CN1204044C - Method for preparing industrial grade and food grade phosphoric acid by wet method phosphoric acid - Google Patents
Method for preparing industrial grade and food grade phosphoric acid by wet method phosphoric acid Download PDFInfo
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- CN1204044C CN1204044C CN 03117850 CN03117850A CN1204044C CN 1204044 C CN1204044 C CN 1204044C CN 03117850 CN03117850 CN 03117850 CN 03117850 A CN03117850 A CN 03117850A CN 1204044 C CN1204044 C CN 1204044C
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Abstract
The present invention relates to a process for preparing industrial phosphoric acid by wet-process phosphoric acid, which successively comprises pretreatment, desulfurization, filtering separation, extraction, deep desulfurization, washing, back extraction and concentration, wherein in the step of the pretreatment comprises, a desulfurizing agent, a defluorinating agent and a decolouring agent are added in the wet-process phosphoric acid; desulfurization, defluorination and decolorization are carried out in one procedure; a reaction temperature is from 60 to 80 DEG C, and the reaction time is from 2 to 4 hours. The method for preparing food phosphoric acid by wet-process phosphoric acid increases a procedure of deep defluorination after the procedure of back extraction on the basis of the processing steps for preparing industrial phosphoric acid. The method simplifies flow, reduces energy consumption and saves costs.
Description
One, technical field
The invention belongs to the preparation method of PHOSPHORIC ACID TECH.GRADE and food grade phosphoric acid, particularly a kind of is the technology that raw material, employing solvent extration become wet phosphoric acid purifying PHOSPHORIC ACID TECH.GRADE or food grade phosphoric acid with the phosphoric acid by wet process.
Two, background technology
The preparation of PHOSPHORIC ACID TECH.GRADE and food grade phosphoric acid can thermal phosphoric acid be a raw material both, can phosphoric acid by wet process be raw material again.Because the production of thermal phosphoric acid power consumption is high, along with energy day is becoming tight, people more are ready to adopt phosphoric acid by wet process, but the phosphoric acid by wet process impurities is higher, it must be purified the requirement that just meet PHOSPHORIC ACID TECH.GRADE and food grade phosphoric acid.About the purification of phosphoric acid by wet process, mainly contain chemical precipitation method, ion exchange method, the Phosphoric Acid Concentration method of purification, solvent extration and crystallization process, at present industrial general employing solvent extration.Though solvent extration is used in industrial production, the detailed data of its flow process and details report are less (sees " phosphoric acid, phosphate fertilizer and composite fertilizer ", chief editor Jiang Shanxiang, Chemical Industry Press, in March, 1999, P
425The 2nd row～P reciprocal
426The 2nd row), especially do not form suitability for industrialized production as yet in China.
" phosphoric acid, phosphate fertilizer and composite fertilizer " (chief editor Jiang Shanxiang, Chemical Industry Press, in March, 1999) introduced the manufacture level phosphoric acid that French Luo Na-Rhone-Poulenc adopted in the book and the solvent extration of food grade phosphoric acid---Central Liqueur flow process (is seen this book P
429～P
430), this flow process is to contain 40～50%P
2O
5Phosphoric acid by wet process be raw material, processing step comprise after clarification, decolouring, extraction, washing, water are stripped, are stripped ester mutually again with the salt solution back extraction, purify ester dearsenification, two and imitate evaporation concentration, defluorinate, extraction agent (solvent) is selected tributyl phosphate for use, washing procedure adds an amount of caustic soda desulfurization, after the back extraction dearsenification, defluorinate processing is carried out in refining acid.Its weak point is: it is uneconomical to improve percentage extraction by interpolation sulfuric acid when 1. extracting, this can increase the follow-up difficulty that removes sulfate radical, it is more thorough that sulfate radical is removed, will increase the NaOH consumption and return the amount of making washing acid by finished acid and also want corresponding increase, reduce the efficient of device.2. this flow process has also increased by a procedure after the water back extraction---salt solution back extraction ester phase.3. dearsenification is wayward in the acid after purification, and dearsenic agent sodium sulphite dissolves in the phosphoric acid, does not note slightly, can cause purifying that sodium ion exceeds standard in the acid.4. density (the 0.97g/cm of tributyl phosphate
3) approaching with the density of water, and viscosity increases much behind the phosphoric acid extraction, can make two-phase phase-splitting difficulty without thinner, it is mutually serious that acid is entrained with machine mutually, therefore must the tributyl phosphate that raffinate is carried secretly in mutually be reclaimed, and increased operation and purified cost.
Three, summary of the invention
The present invention is directed to the deficiency that prior art exists, provide a kind of and prepare the novel method of PHOSPHORIC ACID TECH.GRADE and food grade phosphoric acid with phosphoric acid by wet process, this kind method can be simplified technology, cut down the consumption of energy and cost under the product quality premise guaranteeing.
Provided by the inventionly prepare the method for PHOSPHORIC ACID TECH.GRADE with phosphoric acid by wet process, processing step comprises pre-treatment, desulfurization, filtering separation, extraction, dark desulfurization, washing, back extraction successively and concentrates; Pre-treatment is to add sweetening agent, defluorinating agent, discoloring agent in phosphoric acid by wet process, desulfurization, defluorinate, decolouring is placed on an operation carries out, and sweetening agent is pressed SO in the phosphoric acid
4 2-1～1.3 of stoichiometric ratio is extraordinarily gone into, and defluorinating agent is extraordinarily gone into by 1～1.2 of fluorine content stoichiometric ratio in the phosphoric acid, and the discoloring agent add-on is 0.1～1% of a phosphoric acid quality.60～80 ℃ of temperature of reaction, 2～4 hours reaction times.
The method for preparing food grade phosphoric acid with phosphoric acid by wet process provided by the invention belongs to a total inventive concept with the above-mentioned method for preparing PHOSPHORIC ACID TECH.GRADE, processing step is to increase dark defluorinate operation on the basis of the processing step of above-mentioned preparation PHOSPHORIC ACID TECH.GRADE, and dark defluorinate operation is placed on after the back extraction operation; Pre-treatment is to add sweetening agent, defluorinating agent, discoloring agent, dearsenic agent, removing heavy-metal agent in phosphoric acid by wet process, desulfurization, defluorinate, decolouring, dearsenification, removing heavy-metal is placed on an operation carries out, and sweetening agent is pressed SO in the phosphoric acid
4 2-1～1.3 of stoichiometric ratio is extraordinarily gone into, defluorinating agent is extraordinarily gone into by 1～1.2 of fluorine content stoichiometric ratio in the phosphoric acid, the discoloring agent add-on is 0.1～1% of a phosphoric acid quality, the add-on of dearsenic agent adds with the As stoichiometric ratio in the phosphoric acid, the add-on of removing heavy-metal agent adds with the heavy metal stoichiometric ratio in the phosphoric acid, 60～80 ℃ of temperature of reaction, 2～4 hours reaction times.
In the aforesaid method, the employed sweetening agent of pretreatment process is selected ground phosphate rock for use, and defluorinating agent selects yellow soda ash for use or/and salt of wormwood, and activated carbon selected for use by discoloring agent or/and diatomite, dearsenic agent and sodium sulphite is selected in the removing heavy-metal agent for use or/and thiophosphoric anhydride.
In the aforesaid method, lime carbonate selected for use by the sweetening agent that desulfurization process adds or/and calcium oxide, and the add-on of sweetening agent is with the SO in the phosphoric acid
4 2-1～1.2 of stoichiometric ratio is extraordinarily gone into, 60～80 ℃ of temperature of reaction, 1～3 hour reaction times; Dark desulfurization process is that the organic phase after the extraction is carried out desulfurization, and the sweetening agent of adding is a barium carbonate or/and hydrated barta, and the sweetening agent add-on is by SO in the organic phase
4 2-Stoichiometric ratio adds, 50～60 ℃ of temperature of reaction, reaction times 10～30min.
In the aforesaid method, the extraction agent that extraction process uses is the mixture of tributyl phosphate and kerosene, and the volume percent of kerosene is 20～50%, and the volume percent of tributyl phosphate is 50～80%; Processing parameter: organic phase compares 3～6: 1 with water, and 50～60 ℃ of temperature, organic phase are external phase.
In the aforesaid method, the extraction agent that the back extraction operation is used is soft water, processing parameter: organic phase compares 6～10: 1 with water, 50～60 ℃ of temperature, and water is an external phase.
Dark defluorinate operation in the technical process of preparation food grade phosphoric acid is carried out under vacuum condition, vacuum tightness is 88～95kpa, defluorinating agent is selected active silica for use, and its add-on is extraordinarily gone into 80～90 ℃ of temperature of reaction with 1.3～2 of the stoichiometric ratio of fluorine content in the phosphoric acid.
The present invention has following beneficial effect:
1, defluorinate, desulfurization, decolouring or defluorinate, desulfurization, decolouring, dearsenification, removing heavy-metal all are placed on operation of pre-treatment and finish, not only net effect is better than the effect of proceed step by step but also has simplified technology.
2, dark desulfurization being placed on the extraction back carries out in organic phase, the barium sulfate crystal that generates in organic phase is deposited in the acid mutually soon, the acid of barium sulfate-containing removes to make fertilizer with raffinate after entering extraction tower mutually, thereby not only shortened the time, and solved a difficult problem of separating barium sulfate, in addition, doctor solution consumption is few, sulfate radical removes very thorough, can reach excellent PHOSPHORIC ACID TECH.GRADE standard.
3, comprise three desulfurization in the technical process, can remove sulfate radical to greatest extent, guarantee the quality of product.
4, used extraction agent is the mixture of tributyl phosphate and colorless and odorless kerosene, the density and the viscosity of extraction agent have been reduced, the two-phase phase-splitting is easy, raffinate is carried organic phase secretly and can be ignored, and extraction agent is dissolved in phosphoric acid hardly, so raffinate can reclaim extraction agent without rectifying, be directly used in the fertilizer manufacturing, simplify flow process, reduced energy consumption, saved cost.
Four, description of drawings
Fig. 1 is a kind of process flow sheet for preparing PHOSPHORIC ACID TECH.GRADE with phosphoric acid by wet process provided by the present invention;
Fig. 2 is a kind of process flow sheet for preparing food grade phosphoric acid with phosphoric acid by wet process provided by the present invention.
Five, embodiment
Embodiment 1: the preparation PHOSPHORIC ACID TECH.GRADE
In the present embodiment, raw materials used phosphoric acid by wet process composed as follows:
| P 2O 5 | SO 4 2- | F | Fe | As | Heavy metal (in Pb) | Colourity |
| 50.4％ | 3.5％ | 0.75％ | 0.3％ | 0.0014％ | 0.0025％ | ＞300 |
Serialization is produced, and processing step comprises pre-treatment, desulfurization, filtering separation, extraction, dark desulfurization, washing, back extraction and concentrated as shown in Figure 1 successively.
(1) pre-treatment
Pre-treatment is carried out in pretreatment tank, and sweetening agent is selected the phosphorus concentrate for use, presses SO in the phosphoric acid
4 2-1.1 of stoichiometric ratio is extraordinarily gone into; Defluorinating agent is selected yellow soda ash for use, and add-on is 1.2 times of fluorine content stoichiometric ratio in the phosphoric acid; Discoloring agent is selected activated carbon and diatomite for use, and the add-on of activated carbon is 0.1% (in the raw material phosphoric acid quality), and diatomaceous add-on is 0.1% (in the raw material phosphoric acid quality).60 ℃ of temperature of reaction, 3 hours reaction times.
(2) desulfurization
Desulfurization is carried out in desulfurizer, and sweetening agent is selected lime carbonate for use, presses SO in the phosphoric acid
4 2-1.2 of stoichiometric ratio is extraordinarily gone into; 60 ℃ of temperature of reaction, 2 hours reaction times.
(3) filtering separation
Adopt flame filter press to separate and remove solid matter in the phosphoric acid.
(4) extraction
Extraction is carried out in extraction tank, and extraction agent is the mixture of tributyl phosphate and kerosene, and the volume percent of kerosene is 35%, and the volume percent of tributyl phosphate is 65%; Processing parameter: compare 4: 1 of organic phase and water, 50 ℃ of temperature, organic phase are external phase.
(5) dark desulfurization
Dark desulfurization is carried out in desulfurizer, and sweetening agent is selected barium carbonate for use, by SO in the organic phase
4 2-Stoichiometric ratio adds; 50 ℃ of temperature of reaction, 20 minutes reaction times.
(6) washing
Washing is carried out in rinse bath, compare 20: 1 of organic phase and water, and 50 ℃ of temperature, organic phase are external phase.
(7) back extraction
The equipment of back extraction is the back extraction tower, and extraction agent is a soft water, compare 6: 1 of organic phase and water, and 60 ℃ of temperature, water is an external phase.
(8) concentrate
Promptly be prepared into PHOSPHORIC ACID TECH.GRADE after adopting thickening equipment that purification of phosphoric acid that back extraction obtains is concentrated.
The PHOSPHORIC ACID TECH.GRADE that present embodiment is prepared, relevant components contents such as following table:
| P 2O 5 | SO 4 2- | F | Fe | As | Heavy metal (in Pb) | Colourity |
| 61.5％ | 0.0010％ | 0.0200％ | 0.0020％ | 0.0004％ | 0.0006％ | ＜30 |
Embodiment 2: the preparation food grade phosphoric acid
In the present embodiment, the composition of raw materials used phosphoric acid by wet process is with embodiment 1.Serialization is produced, and processing step comprises that successively pre-treatment, desulfurization, filtering separation, extraction, dark desulfurization, washing, back extraction, dark defluorinate are with concentrated as shown in Figure 2.
In the above-mentioned processing step, except that pre-treatment, dark defluorinate and enrichment process, other each operations are all identical with embodiment 1.
Pre-treatment is carried out in pretreatment tank, and sweetening agent is selected the phosphorus concentrate for use, presses SO in the phosphoric acid
4 2-1.2 of stoichiometric ratio is extraordinarily gone into; Defluorinating agent is selected yellow soda ash for use, press fluorine content stoichiometric ratio in the phosphoric acid 1.1 times; Discoloring agent is selected activated carbon and diatomite for use, and the add-on of activated carbon is 0.1% (in the raw material phosphoric acid quality), and diatomaceous add-on is 0.1% (in the raw material phosphoric acid quality); Sodium sulphite is selected in dearsenic agent and removing heavy-metal agent for use, and the stoichiometric ratio of pressing arsenic and heavy metal in the phosphoric acid adds.60 ℃ of temperature of reaction, 3 hours reaction times.
Dark defluorinate and enrichment process carry out under vacuum condition, and vacuum tightness is 93kpa, and employed equipment is rotatory evaporator, and defluorinating agent is selected active silica for use, and its add-on is 1.6 times of fluorine content stoichiometric ratio in the phosphoric acid; 85 ℃ of temperature of reaction, defluorinate and concentration time are about 3 hours.
The food grade phosphoric acid that present embodiment is prepared, relevant components contents such as following table:
| P 2O 5 | SO 4 2- | F | Fe | As | Heavy metal (in Pb) | Colourity |
| 61.5％ | 0.0015％ | 0.0010％ | 0.0020％ | 0.0001％ | 0.0001％ | ＜20 |
Claims (10)
1, a kind ofly prepare the method for PHOSPHORIC ACID TECH.GRADE with phosphoric acid by wet process, processing step comprises pre-treatment, desulfurization, filtering separation, extraction, dark desulfurization, washing, back extraction successively and concentrates,
Pre-treatment is to add sweetening agent, defluorinating agent, discoloring agent in phosphoric acid by wet process, desulfurization, defluorinate, decolouring is placed on an operation carries out, and sweetening agent is a ground phosphate rock, presses SO in the phosphoric acid
4 2-1～1.3 of stoichiometric ratio is extraordinarily gone into, and defluorinating agent is yellow soda ash or salt of wormwood, extraordinarily goes into by 1～1.2 of fluorine content stoichiometric ratio in the phosphoric acid, discoloring agent is an activated carbon or/and diatomite, and add-on is 0.1～1% of a phosphoric acid quality, 60～80 ℃ of temperature of reaction, 2～4 hours reaction times
The extraction agent that extraction process uses is the mixture of tributyl phosphate and kerosene, processing parameter: organic phase compares 3～6: 1 with water, 50～60 ℃ of temperature, organic phase is an external phase, dark desulfurization process is that the organic phase after the extraction is carried out desulfurization, the sweetening agent that adds is a barium carbonate or/and hydrated barta, and the sweetening agent add-on is by SO in the organic phase
4 2-Stoichiometric ratio adds, 50～60 ℃ of temperature of reaction, reaction times 10～30min.
2, according to claim 1ly prepare the method for PHOSPHORIC ACID TECH.GRADE with phosphoric acid by wet process, it is characterized in that in the extraction agent that the volume percent of kerosene is 20～50%, the volume percent of tributyl phosphate is 50～80%.
3, according to claim 1 and 2ly prepare the method for PHOSPHORIC ACID TECH.GRADE with phosphoric acid by wet process, it is characterized in that sweetening agent that desulfurization process adds is a lime carbonate or/and calcium oxide, the add-on of sweetening agent is with the SO in the phosphoric acid
4 2-1～1.2 of stoichiometric ratio is extraordinarily gone into, 60～80 ℃ of temperature of reaction, 1～3 hour reaction times.
4, according to claim 1 and 2ly prepare the method for PHOSPHORIC ACID TECH.GRADE with phosphoric acid by wet process, it is characterized in that the extraction agent that the back extraction operation is used is soft water, processing parameter: organic phase compares 6～10: 1 with water, 50～60 ℃ of temperature, and water is an external phase.
5, according to claim 3ly prepare the method for PHOSPHORIC ACID TECH.GRADE with phosphoric acid by wet process, it is characterized in that the extraction agent that the back extraction operation is used is soft water, processing parameter: organic phase compares 6～10: 1 with water, 50～60 ℃ of temperature, and water is an external phase.
6, a kind ofly prepare the method for food grade phosphoric acid with phosphoric acid by wet process, the processing step processing step comprises pre-treatment, desulfurization, filtering separation, extraction, dark desulfurization, washing, back extraction, dark defluorinate successively and concentrates,
Pre-treatment is to add sweetening agent, defluorinating agent, discoloring agent, dearsenic agent, removing heavy-metal agent in phosphoric acid by wet process, desulfurization, defluorinate, decolouring, dearsenification, removing heavy-metal is placed on an operation carries out, and sweetening agent is a ground phosphate rock, presses SO in the phosphoric acid
4 2-1～1.3 times of adding of stoichiometric proportion; Defluorinating agent is sodium carbonate or potash; Press 1～1.2 times of adding of fluorine content stoichiometric proportion in the phosphoric acid; Decolorizer is that activated carbon is or/and diatomite; Addition is 0.1～1% of phosphoric acid quality; Hydrodearsenic Catalyst and removing heavy-metal agent are that vulcanized sodium is or/and phosphorus pentasulfide; The addition of Hydrodearsenic Catalyst adds with the As stoichiometric proportion in the phosphoric acid; The addition of removing heavy-metal agent adds with the heavy metal stoichiometric proportion in the phosphoric acid; 60～80 ℃ of reaction temperatures; 2～4 hours reaction time
The extraction agent that extraction process uses is the mixture of tributyl phosphate and kerosene, processing parameter: organic phase compares 3～6: 1 with water, 50～60 ℃ of temperature, organic phase is an external phase, dark desulfurization process is that the organic phase after the extraction is carried out desulfurization, the sweetening agent that adds is a barium carbonate or/and hydrated barta, and the sweetening agent add-on is by SO in the organic phase
4 2-Stoichiometric ratio adds, 50～60 ℃ of temperature of reaction, and reaction times 10～30min,
Dark defluorinate operation is carried out under vacuum condition, and vacuum tightness is 88～95kpa, and defluorinating agent is selected active silica for use, and its add-on is extraordinarily gone into by the stoichiometric ratio 1.3～2 of fluorine content in the phosphoric acid, 80～90 ℃ of temperature of reaction.
7, according to claim 6ly prepare the method for food grade phosphoric acid with phosphoric acid by wet process, it is characterized in that in the extraction agent that the volume percent of kerosene is 20～50%, the volume percent of tributyl phosphate is 50～80%.
8, describedly prepare the method for food grade phosphoric acid with phosphoric acid by wet process according to claim 6 or 7, it is characterized in that sweetening agent that desulfurization process adds is a lime carbonate or/and calcium oxide, the add-on of sweetening agent is with the SO in the phosphoric acid
4 2-1～1.2 of stoichiometric ratio is extraordinarily gone into, 60～80 ℃ of temperature of reaction, 1～3 hour reaction times.
9, describedly prepare the method for food grade phosphoric acid with phosphoric acid by wet process according to claim 6 or 7, it is characterized in that the extraction agent that the back extraction operation is used is soft water, processing parameter: organic phase compares 6～10: 1 with water, 50～60 ℃ of temperature, and water is an external phase.
10, according to claim 8ly prepare the method for food grade phosphoric acid with phosphoric acid by wet process, it is characterized in that the extraction agent that the back extraction operation is used is soft water, processing parameter: organic phase compares 6～10: 1 with water, 50～60 ℃ of temperature, and water is an external phase.
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