CN105347321A - Method for producing ammonium phosphate by using low-grade low-concentration raffinate acid - Google Patents
Method for producing ammonium phosphate by using low-grade low-concentration raffinate acid Download PDFInfo
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- CN105347321A CN105347321A CN201510863254.0A CN201510863254A CN105347321A CN 105347321 A CN105347321 A CN 105347321A CN 201510863254 A CN201510863254 A CN 201510863254A CN 105347321 A CN105347321 A CN 105347321A
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Abstract
The invention discloses a method for producing ammonium phosphate by using low-grade low-concentration raffinate acid. The method includes the steps that the low-grade raffinate acid with the P2O5 concentration of 22-24% is conveyed into a washing system of an ammonium phosphate device as washing liquid to circularly absorb ammonia and dust in tail gas, when the neutralization degree of the raffinate acid washing liquid is 0.6-0.9, the raffinate acid washing liquid is conveyed to a concentration device and is concentrated through heating until the P2O5 concentration is 26-30%, and concentrated slurry and strong phosphoric acid are mixed and then produce an ammonium phosphate product in a neutralization reactor. The low-grade low-concentration raffinate acid is used for absorbing ammonia and the dust in the tail gas of the ammonium phosphate device and then is concentrated through heating, the problem that an acid-insoluble scale layer difficult to clear is prone to generation in the concentration process of the low-grade low-concentration raffinate acid can be solved, and the cost of producing ammonium phosphate by using the low-grade low-concentration raffinate acid is substantially reduced; the usage amount of washing water needed by a tail gas treatment system of the ammonium phosphate device can be reduced, and the production cost of the whole ammonium phosphate device is further reduced.
Description
Technical field
The present invention relates to ammonium phosphate production method, specifically a kind of method utilizing low-grade lower concentration raffinate to produce phosphorus ammonium.
Background technology
Current Wet Phosphoric Acid Market major part adopts solvent extration, can produce a large amount of raffinates in production, and the main digestion method of these raffinates produces chemical fertilizer, according to the difference of raw materials for production and technique, and the P of its raffinate
2o
5concentration difference is larger.There is the technology utilizing raffinate to produce granular monoammonium phosphate or diammonium phosphate at present, raffinate P used
2o
5concentration reaches more than 37%, derives from by P
2o
5the wet phosphoric acid purifying that the higher-grade phosphorus ore of content more than 32% is produced, therefore and be not suitable for the utilization of lower concentration raffinate.
Because phosphate rock resource is more and more poorer, most enterprises all adopts P
2o
5content lower than 30% low-grade phosphate ore, the phosphoric acid by wet process concentration of producing with this kind of phosphorus ore about 40%, adopt solvent extration purification after, gained by-product raffinate P
2o
5concentration is only about 23%, and containing a large amount of impurity such as calcium sulfate, ralstonite type compound, due to raffinate, not only grade is lower but also concentration is also lower, can not directly use on traditional phosphorus ammonium production equipment, otherwise after quality product can be caused not reach requirement, product nutrient and the underproof situation of moisture serious; In addition, low-grade lower concentration raffinate water content is too high, and can cause the water balance difficulty of phosphorus ammonium production equipment, environmental protection pressure is large.Although raffinate water content can be reduced by heating is concentrated, improve raffinate P
2o
5concentration, can directly send in the neutralization reactor of neutralization epitope monoammonium phosphate device for the production of ammonium phosphate product, but because the impurity in raffinate very easily forms at concentration heat exchanger inwall the insoluble dirty layer of acid that hard matter is close, be difficult to removing after high temperature concentrates, tubulation can be caused when fouling is serious to block, concentration operation cannot be proceeded.The dominant of its dirty layer is calcium sulfate, ralstonite type compound, uncrystalline silicon compound and iron aluminium phosphate mutually, they mix mutually, be bonded together, form the insoluble technique rock of acid of hard and compact, cleaning difficulty is very big, cause interchanger to be difficult to steady operation for a long time, make to utilize raffinate cost significantly to increase by method of enrichment.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of method utilizing low-grade lower concentration raffinate to produce phosphorus ammonium is provided, the insoluble dirty layer of acid occurring in concentration process being difficult to remove can be avoided, low-grade lower concentration raffinate can be used by conventional neutralization epitope monoammonium phosphate device.
The present inventor studies discovery: raffinate and ammonia react produce phosphor ammonium slurry, raffinate wherein impurity structure has a very large change, major part is soluble in acid, and gained phosphor ammonium slurry not easily produces fouling in concentration process, and heat exchanger tube is also very easy to cleaning.Therefore, low-grade lower concentration raffinate ammonia or containing NH
+after the material process of ion, can concentrate economically and be used by conventional neutralization epitope monoammonium phosphate device.
The present invention realizes based on above-mentioned research, and step comprises:
(1) the low-grade lower concentration raffinate of wet phosphoric acid purifying device by-product is as the ammonia in the washing system cyclic absorption tail gas of washings feeding monoammonium phosphate device and dust, until raffinate washings degree of neutralization is 0.6 ~ 0.9;
(2) by above-mentioned degree of neutralization 0.6 ~ 0.9 raffinate washings to be sent to concentrating unit heating concentrated, obtained P
2o
5concentration is at 26% ~ 30% enriching slurry;
(3) be sent to after enriching slurry being mixed with strong phosphoric acid in neutralization reactor, produce ammonium phosphate product according to a conventional method.
Raffinate washings concentration is higher, it is fewer that subsequent heat concentrates consumed heat energy, but along with the raising of raffinate washings concentration, it is poorer to the washing effect of tail gas, therefore, step of the present invention (1) gained raffinate washings degree of neutralization preferable range is 0.7 ~ 0.8.
Consider the flowing property of washing tail gas effect and enriching slurry, the P of step of the present invention (2) gained enriching slurry
2o
5concentration preferences is 27% ~ 28%.
Consider that enriching slurry proportion too much can have an impact to quality product, and proportion crosses the usage quantity affecting raffinate at least, raffinate can not digest in time, can restrict the production of purification of phosphoric acid device, therefore, the volume ratio of step (3) enriching slurry and strong phosphoric acid should control in 1:2.8 ~ 3.2.
Beneficial effect of the present invention is: with the ammonia in low-grade lower concentration raffinate absorption tail gas of monoammonium phosphate device and dust, not only can solve with easily generating the insoluble dirty layer problem of acid being difficult to clear up in low-grade lower concentration raffinate concentration process, the cost producing phosphorus ammonium with low-grade lower concentration raffinate is significantly reduced, thus obtains comparatively economic low-grade lower concentration raffinate utilization ways; But also the washing water consumption can saved needed for tail gas of monoammonium phosphate device treatment system, reduce the production cost of whole monoammonium phosphate device further.
Accompanying drawing explanation
Fig. 1 is present invention process schema.
Embodiment
Below in conjunction with accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described.
As shown in Figure 1, the P of wet phosphoric acid purifying device by-product
2o
5concentration is only sent into washing system 4 cyclic absorption of monoammonium phosphate device at the low-grade lower concentration raffinate 1 of about 23% as washings and is come ammonia in self-neutralization and tail gas generated by granulation and dust, is sent to concentrating unit 5 heating 0.6 ~ 0.9 time is concentrated into P until raffinate washings 8 degree of neutralization
2o
5concentration is 26% ~ 30% enriching slurry 9; Again by enriching slurry 9 and the P from phosphoric acid workshop
2o
5concentration be 32% ~ 33% strong phosphoric acid 2 mix after, send in neutralization reactor 6, with gas ammonia 3, neutralization reaction occurs, after reaction, obtained phosphor ammonium slurry 10 is sent to spray granulating in spray granulating machine 7 makes final ammonium phosphate product 11 through concentrated.
The raffinate washings degree of neutralization being sent to concentrating unit 5 is comparatively suitable at 0.7-0.8.
Through the enriching slurry P of concentrating unit 5 gained
2o
5concentration span of control is comparatively suitable 27% ~ 28%.
Enriching slurry 9 controls in 1:2.8 ~ 3.2 scope better with the volume ratio of strong phosphoric acid 2.
Claims (4)
1. utilize low-grade lower concentration raffinate to produce the method for phosphorus ammonium, its step comprises:
(1) the low-grade lower concentration raffinate of wet phosphoric acid purifying device by-product is as the ammonia in the washing system cyclic absorption tail gas of washings feeding monoammonium phosphate device and dust, until raffinate washings degree of neutralization is 0.6 ~ 0.9;
(2) by above-mentioned degree of neutralization 0.6 ~ 0.9 raffinate washings to be sent to concentrating unit heating concentrated, obtained P
2o
5concentration 26% ~ 30% enriching slurry;
(3) be sent to after enriching slurry being mixed with strong phosphoric acid in neutralization reactor, produce ammonium phosphate product according to a conventional method.
2. the method utilizing low-grade lower concentration raffinate to produce phosphorus ammonium according to claim 1, is characterized in that: step (1) gained raffinate washings degree of neutralization is 0.7 ~ 0.8.
3. the method utilizing low-grade lower concentration raffinate to produce phosphorus ammonium according to claim 1, is characterized in that: the P of step (2) gained enriching slurry
2o
5concentration is 27% ~ 28%.
4. the method utilizing low-grade lower concentration raffinate to produce phosphorus ammonium according to claim 1, is characterized in that: the volume ratio of step (3) enriching slurry and strong phosphoric acid is 1:2.8 ~ 3.2.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510863254.0A CN105347321B (en) | 2015-11-27 | 2015-11-27 | The method that phosphorus ammonium is produced using low-grade low concentration raffinate |
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| CN201510863254.0A CN105347321B (en) | 2015-11-27 | 2015-11-27 | The method that phosphorus ammonium is produced using low-grade low concentration raffinate |
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| CN105347321A true CN105347321A (en) | 2016-02-24 |
| CN105347321B CN105347321B (en) | 2017-08-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106348267A (en) * | 2016-08-29 | 2017-01-25 | 宜都兴发化工有限公司 | Method for producing diammonium phosphate with nitrogen and phosphorus containing wastewater |
| CN107161967A (en) * | 2017-06-29 | 2017-09-15 | 宜都兴发化工有限公司 | It is a kind of to add the method and device that raffinate clear liquid produces high-class product diammonium phosphate product |
| CN112624804A (en) * | 2020-12-24 | 2021-04-09 | 安徽六国化工股份有限公司 | Method for producing ammonium phosphate by using low-grade raffinate acid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891504A (en) * | 2010-07-26 | 2010-11-24 | 瓮福（集团）有限责任公司 | Method for producing granular monoammonium phosphate with raffinate |
| CN103896232A (en) * | 2014-03-14 | 2014-07-02 | 中国五环工程有限公司 | Method for preparing industrial grade monoammonium phosphate by using raffinate acid through twice neutralizational process |
-
2015
- 2015-11-27 CN CN201510863254.0A patent/CN105347321B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891504A (en) * | 2010-07-26 | 2010-11-24 | 瓮福（集团）有限责任公司 | Method for producing granular monoammonium phosphate with raffinate |
| CN103896232A (en) * | 2014-03-14 | 2014-07-02 | 中国五环工程有限公司 | Method for preparing industrial grade monoammonium phosphate by using raffinate acid through twice neutralizational process |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106348267A (en) * | 2016-08-29 | 2017-01-25 | 宜都兴发化工有限公司 | Method for producing diammonium phosphate with nitrogen and phosphorus containing wastewater |
| CN106348267B (en) * | 2016-08-29 | 2019-01-29 | 宜都兴发化工有限公司 | A kind of method and device of Nitrogen-and Phosphorus-containing waste water production Diammonium phosphate (DAP) |
| CN107161967A (en) * | 2017-06-29 | 2017-09-15 | 宜都兴发化工有限公司 | It is a kind of to add the method and device that raffinate clear liquid produces high-class product diammonium phosphate product |
| CN112624804A (en) * | 2020-12-24 | 2021-04-09 | 安徽六国化工股份有限公司 | Method for producing ammonium phosphate by using low-grade raffinate acid |
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|---|---|
| CN105347321B (en) | 2017-08-25 |
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