CN100383057C - Method for removing impurities in phosphoric acid and deposition purificant used in the method - Google Patents
Method for removing impurities in phosphoric acid and deposition purificant used in the method Download PDFInfo
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- CN100383057C CN100383057C CNB2005102005068A CN200510200506A CN100383057C CN 100383057 C CN100383057 C CN 100383057C CN B2005102005068 A CNB2005102005068 A CN B2005102005068A CN 200510200506 A CN200510200506 A CN 200510200506A CN 100383057 C CN100383057 C CN 100383057C
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Abstract
The present invention discloses a method for removing impurities in phosphoric acid and a deposition purificant used in the method, and relates to the technical field of the manufacture of phosphoric fertilizers. The present invention has the core of forming objects of the deposition purificant used in the method. A deposition accelerant in the deposition purificant comprises soluble inorganic salt with calcium and barium, and saturated resin; a macromolecular flocculation agent of the deposition purificant at least comprises one kind of polymeric cellulose ether and polyacrylamide; a filtration aid agent of the deposition purificant comprises a plurality of inorganic multiporous bodies and copolymer synthetic resin with a micropore structure and a multiporous structure. The present invention is suitable for removing phosphoric acid produced by a wet method or impurities in a phosphorus ammonium product using the phosphoric acid as raw material. The effect of the present invention can make product purity achieve 99%. Consequently, the present invention satisfies the requirement of phosphorus ammonium fertilizers used for drip irrigation.
Description
Technical field
The present invention relates to phosphate fertilizer manufacturing technology field, especially a kind ofly be used for removing phosphoric acid or be the method and the used precipitation scavenging agent of this method of the phosphorus ammonium fertilizer impurities of raw material with phosphoric acid.
Background technology
The main raw material of making the phosphorus ammonium is a phosphoric acid.Phosphoric acid is to be transformed from Rock Phosphate (72Min BPL), and phosphoric acid makes method with it, can be divided into dry method phosphoric acid and phosphoric acid by wet process.The production of dry method phosphoric acid mainly be by Rock Phosphate (72Min BPL) in electric furnace through pyrolytic decomposition, make phosphorus distil out, being elevated phosphorus through collecting, promptly the yellow phosphorus of based on very high purity makes phosphoric acid with it then.This phosphoric acid is that impurity is few, the phosphoric acid of based on very high purity.But power consumption is very big in process of production, also has environmental issue, and production cost is too high, and industrial scale also is subjected to very big restriction, thereby is not suitable for being used in fertile in the production of phosphorus ammonium.The production of phosphoric acid by wet process mainly is Rock Phosphate (72Min BPL) to be added water grind and to be slurry, then and strong sulfuric acid response, and generates phosphoric acid and calcium sulfate precipitation, obtains calcium sulfate and dilute phosphoric acid after filtering.It is little that the phosphoric acid of this wet production has power consumption, environmental issue is few, production cost is low, be applicable to that mass production is fertile on the phosphorus ammonium, but the phosphoric acid that this processing method is produced, can be with inorganic the sneaking in the dilute phosphoric acid in the Rock Phosphate (72Min BPL) with organic impurity, so there is a large amount of impurity in the phosphoric acid of wet production gained, as metallic cations such as calcium, magnesium, aluminium, iron, sodium, potassium, sulfate radical, silicate, chlorine root, sial acid group and precipitable fouling tendency salt that they constituted are also arranged, also have organism and biological organogel class material.Owing to there is this a large amount of one-tenth dirt material to exist, phosphoric acid by wet process can constantly have the formation of dirt, using with this phosphoric acid is the phosphorus ammonium fertilizer of raw material production, can be because wherein insolubles and foreign matter content be high and influence its purity, do not reach the quality standard of technical grade drip irrigation fertilizer, the picture mud that they can obtain after being dissolved in the water, the material of mixed soup shape can not be used for drip irrigation system, otherwise alluvial and obstruction can take place.At present along with high-tech enters into modern agriculture, the drip irrigation technique of water saving, the fertile environment-friendly type of joint is developed by leaps and bounds abroad, and is also increasing to the demand of the drip irrigation fertilizer that is suitable for the fertigation system at home.Drip irrigation is very urgent with the ammophos demand.How removing phosphate raw material or be impurity contained in the phosphorus ammonium fertilizer of raw material with the phosphoric acid of wet production, is the outstanding problem during the drip irrigation phosphorus ammonium fertilizer is produced.In existing technical scheme, the removal of above-mentioned impurity, be in raw material phosphoric acid or in phosphorus ammonium fertilizer solution, to add precipitation agent, above-mentioned contamination precipitation is separated, obtain meeting the ammonium phosphate product of drip irrigation purity needs again by operations such as concentrated, recrystallize, dryings.The selection that wherein precipitates scavenging agent is crucial, the precipitation scavenging agent can make all kinds of impurity in the phosphoric acid of wet production can obtain precipitation and separate out, thereby remove clean as far as possible, the ideal precipitation agent can obtain thick throw out, thereby help filtering separation and realize filtering automatization continuous production process and flow production greatly, and finally can obtain the very high phosphorus crystalline ammonium product of purity.The drip irrigation fertilizer ammonium phosphate production line that has built up at present all exists not enough in the selection of precipitation scavenging agent, generally mostly is to be made of precipitating inorganic salt and the material that plays filtrating aid function.The calcium ion of wherein precipitating inorganic salt as providing the precipitated sulfur acid group to use with calcium chloride, calcium carbonate stone powder and milk of lime, the material that plays flocculating aids adopts as intumescence stone flour, diatomite in powder, volcanic ash, attapulgite etc.Though this precipitation agent has certain precipitating action, but its effect is still not satisfactory, uses it for precipitation and purifies, and the purity of its product can only reach 97% reluctantly, and be difficult in process of production the throw out filtering separation, productive efficiency can only reach 50%～70% of capacity of equipment.
Summary of the invention
The invention provides the precipitation scavenging agent that is used for removing the phosphoric acid product impurities in a kind of method of removing phosphoric acid impurity and this method, their problems to be solved are that the impurity that will bring in the technology with Wet-process phosphoric acid (WPPA) is to precipitate the product of raw material from phosphoric acid or with phosphoric acid with comparatively thick precipitated form, so that with they filtering separation, thereby improve phosphoric acid or be the purity of the product of raw material with phosphoric acid.
The present invention removes the method for phosphoric acid impurity, it includes and add soluble inorganic salt and the polymeric flocculant that has calcium or barium in phosphoric acid solution, carrying out phosphoric acid precipitates with inorganic porous body and resin-oatmeal as the precipitation scavenging agent that flocculating aids was constituted purifies, and the process portion that the throw out filtering separation is come out, in the described precipitation scavenging agent that adds, also had central a kind of of the poly-ether of cellulose of the saturated resin of precipitation promoter action and a throwing out and polyacrylamide.
Described saturated resin preferably is adsorbed with the saturated resin of metal ion, can also comprise that in described precipitation scavenging agent the interpolymer synthetic resins with micropore and vesicular structure is as flocculating aids.After with the throw out filtering separation in the phosphoric acid, adopt ion exchange resin can further remove foreign ion to filtrate.
The method of above-mentioned removal phosphorus ammonium fertilizer impurity also can be used for removing the impurity of phosphorus ammonium fertilizer solution, be that it includes in phosphorus ammonium fertilizer solution and to add soluble inorganic salt and the polymeric flocculant that has calcium or barium, carrying out phosphoric acid precipitates with inorganic porous body and resin-oatmeal as the precipitation scavenging agent that flocculating aids was constituted purifies, and the process portion that the throw out filtering separation is come out, in the described precipitation scavenging agent that adds, also had central a kind of of the poly-ether of cellulose of the saturated resin of precipitation promoter action and a throwing out and polyacrylamide.
In the method for impurity, described saturated resin preferably is adsorbed with the saturated resin of metal ion in above-mentioned removal phosphorus ammonium fertilizer solution, can also comprise that in described precipitation scavenging agent the interpolymer synthetic resins with micropore and vesicular structure is as flocculating aids.After with the throw out filtering separation in the phosphoric acid, adopt ion exchange resin can further remove foreign ion to filtrate.
In the method for above-mentioned removal phosphoric acid impurity with remove in the precipitation scavenging agent used in the method for impurity in the phosphorus ammonium fertilizer solution, its precipitation promoter includes soluble inorganic salt, saturated resin and the polymeric flocculant of calcium or barium; Its flocculating aids includes the interpolymer synthetic resin powder with the material of inorganic porous body structure and micropore and vesicular structure.
In the above-mentioned precipitation scavenging agent, described saturated resin preferably is adsorbed with the saturated resin of metal ion; Described polymeric flocculant can be to include a kind of in poly-ether of cellulose and the polyacrylamide at least.The constituent weight ratio of above-mentioned precipitation scavenging agent can be: the soluble inorganic salt of described calcium or barium is 45%～60%, and described saturated resin is 5%～10%, and described flocculation agent is 0.5%～1%, and described flocculating aids is 30%～45%.
The brand-new type precipitation scavenging agent of this research invention.Its main composition prescription is:
Technique scheme of the present invention has following beneficial effect to prior art:
Precipitation promoter of the present invention adopts this family macromolecule throw out of saturated resin and calcic, barium soluble inorganic salt to combine, be aided with the inorganic of multi-cellular structure and polymeric retention aid filtering agent again, can reach mineral ion and the isolating purpose of the abundant precipitating of biological organism in the impurity, filterability is good, be convenient to serialization, automatization, the scale operation running of filtering separation, Crystallization Separation is good, and product purity is also high; In precipitation agent, add polymeric flocculant, can make the chap of inorganic salts precipitation body big, make latex obtain dispersive organic-biological body flocculating agglomerating and be beneficial to and remove; Flocculating aids in the precipitation agent is except that adopting prior art several inorganic porous body materials commonly used, also adopt the resin of micropore and porous shape interpolymer, help the filter effect better, more help separating of filtrate and filter mud, obtain the peace and quiet filtrate that impurity removes substantially, condensing crystal after assurance connects, with Crystallization Separation, operations such as drying are along carrying out soon.Also make the filtering separation of post precipitation become simple, be convenient to this operation mechanize, automatization and continuity, carry out to high yield.
Adopt the phosphorus ammonium fertilizer of the phosphoric acid of wet production as the raw material manufacturing, show with the actual effect of precipitation agent of the present invention with the method for removing the impurity in phosphoric acid or the phosphorus ammonium fertilizer: the purity of the final phosphorus ammonium fertilizer that obtains can meet the standard of drip irrigation with fertilizer fully up to 99%.
If after wherein impurity is carried out filtering separation, adopt ion exchange resin further to remove foreign ion to filtrate, can also make product obtain decolouring, can obtain complete water white xln.
Adopt technical scheme of the present invention, can more easily the throw out filtering separation be come out in process of production, bring up to more than 90% thereby productive efficiency can only be able to be reached 50%～70% of capacity of equipment from prior art.
Description of drawings
Fig. 1 is a process frame chart of removing phosphoric acid impurity.
Fig. 2 is a process frame chart of removing phosphorus ammonium fertilizer impurity.
Embodiment
Embodiment 1: making the precipitation scavenging agent that double centner is removed impurities in phosphoric acid, the ammonium phosphate product, is constituent in the following prescription to be mixed according to quantity get final product.
Embodiment 2: making the precipitation scavenging agent that double centner is removed impurities in phosphoric acid, the ammonium phosphate product, is constituent in the following prescription to be mixed according to quantity get final product.
Embodiment 3: the method for removing phosphoric acid impurity.
As shown in Figure 1, phosphoric acid is placed the precipitation refining plant, the precipitation scavenging agent that adds the foregoing description 1 or 2 in 1%～5% ratio, left standstill 12～24 hours, then with supercentrifuge with throw out in the slip and solution separating, the gained throw out can be used for doing composite fertilizer, places in the exchange column spent ion exchange resin to make with extra care gained solution, after treatment the higher purification of phosphoric acid of purity.
Embodiment 4: phosphorus ammonium purifying processing method.
As shown in Figure 2; ammonium phosphate solution is placed settling tank; the precipitation scavenging agent that adds the foregoing description 1 or 2 in 1%～5% ratio; by effects such as precipitation, flocculations; with the impurity macrobeadization; and after leaving standstill 12～24 hours; under the assistance of flocculating aids with supercentrifuge with throw out in the slip and solution separating; thereby obtain high-purity phosphoric acid two ammonium solutions; again by ion exchange unit with its purification and decoloration; scavenging solution again through concentrate, operations such as neutralization, crystallization, separation, drying, finally form purity up to 99% product.
Claims (9)
1. method of removing the phosphoric acid impurities, it includes and add soluble inorganic salt and the polymeric flocculant that has calcium or barium in phosphoric acid solution, carrying out phosphoric acid precipitates with inorganic porous body and resin-oatmeal as the precipitation scavenging agent that flocculating aids was constituted purifies, and the process portion that the throw out filtering separation is come out, it is characterized in that: in the described precipitation scavenging agent that adds, also had central a kind of of the poly-ether of cellulose of the saturated resin of precipitation promoter action and a throwing out and polyacrylamide.
2. the method for removal phosphoric acid impurities according to claim 1 is characterized in that: described saturated resin is the saturated resin that is adsorbed with metal ion; Comprise also that in described precipitation scavenging agent the interpolymer synthetic resins with micropore and vesicular structure is as flocculating aids.
3. the method for removal phosphoric acid impurities according to claim 1 and 2 is characterized in that: after with the throw out filtering separation in the phosphoric acid, adopt ion exchange resin further to remove foreign ion to filtrate.
4. method of removing phosphorus ammonium fertilizer impurity, it includes and add soluble inorganic salt and the polymeric flocculant that has calcium or barium in phosphorus ammonium fertilizer solution, carrying out phosphoric acid precipitates with inorganic porous body and resin-oatmeal as the precipitation scavenging agent that flocculating aids was constituted purifies, and the process portion that the throw out filtering separation is come out, it is characterized in that: in the described precipitation scavenging agent that adds, also had central a kind of of the poly-ether of cellulose of the saturated resin of precipitation promoter action and a throwing out and polyacrylamide.
5. the method for removal phosphorus ammonium fertilizer impurity according to claim 4 is characterized in that: described saturated resin is the saturated resin that is adsorbed with metal ion; Comprise also that in described precipitation scavenging agent the interpolymer synthetic resins with micropore and vesicular structure is as flocculating aids.
6. according to the method for claim 4 or 5 described removal phosphorus ammonium fertilizer impurity, it is characterized in that: after with the throw out filtering separation in the phosphorus ammonium fertilizer solution, adopt ion exchange resin further to remove foreign ion filtrate.
7. precipitation scavenging agent of removing impurities in the phosphoric acid product, it is characterized in that: its precipitation promoter includes soluble inorganic salt, saturated resin and the polymeric flocculant of calcium or barium; Its flocculating aids includes the material of inorganic porous body structure and the interpolymer synthetic resin powder of micropore and vesicular structure.
8. according to the precipitation scavenging agent of impurities in the described removal phosphoric acid product of claim 7, it is characterized in that: described saturated resin is the saturated resin that is adsorbed with metal ion; Described polymeric flocculant includes a kind of in poly-ether of cellulose and the polyacrylamide at least.
9. according to the precipitation scavenging agent of impurities in claim 7 or the 8 described removal phosphoric acid products, it is characterized in that: the weight ratio of its constituent is: the soluble inorganic salt of described calcium or barium is 45%～60%, described saturated resin is 5%～10%, described flocculation agent is 0.5%～1%, and described flocculating aids is 30%～45%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005102005068A CN100383057C (en) | 2005-08-31 | 2005-08-31 | Method for removing impurities in phosphoric acid and deposition purificant used in the method |
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| CNB2005102005068A CN100383057C (en) | 2005-08-31 | 2005-08-31 | Method for removing impurities in phosphoric acid and deposition purificant used in the method |
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| CN1730406A CN1730406A (en) | 2006-02-08 |
| CN100383057C true CN100383057C (en) | 2008-04-23 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102133495B (en) * | 2011-01-20 | 2012-09-26 | 山东金正大生态工程股份有限公司 | Method for purifying acidolysis solution by filter aid and polyacrylamide |
| CN102166452B (en) * | 2011-01-20 | 2012-11-28 | 山东金正大生态工程股份有限公司 | Method for filtration-assisted purification of acidolysis solution obtained in the process of decomposing phosphorite by using nitric acid |
| CN102219198A (en) * | 2011-05-03 | 2011-10-19 | 湖北富邦科技股份有限公司 | Multifunctional sinking agent used in production of phosphoric acid by wet method |
| CN104310328A (en) * | 2014-10-09 | 2015-01-28 | 瓮福（集团）有限责任公司 | Method for primary purification of phosphoric acid by using wet process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02135190A (en) * | 1988-11-17 | 1990-05-24 | Mitsui Petrochem Ind Ltd | Treatment of waste water containing phosphorus |
| CN1608034A (en) * | 2001-10-25 | 2005-04-20 | Imc环球动作公司 | Purification of phosphoric acid plant pond water |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02135190A (en) * | 1988-11-17 | 1990-05-24 | Mitsui Petrochem Ind Ltd | Treatment of waste water containing phosphorus |
| CN1608034A (en) * | 2001-10-25 | 2005-04-20 | Imc环球动作公司 | Purification of phosphoric acid plant pond water |
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