CN102502553A - Method for preparing feed grade calcium hydrogen phosphate from waste water of phosphate fertilizer plant - Google Patents
Method for preparing feed grade calcium hydrogen phosphate from waste water of phosphate fertilizer plant Download PDFInfo
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- CN102502553A CN102502553A CN2011102927263A CN201110292726A CN102502553A CN 102502553 A CN102502553 A CN 102502553A CN 2011102927263 A CN2011102927263 A CN 2011102927263A CN 201110292726 A CN201110292726 A CN 201110292726A CN 102502553 A CN102502553 A CN 102502553A
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Abstract
The invention discloses a method for preparing feed grade calcium hydrogen phosphate from waste water of a phosphate fertilizer plant. The method includes steps that silicon dioxide and sodium chloride are added into waste water, which contains from 0.6 to 1.8% of phosphorous and from 0.50 to 0.80% of fluorine, of the phosphate fertilizer plant to realize primary defluorination; lime milk and sodium fluoride are added into waste water after the primary defluorination, a pH (potential of hydrogen) value ranges from 2.28 to 2.62 at the end point of reaction, flocculating agent with the mass concentration ranging from 0.1% to 1% is added into mixture of the waste water, the lime milk and the sodium fluoride after reaction to realize sedimentation, sedimentation time ranges from 1 hour to 2 hours, and purified filter liquor is prepared after centrifugal filtration; and lime milk is added into the purified filter liquor, reaction condition conditions includes that reaction temperature ranges from 25 DEG C to 38 DEG C, reaction time ranges from 1 hour to 2 hours and stirring speed is 250 revolutions/minute, a pH value ranges from 5.2 to 6.2 at the end point of the reaction, sedimentation continues for 1 hour to 1.5 hours after reaction is completed, centrifugal filtration is carried out, and a product is obtained after a drying process by the aid of filter cakes. The product of the method is high in additional value and resource utilization rate, treatment cost for sewage of the phosphate fertilizer plant is lowered, and environmental pollution is reduced.
Description
Technical field
The invention belongs to chemical technology field, relate in particular to a kind of method that Vanadium Pentoxide in FLAKES is produced calcium hydrophosphate fodder that from phosphate fertilizer plant's waste water, reclaims
Background technology
Calcium hydrophosphate fodder (CaHPO
42H
2O) be a kind of large phosphorus chemical product that wide market outlook are arranged; It is a kind of phosphorus, the good poultry of two kinds of nutritive elements of calcium, cattle food mineral additive of containing, because m (P) wherein: m (Ca)=1:1.29, more approaching with the phosphorus calcium in the animal skeleton than; Simultaneously can all be dissolved in the animal hydrochloric acid in gastric juice again; So get in the animal body easily and participation metabolism, form the needed hormone of human body, enzyme and VITAMINs, keep the phosphorus calcium ratio in the bone; Thereby prevent that animal from because of the caused various diseases of calcium deficiency, promoting animal body to grow fast simultaneously.Its effect of raising obtains generally acknowledging of various countries already.In recent years, along with developing rapidly of China's husbandry, animal husbandry, aquaculture and feed processing industry extensive, intensification develop at a speed unheard of before, and the home market is increasing to the demand of raising calcium.
The working method of calcium hydrophosphate fodder is divided into by-product processing method and chemical process method substantially.The former is a raw material with the assorted bone of animal, and by-product small amounts of phosphoric acid hydrogen calcium is one of method of producing the earliest the phosphatic feed additive when producing gelatine.The product that this method is produced, phosphorus calcium are than suitable, but after mad cow disease had taken place in West Europe, this method was restricted in many countries.The chemical process method also is the phosphorus ore processing method, is divided into Re Fa and wet method usually.Hot method processing method is to be processed into phosphoric acid by electric furnace process yellow phosphorus, is processed into calcium hydrophosphate fodder by phosphoric acid again.Wet processes is normally produced phosphate aqueous solution with the mineral acid decomposing phosphate rock, ins all sorts of ways then to remove the detrimental impurity that phosphorus ore is brought into, produces calcium hydrophosphate fodder with calcium salt or quicklime reaction again.Wet method can be divided into salt acid system, sulfuric acid process, nitrate method etc. again by the mineral acid difference that it adopted.In addition, also has superphosphate of lime aqueous extraction method etc.Chinese patent 200610020230.X discloses " phosphorus ore hydrochloric acid absorption method is produced the method for calcium hydrophosphate fodder and PHOSPHORIC ACID TECH.GRADE ", and detailed process is with salt soak phosphate rock-sulfuric acid stone, acid hydrolysis solution is added thermal distillation reclaim hydrochloric acid, obtains Ca (H simultaneously
2PO
4)
2, with hydrochloric acid and Ca (H
2PO
4)
2After having collected, at remaining CaCl
2Feed CO in the liquid
2, add thermal distillation simultaneously and reclaim hydrochloric acid again, use highly purified Ca (H again
2PO
4)
2With H
2SO
4Metathesis makes PHOSPHORIC ACID TECH.GRADE; PH obtains the calcium hydrophosphate fodder finished product with the milk of lime adjustment.This working method complex process, long reaction time needs to consume a large amount of phosphorus ore resources; Adding thermal distillation, to reclaim the hydrochloric acid energy consumption high, and the waste gas hydrogenchloride that process produces reclaims not exclusively, a large amount of phosphogypsum slags arranged after adding sulfuric acid in process of production, and environment is caused serious pollution.
More than producing the method for calcium hydrophosphate fodder, is that wet method or hot method all are on the basis that is raw material, to produce with phosphorus ore or phosphoric acid.These methods all are faced with the production cost height, and the market competitiveness is low, and to problems such as environmental influence are big.And along with the continuous reduction of phosphorus ore grade, the cost that utilizes Rock Phosphate (72Min BPL) to produce calcium hydrophosphate fodder also can continue to increase.
Summary of the invention
The cost that a kind of value-added content of product that the objective of the invention is to overcome above-mentioned shortcoming and provide is high, resource utilization is high, reduced phosphate fertilizer plant's WWT and reduce the pollution of environment produced the method for calcium hydrophosphate fodder with phosphate fertilizer plant's waste water.
The object of the invention and solve its technical problem underlying and adopt following technical scheme to realize:
Of the present inventionly a kind ofly prepare the method for calcium hydrophosphate fodder, may further comprise the steps with phosphate fertilizer plant's waste water:
(1) pre-treatment of waste water
A, preliminary defluorinate: at phosphorus content is 0.6-1.8%; Fluorine content is to add silicon-dioxide and sodium-chlor in phosphate fertilizer plant's waste water of 0.50-0.80%; Wherein the weight ratio of fluorine content is 1-1.2 ︰ 1 in silicon-dioxide and the waste water, and the weight ratio of fluorine content is 1-3 ︰ 1 in sodium-chlor and the waste water, and reaction conditions is: temperature of reaction is 30-50 ℃; Reaction times is 1-2h, and stirring velocity is 250 rev/mins;
B, degree of depth defluorinate: preliminary defluorinate waste water in add milk of lime, sodium sulphite, the quality of sodium sulphite is 0.0125% of a wastewater quality, the quality of milk of lime is 1.8% of a wastewater quality; Mass concentration is 5-20%, and reaction conditions is: temperature of reaction 30-50 ℃, the reaction times is 1-2h; Stirring velocity is 250 rev/mins; Reaction end pH value is 2.28-2.62, adds the sedimentation of mass concentration 0.1-1% flocculation agent after reaction is accomplished, and the quality of flocculation agent is 0.125% of a charging wastewater quality; Settling time is 1-2h, the filtrating after centrifuging is purified;
(2) preparation calcium hydrophosphate fodder
Add milk of lime in the filtrating after purification, the quality of milk of lime is 1.5% of a wastewater quality, and mass concentration is 5-20%; Reaction conditions is: temperature of reaction 25-38 ℃, the reaction times is 1-2h, and stirring velocity is 250 rev/mins; Reaction end pH value is 5.2-6.2; Reaction finishes back sedimentation 1-1.5h, centrifuging, and filtration cakes torrefaction obtains product.
Above-mentioned a kind ofly produce the method for calcium hydrophosphate fodder with phosphate fertilizer plant's waste water, wherein: the filtrating behind the preparation calcium hydrophosphate fodder product after purifying as the process water of phosphoric acid system.
The present invention compared with prior art; Has tangible beneficial effect; Can be known by above technical scheme: the present invention adopts two step defluorinate methods that phosphate fertilizer plant's waste water is carried out purifying treatment, and then adding milk of lime carries out neutralization reaction and then obtains calcium hydrophosphate fodder in the waste water after purifying.So both effectively recycled the phosphorus in the waste water, also reduced the content of fluorion in the waste water simultaneously, reduced the pollution of waste water environment.The present invention has the following advantages: the one, effectively utilized free phosphorus in phosphate fertilizer plant's waste water, and improve the utilization ratio of resource; The 2nd, reduced the cost of phosphate fertilizer plant's WWT, improved the ability of WWT; The 3rd, for enterprise has increased a fine phosphate product, and owing to produce the with low cost of this product, value-added content of product is high, has the stronger market competitiveness, for enterprise brings great economic benefit; The 4th, reduce phosphorus content and fluorine content in the waste water when reclaiming phosphorus, reduce pollution to environment, society provides technical support for the friendly type of creation environment.
Embodiment
Embodiment 1
A kind ofly prepare the method for calcium hydrophosphate fodder, may further comprise the steps with phosphate fertilizer plant's waste water:
(1) pre-treatment of waste water
A, preliminary defluorinate: in the 2000g phosphate fertilizer plant waste water of phosphorus content 1%, fluorine content 0.50%, add 10g silicon-dioxide and 10g sodium-chlor; Reaction conditions is: temperature of reaction is 30 ℃; Reaction times is 1h; Stirring velocity is 250 rev/mins, obtains P content and be 0.92%, F content is 0.36% preliminary defluorinate water sample;
B, degree of depth defluorinate: in the waste water of preliminary defluorinate, add milk of lime, sodium sulphite, the mass concentration of milk of lime is 5%, and the quality of lime is 36g, and the quality of sodium sulphite is 0.25g.Reaction conditions is: 50 ℃ of temperature of reaction; Reaction times is 2h, and stirring velocity is 250 rev/mins, and reaction end pH value is 2.28; The adding mass concentration was 0.1% flocculant of modified polyacrylamide 10g flocculating settling after reaction was accomplished; Settling time is 1h, the filtrating after centrifuging is purified, and filter cake is the fertilizer grade secondary calcium phosphate;
(2) preparation calcium hydrophosphate fodder
Add milk of lime 30g in the filtrating after purification, the mass concentration of milk of lime is 5%, and reaction conditions is: 30 ℃ of temperature of reaction; Reaction times is 1h, and stirring velocity is 250 rev/mins, and reaction end pH value is 5.2; Reaction finishes back sedimentation 1.5h, centrifuging, and filtration cakes torrefaction obtains product.Result data sees the following form:
Embodiment 2
A kind ofly prepare the method for calcium hydrophosphate fodder, may further comprise the steps with phosphate fertilizer plant's waste water:
(1) pre-treatment of waste water
A, preliminary defluorinate: in the 2000g phosphate fertilizer plant waste water of phosphorus content 1.2%, fluorine content 0.60%, add 13.2g silicon-dioxide and 18.0g sodium-chlor; Reaction conditions is: 40 ℃ of temperature of reaction, 1.5 hours reaction times; 250 rev/mins of mixing speed obtain P content and are 1.13%, F content is 0.42% preliminary defluorinate water sample.
B, degree of depth defluorinate: preliminary defluorinate waste water in add milk of lime, sodium sulphite, the mass concentration of milk of lime is 15%, the quality of lime is 36g, the quality of sodium sulphite is 0.25g.Reaction conditions is: 45 ℃ of temperature of reaction; Reaction times is 2h, and stirring velocity is 250 rev/mins, and reaction end pH value is 2.38; The adding mass concentration was 0.5% flocculant of modified polyacrylamide 5g flocculating settling after reaction was accomplished; Settling time is 1h, the filtrating after centrifuging is purified, and filter cake is the fertilizer grade secondary calcium phosphate;
(2) preparation calcium hydrophosphate fodder
Add milk of lime 30g in the filtrating after purification, the mass concentration of milk of lime is 10%, and reaction conditions is: 38 ℃ of temperature of reaction; Reaction times is 1h, and stirring velocity is 250 rev/mins, and reaction end pH value is 5.6; Reaction finishes back sedimentation 1.5h, centrifuging, and filtration cakes torrefaction obtains product.Result data sees the following form:
Embodiment 3
A kind ofly prepare the method for calcium hydrophosphate fodder, may further comprise the steps with phosphate fertilizer plant's waste water:
(1) pre-treatment of waste water
A, preliminary defluorinate: in the 4000g phosphate fertilizer plant waste water of phosphorus content 0.6%, fluorine content 0.52%, add 20.8g silicon-dioxide and 41.6g sodium-chlor; Reaction conditions is: 50 ℃ of temperature of reaction, 2 hours reaction times; 250 rev/mins of mixing speed obtain P content and are 0.52%, F content is 0.35% preliminary defluorinate water sample.
B, degree of depth defluorinate: preliminary defluorinate waste water in add milk of lime, sodium sulphite, the mass concentration of milk of lime is 20%, the quality of lime is 72g, the quality of sodium sulphite is 0.5g.Reaction conditions is: 50 ℃ of temperature of reaction; Reaction times is 2h, and stirring velocity is 250 rev/mins, and reaction end pH value is 2.5; The adding mass concentration was 1% flocculant of modified polyacrylamide 5g flocculating settling after reaction was accomplished; Settling time is 1h, the filtrating after centrifuging is purified, and filter cake is the fertilizer grade secondary calcium phosphate;
(2) preparation calcium hydrophosphate fodder
Add milk of lime 60g in the filtrating after purification, the mass concentration of milk of lime is 20%, and reaction conditions is: 25 ℃ of temperature of reaction; Reaction times is 2h, and stirring velocity is 250 rev/mins, and reaction end pH value is 6.2; Reaction finishes back sedimentation 1.5h, centrifuging, and filtration cakes torrefaction obtains product.Result data sees the following form:
Embodiment 4
A kind ofly prepare the method for calcium hydrophosphate fodder, may further comprise the steps with phosphate fertilizer plant's waste water:
(1) pre-treatment of waste water
A, preliminary defluorinate: in the 2000g phosphate fertilizer plant waste water of phosphorus content 1.8%, fluorine content 0.8%, add 19.2gSiO2 and 48gNaCl; Reaction conditions is: 45 ℃ of temperature of reaction, 2 hours reaction times; 250 rev/mins of mixing speed obtain P content and are 1.74%, F content is 0.65% preliminary defluorinate water sample.
B, degree of depth defluorinate: preliminary defluorinate waste water in add milk of lime, sodium sulphite, the mass concentration of milk of lime is 20%, the quality of lime is 36g, the quality of sodium sulphite is 0.25g.Reaction conditions is: 50 ℃ of temperature of reaction; Reaction times is 2h, and stirring velocity is 250 rev/mins, and reaction end pH value is 2.62; The adding mass concentration was 1% flocculant of modified polyacrylamide 5g flocculating settling after reaction was accomplished; Settling time is 1h, the filtrating after centrifuging is purified, and filter cake is the fertilizer grade secondary calcium phosphate;
(2) preparation calcium hydrophosphate fodder
Add milk of lime 30g in the filtrating after purification, the mass concentration of milk of lime is 15%, and reaction conditions is: 35 ℃ of temperature of reaction; Reaction times is 2h, and stirring velocity is 250 rev/mins, and reaction end pH value is 6.0; Reaction finishes back sedimentation 1.5h, centrifuging, and filtration cakes torrefaction obtains product.The test-results data see the following form:
According to the inventionly be not limited to the embodiment described in the embodiment, those skilled in the art's technical scheme according to the present invention draws other embodiment, belongs to technological innovation scope of the present invention equally.Obviously, those skilled in the art can carry out various changes and modification to the present invention and not break away from the spirit and scope of the present invention.Like this, belong within the scope of claim of the present invention and equivalent technologies thereof if of the present invention these are revised with modification, then the present invention also is intended to comprise these changes and modification interior.
Claims (2)
1. one kind prepares the method for calcium hydrophosphate fodder with phosphate fertilizer plant's waste water, may further comprise the steps:
(1) pre-treatment of waste water
A, preliminary defluorinate: at phosphorus content is 0.6-1.8%; Fluorine content is to add silicon-dioxide and sodium-chlor in phosphate fertilizer plant's waste water of 0.50-0.80%; Wherein the weight ratio of fluorine content is 1-1.2 ︰ 1 in silicon-dioxide and the waste water, and the weight ratio of fluorine content is 1-3 ︰ 1 in sodium-chlor and the waste water, and reaction conditions is: temperature of reaction is 30-50 ℃; Reaction times is 1-2h, and stirring velocity is 250 rev/mins;
B, degree of depth defluorinate: preliminary defluorinate waste water in add milk of lime, sodium sulphite, the quality of sodium sulphite is 0.0125% of a wastewater quality, the quality of milk of lime is 1.8% of a wastewater quality; Mass concentration is 5-20%, and reaction conditions is: temperature of reaction 30-50 ℃, the reaction times is 1-2h; Stirring velocity is 250 rev/mins; Reaction end pH value is 2.28-2.62, adds the sedimentation of mass concentration 0.1-1% flocculation agent after reaction is accomplished, and the quality of flocculation agent is 0.125% of a charging wastewater quality; Settling time is 1-2h, the filtrating after centrifuging is purified;
(2) preparation calcium hydrophosphate fodder
Add milk of lime in the filtrating after purification, the quality of milk of lime is 1.5% of a wastewater quality, and mass concentration is 5-20%; Reaction conditions is: temperature of reaction 25-38 ℃, the reaction times is 1-2h, and stirring velocity is 250 rev/mins; Reaction end pH value is 5.2-6.2; Reaction finishes back sedimentation 1-1.5h, centrifuging, and filtration cakes torrefaction obtains product.
2. as claimed in claim 1ly a kind ofly produce the method for calcium hydrophosphate fodder with phosphate fertilizer plant's waste water, wherein: the filtrating behind the preparation calcium hydrophosphate fodder product after purifying as the process water of phosphoric acid system.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730655A (en) * | 2012-06-26 | 2012-10-17 | 瓮福（集团）有限责任公司 | Method for preparing phosphoric acid with high density by microwave heating of fertilizer grade phosphoric acid |
| CN103213962A (en) * | 2013-04-19 | 2013-07-24 | 武汉工程大学 | Method for preparing feed-grade calcium hydrophosphate from phosphoric acid-containing mixed acid etching waste liquid |
| CN103435024A (en) * | 2013-08-08 | 2013-12-11 | 瓮福（集团）有限责任公司 | Method for producing feed grade calcium hydrophosphate |
| CN103738931A (en) * | 2013-11-26 | 2014-04-23 | 瓮福（集团）有限责任公司 | Method for production of potassium dihydrogen phosphate from phosphorus-containing acidic wastewater |
| CN104276562A (en) * | 2014-10-30 | 2015-01-14 | 瓮福（集团）有限责任公司 | Method for preparing feed-grade calcium hydrogen phosphate by using washing wastewater produced by phosphoric acid process activated carbon |
| CN106167272A (en) * | 2016-02-23 | 2016-11-30 | 瓮福（集团）有限责任公司 | Utilize the method that Phosphate Fertilizer Industry waste water produces feed grade calcium carbonate |
| CN109153570A (en) * | 2016-05-18 | 2019-01-04 | 凯米拉公司 | The production of phosphatic fertilizer |
| CN112408350A (en) * | 2020-11-03 | 2021-02-26 | 中国五环工程有限公司 | Process for producing feed-grade calcium hydrophosphate from phosphorus-containing wastewater |
| CN113233438A (en) * | 2021-06-15 | 2021-08-10 | 瓮福（集团）有限责任公司 | Method for controlling arsenic and increasing yield of calcium hydrophosphate product |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730655B (en) * | 2012-06-26 | 2013-12-18 | 瓮福（集团）有限责任公司 | Method for preparing phosphoric acid with high density by microwave heating of fertilizer grade phosphoric acid |
| CN102730655A (en) * | 2012-06-26 | 2012-10-17 | 瓮福（集团）有限责任公司 | Method for preparing phosphoric acid with high density by microwave heating of fertilizer grade phosphoric acid |
| CN103213962B (en) * | 2013-04-19 | 2015-05-06 | 武汉工程大学 | Method for preparing feed-grade calcium hydrophosphate from phosphoric acid-containing mixed acid etching waste liquid |
| CN103213962A (en) * | 2013-04-19 | 2013-07-24 | 武汉工程大学 | Method for preparing feed-grade calcium hydrophosphate from phosphoric acid-containing mixed acid etching waste liquid |
| CN103435024A (en) * | 2013-08-08 | 2013-12-11 | 瓮福（集团）有限责任公司 | Method for producing feed grade calcium hydrophosphate |
| CN103738931A (en) * | 2013-11-26 | 2014-04-23 | 瓮福（集团）有限责任公司 | Method for production of potassium dihydrogen phosphate from phosphorus-containing acidic wastewater |
| CN104276562A (en) * | 2014-10-30 | 2015-01-14 | 瓮福（集团）有限责任公司 | Method for preparing feed-grade calcium hydrogen phosphate by using washing wastewater produced by phosphoric acid process activated carbon |
| CN106167272A (en) * | 2016-02-23 | 2016-11-30 | 瓮福（集团）有限责任公司 | Utilize the method that Phosphate Fertilizer Industry waste water produces feed grade calcium carbonate |
| CN109153570A (en) * | 2016-05-18 | 2019-01-04 | 凯米拉公司 | The production of phosphatic fertilizer |
| CN112408350A (en) * | 2020-11-03 | 2021-02-26 | 中国五环工程有限公司 | Process for producing feed-grade calcium hydrophosphate from phosphorus-containing wastewater |
| CN112408350B (en) * | 2020-11-03 | 2023-04-07 | 中国五环工程有限公司 | Process for producing feed-grade calcium hydrophosphate from phosphorus-containing wastewater |
| CN113233438A (en) * | 2021-06-15 | 2021-08-10 | 瓮福（集团）有限责任公司 | Method for controlling arsenic and increasing yield of calcium hydrophosphate product |
| CN113233438B (en) * | 2021-06-15 | 2022-11-01 | 瓮福（集团）有限责任公司 | Method for controlling arsenic and increasing yield of calcium hydrophosphate product |
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Application publication date: 20120620 |