CN107021466B - Sulfuric acid method titanium pigment acid waste water is used for the pretreated closed circulation process of phosphorus ore - Google Patents
Sulfuric acid method titanium pigment acid waste water is used for the pretreated closed circulation process of phosphorus ore Download PDFInfo
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- CN107021466B CN107021466B CN201710272496.1A CN201710272496A CN107021466B CN 107021466 B CN107021466 B CN 107021466B CN 201710272496 A CN201710272496 A CN 201710272496A CN 107021466 B CN107021466 B CN 107021466B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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Abstract
The present invention relates to a kind of production method of calcium hydrophosphate fodder, a kind of sulfuric acid method titanium pigment acid waste water is specifically disclosed for the pretreated closed circulation process of phosphorus ore, comprising the following steps: acid waste water a, is added to phosphorus ore de-magging；B, de-magging slurry is separated by solid-liquid separation；C, de-magging mother liquor is neutralized；D, slurry after neutralization is separated by solid-liquid separation；For being washed to thick metatitanic acid slurry after filtrate clarification；E, to being recycled in return step A after acid waste water moisturizing.The invention has the advantages that 1) substantially reduce the de-magging cost and phosphorus damage of high-magnesium-phosphorus ore, while outlet is had found for the recovery processing of a large amount of acid waste waters；2) closed loop process due to the de-magging mother liquor containing a large amount of impurity for carrying out de-magging generation to phosphorus ore with acid waste water is provided, the problem for hindering this method industrially to promote is overcome；3) combination of sulfuric acid method titanium pigment production technology Yu calcium hydrophosphate fodder production technology is realized.
Description
Technical field
The present invention relates to a kind of production method of calcium hydrophosphate fodder, especially a kind of calcium hydrophosphate fodder was produced
The preprocess method of phosphorus ore in journey.
Background technique
The production technology of usual calcium hydrophosphate fodder are as follows: use high-grade low magnesium phosphorus ore and direct reaction of sulfuric acid, obtain
To phosphoric acid by wet process, enters one section of neutralization chamber after metering, neutralized with milk of lime, the filtering filter residue fertilizer cheap for production prices
Calcium monohydrogen phosphate (white fertilizer), the iron after being neutralized by one section in phosphoric acid, aluminium, the impurity such as sulfate radical are purified；Filtrate enters two sections
Neutralization chamber continues to neutralize with milk of lime, filter liquor return preparing lime milk, filter cake through pneumatic conveying drying, be crushed into product.Its
Exemplary steps can be summarized as follows:
(1) phosphoric acid by wet process is obtained by low magnesium phosphorus ore and sulfuric acid reaction；
(2) in one section of neutralization chamber, phosphoric acid by wet process and milk of lime carry out neutralization reaction, obtain reaction slurry；
(3) filtering reaction slurry obtains one section of filtrate and filter residue；Filter residue is for producing white fertilizer；
(4) in two sections of neutralization chambers, one section of filtrate and milk of lime carry out neutralization reaction, obtain slurry；
(5) filter slurry obtains two sections of filtrates and filter cake, filter cake through pneumatic conveying drying, be crushed into calcium hydrophosphate fodder and produce
Product.
In the production process of calcium monohydrogen phosphate, since magnesium in one section and not can be removed, product is fully entered, is influenced
Product purity, in order to obtain the calcium hydrophosphate fodder product of high-quality generally use high-grade phosphorus ore, low content of magnesium, usually
It is required that content of magnesium is lower than 0.5% (mass fraction).
For many years, the demand with society to phosphor resource is continuously improved, and minable high-grade phosphate rock resource is fewer and fewer,
The decline of phosphorus ore grade, higher impurity content is the problem of we necessarily face.Part of the manufacturer is using sulfuric acid to high-magnesium-phosphorus ore at present
It carries out pretreatment and removes magnesium, phosphoric acid by wet process is then prepared using de-magging phosphorus ore, and then prepare calcium hydrophosphate fodder, the technique
The technical issues of efficiently solving high-magnesium-phosphorus ore production calcium hydrophosphate fodder.But since sulfuric acid is strong acid, not can avoid with
Phosphorus ore antedating response, causes phosphorus to damage, while being difficult to handle containing a large amount of pollutant in de-magging mother liquor, and sulfuric acid consumption is higher to be caused into
This is higher, is difficult to promote in actual production.
Such as a kind of high-magnesium-phosphorus ore de-magging by-product is disclosed in the Chinese patent document of Publication No. CN102992284A
The method of ammonium magnesium phosphate, the patent are to carry out de-magging to high-magnesium-phosphorus ore using sulfuric acid or phosphoric acid, but exist with sulfuric acid de-magging
Above-mentioned defect, and phosphoric acid is at high price, industrially without the possibility of implementation.
Typical sulfuric acid method titanium pigment production technology is as follows:
(1) acidolysis reaction is carried out with ilmenite concentrate or acid-dissolved titanium slag and sulfuric acid, obtains titanyl sulfate solution；
(2) hydrolysing titanyl sulfate solution obtains thick metatitanic acid slurry；
(3) thick metatitanic acid slurry is washed, salt treatment, obtains pretreatment metatitanic acid；
(4) pretreatment metatitanic acid is sent into rotary kiln and calcines output TiO2Product.
Wherein, the technique thick metatitanic acid slurry washed specifically:
(1) primary washing: thick metatitanic acid slurry is separated by solid-liquid separation, a filter cake is obtained；Water is carried out to a filter cake
It washes to remove wherein iron ion, obtains one and wash metatitanic acid cake；One, which washes metatitanic acid cake, adds water to be beaten, and obtains one and washes metatitanic acid slurry；
(2) bleaching reduction: addition bleaching agent and reducing agent in metatitanic acid slurry are washed toward one and is bleached, and it is brilliant that calcining is added
Kind, obtain bleaching slurry；
(3) secondary washing: bleaching slurry is separated by solid-liquid separation, secondary filter cake is obtained；To secondary filter cake washed with
Wherein iron ion is further removed, two is obtained and washes metatitanic acid cake；Two, which wash metatitanic acid cake, adds water to be beaten, and obtains two and washes metatitanic acid slurry
Material.
In sulfate process titanium dioxide production, every production 1t titanium dioxide about generates the waste water that sulfur-bearing acid mass fraction is 2.5% or so
40t or so, the waste water are acid waste water, and the improvement of acid waste water is to solve an important work of titanium white production environmental pollution
Make.
Summary of the invention
It is development and utilization high-magnesium-phosphorus ore resource for producing calcium hydrophosphate fodder, while acid waste water is recycled,
The present invention provides a kind of sulfuric acid method titanium pigment acid waste waters to be used for the pretreated closed circulation process of phosphorus ore.
The technical scheme adopted by the invention is that: sulfuric acid method titanium pigment acid waste water is used for the pretreated closed circulation of phosphorus ore
Technique, comprising the following steps:
A, after phosphorus ore being crushed and is beaten, acid waste water is added thereto and carries out de-magnesium reaction, obtains de-magging slurry；
B, de-magging slurry is separated by solid-liquid separation, obtains de-magging phosphorus ore filter cake and de-magging mother liquor, de-magging phosphorus ore filter cake is sent
Calcium hydrophosphate fodder is produced toward subsequent technique；
C, neutralization reagent is added into de-magging mother liquor to be neutralized, slurry after being neutralized；
D, slurry after neutralization is separated by solid-liquid separation to obtain filter cake and filtrate；
E, after the clarified processing of filtrate, for a washing step in sulfuric acid method titanium pigment production technology to thick metatitanic acid
Slurry is washed, and it is acid waste water that wash water is generated after washing；
F, it is recycled in oxytropism waste water plus after water progress moisturizing processing in return step A, to realize closing
Circulation.
In the present invention, inventor proposes that acid waste water, which can be used, carries out de-magging processing, acid waste water sheet to high-magnesium-phosphorus ore
Body is a kind of byproduct wastewater, is used for phosphorus ore de-magging relative to using sulfuric acid or phosphoric acid de-magging not only to greatly reduce feed grade
The production cost of calcium monohydrogen phosphate, moreover it is possible to reduce sulfuric acid de-magging bring phosphorus damage, and be big in sulfuric acid method titanium pigment production process
The processing of amount acid waste water has found outlet.Experiments have shown that may make magnesium in phosphorus ore after carrying out de-magging to phosphorus ore using acid waste water
Content reduces by 70~95%, and phosphorus loss late is only within 0.1~0.5%.
But inventor has found in research and production, due to containing a large amount of impurities in acid waste water, locates in advance for phosphorus ore
It may lead to the indexs such as phosphorus, fluorine in the de-magging mother liquor generated during reason de-magging due to misoperation, equipment fault lamp reason
Exceeded, the filtrate of generation is difficult to completely remove fluorine therein, phosphorus etc. carrying out sewage treatment using calcium hydroxide.Moreover state
Family must be all water totally enclosed circulations for the environmental requirement of phosphorus product Chemical Manufacture enterprise, must not have production, technique to use
Water discharge.This defect undoubtedly causes serious obstruction to the popularization of the technique.
Invention finds that the main component of the de-magging mother liquor generated during acid waste water pre-treating phosphorite is sulphur under study for action
Acid, ferrous sulfate, magnesium sulfate and micro other impurities.Inventor proposes that it can be neutralized, can by neutralisation treatment
It so that wherein most impurity forms precipitating, can be removed, almost be contained only in obtained filtrate few by being separated by solid-liquid separation
The dissolution calcium sulfate and iron ion of amount, how according to the water quality situation, scientific and reasonable carry out closed circulation utilization is to solve to use
The key of water seal closed loop.
In sulfuric acid method titanium pigment production technology, the one of thick metatitanic acid slurry, which washes in the wash water of process generation, to be contained on a small quantity
Soluble calcium sulfate and iron ion, therefore the process, to the calcium in slurry, the requirement of the impurity such as iron is lower, therefore inventor
It proposes that the primary washing of thick metatitanic acid slurry can will be used for by the de-magging mother liquor of neutralization, filtering, clarifying treatment.
The de-magging mother liquor that the present invention generates acid waste water pre-treating phosphorite accordingly is in the case where being sufficiently stirred, in
PH value of solution, filtering are adjusted with reagent, the clarified processing of filtrate is directly used in washing step of thick metatitanic acid, the wash water of generation
As by-product acid waste water, by-product acid waste water is re-used for phosphorus ore pretreatment, to realize the purpose of closed circulation.Due to pre-
The evaporation for eating liquid and moisture of filter cake causes the closed cycle system total Water to reduce in processing mother liquor N-process, only need to be to being
System carries out appropriate moisturizing.
De-magging phosphorus ore filter cake obtained in step B of the present invention can be pressed directly that is, low magnesium phosphorus ore in traditional handicraft
It is used to produce according to the typical production process of calcium hydrophosphate fodder.Clarifying treatment method described in step E can use common
Standing clarification or the methods of centrifugal sedimentation.
As a further improvement of the present invention, the neutralization terminal of step C are as follows: after obtained neutralization in slurry liquid phase pH >
5, so that neutralization reaction carries out sufficiently, the soluble impurity content after reduction in subsequent filtrate.
As a further improvement of the present invention, the reaction temperature of step A de-magnesium reaction is 40~60 DEG C, the reaction time 30
~90 minutes.It is demonstrated experimentally that maintaining 30~90 minutes reaction time under 40~60 DEG C of reaction temperature, de-magnesium reaction can be made
What is carried out is relatively abundant.
As a further improvement of the present invention, the smashing fineness of phosphorus ore is that 100 mesh percent of pass are greater than 95% in step A,
To promote subsequent de-magnesium reaction with the progress of faster reaction rate.
As a further improvement of the present invention, in step, the de-magging mother liquor obtained using step B breaks phosphorus ore
Slurry.The main purpose for using de-magging mother liquor to be beaten phosphorus ore in the present invention is to reduce the consumption of water in phosphorus ore pulping process, is met
The needs of water balance.
As a further improvement of the present invention, neutralization reagent used in step C is calcium hydroxide reagent.Because using hydrogen
Calcium oxide will not bring a large amount of soluble-salt, the soluble impurity content after reduction in subsequent filtrate into.
As a further improvement of the present invention, neutralization reagent used in step C is calcium hydroxide suspension or carbide slag
Suspension.Calcium hydroxide suspension refers to using calcium oxide is obtained after calcination of calcium carbonate, and water is added and is digested, obtained hydrogen-oxygen
Change calcium suspension；Carbide slag is in PVC production technology after calcium carbide and water reaction after obtained filter pressing with calcium hydroxide, and slurrying obtains；
This programme can further decrease production cost.
The beneficial effects of the present invention are: 1) carry out pretreatment de-magging to high-magnesium-phosphorus ore using titanium white by product acid waste water, greatly
The big de-magging cost for reducing high-magnesium-phosphorus ore and phosphorus damage, while outlet is had found for the recovery processing of a large amount of acid waste waters；2) it provides
The closed loop process of the de-magging mother liquor containing a large amount of impurity due to carrying out de-magging generation to phosphorus ore with acid waste water, overcomes
The problem for hindering this method industrially to promote；3) it realizes sulfuric acid method titanium pigment production technology and calcium hydrophosphate fodder produces
The combination of technique, the by-product that two kinds of technique generates mutually utilizes and closed circulation, has very high economical and environmentally friendly valence
Value.
Detailed description of the invention
Fig. 1 is process flow chart of the invention
Specific embodiment
Below with reference to embodiment, the present invention is further described.
Embodiment:
Acid waste water phosphorus ore is used in accordance with the following methods to pre-process and realize closed circulation:
1, high-magnesium-phosphorus ore (P is taken2O5=28%, MgO=5.0%) 1kg, the de-magging mother liquor in 2kg step 3 is added, uses ball milling
It is 96% that machine, which carries out wet-milling to 100 mesh percent of pass, and obtained ore pulp is injected pretreatment tank；
2, the acid waste water 2.4L of pH=3.1 is added into pretreatment tank, de-magnesium reaction 30min is carried out under the conditions of 50 DEG C
After obtain de-magging slurry；
3, de-magging slurry is separated by solid-liquid separation, obtains de-magging phosphorus ore filter cake and de-magging mother liquor, detect phosphorus ore demagnesium rate, it will
De-magging phosphorus ore filter cake is sent to subsequent technique production calcium hydrophosphate fodder；
4, milk of lime is added into de-magging mother liquor while stirring, the additional amount for controlling milk of lime makes slurry pH=5.2, curing
After 40min, slurry after neutralization is filtered to obtain filter cake and filtrate, filtrate obtains supernatant liquor after standing clarification 30min, examines
Survey clear liquid iron content；
5, thick metatitanic acid slurry (TiO is taken2=300g/l, Fe/TiO2=2000ppm) 1kg, above-mentioned clear liquid is used to wash
The thick metatitanic acid slurry, washing terminal be generate washing lotion in iron content be less than 1000ppm, detection wash after the total titanium of metatitanic acid,
It is beaten iron；
6, it is recycled in return step 2 after carrying out moisturizing to the acid waste water of generation (washing lotion).
7, as procedure described above, circular flow 50 times, every 5 times to phosphorus ore demagnesium rate, clear liquid iron content, the total titanium of metatitanic acid,
Mashing iron carries out analysis comparison, the results are shown in Table 1.
Table 1: phosphorus ore demagnesium rate, clear liquid iron content, the total titanium of metatitanic acid, mashing iron Analysis of test results contrast table
Claims (7)
1. sulfuric acid method titanium pigment acid waste water is used for the pretreated closed circulation process of phosphorus ore, comprising the following steps:
A, after phosphorus ore being crushed and is beaten, acid waste water is added thereto and carries out de-magnesium reaction, obtains de-magging slurry；
B, de-magging slurry is separated by solid-liquid separation, obtains de-magging phosphorus ore filter cake and de-magging mother liquor；
C, neutralization reagent is added into de-magging mother liquor to be neutralized, slurry after being neutralized；
D, slurry after neutralization is separated by solid-liquid separation to obtain filter cake and filtrate；
E, after the clarified processing of filtrate, for a washing step in sulfuric acid method titanium pigment production technology to thick metatitanic acid slurry
It is washed, it is acid waste water that wash water is generated after washing；
F, it is recycled in oxytropism waste water plus after water progress moisturizing processing in return step A, to realize closed circulation.
2. sulfuric acid method titanium pigment acid waste water according to claim 1 is used for the pretreated closed circulation process of phosphorus ore,
Be characterized in that: the neutralization terminal of step C are as follows: after obtained neutralization in slurry liquid phase pH > 5.
3. sulfuric acid method titanium pigment acid waste water according to claim 1 is used for the pretreated closed circulation process of phosphorus ore,
Be characterized in that: the reaction temperature of step A de-magnesium reaction is 40~60 DEG C, and the reaction time is 30~90 minutes.
4. sulfuric acid method titanium pigment acid waste water described in any claim is pre-processed for phosphorus ore according to claim 1~3
Closed circulation process, it is characterised in that: in step A the smashing fineness of phosphorus ore be 100 mesh percent of pass be greater than 95%.
5. sulfuric acid method titanium pigment acid waste water described in any claim is pre-processed for phosphorus ore according to claim 1~3
Closed circulation process, it is characterised in that: in step, the de-magging mother liquor obtained using step B is beaten phosphorus ore.
6. sulfuric acid method titanium pigment acid waste water described in any claim is pre-processed for phosphorus ore according to claim 1~3
Closed circulation process, it is characterised in that: neutralization reagent used in step C be calcium hydroxide reagent.
7. sulfuric acid method titanium pigment acid waste water described in any claim is pre-processed for phosphorus ore according to claim 1~3
Closed circulation process, it is characterised in that: neutralization reagent used in step C be calcium hydroxide suspension or carbide slag it is suspended
Liquid.
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| CN113292055A (en) * | 2021-06-25 | 2021-08-24 | 甘肃东方钛业有限公司 | Method for producing phosphoric acid by recycling waste sulfuric acid and acid wastewater generated in titanium dioxide production process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2111457B1 (en) * | 1995-05-22 | 1999-07-01 | Turol Trading S L | PHOSPHATE FERTILIZER WITH SULFUR AND TRACE ELEMENTS FOR ITS AGRICULTURAL AND INDUSTRIAL USE AND PROCEDURE FOR ITS PREPARATION. |
| CN101759166A (en) * | 2009-12-31 | 2010-06-30 | 四川龙蟒钛业股份有限公司 | Method for pre-treating phosphorite by using acidic waste water in the production process of titanium pigment |
| CN102674277A (en) * | 2012-05-25 | 2012-09-19 | 四川龙蟒钛业股份有限公司 | Method for pre-treating phosphorus rock by mixture of titanium dioxide waste acid and fluorine-containing waste water |
| CN103274462A (en) * | 2013-03-15 | 2013-09-04 | 四川龙蟒钛业股份有限公司 | Method for recycling acidic washing water in rutile titanium dioxide production process |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2111457B1 (en) * | 1995-05-22 | 1999-07-01 | Turol Trading S L | PHOSPHATE FERTILIZER WITH SULFUR AND TRACE ELEMENTS FOR ITS AGRICULTURAL AND INDUSTRIAL USE AND PROCEDURE FOR ITS PREPARATION. |
| CN101759166A (en) * | 2009-12-31 | 2010-06-30 | 四川龙蟒钛业股份有限公司 | Method for pre-treating phosphorite by using acidic waste water in the production process of titanium pigment |
| CN102674277A (en) * | 2012-05-25 | 2012-09-19 | 四川龙蟒钛业股份有限公司 | Method for pre-treating phosphorus rock by mixture of titanium dioxide waste acid and fluorine-containing waste water |
| CN103274462A (en) * | 2013-03-15 | 2013-09-04 | 四川龙蟒钛业股份有限公司 | Method for recycling acidic washing water in rutile titanium dioxide production process |
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Address after: 618200 Mianzhu new town industrial concentration area, Sichuan, Deyang Patentee after: Longbai Sichuan Titanium Co., Ltd Address before: 618200 Mianzhu new town industrial concentration area, Sichuan, Deyang Patentee before: SICHUAN LOMON TITANIUM Co.,Ltd. |