CN209428133U - A kind of crude product sodium pyrophosphate purification produces the device of sodium ascorbyl phosphate and sodium chloride - Google Patents
A kind of crude product sodium pyrophosphate purification produces the device of sodium ascorbyl phosphate and sodium chloride Download PDFInfo
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Abstract
The utility model discloses a kind of phosphorous brine waste by-product crude product sodium pyrophosphate purification production sodium ascorbyl phosphate such as glyphosate mother solution and the devices of sodium chloride product, in crude product sodium pyrophosphate subtractive process, orthophosphates, sodium chloride are separated using the dissolution sex differernce feature of each component and hydrolysate in crude product sodium pyrophosphate under different temperatures, pH value condition and promoter effect, there is reaction advantage, environment-friendly advantage, quality-advantage, cost advantage.Improve phosphoric acid by auxiliary agent, improve crystallization effect, reaction speed is fast, also improves orthophosphates, sodium chloride quality, solves sale problem；Low energy consumption for desalting process, and dissolution is recycled with process waters such as water, slurries in production process, and water consume dosage is small, reduces wastewater flow rate and environmental protection treatment cost.
Description
Technical field
The invention belongs to three-protection design production technical field, the high sodium chloride phosphorus-containing wastewater such as specially a kind of glyphosate mother solution
In the refining plant for the crude product sodium pyrophosphate that burning or high-temperature oxydation obtain, it is particularly suitable for glycine method or IDA method glyphosate
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, and mother liquor is 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.At present at mainstream mother liquor
Science and engineering skill is that mainly have incineration method, high-temperature oxidation, medium temperature oxidizing process, low using oxidizing process degradation mother liquor and recycling P elements
Warm oxidizing process etc. also passes through membrane separation technique or evaporation and concentration recycling sodium chloride and phosphate during mother liquid disposal.Example
Such as: UF membrane recycles sodium chloride and glyphosate and other substances, is concentrated by evaporation recycling glyphosate and sodium chloride, concentrated mother liquor are fixed
Sodium pyrophosphate is recycled to conversion, mother liquor catalytic oxidation recycles phosphate, etc..Every kind of method has superiority and inferiority, several glyphosate masters
Want big producer that different treatment process is respectively adopted, and above-mentioned several techniques are combined processing glyphosate by most enterprises
Mother liquor.Currently, there are concentrated mother liquor orientation conversion production sodium pyrophosphate in Xingfa Group, new Anhua work, Shandong Run Fengdeng company
Device, the obtained main content 40-60% of burnt sodium crude product, sodium chloride content 5-35%, goes back carbonaceous powder, sodium carbonate, sodium bicarbonate, sulfurous
Sour sodium, the impurity such as sodium hydrogensulfite, organic phosphorus.For the route, desalination process is still concentrated in either film process desalination, finally
Contain higher sodium chloride in gained sodium pyrophosphate crude product, also there is certain TOC, so product impurity is more, colour-difference, has
Peculiar smell, main content are low, of poor quality, and the market price is low, and application is also restrained, need further to purify, and improve master and contain
Amount and quality.
Part company takes the mode that crude product sodium pyrophosphate is further produced as disodium hydrogen phosphate to refine, but raw
During production, there are the dissolutions of crude product sodium pyrophosphate slowly, dissolution fluid viscosity is big, processing capacity is small and wastewater flow rate is big, at high cost
Problem, sodium chloride, organophosphorus residue amount are big in phosphate product, of poor quality.Such as a kind of pair of glyphosate mother solution of CN206915770U
The system that phosphor resource after advanced treating is purified.CNIO68098llA is a kind of to prepare sodium pyrophosphate using crude product sodium pyrophosphate
Method and when CN106882781A a kind of crude product sodium pyrophosphate purification production sodium pyrophosphate product the method decolourized it is directly smart
System extracts sodium pyrophosphate, and equally there is also the dissolutions of crude product sodium pyrophosphate during handling crude product sodium pyrophosphate, and slow, lysate glues
Degree 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 special
Point develops new process.
Summary of the invention
The method of crude product sodium pyrophosphate purification production disodium hydrogen phosphate and sodium chloride provided by the present invention, in crude product coke phosphorus
In sour sodium subtractive process, made using each component in crude product sodium pyrophosphate and hydrolysate in different temperatures, pH value condition and auxiliary agent
The characteristics of dissolution sex differernce under, separates orthophosphates, sodium chloride.Using phosphoric acid and with oxidizing substance at auxiliary agent
Reason promotes the dissolution of by-product crude product sodium pyrophosphate, hydrolysis and crystallization, changes phosphoric acid while removing impurity, improves crystallization effect
Fruit improves orthophosphates, sodium chloride quality.In production process, mother liquor and dissolution after purification to be taken out to orthophosphates are used
Water, slurry and process water are recycled, and water consume dosage and waste water yield significantly reduce, and reduce environmental protection treatment pressure
Power and cost.
According to market sale needs, the orthophosphates can specifically be produced as sodium dihydrogen phosphate, disodium hydrogen phosphate, tricresyl phosphate
The mixture of sodium or sodium dihydrogen phosphate, the mixture of disodium hydrogen phosphate or disodium hydrogen phosphate, tertiary sodium phosphate.Tune can specifically be passed through
The technic indexs such as whole temperature, pH value are realized.
First sodium chloride is extracted in filtering from the mixed slurry after the dissolution of crude product sodium pyrophosphate, hydrolysis, then extracts from filtrate
Orthophosphates.Then the sodium chloride crude product and orthophosphates crude product that extract are refined respectively.Filter B is separating positive phosphorus
Liquor B obtained in hydrochlorate process returns to hydrolysis kettle and carries out recycled.Orthophosphates crude product and sodium chloride crude product are purified
Cleaning solution or filtrate in journey return to hydrolysis kettle and are applied.Specific device structure is as follows:
A kind of crude product sodium pyrophosphate purification produces the device of orthophosphoric acid sodium salt and sodium chloride, hydrolysis kettle bottom and filter A
Connection；Filter device A is connect with heat exchanger, and heat exchanger is connect with mixer, and mixer is connect with filter C, filter C and knot
Brilliant kettle connection, crystallization kettle are connect with filter B, and filter B is connect with material device B is washed, and are washed material device B and are connected to phosphate depth
Refining plant.
The filter B is washed material device B and is connect respectively through pipeline with heat exchanger, heat exchanger connected water storage tank again with
Heater connection, heater are 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 depth
Refining plant is connected to heat exchanger all the way.Heater is connected to through pipeline washes material device A.
It is provided with pyrophosphoric acid crude product on the hydrolysis kettle and enters pipeline, phosphoric acid pipeline, auxiliary agent pipeline, water pipeline, steam
Pipeline.
Material device A is washed, washes and expects that being provided with water on device B enters pipeline.
Crystallization water pipeline is provided on crystallization kettle.
The technical solution of the utility model 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,
Unit time treating capacity is big, and monomer unit production capacity greatly improves.Only 5-20min can be completely dissolved, compared with 2. economy, environmental benefit
It is good.Crude product sodium pyrophosphate purify the later mother liquor (i.e. liquor B) of orthophosphates can with recycled, the dissolution of crude product sodium pyrophosphate and
In hydrolytic process, the water and sodium pyrophosphate applied in process water are combined (hydrolysis and hydration reaction), in addition system
Water system is finally produced in the form of orthophosphates combination water, it is only necessary to regular minute quantity row is dense, the water money in reuse technology water
Source is recycled.The sodium chloride cause and effect in crude product sodium pyrophosphate is saturated and is precipitated and realizes separation simultaneously.Therefore purification purification
Wastewater flow rate reduces 92% or more for extracting other techniques such as phosphate with respect to catalytic wet oxidation in the process.Maximizing
It improves the purity of orthophosphates and reduces 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.This method
The cost for recycling sodium chloride is far below the cost that sodium chloride is recycled using evaporating concentrating method, 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 burnt using phosphoric acid
The dissolution of sodium phosphate crude product does not introduce new anionic impurity, while the carbon that will be generated during the waste water incinerations such as glyphosate mother solution
The removal of the anionic impurities such as acid group, 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 have increasing
The white and effect of eliminating the unusual smell, while promoting colloid dispergation in mixed system, material particle is fully dispersed, reduces viscosity of sludge, institute
It is good with crystallization effect, synergistic effect, gained orthophosphates crystal and sodium chloride crystal are further produced under these types effect
Purity is high.(3) because crude product sodium pyrophosphate purifies orthophosphates, later mother liquor system comes back to recycled in system,
Washing water can be improved as far as possible, improves the purity of orthophosphates in waste water acceptable range limits, sodium chloride,
The features impurity index such as non-positive phosphorus substance significantly improves.(4) the mother liquor system after sodium chloride purification comes back to circulating sleeve in system
With so can improve as far as possible washing water in waste water acceptable range limits, improve the purity of sodium chloride.(5)
Sodium chloride content can be down to 0.1% or so in the orthophosphates of this method recycling, and sodium chloride content level is far below traditional handicraft essence
The level of system gained sodium pyrophosphate or orthophosphates 3-15% sodium chloride.
Detailed description of the invention
Fig. 1 is the structure drawing of device of crude product sodium pyrophosphate purification production sodium ascorbyl phosphate and sodium chloride, wherein 1. hydrolysis kettles,
2. filter A, 3. wash material device A, 4. heat exchangers, 5. water storage tanks, 6. mixers, 7. filter C, 8. crystallization kettles, 9. filters
B, 10. wash material device B, 11. phosphate deep refining devices, 12. heaters, 13. sodium chloride deep refining devices.
Specific embodiment
A kind of crude product sodium pyrophosphate purification produces the device of orthophosphoric acid sodium salt and sodium chloride, 1 bottom of hydrolysis kettle and filter
A2 connection；Filter device A 2 is connect with heat exchanger 4, and heat exchanger 4 is connect with mixer 6, and mixer 6 is connect with filter C 7,
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 is washed
Material device B 10 is connected to phosphate 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, steam
Pipeline.
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.
The method that production sodium ascorbyl phosphate and sodium chloride are purified to crude product sodium pyrophosphate using above-mentioned apparatus, including walk as follows
It is rapid:
1. initial when driving, by crude product sodium pyrophosphate and water according to 1:(0.5-2.0) mass ratio in hydrolysis kettle (hydrolysis
Pond) mixed, phosphoric acid control mixed material pH value is added dropwise in 1.0-8.8 range, control 80-95 DEG C at a temperature of stir 5-
60min makes crude product sodium pyrophosphate dissolve and hydrolyze；
2. during continuous operation, by crude product sodium pyrophosphate, (filter B is through heat exchanger heat exchange again through adding with process water is applied
Other process waters described in liquor B 2, cleaning solution A and implementation steps after the heating of hot device) according to 1:(0.5-2.0) quality
Than being mixed in hydrolysis kettle (hydrolytic tank), phosphoric acid control mixed material pH value is added dropwise in 1.0-8.8 range, controls in 80-95
5-60min is stirred at a temperature of DEG C makes crude product sodium pyrophosphate dissolve and hydrolyze；
3. crude product sodium pyrophosphate is after completely dissolution, oxidisability auxiliary agent sodium perchlorate, chlorine are added into hydrolysis kettle (hydrolytic tank)
One or more of sour sodium, sodium chlorite, sodium hypochlorite, carry out oxidation and colloidal sol reaction, and the additional amount of auxiliary agent is pyrophosphoric acid
The 0.005%(50ppm of sodium crude product quality) -2.5%；After the auxiliary agent is added, solution viscosity is reduced, and solution rate is further promoted.
As crude product dissolves, phosphate and sodium chloride content are incrementally increased in mixed solution, and sodium chloride is first reached because solubility is relatively small
To satisfying, when crude product continues investment, sodium chloride constantly crystallizes precipitation, phosphatic content is constantly promoted in system,
The oxidisability auxiliary agent, it is therefore preferable to which one of sodium hypochlorite, sodium chlorite, sodium chlorate or sodium perchlorate are several
The mixture of kind.It is further preferred that being sodium chlorate, sodium chlorite；
4. discharging filtering while hot, obtains filtrate A and filter residue A.The filtrate A of heat after heat exchanger and cold liquor B 1 exchange heat,
It carries out being mixed to get solution A -2 in mixer with alkali, controls the pH value of mixed solution A -2 in 8-10 range, generate phosphoric acid hydrogen
Disodium,
The alkali is the combination of one or more of sodium hydroxide, sodium carbonate, sodium bicarbonate；
5. solution A -2 goes to crystallization kettle after filter C filters out a small amount of impurity, the temperature for controlling slurries is 80-105 DEG C,
The mass ratio of the crystal of addition suitable quantity of water and anhydrous orthophosphates into crystallization kettle, water and crude product coke sodium is (0.5-3): 1, it is anhydrous
The crystal of orthophosphates accounts for the 0.01-0.1% of crude product orthophosphoric acid quality；Control 0-30 DEG C of crystallisation by cooling 2-8h of temperature.Temperature-fall period
In, the disodium hydrogen phosphate dodecahydrate crystal being saturated first and the sodium chloride solution being closely saturated；As temperature further drops
Low, the disodium hydrogen phosphate hydrate in slurry constantly crystallizes precipitation, and sodium chloride stays in slurry mother liquor because solubility decline is smaller
It is not precipitated.Sufficient crystallising slurry is through the isolated liquor B of filter device B and filter residue B；
6. cold liquor B is gone to after heater further heats after heat exchanger and the filtrate A of heat heat exchange and returns to hydrolysis kettle
Carry out recycled.Filter residue B is disodium hydrogen phosphate crude product, goes to wash and expects that device B obtains disodium hydrogen phosphate dodecahydrate product.
The disodium hydrogen phosphate dodecahydrate obtained herein can also go to orthophosphates deep refining device and further purify；
7. filter residue A is thick sodium chloride product, successively goes to wash and expect that device A obtains sodium chloride crude product.Sodium chloride crude product is also
Sodium chloride deep refining device can be gone to further to purify.
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 hydrolysis
Kettle is applied.
The device can be also used for using crude product sodium pyrophosphate produce tertiary sodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate or
Sodium pyrophosphate.
Claims (7)
1. the device of a kind of crude product sodium pyrophosphate purification production sodium ascorbyl phosphate and sodium chloride, it is characterised in that:
Hydrolysis kettle (1) bottom is connect with filter A(2)；Filter A(2) it is connect with heat exchanger (4), heat exchanger (4) and mixer
(6) connect, mixer (6) is connect, filter C(7 with filter C(7)) it is connect with crystallization kettle (8), crystallization kettle (8) and filter
B(9) connect, filter B (9) with wash material device B(10) connect, wash expect device B(10) be connected to phosphate deep refining device
(11).
2. the device of crude product sodium pyrophosphate purification production sodium ascorbyl phosphate according to claim 1 and sodium chloride, feature exist
In: filter B (9) washes material device B(10) connect respectively through pipeline with heat exchanger (4), heat exchanger (4) is through connecting water storage tank (5)
It is connect again with heater (12), heater (12) is connected to hydrolysis kettle (1).
3. the device of crude product sodium pyrophosphate purification production sodium ascorbyl phosphate according to claim 1 and sodium chloride, feature exist
In: filter A(2) bottom through pipeline with wash material device A(3) connect, wash material device A(3) to be connected to sodium chloride depth all the way smart
Device (13) processed, is connected to heat exchanger (4) all the way.
4. the device of crude product sodium pyrophosphate purification production sodium ascorbyl phosphate according to claim 2 and sodium chloride, feature exist
In: heater (12) is connected to through pipeline and washes material device A(3).
5. the device of crude product sodium pyrophosphate purification production sodium ascorbyl phosphate according to claim 1 and sodium chloride, feature exist
In: pyrophosphoric acid crude product, which is provided with, on the hydrolysis kettle (1) enters pipeline, phosphoric acid pipeline, auxiliary agent pipeline, water pipeline, steam pipe
Line.
6. the device of crude product sodium pyrophosphate purification production sodium ascorbyl phosphate according to claim 3 and sodium chloride, feature exist
In: wash material device A(3), wash material device B(10) on be provided with process water and enter pipeline.
7. the device of crude product sodium pyrophosphate purification production sodium ascorbyl phosphate according to claim 1 and sodium chloride, feature exist
In: crystallization kettle is provided with crystallization water pipeline on (8).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109399593A (en) * | 2018-12-28 | 2019-03-01 | 湖北泰盛化工有限公司 | A kind of method that the purification of crude product sodium pyrophosphate produces disodium hydrogen phosphate and sodium chloride |
| CN110812877A (en) * | 2019-10-12 | 2020-02-21 | 西安交通大学 | Glyphosate mother liquor treatment method and device |
| CN114148996A (en) * | 2021-10-29 | 2022-03-08 | 雷波凯瑞磷化工有限责任公司 | Method for producing sodium pyrophosphate and sodium chloride by purifying crude sodium pyrophosphate |
| CN115448514A (en) * | 2022-07-28 | 2022-12-09 | 南通江山农药化工股份有限公司 | Process method for treating organophosphorus wastewater and recycling potassium chloride |
-
2018
- 2018-12-27 CN CN201822217931.3U patent/CN209428133U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109399593A (en) * | 2018-12-28 | 2019-03-01 | 湖北泰盛化工有限公司 | A kind of method that the purification of crude product sodium pyrophosphate produces disodium hydrogen phosphate and sodium chloride |
| CN110812877A (en) * | 2019-10-12 | 2020-02-21 | 西安交通大学 | Glyphosate mother liquor treatment method and device |
| CN114148996A (en) * | 2021-10-29 | 2022-03-08 | 雷波凯瑞磷化工有限责任公司 | Method for producing sodium pyrophosphate and sodium chloride by purifying crude sodium pyrophosphate |
| CN115448514A (en) * | 2022-07-28 | 2022-12-09 | 南通江山农药化工股份有限公司 | Process method for treating organophosphorus wastewater and recycling potassium chloride |
| CN115448514B (en) * | 2022-07-28 | 2023-08-29 | 南通江山农药化工股份有限公司 | Process method for treating organophosphorus wastewater and recycling potassium chloride |
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