CN105502322A - Method for preparing alkali metal phosphate by using wet process crude phosphoric acid - Google Patents
Method for preparing alkali metal phosphate by using wet process crude phosphoric acid Download PDFInfo
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- CN105502322A CN105502322A CN201610031528.4A CN201610031528A CN105502322A CN 105502322 A CN105502322 A CN 105502322A CN 201610031528 A CN201610031528 A CN 201610031528A CN 105502322 A CN105502322 A CN 105502322A
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- alkali metal
- phosphoric acid
- metal phosphate
- extraction
- phosphate
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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
- C01B25/30—Alkali metal phosphates
- C01B25/305—Preparation from phosphorus-containing compounds by alkaline treatment
Abstract
The invention relates to a method for preparing alkali metal phosphate by using wet process crude phosphoric acid. The method comprises the following steps: 1) extracting the wet process crude phosphoric acid by using an extractant, and then carrying out separation to obtain a water phase and an organic phase containing organic phosphate; 2) carrying out extraction and reaction on an alkali metal hydroxide aqueous solution or an alkali metal carbonate aqueous solution and the organic phase containing the organic phosphate obtained in the step 1) at the same time, and carrying out separation to obtain a water phase containing alkali metal phosphate and an organic phase; and 3) carrying out after treatment on the water phase containing the alkali metal phosphate obtained in the step 2) to obtain the alkali metal phosphate. According to the method provided by the invention, the alkali metal hydroxide aqueous solution or the alkali metal carbonate aqueous solution of which the alkalinity is stronger than that of the extractant is adopted as a back-extractant, back extraction can be carried out without washing and concentration of the organic phase obtained by extraction, and the process of the back extraction combines the reaction for preparing the alkali metal phosphate and the recovery of the extractant, so that the process flow is greatly shortened, the equipment investment is reduced, the production cost is reduced, the reaction condition is mild, and the product quality is high.
Description
Technical field
The invention belongs to inorganic chemical industry production field, relate to a kind of method that wet method crude phosphoric acid prepares alkali metal phosphate.
Background technology
Alkali metal phosphate is generally sodium salt, sylvite etc., is widely used in food, petrochemical complex, medicine and feed etc.Current domestic production alkali metal phosphate is mainly obtained by refining phosphoric acid and oxyhydroxide or carbonate reaction, is divided into thermal phosphoric acid route and phosphoric acid by wet process route according to the source of raw material phosphoric acid.Thermal phosphoric acid route take yellow phosphorus as raw material, through the obtained technical grade of the reaction such as oxidation, aquation phosphoric acid again with alkali reaction, process is simple, and technology is comparatively ripe, and obtained phosphoric acid salt quality is high.But thermal phosphoric acid route requires higher to phosphorus ore taste, and seriously polluted, energy consumption and cost are all higher, thus present stage increasing research steering in a wet process phosphoric acid be on the production line of raw material.Phosphoric acid by wet process route namely adopt mineral acid decomposing phosphate rock made of stones phosphorus bronsted lowry acids and bases bronsted lowry or the reaction of corresponding an alkali metal salt produce alkali metal phosphate, because its cost is low and pollute little compared with thermal phosphoric acid, therefore obtain the favor of more and more investigator.Phosphoric acid by wet process is because requiring low to phosphorus ore taste, therefore obtained wet method crude phosphoric acid impurity is many and concentration is lower, have to pass through purifying, concentrated after just can enter the phosphate product that subsequent reactions prepares technical grade or food grade.
The purification process of phosphoric acid by wet process mainly contains chemical precipitation method, crystallization process, ion exchange method, organic solvent extractionprocess etc., and wherein machine solvent extration is the one be most widely used at present.Organic extraction solvent roughly can be divided into alcohols, ester class, ethers, ketone, amides etc., these solvent major parts are all through repeatedly extracting, stripping to the wet method crude phosphoric acid of high density, just can play the effect of purifying after concentrated, and the object reaching purifying is difficult to the phosphoric acid by wet process of lower concentration.
Chinese patent CN1308228 discloses extraction solvent and the extracting process thereof that a kind of wet phosphoric acid purifying produces food grade phosphoric acid, it uses three butoxyethyl phosphate: isopropyl ether: hexalin forms liquid hybrid extraction solvent, the method before extraction must by the pre-treatment of wet method crude phosphoric acid and to be concentrated into concentration be more than 60%, again through multi-stage solvent extraction and reextraction, food grade phosphoric acid is obtained after concentrated, not only energy consumption is high, technique is loaded down with trivial details but also percentage extraction is not high, high to the concentration requirement of raw phosphoric acid, be unfavorable for industrial applications.
CN101525130B relates to a kind of technique of purifying and producing industrial phosphoric acid by wet-process phosphoric acid, and this technique extracts after thick phosphoric acid by wet process desulfurization defluorinate process; Organic phase washing after extraction; Organic phase back extraction after washing; After stripping, refining the concentrating of aqueous phase obtains PHOSPHORIC ACID TECH.GRADE.This invention can only have good effect of extracting to the wet method crude phosphoric acid that phosphorus acid content is 21 ~ 38wt%; Want organic phase to want pickling after extraction, produce spent acid and not easily process; The low need of the phosphoric acid concentration that back extraction obtains concentrate, power consumption; And also will to the first pre-treatment of raw phosphoric acid before extraction.
CN104591114A has invented a kind of mixed solvent being applicable to lower concentration phosphoric acid by wet process extracting and purifying, namely a kind of by extraction agent, properties-correcting agent, the mixture of thinner composition.Wherein the volume of extraction agent accounts for 10 ~ 40% of mixed solvent cumulative volume; Properties-correcting agent accounts for 20 ~ 80% of mixed solvent cumulative volume; Thinner accounts for 20 ~ 60% of mixed solvent cumulative volume.In the operating temperature range of 20 ~ 50 DEG C, this organic mixed solvent has higher efficiency when low phosphorus acid extraction, and has certain effect with being separated of phosphate radical to chlorion.Because this mixed solvent can only have obvious effect of extracting when low phosphorus acid extraction, there is certain limitation; And during this invention back extraction, adopt neutral salt solution, organic extractant low as strippant reextraction efficiency to be difficult to regeneration; In addition this mixed solvent can not thoroughly separating chlorine ion and phosphate radical, and the potassium dihydrogen phosphate obtained after causing potassium chloride solution and organophosphate to carry out back extraction contains muriate, because of the two bad separation, affects quality product.
Wet method crude phosphoric acid can react obtained corresponding alkali metal phosphate to oxyhydroxide or an alkali metal salt after the purifyings such as extraction, back extraction.Organic solvent extractionprocess is one of phosphoric acid by wet process method preparing alkali metal phosphate, also has more report at present to the research of this respect.
Chinese patent CN101979311A discloses a kind of method that purifying phosphoric acid is in a wet process raw material abstraction method manufacture potassium primary phosphate and nitrogen-phosphorus-potassium compound fertilizer.The method in a wet process purifying phosphoric acid, Repone K is raw material, and octanol and octylame are that extraction agent carries out extracting, aqueous phase carries out crystallization and obtains potassium dihydrogen phosphate product; Organic phase saturated ammonium chloride solution stirs and strips, and recycles after phase-splitting after organic phase washing.Although the method extraction efficiency is high, selectivity is good, and need add EDTA during extraction affects quality product, and strippant ammonium chloride solution will lead to ammonia to saturated increase cost, and extraction and back-extraction process all needs insulation, power consumption.
Application number be 201410035386.X patent discloses a kind of method that phosphoric acid by wet process prepares tertiary sodium phosphate, this invention utilizes carboxamide and wet-process phosphoric acid reaction, through crystallisation by cooling, be separated and obtain intermediate, then this intermediate and sodium hydroxide are reacted prepare tertiary sodium phosphate product.The method will carry out removal of impurities, the technique such as concentrated to phosphoric acid by wet process before use phosphoric acid, all need strict control, operation more loaded down with trivial details with the reaction conditions that carboxamide prepares intermediate and intermediate and alkali reaction preparing phosphoric acid trisodium, and observable index is higher, unstable product quality.
In sum, there is more research although purify wet method crude phosphoric acid extraction and utilize extraction process to produce alkali metal phosphate at present, but still deposit some problems.As not yet found, a kind of organic solvent can realize having highly selective and high percentage extraction to the wet method crude phosphoric acid of different concns; Extraction process exists high to phosphoric acid by wet process quality requirements when preparing alkali metal phosphate, technical process is long, obtained unstable product quality, the problems such as cost is higher.
Summary of the invention
The present invention is directed to the technological deficiency that the above prior art exists, provide a kind of method that wet method crude phosphoric acid prepares alkali metal phosphate.The present invention adopts alkalescence to be better than the alkali metal hydroxide aqueous solution of extraction agent or aqueous alkali carbonate solution as strippant, without the need to stripping to extracting the organic phase washing concentrating obtained, the recovery of the reaction and extraction agent of preparing alkali metal phosphate unites two into one by reextraction process, substantially reduce technical process, reduce facility investment, reduce production cost, reaction conditions is gentle, and quality product is high.
The present invention is achieved by the following technical solutions:
Wet method crude phosphoric acid prepares a method for alkali metal phosphate, comprises the following steps:
1) wet method crude phosphoric acid is separated after extraction agent extraction the organic phase obtaining aqueous phase and contain organophosphate;
2) by alkali metal hydroxide aqueous solution or aqueous alkali carbonate solution and step 1) the extraction limit, organic phase limit containing organophosphate that obtains react, is separated the aqueous phase obtaining organic phase and contain alkali metal phosphate;
3) by step 2) obtain obtain alkali metal phosphate containing the aqueous phase of alkali metal phosphate through aftertreatment.
Preferably, step 2) in be separated the organic phase that obtains and be circulated to step 1) use as extraction agent.
Preferably, step 1) in, the percentage extraction controlling wet method crude phosphoric acid single extraction is greater than 85%.The percentage extraction of described control wet method crude phosphoric acid single extraction is greater than 85% and specifically refers to, wet method crude phosphoric acid is when extraction agent extracts, the percentage extraction of first time extraction gained organic phase is greater than 85%, the molar weight > 85% of phosphoric acid in the front wet method crude phosphoric acid of molar weight/extraction of the organophosphate namely contained in organic phase after extraction.
Preferably, step 1) in, when wet method crude phosphoric acid after single extraction in gained aqueous phase wet method crude phosphoric acid the rate of recovery lower than 95% time, after single extraction, gained aqueous phase makes total percentage extraction of wet method crude phosphoric acid reach more than 95% through reextraction again.After single extraction in gained aqueous phase wet method crude phosphoric acid the rate of recovery=(before single extraction in aqueous phase in wet method crude phosphoric acid phosphoric acid molar weight-single extraction after the molar weight of phosphoric acid that contains in aqueous phase) molar weight of phosphoric acid in wet method crude phosphoric acid in aqueous phase before/single extraction.
Preferably, step 1) in, during each extraction, the volume ratio of described extraction agent and described wet method crude phosphoric acid is 1 ~ 10:1, as 1 ~ 2.5:1,2.5 ~ 3:1,3 ~ 4:1,4 ~ 6:1 or 6 ~ 10:1, extraction time is 10 ~ 120min, as 10 ~ 20min, 20 ~ 40min, 40 ~ 60min, 60 ~ 90min or 90 ~ 120min.
Preferably, the difficult water-soluble weakly alkaline organic solvent of described extraction agent.Preferred, described extraction agent is organic amine organic solvent, as Tributylamine, trioctylamine or tri-iso-octylamine.Preferred further, described extraction agent is trioctylamine.The described water that is insoluble in refers to that the solubleness in water is less than 0.1g/L.
Preferably, step 1) in, described extraction agent is mixed extractant, described mixed extractant comprises the weakly alkaline organic solvent and thinner that are insoluble in water, described thinner is the organic solvent that water-insoluble viscosity is little, the volume ratio of described the weakly alkaline organic solvent and described thinner that are insoluble in water is 1 ~ 10:1, and as 1 ~ 2:1,2 ~ 5:1 or 5 ~ 10:1, preferred volume ratio is 2 ~ 5:1.Described extraction agent can be Tributylamine, trioctylamine or tri-iso-octylamine, and described thinner can be kerosene or chloroform.Preferred, described extraction agent is trioctylamine.Describedly water-insolublely refer to that the solubleness in water is less than 0.8g/L, described viscosity is little refers to that viscosity is less than 0.6mPas.
Above-mentioned extraction agent or mixed extractant are applicable to different H
3pO
4the extraction of the wet method crude phosphoric acid of concentration, preferably, the H of wet method crude phosphoric acid
3pO
4concentration is 5 ~ 85wt%, as 5 ~ 10wt%, 10 ~ 30wt%, 30 ~ 40wt%, 40 ~ 60wt% or 60 ~ 85wt%.
Preferably, step 2) in, the concentration of described alkali metal hydroxide aqueous solution or aqueous alkali carbonate solution is 10wt% ~ saturated solution.
Preferably, step 2) in, when described alkali metal phosphate is dihydrogen phosphate, the mol ratio of alkalimetal ion and phosphate radical is 1 ~ 1.05:1; When described alkali metal phosphate is monohydric phosphate, the mol ratio of alkalimetal ion and phosphate radical is 2 ~ 2.05:1; When described alkali metal phosphate is phosphoric acid salt, the mol ratio of alkalimetal ion and phosphate radical is 3 ~ 3.05:1.
Preferably, step 2) in, when described alkali metal phosphate is dihydrogen phosphate, the pH value controlling the aqueous phase containing alkali metal phosphate is 4 ~ 5; When described alkali metal phosphate is monohydric phosphate, the pH value controlling the aqueous phase containing alkali metal phosphate is 8 ~ 9.5; When described alkali metal phosphate is phosphoric acid salt, the pH value controlling the aqueous phase containing alkali metal phosphate is 10.5 ~ 12.
Preferably, step 2) in, described is 10wt% ~ saturated solution containing the concentration of alkali metal phosphate in the aqueous phase of alkali metal phosphate.
Preferably, step 3) in, described aftertreatment is concentrated, crystallization and oven dry.
Know-why of the present invention is as follows, refers to extraction agent in equation with E:
H
3PO
4+E→H
3PO
4·E
H
3PO
4·E+A
2CO
3→A
xH
yPO
4+CO
2+E
Or
H
3PO
4+E→H
3PO
4·E
H
3PO
4·E+AOH→A
xH
yPO
4+H
2O+E
The present invention at least has one of following beneficial effect:
(1) the present invention adopts the wet method crude phosphoric acid of non-water-soluble weakly alkaline organic solvent to different phosphate acid concentration to extract, also the mixed extractant of non-water-soluble weakly alkaline organic solvent and thinner composition can be adopted to extract, there is highly selective and percentage extraction, through reextraction, phosphoric acid extraction rate can reach more than 99%, substantially produce without spent acid, realize efficiently, phosphoric acid extraction from aqueous phase fast, effectively can remove a large amount of impurity in wet method crude phosphoric acid simultaneously, reach the object of purification of crude phosphoric acid;
(2) the present invention adopts alkalescence to be better than the alkali metal hydroxide aqueous solution of extraction agent or aqueous alkali carbonate solution as strippant, extraction limit, limit is reacted, without the need to stripping to extracting the organic phase washing concentrating obtained, the recovery of the reaction and extraction agent of preparing alkali metal phosphate unites two into one by reextraction process, substantially reduce technical process, reduce facility investment, reduce production cost; The present invention adopts the stronger basic metal of alkalescence or aqueous alkali carbonate solution as strippant because stripping, and is easily extracted by phosphate radical, and obtains alkali metal phosphate and CO after stripping
2or alkali metal phosphate and water, do not introduce other difficult separating impurity, the fine separating-purifying of product, good product quality;
(3) wet method crude phosphoric acid extraction of the present invention, reextraction and alkali metal phosphate the process such as to be produced and are all carried out more complete, and selectivity is high, and the quality of the alkali metal phosphate obtained can reach the quality that food-grade alkali metal phosphate prepared by thermal phosphoric acid.
Embodiment
Below by way of specific specific examples, technical scheme of the present invention is described.Should be understood that one or more method stepss that the present invention mentions do not repel and before and after described combination step, also to there is additive method step or can also insert additive method step between these steps clearly mentioned; Should also be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.And, except as otherwise noted, the numbering of various method steps is only the convenient tool differentiating various method steps, but not be ordering or the enforceable scope of restriction the present invention of restriction various method steps, the change of its relativeness or adjustment, when changing technology contents without essence, when being also considered as the enforceable category of the present invention.
Embodiment 1
1) by phosphoric acid concentration be 5% wet method crude phosphoric acid and trioctylamine by volume 1:1 extract after mixing, control extraction time is 10min, after twice extraction, in aqueous phase, the total yield of phosphoric acid is 97.5%, is separated and obtains aqueous phase and the organic phase containing trioctylamine phosphoric acid;
2) be the Na of 10wt% by concentration
2cO
3solution and step 1) the trioctylamine phosphoric acid organic phase that obtains mixes and strips, control Na simultaneously
+with PO
4 3-mol ratio be 1:1, when the pH of aqueous phase is 4 ~ 5, extraction is completely, is separated and obtains NaH
2pO
4solution and trioctylamine, trioctylamine is back to step 1 after reclaiming) continue extraction wet method crude phosphoric acid;
3) step 2) NaH that obtains
2pO
4solution obtains the food grade NaH meeting GB25561-2010 after the process such as concentrated, crystallization, oven dry
2pO
4.
Embodiment 2
1) by phosphoric acid concentration be 10% wet method crude phosphoric acid, extraction after the 2:5:1 mixing by volume of Tributylamine and chloroform, control extraction time is 40min, after twice extraction, in aqueous phase, the total yield of phosphoric acid is 98%, is separated the mixing organic phase obtaining aqueous phase and contain Tributylamine phosphoric acid and chloroform;
2) by concentration being KOH solution and the step 1 of 10wt%) organic phase that mixes containing Tributylamine phosphoric acid that obtains mixes and strips, control K
+with PO
4 3-mol ratio be 1.05:1, when the pH of aqueous phase solution is 4 ~ 5, extraction completely, is separated obtain KH
2pO
4solution and Tributylamine, chloroform mixed solvent, Tributylamine, chloroform mixed solvent are back to step 1 after reclaiming) continue extraction wet method crude phosphoric acid;
3) step 2) KH that obtains
2pO
4solution obtains the food grade KH meeting GB25560-2010 after the process such as concentrated, crystallization, oven dry
2pO
4.
Embodiment 3
1) by phosphoric acid concentration be 30% wet method crude phosphoric acid, extraction after the 1:3:3 mixing by volume of trioctylamine and chloroform, control extraction time is 20min, after single extraction, in aqueous phase, the total yield of phosphoric acid is 96%, is separated the mixing organic phase obtaining aqueous phase and contain trioctylamine phosphoric acid and chloroform;
2) by concentration being NaOH solution and the step 1 of 20wt%) the trioctylamine phosphoric acid organic phase that obtains mixes and strips, control Na
+with PO
4 3-mol ratio be 2:1, when the pH of aqueous phase is 8 ~ 9.5, extraction is completely, is separated and obtains Na
2hPO
4solution and trioctylamine, chloroform mixed solvent, trioctylamine, chloroform mixed solvent are back to step 1 after reclaiming) continue extraction wet method crude phosphoric acid;
3) step 2) Na that obtains
2hPO
4solution obtains the food grade Na meeting GB25568-2010 after the process such as concentrated, crystallization, oven dry
2hPO
4.
Embodiment 4
1) by phosphoric acid concentration be 40% wet method crude phosphoric acid and tri-iso-octylamine by volume 1:4 extract after mixing, control extraction time is 60min, after twice extraction, in aqueous phase, the total yield of phosphoric acid is 98.5%, is separated and obtains aqueous phase and the organic phase containing tri-iso-octylamine phosphoric acid;
2) by concentration being NaOH solution and the step 1 of 30wt%) the tri-iso-octylamine phosphoric acid organic phase that obtains mixes and strips, control Na
+with PO
4 3-mol ratio be 2.05:1, when the pH of aqueous phase is 8 ~ 9.5, extraction is completely, is separated and obtains Na
2hPO
4solution and tri-iso-octylamine, tri-iso-octylamine is back to step 1 after reclaiming) continue extraction wet method crude phosphoric acid;
3) step 2) Na that obtains
2hPO
4solution obtains the food grade Na meeting GB25568-2010 after the process such as concentrated, crystallization, oven dry
2hPO
4.
Embodiment 5
1) by phosphoric acid concentration be 60% wet method crude phosphoric acid, extraction after the 1:6:3 mixing by volume of trioctylamine and kerosene, control extraction time is 90min, after twice extraction, in aqueous phase, the total yield of phosphoric acid is 98%, is separated and obtains aqueous phase and the organic phase containing trioctylamine phosphoric acid, kerosene;
2) be the K of 40wt% by concentration
2cO
3solution and step 1) obtain trioctylamine phosphoric acid, kerosene organic phase mix and strip, control K
+with PO
4 3-mol ratio be 3:1, when the pH of aqueous phase is 10.5 ~ 12, extraction is completely, is separated and obtains K
3pO
4solution and trioctylamine, kerosene mixed solvent, trioctylamine, kerosene mixed solvent are back to step 1 after reclaiming) continue extraction wet method crude phosphoric acid;
3) step 2) K that obtains
3pO
4solution obtains the food grade K meeting GB25563-2010 after the process such as concentrated, crystallization, oven dry
3pO
4.
Embodiment 6
1) by phosphoric acid concentration be 85% wet method crude phosphoric acid, extraction after the 1:10:1 mixing by volume of trioctylamine and chloroform, control extraction time is 120min, after twice extraction, in aqueous phase, the total yield of phosphoric acid is 99%, is separated and obtains aqueous phase and the organic phase containing trioctylamine phosphoric acid, chloroform;
2) by Na that concentration is saturated
2cO
3solution and step 1) strip mixing containing the organic phase of trioctylamine phosphoric acid of obtaining, control Na
+with PO
4 3-mol ratio be 3.05:1, when the pH of aqueous phase is 10.5 ~ 12, extraction is completely, is separated and obtains Na
3pO
4solution and trioctylamine, chloroform mixed solvent, trioctylamine, chloroform mixed solvent are back to step 1 after reclaiming) continue extraction wet method crude phosphoric acid;
3) step 2) Na that obtains
3pO
4solution obtains the food grade Na meeting HG/T2517-93 after the process such as concentrated, crystallization, oven dry
3pO
4.
The above; be only preferred embodiment of the present invention; not to any formal and substantial restriction of the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the inventive method, also can make some improvement and supplement, these improve and supplement and also should be considered as protection scope of the present invention.All those skilled in the art, without departing from the spirit and scope of the present invention, a little change made when utilizing disclosed above technology contents, the equivalent variations of modifying and developing, be Equivalent embodiments of the present invention; Meanwhile, all according to substantial technological of the present invention to the change of any equivalent variations that above-described embodiment is done, modify and differentiation, all still belong in the scope of technical scheme of the present invention.
Claims (11)
1. prepare a method for alkali metal phosphate with wet method crude phosphoric acid, it is characterized in that, comprise the following steps:
1) wet method crude phosphoric acid is separated after extraction agent extraction the organic phase obtaining aqueous phase and contain organophosphate;
2) by alkali metal hydroxide aqueous solution or aqueous alkali carbonate solution and step 1) the extraction limit, organic phase limit containing organophosphate that obtains react, is separated the aqueous phase obtaining organic phase and contain alkali metal phosphate;
3) by step 2) obtain obtain alkali metal phosphate containing the aqueous phase of alkali metal phosphate through aftertreatment.
2. wet method crude phosphoric acid according to claim 1 prepares the method for alkali metal phosphate, it is characterized in that, step 2) in be separated the organic phase that obtains and be circulated to step 1) use as extraction agent.
3. wet method crude phosphoric acid according to claim 1 prepares the method for alkali metal phosphate, it is characterized in that, step 1) in, the percentage extraction controlling wet method crude phosphoric acid single extraction is greater than 85%.
4. wet method crude phosphoric acid according to claim 1 prepares the method for alkali metal phosphate, it is characterized in that, step 1) in, when wet method crude phosphoric acid after single extraction in gained aqueous phase wet method crude phosphoric acid the rate of recovery lower than 95% time, after single extraction, gained aqueous phase makes total percentage extraction of wet method crude phosphoric acid reach more than 95% through reextraction again.
5. wet method crude phosphoric acid according to claim 1 prepares the method for alkali metal phosphate, it is characterized in that, step 1) in, when extracting, the volume ratio of described extraction agent and described wet method crude phosphoric acid is 1 ~ 10:1, and extraction time is 10 ~ 120min at every turn.
6. wet method crude phosphoric acid according to claim 1 prepares the method for alkali metal phosphate, it is characterized in that, the difficult water-soluble weakly alkaline organic solvent of described extraction agent.
7. wet method crude phosphoric acid according to claim 1 prepares the method for alkali metal phosphate, it is characterized in that, step 1) in, described extraction agent is mixed extractant, described mixed extractant comprises the weakly alkaline organic solvent and thinner that are insoluble in water, described thinner is the organic solvent that water-insoluble viscosity is little, described in be insoluble in water the volume ratio of weakly alkaline organic solvent and described thinner be 1 ~ 10:1.
8. wet method crude phosphoric acid according to claim 1 prepares the method for alkali metal phosphate, it is characterized in that, step 2) in, the concentration of described alkali metal hydroxide aqueous solution or aqueous alkali carbonate solution is 10wt% ~ saturated solution.
9. wet method crude phosphoric acid according to claim 1 prepares the method for alkali metal phosphate, it is characterized in that, step 2) in, when described alkali metal phosphate is dihydrogen phosphate, the mol ratio of alkalimetal ion and phosphate radical is 1 ~ 1.05:1; When described alkali metal phosphate is monohydric phosphate, the mol ratio of alkalimetal ion and phosphate radical is 2 ~ 2.05:1; When described alkali metal phosphate is phosphoric acid salt, the mol ratio of alkalimetal ion and phosphate radical is 3 ~ 3.05:1.
10. wet method crude phosphoric acid according to claim 1 prepares the method for alkali metal phosphate, it is characterized in that, step 2) in, when described alkali metal phosphate is dihydrogen phosphate, the pH value controlling the aqueous phase containing alkali metal phosphate is 4 ~ 5; When described alkali metal phosphate is monohydric phosphate, the pH value controlling the aqueous phase containing alkali metal phosphate is 8 ~ 9.5; When described alkali metal phosphate is phosphoric acid salt, the pH value controlling the aqueous phase containing alkali metal phosphate is 10.5 ~ 12.
11. wet method crude phosphoric acid according to claim 1 prepare the method for alkali metal phosphate, it is characterized in that, step 2) in, described is 10wt% ~ saturated solution containing the concentration of alkali metal phosphate in the aqueous phase of alkali metal phosphate.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1929443A (en) * | 1930-08-26 | 1933-10-10 | American Agricultural Chem Co | Process for obtaining alkali metal phosphates |
| US4678650A (en) * | 1984-04-06 | 1987-07-07 | Hoechst Aktiengesellschaft | Process for making an alkali phosphate solution |
| CN1258636A (en) * | 1999-12-30 | 2000-07-05 | 清华大学 | Alternate extraction-counter extraction process of producing phosphate |
-
2016
- 2016-01-18 CN CN201610031528.4A patent/CN105502322A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1929443A (en) * | 1930-08-26 | 1933-10-10 | American Agricultural Chem Co | Process for obtaining alkali metal phosphates |
| US4678650A (en) * | 1984-04-06 | 1987-07-07 | Hoechst Aktiengesellschaft | Process for making an alkali phosphate solution |
| CN1258636A (en) * | 1999-12-30 | 2000-07-05 | 清华大学 | Alternate extraction-counter extraction process of producing phosphate |
Non-Patent Citations (3)
| Title |
|---|
| 周霞 等: "溶剂萃取法净化磷酸中氟的研究", 《应用化工》 * |
| 江玉明 等: "萃取法抽取磷酸二氢钾", 《盐湖研究》 * |
| 田恒水 等: "液一液萃取法从湿法磷酸中脱氟制饲料磷酸氢钙", 《华东化工学院学报》 * |
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Application publication date: 20160420 |