CN109704299A - The method that phosphate discharge liquid prepares potassium dihydrogen phosphate - Google Patents
The method that phosphate discharge liquid prepares potassium dihydrogen phosphate Download PDFInfo
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- CN109704299A CN109704299A CN201910151064.4A CN201910151064A CN109704299A CN 109704299 A CN109704299 A CN 109704299A CN 201910151064 A CN201910151064 A CN 201910151064A CN 109704299 A CN109704299 A CN 109704299A
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- orlon
- potassium hydroxide
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Abstract
The invention discloses the methods that phosphate discharge liquid prepares potassium dihydrogen phosphate.Solid potassium hydroxide is mixed with phosphate discharge liquid；Orlon stirring is added, brownish black jelly is wound by Orlon, sticks and takes out of, the color of system shoals, and pH is less than 1；As acid-base neutralization reaction terminates, system temperature is reduced, and is had transparent crystal to generate and is increased rapidly；Solid potassium hydroxide stirring, Orlon stirring are added in two portions again, the color of system further shoals, while crystal further increases；Stirring, it is cooling, allow crystallizing system aging 2h or more；Filtering, obtains white crystals thing.Solve the problems, such as that the phosphate discharge liquid accumulation coloration generated during phosphorous pesticide producing is too deep and influences its resource utilization, by the way that Orlon is added in the very exothermic reaction process of sum in acidolysis, decolorizing effect significantly improves, so that the color of the agricultural potassium dihydrogen phosphate of final products is more shallow, purity is higher.
Description
Technical field
The invention belongs to waste resource utilization technology fields, and in particular to a kind of phosphate discharge liquid prepares potassium dihydrogen phosphate
Method.
Background technique
Oxazole method technique produces vitamin B6, and the production of the production of glyphosate, the production of alachlor, butachlor all generates height
The phosphoric acid waste of concentration.It is protected in the time of attention degree not enough in our Environmentals, the production of these target products
After discarded phosphoric acid in technique is neutralized with soda or water body or part are directly discharged into the shape of mixed salt (sodium chloride+sodium phosphate)
Very inexpensively society is given in processing to formula.It seriously polluted environment and waste valuable phosphor resource.
At present the method for preparing agricultural potassium dihydrogen phosphate of domestic contrast maturation be after preparing phosphoric acid with phosphorus-containing ore with height
The sulfuric acid of concentration is mixed to form nitration mixture, then hybrid reaction is prepared containing biphosphate according to a certain percentage with solid potassium chloride
The mixture of potassium, dipotassium hydrogen phosphate etc..
Pesticide discards the production technology that phosphoric acid is mainly derived from Acetochlor.Its main production process is seven amine of the first and second base of 2,6-
It is reacted with monoxone and phosphorus trichloride, generates the first and second base of 2,6- -2- chloro acetanilide, ethyl alcohol and polyformaldehyde and hydrochloric acid exists
Lower reaction generates chloromethyl ethyl ether, and 2,6- first and second base -2- chloro acetanilides and chloromethyl ethyl ether are condensed, and generates second
Careless amine.It is decolorising agent problem through testing handy this waste phosphoric acid legal most crucial problem of agricultural potassium dihydrogen phosphate for preparing in, because
The decolorizing effect of common bleaching agent activated carbon is unsatisfactory.
Summary of the invention
Present invention aims at the crystalline mother solution accumulation colorations occurred in the production process for solving Acetochlor to influence deeply very much
The problem of its resource utilization, discards phosphoric acid to pesticide and carries out effective decolorization, and recycling benefit is further carried out to it
With.
In order to achieve the above objectives, as follows using technical solution:
The method that phosphate discharge liquid prepares potassium dihydrogen phosphate, comprising the following steps:
1) solid potassium hydroxide is mixed with phosphate discharge liquid, liquid level has brownish black jelly to gather；It is short that polyacrylonitrile is added
Brownish black jelly is wound by Orlon, sticks and take out of by fiber stirring, and the color of system shoals, and pH is less than
1；As acid-base neutralization reaction terminates, system temperature is reduced, and is had transparent crystal to generate and is increased rapidly；
2) solid potassium hydroxide stirring is added again, Orlon stirring is added, brownish black jelly is passed through
Orlon winding is sticked and is taken out of, and the color of system further shoals, and pH is less than 1；
3) solid potassium hydroxide stirring is added again, Orlon stirring is added, brownish black jelly is passed through
Orlon winding is sticked and is taken out of, and the color of system further shoals, and pH is greater than 1 less than 3, while crystal is further
Increase；
4) it stirs, it is cooling, allow crystallizing system aging 2h or more；Filtering, obtains white crystals thing.
According to the above scheme, the phosphate discharge liquid derives from the production technology of Acetochlor；Wherein phosphorus acid content is 10wt%-
60wt%.
According to the above scheme, potassium hydroxide content is 10wt%-85wt% in the solid potassium hydroxide.
According to the above scheme, the Orlon length is 0.1mm-15mm.
According to the above scheme, potassium hydroxide used and phosphoric acid molar ratios are 1:(0.5-2.5).
Under decolorising agent micro and in phosphoric acid in pigment affinity comparison procedure, glass capillary is used first, takes work
Property charcoal be placed in the water in observation pond of submicroscopic visualization device, it is discarded separately to draw Synthetic Process of Acetochlor with glass capillary
Coloured phosphoric acid, the motion conditions of observation micro activated carbon particle and coloured micelle in phosphoric acid.Coloured micelle is not almost seen in 0-45min
There is sorption phenomenon with active carbon particle.Therefore, active carbon is not suitable for making the de- of the discarded coloured phosphoric acid of Synthetic Process of Acetochlor
Toner.Another plus 1mL dodecane is placed in the water in observation pond of submicroscopic visualization device, and oil-water interfaces are very clear.Use capillary
Glass tube draws the coloured phosphoric acid of discarding that micro Synthetic Process of Acetochlor generates and is respectively placed in water phase and oily phase.Coloured micelle is obvious
It is enriched with to oil-water interfaces.This shows that coloring matter has certain interfacial activity in phosphoric acid.Finally in submicroscopic visualization device
Observation pond water in a few root polypropylene nitrile staple fibers are added, after sufficiently soaking, with glass capillary draw Acetochlor production
What technique generated discards in coloured phosphoric acid micro entrance observation pond.The case where coloured micelle is adsorbed is observed with 0-45min.Observation
Show have the coloured micelle of dozens of by sorption within the observation period in every millimeter of segment of fiber.This shows that Orlon is made
For the reasonable of decolorising agent.
The beneficial effects of the invention are that:
Solving the phosphate discharge liquid accumulation coloration generated during phosphorous pesticide producing influences its resource utilization deeply very much
The problem of, by the way that Orlon is added in the very exothermic reaction process of sum in acidolysis, decolorizing effect is significantly improved,
So that the color of the agricultural potassium dihydrogen phosphate of final products is more shallow, purity is higher.
Specific embodiment
Following embodiment further illustrates technical solution of the present invention, but not as limiting the scope of the invention.
By the character of pesticide waste phosphoric acid it is found that its pH value less than 1, has the breath of dense organic matter, 60 DEG C of heating, which has, chokes
The sour gas of people is excessive.It can be obtained through test and contain organic volatile matter 1wt%-2wt%, organic pigment 1.0wt%- in raw material
1.6wt%, hydrochloric acid 1wt% or so, substantially used spent acid are the nitration mixture of the hydrochloric acid and 50wt% phosphoric acid composition of 1wt%,
Bivalent metal ion is substantially free of in mixed acid system.Therefore pigment source is in organic matter.
120 grams of 85wt% solid potassium hydroxides are taken, 250mL waste phosphoric acid is stand-by.100g85% solid potassium hydroxide is put into
In the beaker of 500mL capacity, 250mL waste phosphoric acid is poured into 500mL beaker, acid-base neutralization reaction is violent, with a large amount of steam
Cup is gone out, upper layer shows as white dense foam uplink and quickly vanishes in cup.After white foam is vanished, liquid surface has palm fibre
Dark gum gathers.Wherein brownish black jelly is organic pigment.The Orlon of phosphoric acid quality 1% is taken, in batches
Secondary to lose in beaker, brownish black jelly is taken in stirring out of.With brownish black jelly by fiber winding, stick and take beaker out of,
The color of system shoals.Acid-base neutralization reaction is a strong exothermal reaction.In reaction process, the color of system is by pale brown transparent turn
Turn to the opaque muddy shape of milk yellow.The carry out system overflowed with stirring and steam is gradually converted to transparence, temperature drop
Low, transparent crystal also increases rapidly.Steam is excessive, has taken away many moisture, has also taken organic volatile part out of.It is tried with wide pH value
The pH value of paper survey system.At this moment system is still in highly acid.pH<1.10g 85wt% solid potassium hydroxide is added, stirring adds
Enter the decoloration staple fiber of above-mentioned preparation, system fever local boiling, stirring takes out decoloration object, system pH after reacting calmness
Less than 1.10g 85wt% solid potassium hydroxide is added, the decoloration staple fiber of above-mentioned preparation, system fever part boiling is added in stirring
It rises, stirs, after reacting calmness, take out decoloration object, for the pH value of system less than 3, the crystal of system is more.Stirring, it is cooling, it stirs
It mixes, allows crystallizing system aging 2 hours.With filtered on buchner funnel, it is contemplated that be sour elastomer systems, do not have to general filter paper, use instead
Polypropylene fiber nonwoven cloth does filter cloth.White crystals thing 212g, colorless and transparent crystalline mother solution 145mL are weighed after filtering.With hydrogen-oxygen
Calculating a yield on the basis of change potassium is 85.5wt%.
With a yield 64wt% of liquid sodium hydroxide alkali and waste phosphoric acid Response calculation, total recovery 95wt% compares it
Process flow benefit is not much different.But it selects the economic benefit of solid potassium hydroxide alkali to want high, therefore selects solid potassium hydroxide alkali
It is reacted with pesticide waste phosphoric acid and prepares agricultural potassium dihydrogen phosphate.
Embodiment 1
120 grams of 85wt% solid potassium hydroxides are taken, 250mL (about 165g) waste phosphoric acid is stand-by.By 100g85% solid hydrogen-oxygen
Change potassium to be put into the beaker of 500mL capacity, 250mL waste phosphoric acid be poured into 500mL beaker, acid-base neutralization reaction.Take phosphoric acid matter
The Orlon of amount 1%, length is about 2mm ± 5mm, is lost in beaker in batches, is stirred, by brownish black jelly band
Out.10g 85wt% solid potassium hydroxide is added, stirring is added the decoloration staple fiber of above-mentioned preparation, and system is generated heat local boiling,
Stirring takes out decoloration object after reacting calmness.10g 85wt% solid potassium hydroxide is added, the de- of above-mentioned preparation is added in stirring
Color staple fiber, system generate heat local boiling, stirring, after reacting calmness, take out decoloration object, the pH value of system less than 3, system
Crystal is more.Stirring, cooling, stirring allows crystallizing system aging 2 hours.With filtered on buchner funnel, polypropylene fiber nonwoven cloth
Do filter cloth.White crystals thing 212g, colorless and transparent crystalline mother solution 145mL are weighed after filtering.One is calculated on the basis of potassium hydroxide
Secondary yield is 85.5wt%.
Embodiment 2
125 grams of 85wt% solid potassium hydroxides are taken, 250mL (about 165g) waste phosphoric acid is stand-by.By 100g85% solid hydrogen-oxygen
Change potassium to be put into the beaker of 500mL capacity, 250mL waste phosphoric acid be poured into 500mL beaker, acid-base neutralization reaction.Take phosphoric acid matter
The Orlon of amount 1%, length is about 2mm ± 5mm, is lost in beaker in batches, is stirred, by brownish black jelly band
Out.15g 85wt% solid potassium hydroxide is added, stirring is added the decoloration staple fiber of above-mentioned preparation, and system is generated heat local boiling,
Stirring takes out decoloration object after reacting calmness.10g 85wt% solid potassium hydroxide is added, the de- of above-mentioned preparation is added in stirring
Color staple fiber, system generate heat local boiling, stirring, after reacting calmness, take out decoloration object, the pH value of system less than 3, system
Crystal is more.Stirring, cooling, stirring allows crystallizing system aging 2 hours.With filtered on buchner funnel, polypropylene fiber nonwoven cloth
Do filter cloth.White crystals thing 220g, colorless and transparent crystalline mother solution 145mL are weighed after filtering.One is calculated on the basis of potassium hydroxide
Secondary yield is 86.5wt%.
Embodiment 3
The phosphoric acid generated during oxazole method technique production vitamin B6 and hydrochloric acid mixture 1000mL are taken, is removed through distillation
Go hydrochloric acid stand-by.Distillation end point is that vapour phase middle acid substance is not detected.At this moment brownish black thick liquid is phosphoric acid.Visual phosphorus
Acid concentration difference need to add water adjustment phosphoric acid concentration to be 34%-60%.In experiment, phosphoric acid concentration is adjusted to 46% (wt).Take 125
Gram 85wt% solid potassium hydroxide, 260mL (about 165g) waste phosphoric acid are stand-by.100g85% solid potassium hydroxide is put into 500mL
In the beaker of capacity, 250mL waste phosphoric acid is poured into 500mL beaker, acid-base neutralization reaction.Take the polypropylene of phosphoric acid quality 1%
Nitrile staple fiber, length are about 2mm ± 5mm, are lost in beaker in batches, and brownish black jelly is taken in stirring out of.15g is added
The decoloration staple fiber of above-mentioned preparation, system fever local boiling, stirring, wait react is added in 85wt% solid potassium hydroxide, stirring
After calmness, decoloration object is taken out.10g 85wt% solid potassium hydroxide is added, the decoloration staple fiber of above-mentioned preparation, body is added in stirring
System's fever local boiling, stirring take out decoloration object, for the pH value of system less than 3, the crystal of system is more after reacting calmness.
Stirring, cooling, stirring allows crystallizing system aging 2 hours.With filtered on buchner funnel, polypropylene fiber nonwoven cloth does filter cloth.Filtering
White crystals thing 218g, colorless and transparent crystalline mother solution 145mL are weighed afterwards.A yield is calculated on the basis of potassium hydroxide is
83.5wt%.
Claims (5)
1. the method that phosphate discharge liquid prepares potassium dihydrogen phosphate, it is characterised in that the following steps are included:
1) solid potassium hydroxide is mixed with phosphate discharge liquid, liquid level has brownish black jelly to gather；Orlon is added
Brownish black jelly is wound by Orlon, sticks and take out of by stirring, and the color of system shoals, and pH is less than 1；With
Acid-base neutralization reaction terminate, system temperature reduces, and has transparent crystal to generate and increases rapidly；
2) solid potassium hydroxide stirring is added again, Orlon stirring is added, brownish black jelly is passed through poly- third
The winding of alkene nitrile staple fiber is sticked and is taken out of, and the color of system further shoals, and pH is less than 1；
3) solid potassium hydroxide stirring is added again, Orlon stirring is added, brownish black jelly is passed through poly- third
The winding of alkene nitrile staple fiber is sticked and is taken out of, and the color of system further shoals, and pH is greater than 1 less than 3, while crystal further increases；
4) it stirs, it is cooling, allow crystallizing system aging 2h or more；Filtering, obtains white crystals thing.
2. the method that phosphate discharge liquid as described in claim 1 prepares potassium dihydrogen phosphate, it is characterised in that the phosphate discharge liquid source
In the production technology of Acetochlor；Wherein phosphorus acid content is 10%-60%.
3. the method that phosphate discharge liquid as described in claim 1 prepares potassium dihydrogen phosphate, it is characterised in that the solid potassium hydroxide
Middle potassium hydroxide content is 10%-85wt%.
4. the method that phosphate discharge liquid as described in claim 1 prepares potassium dihydrogen phosphate, it is characterised in that the short fibre of polyacrylonitrile
Dimension length is 0.1mm-15mm.
5. the method that phosphate discharge liquid as described in claim 1 prepares potassium dihydrogen phosphate, it is characterised in that potassium hydroxide and phosphorus used
Sour molar ratio is 1:(0.5-2.5).
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Cited By (2)
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| CN110483125A (en) * | 2019-08-02 | 2019-11-22 | 史丹利化肥当阳有限公司 | Utilize the method for waste phosphoric acid production S-based compound fertilizer raw material |
| RU2776120C1 (en) * | 2021-10-05 | 2022-07-13 | Акционерное общество "Объединенная химическая компания "УРАЛХИМ" (АО "ОХК "УРАЛХИМ") | Method for producing potassium monoposphate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110483125A (en) * | 2019-08-02 | 2019-11-22 | 史丹利化肥当阳有限公司 | Utilize the method for waste phosphoric acid production S-based compound fertilizer raw material |
| CN110483125B (en) * | 2019-08-02 | 2022-03-04 | 史丹利化肥当阳有限公司 | Method for producing raw material for sulfur-based compound fertilizer by using waste phosphoric acid |
| RU2776120C1 (en) * | 2021-10-05 | 2022-07-13 | Акционерное общество "Объединенная химическая компания "УРАЛХИМ" (АО "ОХК "УРАЛХИМ") | Method for producing potassium monoposphate |
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Application publication date: 20190503 |