CN100389061C - Wet method purification method for phosphate or soluble phosphate - Google Patents
Wet method purification method for phosphate or soluble phosphate Download PDFInfo
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- CN100389061C CN100389061C CNB2005100193128A CN200510019312A CN100389061C CN 100389061 C CN100389061 C CN 100389061C CN B2005100193128 A CNB2005100193128 A CN B2005100193128A CN 200510019312 A CN200510019312 A CN 200510019312A CN 100389061 C CN100389061 C CN 100389061C
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Abstract
The present invention relates to a purification method of wet-process phosphorous acid or soluble phosphate, which is characterized in that the purification method comprises the following steps: 1) preparing emulsion via adding surfactant into organic solvent with a quality ratio of 0.01: 1 to 100: 1; 2) preparing solution via adding interface dissolution process promoter to the emulsion, with promotor quality taking 0.1% to 30% in the quality of the emulsion; 3) preparing emulsion via adding, mixing and stirring water solution of wet-process phosphorous acid or soluble phosphate to the solution with a quality ratio of 20: 80 to 70: 30; 4) stirring the emulsion and letting stand for delamination, and separating liquid to obtain liquid in lower layer namely the water solution of the phosphorous acid or the soluble phosphate. The method can eliminate various high valence metal cations from the wet-process phosphoric acid or phosphate produced from the wet-process phosphorous acid as raw material in high speed and low cost. Via the method, the purifying rate of trivalent metal cations in the wet-process phosphoric acid and the soluble phosphate thereof reaches 97%, and the purifying rate of the divalent metal cations reaches 93%.
Description
Technical field
The invention belongs to the chemical products production field, be specifically related to a kind of phosphoric acid by wet process or be the purifying method of the soluble phosphate of raw material production with the phosphoric acid by wet process.
Background technology
The end-use of phosphoric acid depends on its purity, and phosphoric acid by wet process is produced with natural Rock Phosphate (72Min BPL), so it also contains plurality of impurity ions except phosphoric acid.For this reason, phosphoric acid by wet process always can not be used and can only make fertilizer material as the raw material of some industrial production (as necessary foodstuffs industry with high-purity phosphoric acid, electronic material industry etc.).Generally contain CaO 0.3～0.5% in the phosphoric acid by wet process, MgO 1.18%, Al
2O
30.26%, Fe 0.27%, also has SiO in addition
2, F
-, SO
4 2-Deng foreign ion, how to make the product of production purify the hot issue that becomes phosphatization worker industry.The wet phosphoric acid purifying method is a lot, concludes and gets up to have following 5 types: 1) ion-exchange-resin process; 2) crystallization process; 3) electroosmose process; 4) solvent extration; 5) chemical precipitation method.
Ion-exchange-resin process: be based on H with the refining phosphoric acid by wet process of ion exchange resin
+The H of the Zeo-karb of type
+Ion can replace metal ion contained in the thick acid, and phosphate type or OH
-The anionite-exchange resin of type then may be replaced the ion of vitriol, fluorochemical and silicofluoride, thereby reaches the purpose of purification.Resin after the exchange then uses acid (resin cation (R.C.)) or alkali (resin anion(R.A)) processing to regenerate.From document as can be known, H
+The type Zeo-karb can remove most of Mg from thick acid
2+, Ca
2+, but to Al
3+, Fe
3+Both remove less, and this is because Al
3+Fe can be combined with fluorochemical
3+Can combine with phosphoric acid salt.Therefore, ion exchange method generally just cooperates as a kind of aided process in the whole process with other method.
Crystallization process: be about to the method that the phosphoric acid crystallization is separated out, separate out the difference of mode according to phosphoric acid, crystallization process can divide: H is separated out in (1) crystallization in the high concentration phosphorus acid solution
3PO
4(42.35 ℃ of fusing points) or H
3PO
40.5H
2O (29.32 ℃ of fusing points) crystalline method; (2) phosphatic method is separated out in crystallization; (3) crystallization forms double salt.To preceding two kinds of methods, because the phosphoric acid by wet process foreign matter content is more, direct crystallization is difficulty quite, forms mixed crystal easily, and often need carry out repeatedly crystallization.The crystallization process that generates double salt mainly contains urea phosphate method and melamine phosphate method.
Electroosmose process: electrodialysis is to utilize ion-exchange membrane that the characteristic that ion selectivity sees through is purified PO to some Chemicals
4 3-Adsorptive power on strong alkali anion exchange membrane is greater than most of anionic adsorptive poweies, and its rate of adsorption is again much larger than some anionic rate of adsorption.Therefore can utilize anion-exchange membrane to remove positively charged ion and some negatively charged ion in the phosphoric acid.Utilize this method, under the condition of low current density and lower concentration raw material, can purifying industrial phosphoric acid producing high-purity phosphoric acid, but to SO
4 2-Inrichment is arranged, therefore need to remove SO with chemical method earlier
4 2-, also need solve the current efficiency problem in actual applications.
Solvent extration: the organic solvent of phosphoric acid by wet process with water-insoluble or low water solubility fully contacted, make phosphoric acid enter the organic solvent phase, use less water cleaning solvent phase again, water is stripped then, make phosphoric acid purification, after the extraction, phosphoric acid purity improves greatly more than double.This method phosphoric acid distribution in water and organic phase usually is unfavorable for extraction, so before adopting this method to purify, concentrates raw material phosphoric acid and can improve percentage extraction.
Chemical precipitation method:, add corresponding precipitation agent to remove partial cation or negatively charged ion according to foreign ion character.This method is simple to operate and can reach higher yield.But it is generally not high that impurity is removed rate.
(emulsion liquid membrane, ELM) technology ELM technology is a kind of emerging isolation technique that occurs late 1960s to emulsion liquid membrane, existing so far very big development.In fields such as wastewater treatment, " wet method " metallurgy, petrochemical complex, medical and health extensive studies and utilization are arranged all.Emulsion liquid membrane technology has been simulated biomembranous separation function, and the characteristic of having used parents' molecular structure that tensio-active agent has realizes separating, and has quick, single-minded, characteristic of low energy consumption, is particularly suitable for the separation of lower concentration material.
Summary of the invention
At the shortcoming that above-mentioned phosphoric acid by wet process or soluble phosphate purifying method exist, the object of the present invention is to provide that a kind of cost is low, the purifying method of the phosphoric acid by wet process of good separating effect or soluble phosphate.
To achieve these goals, technical scheme of the present invention is: the purifying method of phosphoric acid by wet process or soluble phosphate, described soluble phosphate are to be the soluble phosphate of raw material production with the phosphoric acid by wet process, it is characterized in that comprising the steps:
1). preparation milk sap: add tensio-active agent in organic solvent, the mass ratio of organic solvent and tensio-active agent is 0.01: 1～100: 1; It is 8～18 water soluble surfactant active that the preparation oil-in-water emulsion is selected HLB value for use, and preparing Water in Oil emulsion, to select the HLB value for use be 3.5～6 oil soluble surfactant;
2). add interface dissolution process promotor obtain solution in the milk sap, interface dissolution process promotor accounts for 0.1%～30% of milk sap quality;
3). add phosphoric acid by wet process or soluble phosphoric acid salt brine solution in solution, the mass ratio of solution and phosphoric acid by wet process or soluble phosphoric acid salt brine solution is 20: 80～70: 30, mixes to stir to be mixed with emulsion;
4). emulsion leaves standstill after stirring, clear liquor is separatory behind standing sedimentation, getting lower floor's liquid is phosphoric acid or soluble phosphoric acid salt brine solution, and the purification rate of trivalent metal cation reaches 97% in phosphoric acid that obtains or the soluble phosphoric acid salt brine solution, and the purification rate of divalent metal reaches 93%.
Organic solvent is any one or any mixing more than two kinds in ethylbenzene, xylol, industrial naptha, gasoline, hexanaphthene, tetrachloromethane, the hexane in the described step 1), and during any mixing more than two kinds, its proportioning is any proportioning.Of the present inventionly contain two kinds more than two kinds arbitrarily, below identical.
The water soluble surfactant active is any one or any mixing more than two kinds in trihydroxy ethylamine stearate, hexadecanol sulfuric ester sodium salt, hexadecanol Soxylat A 25-7, fatty acid alkali metal salt, AEO-9, TX-10, Tween-60, the Tween-40 in the described step 1), during any mixing more than two kinds, its proportioning is any proportioning.
Oil soluble surfactant is any one or any mixing more than two kinds in Zerol, hexadecanol ether-2, Arlacel-60, Arlacel-20, stearic acid, the vegetable fatty acid in the described step 1), during any mixing more than two kinds, its proportioning is any proportioning.
Described step 2) dissolution process promotor in median surface is any one or any mixing more than two kinds in methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, isopropylcarbinol, amylalcohol, primary isoamyl alcohol, glycerine, hexalin, acetate, the propionic acid, during any mixing more than two kinds, its proportioning is any proportioning.
Mixing churning time in the described step 3) is 0.1～24 hour.Stirring reacts completely foreign ion.
Time of repose is 0.5～48 hour in the described step 4).
The invention provides the method that a kind of emulsion liquid membrane isolation technique is come purification of wet process phosphoric acid or its soluble phosphate.This emulsion liquid membrane isolation technique simulated biomembranous separation function, and the characteristic of having used parents' molecular structure that tensio-active agent has realizes separating, and has quick, single-minded, characteristic of low energy consumption, is particularly suitable for the separation of lower concentration material.Metal ion exists with the acid salt form in than low ph environment, and the salt of high price metallic cations such as Al, Ca, Fe has bigger solubleness in phosphoric acid or soluble phosphoric acid salt brine solution.The present invention mixes with the emulsion for preparing by the aqueous solution with phosphoric acid by wet process or its soluble phosphate, has formed the interfacial phase of oil and water.In the present invention, tensio-active agent can reduce the surface tension of oil phase and aqueous phase interface rapidly, the solubleness of salt in oil phase at the high-valency metal foreign ion of aqueous phase is improved relatively, and the solubleness in phosphoric acid or its soluble phosphoric acid salt brine solution reduces relatively.In operation, constantly remove the organic phase that contains high volence metal ion, replenish the new organic phase that does not contain high volence metal ion, reach the purpose of purification of wet process phosphoric acid or its soluble phosphoric acid salt brine solution like this by the emulsion liquid membrane isolation technique.Solvent source is abundant, in larger production, solvent be easy to reclaim and reusability good, the few and easy processing of waste liquid amount, cost method of specific heat phosphoric acid is low, has tangible economic benefit.In addition, purify acid and reach technical grade, can make the purification rate of trivalent metal cation in phosphoric acid or its soluble phosphoric acid salt brine solution reach 97%, the purification rate of divalent metal reaches 93%.Compare with existing several purifying methods, equipment required for the present invention is simple, technical process short, easy to operate, separation costs is lower, good separating effect.
Embodiment
Embodiment one:
Add trihydroxy ethylamine stearate 4.1491g in the Florence flask that fills the 50ml ethylbenzene, measure 5ml methyl alcohol and add in the bottle, add phosphoric acid by wet process 25ml again, put into stirrer, induction stirring 2 hours leaves standstill layering in 30 minutes, and separatory gets the phosphoric acid that lower floor purifies.
Embodiment two:
Add Tween-60 0.7762g in the Florence flask that fills the 10ml ethylbenzene, measure the 5ml dehydrated alcohol and add in the bottle, add phosphoric acid by wet process 20ml again, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment three:
Add stearic acid 2.3284g in the Florence flask that fills the 20ml ethylbenzene, add the 5ml Virahol, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 30 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment four:
Add Tween-40 0.7762g in the Florence flask that fills 10ml xylol (a kind of Industrial products), add the 5ml dehydrated alcohol, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 30 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment five:
Add Arlacel-60 1.5571g in the Florence flask that fills the 20ml ethylbenzene, add the 5ml propyl alcohol, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 30 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment six:
Add trihydroxy ethylamine stearate 1.7791g in the Florence flask that fills the 20ml xylol, add the 5ml propyl alcohol, measure phosphoric acid by wet process 40ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 30 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment seven:
Add Zerol 3.6952g in the Florence flask that fills the 25ml ethylbenzene, add 15ml glycerine, measure phosphoric acid by wet process 30ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 30 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment eight:
Add Zerol 3.6686g in the Florence flask that fills 20ml gasoline, add 15ml glycerine, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 0.5 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment nine:
Add Arlacel-60 0.7251g in the Florence flask that fills 10ml gasoline, 10ml ethylbenzene, add the 5ml dehydrated alcohol, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 0.5 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment ten:
Add Arlacel-60 0.7289g in the Florence flask that fills 6ml gasoline, 4ml hexanaphthene, add 10ml acetate, measure phosphoric acid by wet process 15ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 11
Add Arlacel-20 0.8356g in the Florence flask that fills 15ml xylol, 5ml hexanaphthene, add 10ml methyl alcohol, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 1 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 12:
Add Arlacel-20 0.5678g in the Florence flask that fills 10ml industrial naptha, 10ml xylol, add 5ml methyl alcohol and 5ml acetate, measure phosphoric acid by wet process 25ml and add in the bottle, put into stirrer, induction stirring 1 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 13:
Stearic acid 2.5678g in the Florence flask that fills the 20ml ethylbenzene adds 5ml acetate, measures phosphoric acid by wet process 25ml and adds in the bottle, puts into stirrer, and induction stirring 1 hour gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 14:
Add hexadecanol sulfuric ester sodium salt 3.7864g in the Florence flask that fills the 20ml industrial naptha, add the 5ml dehydrated alcohol, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 1 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 15:
Add vegetable fatty acid 5.6319g in the Florence flask that fills the 20ml ethylbenzene, add 15ml glycerine, measure phosphoric acid by wet process 30ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 16:
Add sodium stearate 3.7864g in the Florence flask that fills the 20ml industrial naptha, add 10ml glycerine and 5ml acetate, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 1 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 17:
Add Tween-40 0.8672g in the Florence flask that fills the 15ml industrial naptha, add 5ml acetate, measure phosphoric acid by wet process 15ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 18:
Add stearic acid 3.8746g in the Florence flask that fills the 20ml hexanaphthene, add the 10ml butanols, get phosphoric acid by wet process 15ml and add in the bottle, put into stirrer, induction stirring 0.5 hour gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 19:
Add Tween-60 0.8861g in the Florence flask that fills the 10ml hexanaphthene, add the 5ml propionic acid, measure phosphoric acid by wet process 10ml and add in the bottle, put into stirrer, induction stirring 0.5 hour gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 20:
Add hexadecanol sulfuric ester sodium salt 3.6766g in filling the hexane Florence flask of 15ml, add the 10ml amylalcohol, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 0.5 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 21:
Add AEO-9 0.7271g in the Florence flask that fills the 10ml xylol, add the 5ml amylalcohol, measure phosphoric acid by wet process 15ml and add in the bottle, put into stirrer, induction stirring 1 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 22:
Add AEO-9 0.8672g in the Florence flask that fills the 20ml tetrachloromethane, add 5ml glycerine and 5ml dehydrated alcohol, measure phosphoric acid by wet process 25ml and add in the bottle, put into stirrer, induction stirring 0.5 hour gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 23:
Add TX-10 2.5864g in the Florence flask that fills the 15ml tetrachloromethane, add the 5ml primary isoamyl alcohol, measure phosphoric acid by wet process 15ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 24:
Add hexadecanol sulfuric ester sodium salt 2.8672g in the Florence flask of Sheng 20ml tetrachloromethane, add 10ml propionic acid and 5ml Virahol, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 1 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 25:
Add vegetable fatty acid 1.6865g in the Florence flask that fills the 10ml hexane, add 10ml glycerine, measure phosphoric acid by wet process 15ml and add in the bottle, put into stirrer, induction stirring 0.5 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 26:
Add Arlacel-60 1.5751g in the Florence flask that fills the 10ml hexane, add the 5ml butanols, measure phosphoric acid by wet process 15ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 27:
Add trihydroxy ethylamine stearate salt 0.5864g in the Florence flask that fills the 20ml hexanaphthene, add the 5ml dehydrated alcohol, measure phosphoric acid by wet process 15ml and add in the bottle, put into stirrer, induction stirring 0.5 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 28:
Add Tween-40 0.8564g in the Florence flask that fills the 15ml hexanaphthene, add 15ml glycerine, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 29:
Add stearic acid 2.5874g in the Florence flask that fills the 15ml hexanaphthene, add 15ml glycerine, measure phosphoric acid by wet process 20ml and add in the bottle, put into stirrer, induction stirring 1.5 hours gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 30:
Add vegetable tallow acid-proof 2.5864g in the Florence flask that fills the 20ml tetrachloromethane, add 15ml glycerine, measure phosphoric acid by wet process 30ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the phosphoric acid that lower floor purifies.
The embodiment hentriaconta-:
Add hexadecanol Soxylat A 25-7 3.5684g in the Florence flask that fills the 20ml ethylbenzene, add the 10ml hexalin, measure phosphoric acid by wet process 25ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 32:
Add hexadecanol ether-22.5762g in the Florence flask that fills the 20ml xylol, add 5ml methyl alcohol and 10ml Virahol, measure phosphoric acid by wet process 25ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the phosphoric acid that lower floor purifies.
Embodiment 33:
Add hexadecanol ether-23.0662g in the Florence flask that fills the 20ml xylol, add 10ml methyl alcohol and 5ml primary isoamyl alcohol, measure phosphoric acid by wet process ammonium dihydrogen aqueous solution 20ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the ammonium dihydrogen phosphate aqueous solution that lower floor must purify.
Embodiment 34:
Add Tween-60 0.7762g in the Florence flask that fills the 10ml ethylbenzene, add the 5ml dehydrated alcohol, add phosphoric acid by wet process ammonium dihydrogen aqueous solution 15ml again, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the ammonium dihydrogen phosphate aqueous solution that lower floor purifies.
Embodiment 35:
Add stearic acid 2.3284g in the Florence flask that fills the 20ml ethylbenzene, add the 5ml Virahol, measure phosphoric acid by wet process ammonium dihydrogen aqueous solution 20ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 30 minutes, separatory gets the ammonium dihydrogen phosphate aqueous solution that lower floor purifies.
Embodiment 36:
Add trihydroxy ethylamine stearate 0.7791g in the Florence flask that fills the 20ml xylol, add the 5ml propyl alcohol, measure phosphoric acid by wet process sodium dihydrogen aqueous solution 25ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 30 minutes, separatory gets the biphosphate sodium water solution that lower floor purifies.
Embodiment 37:
Add Zerol 4.3552g in the Florence flask that fills the 25ml ethylbenzene, add 10ml glycerine, measure phosphoric acid by wet process sodium dihydrogen aqueous solution 25ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 30 minutes, separatory gets the biphosphate sodium water solution that lower floor purifies.
Embodiment 38:
In the Florence flask that fills the 40ml industrial naptha, add higher fatty acid sodium salt 3.2686g, Zerol 0.1356g, add the 15ml dehydrated alcohol, measure phosphoric acid by wet process sodium dihydrogen aqueous solution 15ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the biphosphate sodium water solution that lower floor purifies.
Embodiment 39:
Add Arlacel-60 0.1251g in the Florence flask that fills the 20ml industrial naptha, add the 5ml dehydrated alcohol, measure phosphoric acid by wet process potassium dihydrogen aqueous solution 15ml and add in the bottle, put into stirrer, induction stirring 0.5 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the potassium dihydrogen phosphate aqueous solution that lower floor purifies.
Embodiment 40:
Add Arlacel-60 0.2289g in the Florence flask that fills the 10ml industrial naptha, add 10ml ethanol, measure phosphoric acid by wet process potassium dihydrogen aqueous solution 15ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the potassium dihydrogen phosphate aqueous solution that lower floor purifies.
Embodiment 41:
Add Arlacel-20 0.3356g in the Florence flask that fills the 20ml xylol, add 10ml methyl alcohol, measure phosphoric acid by wet process potassium dihydrogen aqueous solution 15ml and add in the bottle, put into stirrer, induction stirring 1 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the potassium dihydrogen phosphate aqueous solution that lower floor purifies.
Embodiment 42:
Add Arlacel-20 2.7568g in the Florence flask that fills the 20ml industrial naptha, add 10ml methyl alcohol, measure phosphoric acid by wet process hydrogen two aqueous ammonium 25ml and add in the bottle, put into stirrer, induction stirring 1 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the ammonium dibasic phosphate aqueous solution that lower floor purifies.
Embodiment 43:
Stearyl Amine 1.5768g in the Florence flask that fills the 20ml ethylbenzene adds 5ml acetate, measures phosphoric acid by wet process hydrogen two aqueous ammonium 20ml and adds in the bottle, puts into stirrer, and induction stirring 1 hour gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the ammonium dibasic phosphate aqueous solution that lower floor purifies.
Embodiment 44:
Add hexadecanol sulfuric ester sodium salt 3.7864g in the Florence flask that fills the 20ml industrial naptha, add the 5ml dehydrated alcohol, measure phosphoric acid by wet process hydrogen two aqueous ammonium 15ml and add in the bottle, put into stirrer, induction stirring 1 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the ammonium dibasic phosphate aqueous solution that lower floor purifies.
Embodiment 45:
Add vegetable fatty acid 3.5319g in the Florence flask that fills the 20ml ethylbenzene, add 15ml glycerine, measure phosphoric acid by wet process disodium hydrogen aqueous solution 25ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the Sodium phosphate dibasic aqueous solution that lower floor purifies.
Embodiment 46:
Add sodium stearate 2.6564g in the Florence flask that fills the 20ml industrial naptha, add 15ml glycerine, measure phosphoric acid by wet process disodium hydrogen aqueous solution 35ml and add in the bottle, put into stirrer, induction stirring 1 hour gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the Sodium phosphate dibasic aqueous solution that lower floor purifies.
Embodiment 47:
In the Florence flask that fills the 20ml industrial naptha, add Tween-40 0.8762g, sodium stearate 0.3125g, add 10ml acetate, measure phosphoric acid by wet process disodium hydrogen aqueous solution 25ml and add in the bottle, put into stirrer, induction stirring 2 hours gets milky mixture; Leave standstill layering in 60 minutes, separatory gets the Sodium phosphate dibasic aqueous solution that lower floor purifies.
Embodiment 48:
Add potassium stearate 3.8276g, TX-10 0.2038g in the Florence flask that fills the 20ml hexanaphthene, add the 15ml butanols, get phosphoric acid by wet process hydrogen two aqueous solutions of potassium 30ml and add in the bottle, put into stirrer, induction stirring 1.5 hours gets milky mixture; Leave standstill layering in 90 minutes, separatory gets the aqueous dibasic potassium phosphate solution that lower floor purifies.
The bound value of organic solvent of the present invention, tensio-active agent, interface dissolution process promotor, and concrete separately thing can both realize the present invention.
Claims (6)
1. the purifying method of phosphoric acid by wet process or soluble phosphate is characterized in that comprising the steps: 1). preparation milk sap: add tensio-active agent in organic solvent, the mass ratio of organic solvent and tensio-active agent is 0.01: 1～100: 1; It is 8～18 water soluble surfactant active that the preparation oil-in-water emulsion is selected HLB value for use, and preparing Water in Oil emulsion, to select the HLB value for use be 3.5～6 oil soluble surfactant;
Described organic solvent is any one or two or more the mixing arbitrarily in ethylbenzene, xylol, gasoline, tetrachloromethane, hexanaphthene, the hexane, and during any mixing more than two kinds, its proportioning is any proportioning;
2). add interface dissolution process promotor obtain solution in the milk sap, interface dissolution process promotor accounts for 0.1%～30% of milk sap quality;
Described interface dissolution process promotor is any one or any mixing more than two kinds in methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, isopropylcarbinol, amylalcohol, primary isoamyl alcohol, glycerine, hexalin, acetate, the propionic acid, during any mixing more than two kinds, its proportioning is any proportioning;
3). add phosphoric acid by wet process or soluble phosphoric acid salt brine solution in solution, the mass ratio of solution and phosphoric acid by wet process or soluble phosphoric acid salt brine solution is 20: 80～70: 30, mixes to stir to be mixed with emulsion;
4). emulsion leaves standstill after stirring, and clear liquor is separatory behind standing sedimentation, and getting lower floor's liquid is phosphoric acid or soluble phosphoric acid salt brine solution.
2. the purifying method of phosphoric acid by wet process according to claim 1 or soluble phosphate, it is characterized in that: the water soluble surfactant active is any one or any mixing more than two kinds in the trihydroxy ethylamine stearate, hexadecanol sulfuric ester sodium salt, hexadecanol Soxylat A 25-7, fatty acid alkali metal salt, AEO-9, TX-10, Tween-60, Tween-40 in the described step 1), during any mixing more than two kinds, its proportioning is any proportioning.
3. the purifying method of phosphoric acid by wet process according to claim 1 or soluble phosphate, it is characterized in that: oil soluble surfactant is any one or any mixing more than two kinds in Zerol, hexadecanol ether-2, Arlacel-60, Arlacel-20, stearic acid, the vegetable fatty acid in the described step 1), during any mixing more than two kinds, its proportioning is any proportioning.
4. the purifying method of phosphoric acid by wet process according to claim 1 or soluble phosphate is characterized in that: mixing churning time in the described step 3) is 0.1～24 hour.
5. the purifying method of phosphoric acid by wet process according to claim 1 or soluble phosphate is characterized in that: time of repose is 0.5～48 hour in the described step 4).
6. the purifying method of phosphoric acid by wet process according to claim 1 or soluble phosphate is characterized in that: described gasoline is industrial naptha.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3903247A (en) * | 1973-07-18 | 1975-09-02 | Imi Tami Institute Research | Cleaning of phosphoric acid |
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| US3903247A (en) * | 1973-07-18 | 1975-09-02 | Imi Tami Institute Research | Cleaning of phosphoric acid |
Non-Patent Citations (4)
| Title |
|---|
| 乳状液膜状去除湿法磷酸中Mg(Ⅱ)的研究. 高枫等.当代化工，第34卷第2期. 2005 |
| 乳状液膜状去除湿法磷酸中Mg(Ⅱ)的研究. 高枫等.当代化工，第34卷第2期. 2005 * |
| 液膜分离技术净化湿法磷酸中的镁离子. 高枫等.当代化工，第33卷第2期. 2000 |
| 液膜分离技术净化湿法磷酸中的镁离子. 高枫等.当代化工，第33卷第2期. 2000 * |
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Assignee: Wuhan Tianyi Chemical Co., Ltd. Assignor: Wuhan Chemistry College Contract record no.: 2010420000168 Denomination of invention: Wet method purification method for phosphate or soluble phosphate Granted publication date: 20080521 License type: Exclusive License Open date: 20060426 Record date: 20100919 |
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