultaneously
Recycling leaching extracts phosphorus out, and leaching extracts remaining impurity out with mother liquor oxidation processes.
Preferably, the alcoholic solution evaporation recycling alcohol after leaching extraction, obtained phosphorous concentrate deoxidation recycling, the alcohol of recycling
Recycled.
Hydrochloric acid is back to glyphosate mother solution postprocessing working procedures, for adjusting mother liquor pH value, while recycling the phosphorus for soaking and extracting out,
Remaining impurity is with mother liquor oxidation processes.
The alcohol is the mixture of one or more of methanol, ethyl alcohol, propyl alcohol, isopropanol, butanol.
(3) sodium dihydrogen phosphate Product recycling: it will mix, control in mixer with alkali after the cooling of filtrate described in step (2)
Mixed solution pH value processed generates sodium dihydrogen phosphate, goes to crystallization kettle after filter filters out impurity, expecting in 4.0-7.0 range
When slurry temperature degree is down to 30-90 DEG C, water and biphosphate sodium crystal are added into crystallization kettle, later again in the case where temperature is 0-30 DEG C
Sodium dihydrogen phosphate dihydrate is precipitated in crystallisation by cooling 2-8h, and the slurry filtration after sufficient crystallising is separated, two hypophosphite monohydrates are obtained
Sodium dihydrogen product.
Mother liquor in aforementioned (3) after separation sodium dihydrogen phosphate is cold saturation phosphate solution, and sodium chloride content is close
Saturation returns to dissolution kettle and carries out recycled, continues to dissolve crude product sodium pyrophosphate.
The crude product sodium pyrophosphate is the phosphorous sodium chloride-containing waste water such as glyphosate mother solution, pmida mother liquor burned or
The sodium pyrophosphate crude product that high-temperature oxydation obtains, be grey, canescence or grey black powdery, bulk, granular mixture,
Main component is sodium pyrophosphate and sodium chloride, sodium pyrophosphate main content 40-85%, sodium chloride content 3-40%, total organic carbon
In 0.2% or so, the also impurity such as containing sodium carbonate, sodium bicarbonate, sodium sulfite, sodium hydrogensulfite, organic phosphorus.Its aqueous solution pH
Value is 10.0 or so.
The mass ratio of the crude product sodium pyrophosphate and water is 1:(0.5-2.0).The water is process water, process water
For after crystallization kettle slurry filtration filtrate and sodium chloride, sodium dihydrogen phosphate wash material, the process water in subtractive process.
The additional amount of oxidisability auxiliary agent described in the step (2) is the 0.005%- of sodium pyrophosphate crude product quality
2.5%.
Oxidisability auxiliary agent described in the step (2) is sodium perchlorate, in sodium chlorate, sodium chlorite, sodium hypochlorite
Any one or the combination of several of them.Preferred embodiment is the mixture that the oxidisability auxiliary agent is sodium chlorate and sodium hypochlorite, excellent
Its mass ratio of selection of land is 1:(0.2-1.2).
Alkali described in the step (3) is the combination of one or more of sodium hydroxide, sodium carbonate, sodium bicarbonate.
The mass ratio of the water and crude product sodium pyrophosphate is (0-5): 1.；The weight of biphosphate sodium crystal is that crude product is burnt
The 0.05-0.2% of sodium phosphate.Preferably 0.1%.
The crude product sodium pyrophosphate is that the phosphorous sodium chloride-containing waste water such as glyphosate mother solution is burned or high-temperature oxydation obtains
Sodium pyrophosphate crude product.
(4) Recycling Mother Solution is applied:
Water, 30% or so sodium chloride and 10% or so the phosphate that mother liquor (i.e. liquor B) ingredient is about 60%.It is cold
Liquor B go to technique water storage tank after heat exchanger and the filtrate A of heat heat exchange, then heated device further heat after return to it is molten
It solves kettle and carries out recycled, continue to dissolve crude product sodium pyrophosphate.
(5) optimum condition
Preferably, using the liquor B 2 of the heat after heat exchanger preheating and heater are heated to filter residue A (i.e. sodium chloride)
It carries out washing material, gained cleaning solution A is back to use hydrolysis kettle recycled.
Preferably, the washing of material device B and orthophosphates deep refining device in purification orthophosphates product process is washed
Liquid or filtrate return to hydrolysis kettle and are applied.
The present invention also provides a kind of crude product sodium pyrophosphates to purify production sodium dihydrogen phosphate and sodium chloride in the above content
Device, hydrolysis kettle bottom are connect with filter A；Filter device A is connect with heat exchanger, and heat exchanger is connect with mixer, mixer
It is connect with filter C, filter C is connect with crystallization kettle, and crystallization kettle is connect with filter B, and filter B connects with material device B is washed
It connects, washes material device B and be connected to phosphate deep refining device.The filter B washes material device B respectively through pipeline and heat exchange
Device connection, heat exchanger are connect with heater again through connecting water storage tank, and heater is connected to hydrolysis kettle.
The bottom filter A is connect through pipeline with material device A is washed, and is washed material mono- tunnel device A and is connected to sodium chloride deep refining dress
(13) are set, are connected to heat exchanger (4) all the way.
Wash the connecting pipe that material device A is connected between heater and hydrolysis kettle through pipeline line.
Technical solution of the present invention has the following beneficial effects:
1. the advantage of reaction, power savings advantages are obvious.This method dissolution, the speed of hydrolysis sodium pyrophosphate crude product is fast, reaction is thorough
Bottom, unit time treating capacity is big, and monomer unit production capacity greatly improves.Only 5-20min can be completely dissolved, and dissolution time relatively passes
System technique substantially shortens.
2. economy, environmental benefit are good.Crude product sodium pyrophosphate purifies the later mother liquor of biphosphate sodium salt, and (i.e. specification is attached
The liquor B of filter device B in figure) it can be applied in process water with recycled, the dissolution of crude product sodium pyrophosphate in hydrolytic process
Water and sodium pyrophosphate be combined (hydrolysis and hydration reaction), the water in addition system is finally combined with orthophosphates
The form of water produces system, it is only necessary to which regular minute quantity row is dense, and the water resource in reuse technology water is recycled.It is thick simultaneously
Realization separation is precipitated because of saturation for sodium chloride in product sodium pyrophosphate.Therefore wastewater flow rate is urged with respect to wet type in purification purification process
Reduce 92% or more for other techniques such as change oxidative extraction phosphate.Maximizing raising orthophosphates purity and
Reduce waste water yield, environmental benefit is very prominent, good economy performance.
3. this method can recycle sodium chloride product, chlorine resource is recycled, reduces the discharge amount liquid and waste slag produced containing chlorine.The party
The cost that method recycles sodium chloride is far below the cost using evaporating concentrating method recycling sodium chloride, and quality might as well.
4. orthophosphates obtained by this method and sodium chloride product impurity are few, purity is high.(1) this method is accelerated using phosphoric acid
The dissolution of sodium pyrophosphate crude product does not introduce new anionic impurity, while the waste water incinerations such as glyphosate mother solution being generated in the process
The removal of the anionic impurities such as carbonate, bicarbonate radical, inferior sulfate radical, sulfate radical, the removal of sulfide reduce product peculiar smell.
(2) this method is using oxidisability auxiliary agent on the one hand by TOC, COD and NH remaining in mother liquor burning process3- N oxidation removal, and
It brightens and eliminates the unusual smell effect, while promoting colloid dispergation in mixed system, material particle is fully dispersed, reduces feed liquid
Viscosity further produces synergistic effect, gained orthophosphates crystal and chlorine under these types effect so crystallization effect is good
Change sodium crystal purity is high.(3) it comes back in system and recycles because of the later mother liquor system of crude product sodium pyrophosphate purification orthophosphates
It applies, so can improve washing water in waste water acceptable range limits, improve the purity of sodium dihydrogen phosphate,
The features impurity indexs such as sodium chloride, non-positive phosphorus substance significantly improve.(4) the mother liquor system after sodium chloride purification comes back to system
Middle recycled, so can improve as far as possible washing water in waste water acceptable range limits, improve sodium chloride
Purity.(5) chloride content is down to 0.10% in the sodium dihydrogen phosphate of this method recycling, compared to Nantong rivers and mountains, Hubei
The chloride level of sodium dihydrogen phosphate 1% or so obtained by the companies such as Xing Fa traditional handicraft, residues of chloride figureofmerit significantly drop
It is low.
5. phosphorus residual quantity is very low in sodium chloride product, glyphosate reaches within 0.05%, within total phosphorus 0.15%.With this
P elements recycle also more thoroughly simultaneously.It is further preferred that using the alcoholic solution or alcoholic solution of hydrochloric acid or hydrogen chloride to obtaining
Sodium chloride product carry out extracting and refining when residue of glyphosate is reduced within 0.02% (mass ratio), total phosphorus is reduced to
Within 0.08%.
Because the later mother liquor system of crude product sodium pyrophosphate purification sodium ascorbyl phosphate comes back to recycled in system,
Washing water can be improved as far as possible in waste water acceptable range limits, while improving sodium chloride quality, reduced
The loss of sodium ascorbyl phosphate.
Detailed description of the invention
Fig. 1 is the process flow chart of crude product sodium pyrophosphate purification production sodium dihydrogen phosphate and sodium chloride, wherein 1. hydrolysis
Kettle, 2. filter A, 3. wash material device A, 4. heat exchangers, 5. water storage tanks, 6. mixers, 7. filter C, 8. crystallization kettles, 9. mistakes
Filter B, 10. wash material device B, 11. phosphate deep refining devices, 12. heaters, 13. sodium chloride deep refining devices.
Specific embodiment
Embodiment 1
A kind of method that the purification of crude product sodium pyrophosphate produces sodium dihydrogen phosphate and sodium chloride
In the process program, it is high that sodium dihydrogen phosphate crystallizes biphosphate sodium content in post mother liquor, and consume phosphoric acid amount compared with
Greatly, but because sodium dihydrogen phosphate hydration level is small and mother liquor is recycled, so overall cost is also advantageous.The process program is outstanding
It is suitable for having the enterprise of five sodium of phosphoric acid, six inclined corollary apparatus.
1. ingredient: when initial driving, by crude product sodium pyrophosphate and water according to the mass ratio of 1:1 at hydrolysis kettle (hydrolytic tank)
It is mixed, phosphoric acid control mixed material pH value is added dropwise 3.5.
During continuous operation, by crude product sodium pyrophosphate, (liquor B 2 washes the washing of material device A out with process water is applied
Other process waters described in liquid A and implementation steps) it is mixed according to the mass ratio of 1:1 in hydrolysis kettle (hydrolytic tank), it is added dropwise
Phosphoric acid controls mixed material pH value 3.5.
After crude product sodium pyrophosphate is partly dissolved, oxidisability auxiliary agent sodium chlorate and time chlorine are added into hydrolysis kettle (hydrolytic tank)
The mixture of sour sodium, carries out oxidation and colloidal sol reaction, and the additional amount of auxiliary agent is the 0.015% of sodium pyrophosphate crude product quality；It is added
After the auxiliary agent, solution viscosity is reduced, and solution rate is further promoted；Control keeps crude product burnt in 90 DEG C of at a temperature of stirring 30min
Sodium phosphate is sufficiently dissolved and is hydrolyzed；
The oxidisability auxiliary agent is sodium chlorate and the sodium hypochlorite mixture of 1:1 in mass ratio.
2. analysing salt: as crude product dissolves, phosphate and sodium chloride content are incrementally increased in mixed solution, and sodium chloride is because molten
Xie Du is relatively small, first reaches saturation, and when crude product continues investment, sodium chloride constantly crystallizes precipitation, phosphatic contains in system
Amount is constantly promoted.
3. sodium chloride Product recycling: discharging filtering while hot obtains filtrate A and filter residue A.Filter residue A is that thick sodium chloride produces
Product are washed material and obtain sodium chloride product, can also be gone to sodium chloride deep refining device and further be purified.Burnt phosphorus in filtrate A
Sour sodium, sodium chloride, which have been satisfied, to be reached and state.
4. orthophosphates Product recycling:
The filtrate A of heat carries out mixing in mixer after heat exchanger and cold liquor B 1 exchange heat with alkali sodium hydroxide
To solution A 2, the pH value of mixed solution A 2 is controlled 6.5, gradually generates sodium dihydrogen phosphate.Solution A 2 filters out few through filter C
Crystallization kettle is gone to after amount impurity.
When slurry temperature is reduced to 55-60 DEG C, suitable quantity of water and biphosphate sodium crystal are added into crystallization kettle, it is described
The mass ratio of the crystallization water and crude product coke sodium is 1:1, and biphosphate sodium crystal accounts for the 0.1% of crude product sodium dihydrogen phosphate weight, is controlled
20 DEG C of crystallisation by cooling 5h of temperature.In temperature-fall period, sodium dihydrogen phosphate solubility rapid decrease reaches hypersaturated state, di(2-ethylhexyl)phosphate
Hydrogen sodium crystal is constantly precipitated.Solubility with temperature decline of the sodium chloride in mixed solution is smaller, therefore sodium chloride stays in slurry
It is not precipitated in mother liquor.
Slurry after sufficient crystallising is gone to filter B and is separated by filtration, and obtained filter residue B is sodium dihydrogen phosphate product (two
Hypophosphite monohydrate sodium dihydrogen).Obtained sodium dihydrogen phosphate can also go to deep refining device and further purify.
5. Recycling Mother Solution is applied:
Water, 30% or so sodium chloride and 10% or so the phosphate that mother liquor (i.e. liquor B) ingredient is about 60%.It is cold
Liquor B go to technique water storage tank after heat exchanger and the filtrate A of heat heat exchange, then heated device further heat after return to it is molten
It solves kettle and carries out recycled, continue to dissolve crude product sodium pyrophosphate.
Preferably, using the liquor B 2 of the heat after heat exchanger preheating and heater are heated to filter residue A (i.e. sodium chloride)
It carries out washing material, gained cleaning solution A is back to use hydrolysis kettle recycled.
Preferably, the washing of material device B and orthophosphates deep refining device in purification orthophosphates product process is washed
Liquid or filtrate return to hydrolysis kettle and are applied.
Preferably, cleaning solution or filtrate of the sodium chloride deep refining device in purification sodium chloride product process return to water
Solution kettle is applied.
Table 2: crude product sodium pyrophosphate hydrolysate and sodium chloride dissolubility data
Embodiment 2
A kind of crude product sodium pyrophosphate purification produces the device of sodium pyrophosphate and sodium chloride, 1 bottom of hydrolysis kettle and filter A2
Connection；Filter device A2 is connect with heat exchanger 4, and heat exchanger 4 is connect with mixer 6, and mixer 6 is connect with filter C 7, mistake
Filter C 7 is connect with crystallization kettle 8, and crystallization kettle 8 is connect with filter B 9, and filter B 9 is connect with material device B 10 is washed, and washes material
Device B 10 is connected to sodium pyrophosphate deep refining device 11.
Filter B 9 washes and expects that device B 10 is connect through pipeline with heat exchanger 4 respectively, and heat exchanger 4 is through connecting water storage tank 5 again
It is connect with heater 12, heater 12 is connected to hydrolysis kettle 1.
2 bottom filter A is connect through pipeline with material device A 3 is washed, and is washed material 3 one tunnel device A and is connected to sodium chloride depth
Refining plant 13 is connected to heat exchanger 4 all the way.
Heater 12 is connected to through pipeline washes material device A 3.
It is provided with pyrophosphoric acid crude product on the hydrolysis kettle 1 and enters pipeline, phosphoric acid pipeline, auxiliary agent pipeline, water pipeline, steaming
Steam pipe line.
Material device A 3 is washed, washes and expects that being provided with water on device B 10 enters pipeline.
Crystallization water pipeline is provided on crystallization kettle 8.
Claims (8)
1. a kind of method of crude product sodium pyrophosphate purification production sodium dihydrogen phosphate and sodium chloride, it is characterised in that:
(1) ingredient and analysis salt: crude product sodium pyrophosphate and water are mixed, and phosphoric acid control mixed material pH value is added dropwise in 0.5-4.5 model
Enclose, be added oxidisability auxiliary agent after 70-120 DEG C at a temperature of stirring 5-60min make crude product sodium pyrophosphate dissolve and hydrolysis；
(2) sodium chloride Product recycling: slurry in hydrolysis kettle as described in step (1) is discharged filtering while hot, obtains sodium chloride production
Product and filtrate；
(3) it sodium dihydrogen phosphate Product recycling: will be mixed in mixer after the cooling of filtrate described in step (2) with alkali, control is mixed
Solution ph is closed in 4.0-7.0 range, sodium dihydrogen phosphate is generated, crystallization kettle is gone to after filter filters out impurity, in slurry temperature
When degree is down to 30-90 DEG C, water and biphosphate sodium crystal are added into crystallization kettle, cooling knot at being again later 0-30 DEG C in temperature
Sodium dihydrogen phosphate dihydrate is precipitated in brilliant 2-8h, and the slurry filtration after sufficient crystallising is separated, and obtains sodium dihydrogen phosphate dihydrate production
Product.
2. the method for crude product sodium pyrophosphate purification production sodium dihydrogen phosphate according to claim 1 and sodium chloride, feature
Be: the crude product sodium pyrophosphate is glyphosate mother solution, the phosphorous sodium chloride-containing waste water of pmida mother liquor is burned or high temperature oxygen
Change the sodium pyrophosphate crude product that obtained main component is sodium pyrophosphate and sodium chloride, be grey, canescence or grey black powdery,
Blocky, granular mixture, main component are sodium pyrophosphate and sodium chloride, the main content 40-85% of sodium pyrophosphate, sodium chloride
Content 3-35%, total organic carbon is in 0.1-0.3%, also containing sodium carbonate, sodium bicarbonate, sodium sulfite, sodium hydrogensulfite, organic phospha
Matter, pH value of water solution 9.5-10.55.
3. the method for crude product sodium pyrophosphate purification production sodium dihydrogen phosphate according to claim 1 and sodium chloride, feature
Be: the mass ratio of crude product sodium pyrophosphate and water as described in step (1) is 1:(0.5-2.0).
4. the method for crude product sodium pyrophosphate purification production sodium dihydrogen phosphate according to claim 1 and sodium chloride, feature
Be: the additional amount of oxidisability auxiliary agent described in step (2) is the 0.005%-2.5% of sodium pyrophosphate crude product quality.
5. the method for crude product sodium pyrophosphate purification production sodium dihydrogen phosphate according to claim 1 and sodium chloride, feature
Be: oxidisability auxiliary agent described in step (2) is sodium perchlorate, sodium chlorate, sodium chlorite, any one in sodium hypochlorite
Or several combination.
6. the method for crude product sodium pyrophosphate purification production sodium dihydrogen phosphate according to claim 1 and sodium chloride, feature
Be: alkali described in step (3) is sodium chlorate, the sodium hypochlorite mixture of 1:0.2-1.2 in mass ratio.
7. the method for crude product sodium pyrophosphate purification production sodium dihydrogen phosphate according to claim 1 and sodium chloride, feature
Be: the mass ratio of crude product sodium pyrophosphate is (0-5) in the quality and raw material of the water of addition described in step (3): 1；Di(2-ethylhexyl)phosphate
The weight of hydrogen sodium crystal is the 0.05-0.2% of the sodium dihydrogen phosphate of production.
8. the method for crude product sodium pyrophosphate purification production sodium dihydrogen phosphate according to claim 1 and sodium chloride, feature
It is: when slurry solution is down to 40-50 DEG C, water and biphosphate sodium crystal is added.
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| CN110407871B (en) * | 2019-08-30 | 2022-04-08 | 湖北泰盛化工有限公司 | Glyphosate crystallization device and crystallization method |
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