CN102267691A - Settling agent for wet phosphoric acid refining desulfuration and using method thereof - Google Patents
Settling agent for wet phosphoric acid refining desulfuration and using method thereof Download PDFInfo
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- CN102267691A CN102267691A CN 201110185944 CN201110185944A CN102267691A CN 102267691 A CN102267691 A CN 102267691A CN 201110185944 CN201110185944 CN 201110185944 CN 201110185944 A CN201110185944 A CN 201110185944A CN 102267691 A CN102267691 A CN 102267691A
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- phosphoric acid
- sinking agent
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- ether
- flocculant
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 291
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 149
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 105
- 238000007670 refining Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 239000007864 aqueous solution Substances 0.000 claims abstract description 24
- 159000000009 barium salts Chemical class 0.000 claims abstract description 21
- 239000002893 slag Substances 0.000 claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 229910052788 barium Inorganic materials 0.000 claims abstract description 7
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 90
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 80
- -1 polyoxyethylene Polymers 0.000 claims description 60
- 241000047703 Nonion Species 0.000 claims description 36
- 239000004094 surface-active agent Substances 0.000 claims description 33
- 238000004062 sedimentation Methods 0.000 claims description 31
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 22
- 230000023556 desulfurization Effects 0.000 claims description 19
- 229910019142 PO4 Inorganic materials 0.000 claims description 18
- 230000001186 cumulative effect Effects 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 18
- 239000010452 phosphate Substances 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 12
- NJPQAIBZIHNJDO-UHFFFAOYSA-N 1-dodecylpyrrolidin-2-one Chemical compound CCCCCCCCCCCCN1CCCC1=O NJPQAIBZIHNJDO-UHFFFAOYSA-N 0.000 claims description 11
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 11
- 244000060011 Cocos nucifera Species 0.000 claims description 11
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 11
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229920002125 Sokalan® Polymers 0.000 claims description 9
- 239000004584 polyacrylic acid Substances 0.000 claims description 9
- 150000003016 phosphoric acids Chemical class 0.000 claims description 7
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 5
- 229920002432 poly(vinyl methyl ether) polymer Polymers 0.000 claims description 5
- 238000001914 filtration Methods 0.000 abstract description 33
- 230000000694 effects Effects 0.000 abstract description 14
- 239000000243 solution Substances 0.000 abstract description 8
- 239000003945 anionic surfactant Substances 0.000 abstract description 2
- 239000008394 flocculating agent Substances 0.000 abstract 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 58
- 239000002245 particle Substances 0.000 description 17
- 239000002244 precipitate Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000007787 solid Substances 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 230000003311 flocculating effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
Abstract
The invention discloses a settling agent for wet phosphoric acid refining desulfuration. The settling agent is 0.1 to 1 mass percent aqueous solution; and the solute of the settling agent comprises nonionic flocculating agent and anionic surfactant in a mass ratio of 1: (0-75). A using method of the settling agent comprises the following steps of: adding barium salt into 75 percent phosphoric acid which is at the temperature of 60 DEG C and refined by extracting, wherein the stoichiometric ratio of the barium element in the barium salt to sulfate radicals in the phosphoric acid is 1:1; and continuously stirring the solution for 2 hours, adding the settling agent in a volume which is 0.05 to 1 percent of the volume of the phosphoric acid with stirring, continuously stirring the solution for 5 minutes to obtain phosphoric acid solution, putting the phosphoric acid solution into a settling tank, settling for 4 hours, filtering clear solution and settling slag respectively, delivering the total filtrate obtained by filtration to a concentration device, and performing concentration to obtain 85 percent industrial phosphoric acid. The using method is short in time, high in filtration speed, good in desulfuration effect and low in cost.
Description
Technical field
The present invention relates to a kind of sulfur removal technology of phosphoric acid by wet process, relate in particular to a kind of sinking agent and using method thereof that is used for the wet phosphoric acid refining desulfurization, specifically be applicable to 75% phosphoric acid through extracting and refining is carried out desulfurization to produce 85% industrial phosphoric acid.
Background technology
At present, in the process of the refining phosphoric acid by wet process of solvent extration because the sulfate radical that ortho acid brings also has and is extracted on a small quantity and can not be removed fully, back extraction later on still can a residual part in strip liquor, through concentrating, the sulfate radical content in product industry 85% phosphoric acid is exceeded standard.For this reason, must add barium salt makes sulfate radical generate barium sulfate precipitate and removes.Barium sulfate is a kind of water-fast white solid, its particle when forming is very tiny, and when especially removing sulfate radical in solvent extraction purified phosphoric acid, the diameter of the barium sulfate particle of its generation has only 0.2 micron even littler, if direct filtration is then very easily worn filter.Simultaneously, because the influence of solubility product, in the solution that is lower than 75% phosphoric acid, barium sulfate can not be precipitated out fully, so phosphoric acid concentration must reach 75% at least.
For addressing the above problem, the one, must generate barium sulfate particle in more than or equal to 75% phosphoric acid in concentration, can guarantee that just barium sulfate precipitates fully, thereby remove sulfate radical fully; The 2nd, must wait for that the barium sulfate precipitate particle is long to enough filtering greatly the time again, thereby avoid wearing filter.But because the viscosity of 75% phosphoric acid is very big, thereby adds the barium sulfate particle that barium salt generates in 75% phosphoric acid, must be incubated 40 hours under 40 ℃ of temperature and just can make the barium sulfate precipitate particle long to enough big so that filter, spended time is longer.Nonetheless, because 75% phosphoric acid viscosity is big, filtration velocity can be very slow, even add flocculating aids, filtration velocity is also very slow all the time.
Domestic separation method to barium sulfate in the solution also has some reports, on December calendar year 2001 " chemical engineer " magazine, propose in disclosed " research of ultra-fine barium sulfate particulate flocculating settling " literary composition as flocculation agent barium sulfate to be carried out flocculating settling with Tai-Ace S 150, polyacrylamide respectively such as Li Jun equality, to reach the purpose of separating barium sulfate, but experimental data and conclusion from article, settled effect is not very good, clear liquid accounts for 50% greatly, arch formation is fairly obvious, satisfy need of industrial production, also have very long stretch to walk.In addition, Shangfang is given birth and is proposed to adopt horizontal settling centrifuge to substitute leaf-type vacuum filter or chamber filter press to enhance productivity in September, 2005 " inorganic chemicals industry " magazine in " research of horizontal settling centrifuge precipitation separation barium sulfate " literary composition, but data from article, separating effect is not fully up to expectations, and operational condition is too harsh.In addition, these two pieces of articles at all be under non-phosphoric acid system to the separation of barium sulfate, thereby can not solve long, the slower problem of filtration velocity of spended time that occurs in the 75% phosphoric acid desulfurization behind the extracting and refining.
The Chinese patent patent No. is ZL200510019748.7, and Granted publication day is the method that the patent of invention on February 14th, 2007 discloses solids and fluorine in a kind of quick removal wet method crude phosphoric acid, and this method is earlier at P
2O
5Mass content is to add yellow soda ash in 20%～54% raw phosphoric acid, stirring reaction 1～1.2 hour, subsequently, add sinking agent, sinking agent is that total mass concentration that flocculant in non-ion type and anion surfactant are mixed with by mass ratio 1: 25～75 is 1%～10% the aqueous solution, and the sinking agent add-on is 0.1%～5% of a raw phosphoric acid volume, 5～24 hours settling times, get the clarification phosphoric acid of liquid≤20% on earth, the solid content＜0.5wt% of phosphoric acid clear liquid, fluorine decreasing ratio 〉=84%.Though this invention can be removed solids and fluorine in the wet method crude phosphoric acid fast by sinking agent, but it and be not suitable for extracting and refining after the removal of sulfate radical in 75% phosphoric acid, its reason is as follows: at first, the system difference, this invents wet method crude phosphoric acid to be processed, the kind of the impurity that it contains and content are all very many, and present system to be processed is through 75% phosphoric acid by wet process behind the extracting and refining, beyond its foreign matter content sulfate radical, other have all met the requirement of PHOSPHORIC ACID TECH.GRADE, as seen, the system difference causes the filtering object difference, and different filtering objects will require different sinking agents; Secondly, sinking agent at the object difference: the sinking agent that this invention is taked is at the solid sediment in the raw phosphoric acid, comprise calcium, iron, the aluminium of calcium sulfate, phosphoric acid, double salt and the fluorine or the silicofluoride etc. of potassium, and now to be processed be barium sulfate, object is obviously different, if firmly with the sinking agent in this invention, then its specific aim just a little less than, effect of settling is also just relatively poor, thereby can not solve existing issue; The 3rd, the outside temperature difference of sinking agent effect: the outside temperature of the sinking agent effect that this invention is adopted is 60 ℃ of 15 –, and present environment is self temperature of 75% phosphoric acid behind the extracting and refining, this temperature is more than or equal to 60 ℃, under this high temperature, the stability of the sinking agent in this invention will reduce greatly, diminishes the realization of its effect of settling.
Summary of the invention
The objective of the invention is to overcome long, slower defective and the problem of filtration velocity of the spended time that exists in the prior art, a kind of spended time is short, filtration velocity is used for the wet phosphoric acid refining desulfurization faster sinking agent and using method thereof are provided.
For realizing above purpose, technical solution of the present invention is:
A kind of sinking agent that is used for the wet phosphoric acid refining desulfurization, this sinking agent are a kind of aqueous solution, and its solute is flocculant in non-ion type and aniorfic surfactant;
Described sinking agent is that mass percent concentration is the aqueous solution of 1 ‰ – 10 ‰, and the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:0 – 75;
Described flocculant in non-ion type is a kind of of octadecyl polyoxyethylene (4) ether, coconut oleoyl amine polyoxyethylene (6) ether, polyvinyl methyl ether, polyacrylamide, N – dodecyl pyrrolidone, poly-alkane base phenol – oxyethane or any two kinds of preparing by the mass ratio of 1:1;
Described aniorfic surfactant is a kind of of polyacrylic acid isopropyl ester, alkyl phosphate diethanolamine salt, isooctyl alcohol polyoxyethylene groups ether phosphate, alcohol ether phosphate monoester.
The mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:0 – 75 in the described sinking agent.
Described flocculant in non-ion type is a kind of of octadecyl polyoxyethylene (4) ether, coconut oleoyl amine polyoxyethylene (6) ether, N – dodecyl pyrrolidone or any two kinds of preparing by the mass ratio of 1:1;
Described aniorfic surfactant is a kind of of polyacrylic acid isopropyl ester, alkyl phosphate diethanolamine salt, isooctyl alcohol polyoxyethylene groups ether phosphate, alcohol ether phosphate monoester.
A kind of using method that is used for the sinking agent of wet phosphoric acid refining desulfurization, this using method may further comprise the steps successively:
The first step: be not less than 60 ℃ passing through in 75% phosphoric acid of extracting and refining in the liquid temperature, measure the content of sulfate radical in this phosphoric acid earlier, add barium salt again under the state that stirs, the stoichiometric ratio of barium element is 1:1 in sulfate radical and the barium salt, continues to stir 2 hours then to obtain mixed solution;
Second step: under the state that stirs sinking agent is added in the above-mentioned mixed solution earlier, the volume of sinking agent is 0.5 ‰ – 10 ‰ of phosphoric acid volume, continues to stir 5 minutes again to obtain the phosphoric acid feed liquid, then the phosphoric acid feed liquid is put into subsider and carries out sedimentation;
The 3rd step: after the sedimentation in 4 hours, collect the clear liquid on phosphoric acid feed liquid top earlier, this clear liquid accounts for 80 – 90% of phosphoric acid feed liquid cumulative volume, plate-and-frame filter press with existing precoated layer filters clear liquid again, collect remaining sedimentation slag then and filter, the total filtrate that will cross cleaner liquid, sedimentation slag gained is again delivered to concentrating unit and is concentrated to obtain 85% industrial phosphoric acid.
In described second step, the volume of sinking agent is 0.5 ‰ – 10 ‰ of phosphoric acid volume.
Compared with prior art, beneficial effect of the present invention is:
1, the application system of a kind of sinking agent that is used for the wet phosphoric acid refining desulfurization of the present invention and using method thereof is not less than 60 ℃ 75% phosphoric acid through extracting and refining for the liquid temperature, the sulfur method that the present invention takes is for adding barium salt earlier to generate barium sulfate particle in phosphoric acid, add the barium sulfate particle of the sinking agent of unique design again with the precipitation generation, then the clear liquid after the sedimentation, sedimentation slag are filtered to obtain total filtrate, concentrate total filtrate at last and can obtain 85% industrial phosphoric acid, at this moment, whole sweetening process finishes fully.In the whole process, at first, because concentration of phosphoric acid is 75%, thereby the barium sulfate that generates can be precipitated out fully, and sweetening effectiveness is fine; Secondly, owing to only need to remove sulfate radical, thereby the consumption of sinking agent is less, be 0.5 ‰ – 10 ‰ of phosphoric acid volume only, reduced cost, and when the volume of sinking agent is 0.5 ‰ – 10 ‰ of phosphoric acid volume, not only can guarantee sweetening effectiveness, and cost reduction effect is more obvious; The 3rd, because the prescription of the sinking agent of taking and the specific aim of usage quantity are stronger, thereby only need sedimentation can make the barium sulfate precipitate particle long in 4 hours to enough big, compare with 40 hours of prior art, time shortens greatly, moreover, filtration velocity also increases greatly, is more than 25 times of feed liquid with sinking agent with the filtration velocity of the later feed liquid of sinking agent sedimentation.Therefore not only spended time is short, filtration velocity is very fast in the present invention, and sweetening effectiveness is better, cost is lower.
2, a kind of sinking agent and using method depressant prescription thereof that is used for the wet phosphoric acid refining desulfurization of the present invention is that mass percent concentration is the aqueous solution of 1 ‰ – 10 ‰, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:0 – 75, wherein, flocculant in non-ion type is octadecyl polyoxyethylene (a 4) ether, coconut oleoyl amine polyoxyethylene (6) ether, polyvinyl methyl ether, polyacrylamide, N – dodecyl pyrrolidone, poly-alkane base phenol – oxyethane a kind of or any two kinds of preparing by the mass ratio of 1:1, better choice is octadecyl polyoxyethylene (a 4) ether, coconut oleoyl amine polyoxyethylene (6) ether, N – dodecyl pyrrolidone a kind of or any two kinds of preparing by the mass ratio of 1:1, and aniorfic surfactant is the polyacrylic acid isopropyl ester, the alkyl phosphate diethanolamine salt, isooctyl alcohol polyoxyethylene groups ether phosphate, alcohol ether phosphate monoester a kind of, this design is and the sedimentation object, depositional temperature correlation.Because what the present invention is directed to is 75% phosphoric acid behind the extracting and refining, not only viscosity is big, the temperature height, and the impurity that needs to remove only is sulfate radical, thereby selecting flocculant in non-ion type, during the combination of aniorfic surfactant, big at 75% phosphoric acid viscosity, the very tiny filtration that causes of barium sulfate precipitate particle very the factors such as interaction of difficulty and flocculation agent and tensio-active agent to flocculant in non-ion type, the kind of aniorfic surfactant and consumption have carried out rational screening, not only can guarantee sweetening effectiveness preferably, and under more than or equal to 60 ℃ temperature, can also keep stable character, cost is also lower, simultaneously, concentration for sinking agent also has screening, promptly select the sinking agent of low concentration (1 ‰ – 10 ‰), the sinking agent of lower concentration not only can guarantee to realize sweetening effectiveness, and cost is lower.Therefore not only sweetening effectiveness is better, stable in properties in the present invention, and cost is lower.
Embodiment
The present invention is further detailed explanation below in conjunction with embodiment.
A kind of sinking agent that is used for the wet phosphoric acid refining desulfurization, this sinking agent are a kind of aqueous solution, and its solute is flocculant in non-ion type and aniorfic surfactant;
Described sinking agent is that mass percent concentration is the aqueous solution of 1 ‰ – 10 ‰, and the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:0 – 75;
Described flocculant in non-ion type is a kind of of octadecyl polyoxyethylene (4) ether, coconut oleoyl amine polyoxyethylene (6) ether, polyvinyl methyl ether, polyacrylamide, N – dodecyl pyrrolidone, poly-alkane base phenol – oxyethane or any two kinds of preparing by the mass ratio of 1:1;
Described aniorfic surfactant is a kind of of polyacrylic acid isopropyl ester, alkyl phosphate diethanolamine salt, isooctyl alcohol polyoxyethylene groups ether phosphate, alcohol ether phosphate monoester.
The mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:0 – 75 in the described sinking agent.
Described flocculant in non-ion type is a kind of of octadecyl polyoxyethylene (4) ether, coconut oleoyl amine polyoxyethylene (6) ether, N – dodecyl pyrrolidone or any two kinds of preparing by the mass ratio of 1:1;
Described aniorfic surfactant is a kind of of polyacrylic acid isopropyl ester, alkyl phosphate diethanolamine salt, isooctyl alcohol polyoxyethylene groups ether phosphate, alcohol ether phosphate monoester.
The principle of sinking agent is described as follows:
The phosphoric acid that the present invention is directed to be the liquid temperature be not less than 60 ℃ through 75% phosphoric acid of extracting and refining, not only viscosity is big, temperature is high, and the impurity that contains only is sulfate radical, the particle that adds the barium sulfate that generates behind the barium salt is very little.In order to improve sweetening effectiveness, shorten the operating time, to improve filtration velocity, not only to overcome the barium sulfate particle of the big characteristics of phosphoric acid viscosity, formation enough big in requirement, and the time that barium sulfate particle is grown up also must be short, thereby added sinking agent.Under lower temperature, under 40 ℃, the viscosity of phosphoric acid is higher, reaction for barium salt and sulfate radical is unfavorable, and when temperature was brought up to 60 ℃, sinking agent will be more obvious to the absorption coagulation effect of barium sulfate particle, therefore, this sinking agent must be not less than 60 ℃ pass through in the liquid temperature and keep stable character in 75% phosphoric acid of extracting and refining, only in this way just can give full play to its effect of settling.
For realizing above effect, the present invention has carried out unique design to the kind and the consumption of mass percent concentration, flocculant in non-ion type and the aniorfic surfactant of sinking agent.The akin material of flocculant in non-ion type, aniorfic surfactant that some and the present invention adopt, because effect is bad under this phosphoric acid concentration, can not realize above effect, thereby do not taked, as alkyl benzene sulphonate (ABS) and sodium salt, sodium laurylsulfonate etc., they can introduce the sulfonic acid of similar sulfate radical, can cause sulfate radical defective.
A kind of using method that is used for the sinking agent of wet phosphoric acid refining desulfurization, this using method may further comprise the steps successively:
The first step: be not less than 60 ℃ passing through in 75% phosphoric acid of extracting and refining in the liquid temperature, measure the content of sulfate radical in this phosphoric acid earlier, add barium salt again under the state that stirs, the stoichiometric ratio of barium element is 1:1 in sulfate radical and the barium salt, continues to stir 2 hours then to obtain mixed solution;
Second step: under the state that stirs sinking agent is added in the above-mentioned mixed solution earlier, the volume of sinking agent is 0.5 ‰ – 10 ‰ of phosphoric acid volume, continues to stir 5 minutes again to obtain the phosphoric acid feed liquid, then the phosphoric acid feed liquid is put into subsider and carries out sedimentation;
The 3rd step: after the sedimentation in 4 hours, collect the clear liquid on phosphoric acid feed liquid top earlier, this clear liquid accounts for 80 – 90% of phosphoric acid feed liquid cumulative volume, plate-and-frame filter press with existing precoated layer filters clear liquid again, collect remaining sedimentation slag then and filter, the total filtrate that will cross cleaner liquid, sedimentation slag gained is again delivered to concentrating unit and is concentrated to obtain 85% industrial phosphoric acid.
In described second step, the volume of sinking agent is 0.5 ‰ – 1 ‰ of phosphoric acid volume.
User's ratio juris is described as follows:
In the first step 60 ℃ are self temperature of 75% phosphoric acid, it is the temperature that flow process is gone to this, the viscosity of phosphoric acid is relatively low under this temperature, favourable for barium salt and sulfate radical reaction generation barium sulfate precipitate, simultaneously, best to the coagulation effect of barium sulfate particle at 60 ℃ of following sinking agents, 2 hours churning time then is more complete for what the reaction that generates barium sulfate can be carried out.
The purpose that adds sinking agent in second step is to make barium sulfate particle to flocculate bigger sedimented particle in the short period of time, the shortening time, is convenient to filter.The purpose that adds sinking agents according to 0.5 ‰ – 10 ‰ of phosphoric acid volume is to be convenient to sedimentation, if adopt 0.5 ‰ below or the ratios more than 10 ‰, and then can't sedimentation.
4 hours settling time is 60 ℃ a envrionment temperature and the acting in conjunction that adds sinking agent in the 3rd step.
Comparative Examples:
Be not less than 60 ℃ passing through in 75% phosphoric acid of extracting and refining in the liquid temperature, in measuring phosphoric acid, behind the sulfate radical content, under agitation add barium salt, and continue to stir 2 hours according to sulfate radical content stoichiometric 100%; Get the phosphoric acid feed liquid and filter with the plate-and-frame filter press that precoated layer is arranged, filtration velocity is 0.576M
3/ dM
2, cleaner liquid send concentrating unit further to be concentrated into 85% phosphoric acid, promptly gets qualified product 85% industrial phosphoric acid.
Embodiment 1:
A kind of using method that is used for the sinking agent of wet phosphoric acid refining desulfurization, this using method may further comprise the steps successively:
The first step: be not less than 60 ℃ passing through in 75% phosphoric acid of extracting and refining in the liquid temperature, measure the content of sulfate radical in this phosphoric acid earlier, add barium salt again under the state that stirs, the stoichiometric ratio of barium element is 1:1 in sulfate radical and the barium salt, continues to stir 2 hours then to obtain mixed solution;
Second step: under the state that stirs sinking agent is added in the above-mentioned mixed solution earlier, the volume of sinking agent is 0.5 ‰ of a phosphoric acid volume, continues to stir 5 minutes again to obtain the phosphoric acid feed liquid, then the phosphoric acid feed liquid is put into subsider and carries out sedimentation;
The 3rd step: after the sedimentation in 4 hours, collect the clear liquid on phosphoric acid feed liquid top earlier, this clear liquid accounts for 80% of phosphoric acid feed liquid cumulative volume, and the plate-and-frame filter press with existing precoated layer filters clear liquid again, and filtration velocity is 25M
3/ dM
2, to collect remaining sedimentation slag then and filter, the total filtrate that will cross cleaner liquid, sedimentation slag gained is again delivered to concentrating unit and is concentrated to obtain 85% industrial phosphoric acid.
Described sinking agent is that mass percent concentration is 10 ‰ the aqueous solution, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:5, wherein, flocculant in non-ion type is a kind of of octadecyl polyoxyethylene (4) ether, coconut oleoyl amine polyoxyethylene (6) ether, polyvinyl methyl ether, polyacrylamide, N – dodecyl pyrrolidone, poly-alkane base phenol – oxyethane or any two kinds of preparing by the mass ratio of 1:1; Aniorfic surfactant is a kind of of polyacrylic acid isopropyl ester, alkyl phosphate diethanolamine salt, isooctyl alcohol polyoxyethylene groups ether phosphate, alcohol ether phosphate monoester.
Embodiment 2:
Step is with embodiment 1, and difference is: the volume of sinking agent is 0.8 ‰ of a phosphoric acid volume, and clear liquid accounts for 85% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 26M
3/ dM
2, sinking agent is that mass percent concentration is 3 ‰ the aqueous solution, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:15.
Embodiment 3:
Step is with embodiment 1, and difference is: the volume of sinking agent is 1 ‰ of a phosphoric acid volume, and clear liquid accounts for 90% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 25M
3/ dM
2, sinking agent is that mass percent concentration is 5 ‰ the aqueous solution, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:25.
Embodiment 4:
Step is with embodiment 1, and difference is: the volume of sinking agent is 6 ‰ of a phosphoric acid volume, and clear liquid accounts for 85% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 24M
3/ dM
2, sinking agent is that mass percent concentration is 8 ‰ the aqueous solution, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:35.
Embodiment 5:
Step is with embodiment 1, and difference is: the volume of sinking agent is 10 ‰ of a phosphoric acid volume, and clear liquid accounts for 90% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 25M
3/ dM
2, sinking agent is that mass percent concentration is 1 ‰ the aqueous solution, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:75.
Embodiment 6:
A kind of using method that is used for the sinking agent of wet phosphoric acid refining desulfurization, this using method may further comprise the steps successively:
The first step: be not less than 60 ℃ passing through in 75% phosphoric acid of extracting and refining in the liquid temperature, measure the content of sulfate radical in this phosphoric acid earlier, add barium salt again under the state that stirs, the stoichiometric ratio of barium element is 1:1 in sulfate radical and the barium salt, continues to stir 2 hours then to obtain mixed solution;
Second step: under the state that stirs sinking agent is added in the above-mentioned mixed solution earlier, the volume of sinking agent is 0.5 ‰ of a phosphoric acid volume, continues to stir 5 minutes again to obtain the phosphoric acid feed liquid, then the phosphoric acid feed liquid is put into subsider and carries out sedimentation;
The 3rd step: after the sedimentation in 4 hours, collect the clear liquid on phosphoric acid feed liquid top earlier, this clear liquid accounts for 80% of phosphoric acid feed liquid cumulative volume, and the plate-and-frame filter press with existing precoated layer filters clear liquid again, and filtration velocity is 25M
3/ dM
2, to collect remaining sedimentation slag then and filter, the total filtrate that will cross cleaner liquid, sedimentation slag gained is again delivered to concentrating unit and is concentrated to obtain 85% industrial phosphoric acid.
Described sinking agent is that mass percent concentration is 10 ‰ the aqueous solution, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:5, wherein, flocculant in non-ion type is a kind of of octadecyl polyoxyethylene (4) ether, coconut oleoyl amine polyoxyethylene (6) ether, N – dodecyl pyrrolidone or any two kinds of preparing by the mass ratio of 1:1; Aniorfic surfactant is a kind of of polyacrylic acid isopropyl ester, alkyl phosphate diethanolamine salt, isooctyl alcohol polyoxyethylene groups ether phosphate, alcohol ether phosphate monoester.
Embodiment 7:
Step is with embodiment 6, and difference is: the volume of sinking agent is 0.8 ‰ of a phosphoric acid volume, and clear liquid accounts for 85% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 26M
3/ dM
2, sinking agent is that mass percent concentration is 3 ‰ the aqueous solution, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:15.
Embodiment 8:
Step is with embodiment 6, and difference is: the volume of sinking agent is 1 ‰ of a phosphoric acid volume, and clear liquid accounts for 90% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 25M
3/ dM
2, sinking agent is that mass percent concentration is 5 ‰ the aqueous solution, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:25.
Embodiment 9:
Step is with embodiment 6, and difference is: the volume of sinking agent is 6 ‰ of a phosphoric acid volume, and clear liquid accounts for 85% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 24M
3/ dM
2, sinking agent is that mass percent concentration is 8 ‰ the aqueous solution, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:35.
Embodiment 10:
Step is with embodiment 6, and difference is: the volume of sinking agent is 10 ‰ of a phosphoric acid volume, and clear liquid accounts for 90% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 25M
3/ dM
2, sinking agent is that mass percent concentration is 1 ‰ the aqueous solution, the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:75.
Embodiment 11:
A kind of using method that is used for the sinking agent of wet phosphoric acid refining desulfurization, this using method may further comprise the steps successively:
The first step: be not less than 60 ℃ passing through in 75% phosphoric acid of extracting and refining in the liquid temperature, measure the content of sulfate radical in this phosphoric acid earlier, add barium salt again under the state that stirs, the stoichiometric ratio of barium element is 1:1 in sulfate radical and the barium salt, continues to stir 2 hours then to obtain mixed solution;
Second step: under the state that stirs sinking agent is added in the above-mentioned mixed solution earlier, the volume of sinking agent is 0.5 ‰ of a phosphoric acid volume, continues to stir 5 minutes again to obtain the phosphoric acid feed liquid, then the phosphoric acid feed liquid is put into subsider and carries out sedimentation;
The 3rd step: after the sedimentation in 4 hours, collect the clear liquid on phosphoric acid feed liquid top earlier, this clear liquid accounts for 80% of phosphoric acid feed liquid cumulative volume, and the plate-and-frame filter press with existing precoated layer filters clear liquid again, and filtration velocity is 25M
3/ dM
2, to collect remaining sedimentation slag then and filter, the total filtrate that will cross cleaner liquid, sedimentation slag gained is again delivered to concentrating unit and is concentrated to obtain 85% industrial phosphoric acid.
Described sinking agent is that mass percent concentration is 10 ‰ the aqueous solution, its solute only is a flocculant in non-ion type, and flocculant in non-ion type is a kind of of octadecyl polyoxyethylene (4) ether, coconut oleoyl amine polyoxyethylene (6) ether, N – dodecyl pyrrolidone or any two kinds of preparing by the mass ratio of 1:1.
Embodiment 12:
Step is with embodiment 11, and difference is: the volume of sinking agent is 0.8 ‰ of a phosphoric acid volume, and clear liquid accounts for 85% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 26M
3/ dM
2, sinking agent is that mass percent concentration is 3 ‰ the aqueous solution.
Embodiment 13:
Step is with embodiment 11, and difference is: the volume of sinking agent is 1 ‰ of a phosphoric acid volume, and clear liquid accounts for 90% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 25M
3/ dM
2, sinking agent is that mass percent concentration is 5 ‰ the aqueous solution.
Embodiment 14:
Step is with embodiment 11, and difference is: the volume of sinking agent is 6 ‰ of a phosphoric acid volume, and clear liquid accounts for 85% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 24M
3/ dM
2, sinking agent is that mass percent concentration is 8 ‰ the aqueous solution.
Embodiment 15:
Step is with embodiment 11, and difference is: the volume of sinking agent is 10 ‰ of a phosphoric acid volume, and clear liquid accounts for 90% of phosphoric acid feed liquid cumulative volume, and filtration velocity is 25M
3/ dM
2, sinking agent is that mass percent concentration is 1 ‰ the aqueous solution.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the above is only own for specific embodiments of the invention; be not limited to the present invention; all within claim of the present invention, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. sinking agent that is used for the wet phosphoric acid refining desulfurization, this sinking agent is a kind of aqueous solution, its solute is flocculant in non-ion type and aniorfic surfactant, it is characterized in that:
Described sinking agent is that mass percent concentration is the aqueous solution of 1 ‰ – 10 ‰, and the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:0 – 75;
Described flocculant in non-ion type is a kind of of octadecyl polyoxyethylene (4) ether, coconut oleoyl amine polyoxyethylene (6) ether, polyvinyl methyl ether, polyacrylamide, N – dodecyl pyrrolidone, poly-alkane base phenol – oxyethane or any two kinds of preparing by the mass ratio of 1:1;
Described aniorfic surfactant is a kind of of polyacrylic acid isopropyl ester, alkyl phosphate diethanolamine salt, isooctyl alcohol polyoxyethylene groups ether phosphate, alcohol ether phosphate monoester.
2. a kind of sinking agent that is used for the wet phosphoric acid refining desulfurization according to claim 1 is characterized in that: the mass ratio of flocculant in non-ion type and aniorfic surfactant is 1:0 – 75 in the described sinking agent.
3. a kind of sinking agent that is used for the wet phosphoric acid refining desulfurization according to claim 1 is characterized in that: described flocculant in non-ion type is a kind of of octadecyl polyoxyethylene (4) ether, coconut oleoyl amine polyoxyethylene (6) ether, N – dodecyl pyrrolidone or any two kinds of preparing by the mass ratio of 1:1;
Described aniorfic surfactant is a kind of of polyacrylic acid isopropyl ester, alkyl phosphate diethanolamine salt, isooctyl alcohol polyoxyethylene groups ether phosphate, alcohol ether phosphate monoester.
4. claim 1,2 or 3 described a kind of using method that are used for the sinking agent of wet phosphoric acid refining desulfurization is characterized in that this using method may further comprise the steps successively:
The first step: be not less than 60 ℃ passing through in 75% phosphoric acid of extracting and refining in the liquid temperature, measure the content of sulfate radical in this phosphoric acid earlier, add barium salt again under the state that stirs, the stoichiometric ratio of barium element is 1:1 in sulfate radical and the barium salt, continues to stir 2 hours then to obtain mixed solution;
Second step: under the state that stirs sinking agent is added in the above-mentioned mixed solution earlier, the volume of sinking agent is 0.5 ‰ – 10 ‰ of phosphoric acid volume, continues to stir 5 minutes again to obtain the phosphoric acid feed liquid, then the phosphoric acid feed liquid is put into subsider and carries out sedimentation;
The 3rd step: after the sedimentation in 4 hours, collect the clear liquid on phosphoric acid feed liquid top earlier, this clear liquid accounts for 80 – 90% of phosphoric acid feed liquid cumulative volume, plate-and-frame filter press with existing precoated layer filters clear liquid again, collect remaining sedimentation slag then and filter, the total filtrate that will cross cleaner liquid, sedimentation slag gained is again delivered to concentrating unit and is concentrated to obtain 85% industrial phosphoric acid.
5. a kind of using method that is used for the sinking agent of wet phosphoric acid refining desulfurization according to claim 4 is characterized in that: in described second step, the volume of sinking agent is 0.5 ‰ – 10 ‰ of phosphoric acid volume.
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Cited By (9)
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|---|---|---|---|---|
| CN102556991A (en) * | 2012-01-11 | 2012-07-11 | 吴杰 | Pre-treatment method applied to wet process phosphoric acid extraction and refining through composite extracting agents |
| CN103332666A (en) * | 2013-07-10 | 2013-10-02 | 湖北兴发化工集团股份有限公司 | Settling agent in wet-method phosphoric acid concentration processing process |
| CN104591110A (en) * | 2015-01-13 | 2015-05-06 | 四川省汉源化工总厂 | Method for preparing low-sulfur-content calcium dihydrogen phosphate by concentrating wet-process phosphoric acid |
| CN105439109A (en) * | 2015-12-29 | 2016-03-30 | 中国海洋石油总公司 | Concentration method of wet-process phosphoric acid |
| CN105944451A (en) * | 2016-05-16 | 2016-09-21 | 吴立新 | Polymerizing agent for flocculating barium sulfate during wet process phosphoric acid refinement and flocculating method adopting polymerizing agent |
| CN105948212A (en) * | 2016-06-16 | 2016-09-21 | 上海华友金裕微电子有限公司 | Organic acid sinking agent preparing method |
| CN114671419A (en) * | 2022-04-06 | 2022-06-28 | 武汉强盛科技有限公司 | Settling agent and method for rapidly reducing solid content of wet-process phosphoric acid |
| WO2022140804A1 (en) * | 2020-12-21 | 2022-06-30 | Tu Trinh Hong | Method for filtering impurities in concentrated extracted phosphoric acid for enhancement of diammonium phosphate fertilizer content and for treatment of post-filtration solid waste into phosphate fertilizer, np fertilizer or npk fertilizer. |
| CN115092898A (en) * | 2022-06-21 | 2022-09-23 | 云南磷化集团有限公司 | Method for removing sulfate radical in wet-process phosphoric acid by using yellow phosphorus slag |
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| CN102556991A (en) * | 2012-01-11 | 2012-07-11 | 吴杰 | Pre-treatment method applied to wet process phosphoric acid extraction and refining through composite extracting agents |
| CN102556991B (en) * | 2012-01-11 | 2013-11-20 | 吴杰 | Pre-treatment method applied to wet process phosphoric acid extraction and refining through composite extracting agents |
| CN103332666A (en) * | 2013-07-10 | 2013-10-02 | 湖北兴发化工集团股份有限公司 | Settling agent in wet-method phosphoric acid concentration processing process |
| CN103332666B (en) * | 2013-07-10 | 2015-11-18 | 湖北兴发化工集团股份有限公司 | Sinking agent in a kind of wet-process phosphoric acid concentration treating processes |
| CN104591110A (en) * | 2015-01-13 | 2015-05-06 | 四川省汉源化工总厂 | Method for preparing low-sulfur-content calcium dihydrogen phosphate by concentrating wet-process phosphoric acid |
| CN105439109A (en) * | 2015-12-29 | 2016-03-30 | 中国海洋石油总公司 | Concentration method of wet-process phosphoric acid |
| CN105944451A (en) * | 2016-05-16 | 2016-09-21 | 吴立新 | Polymerizing agent for flocculating barium sulfate during wet process phosphoric acid refinement and flocculating method adopting polymerizing agent |
| CN105948212A (en) * | 2016-06-16 | 2016-09-21 | 上海华友金裕微电子有限公司 | Organic acid sinking agent preparing method |
| WO2022140804A1 (en) * | 2020-12-21 | 2022-06-30 | Tu Trinh Hong | Method for filtering impurities in concentrated extracted phosphoric acid for enhancement of diammonium phosphate fertilizer content and for treatment of post-filtration solid waste into phosphate fertilizer, np fertilizer or npk fertilizer. |
| CN114671419A (en) * | 2022-04-06 | 2022-06-28 | 武汉强盛科技有限公司 | Settling agent and method for rapidly reducing solid content of wet-process phosphoric acid |
| CN114671419B (en) * | 2022-04-06 | 2024-04-12 | 武汉强盛科技有限公司 | Settling agent and method for rapidly reducing solid content of wet-process phosphoric acid |
| CN115092898A (en) * | 2022-06-21 | 2022-09-23 | 云南磷化集团有限公司 | Method for removing sulfate radical in wet-process phosphoric acid by using yellow phosphorus slag |
| CN115092898B (en) * | 2022-06-21 | 2023-09-19 | 云南磷化集团有限公司 | Method for removing sulfate radical in wet-process phosphoric acid by utilizing yellow phosphorus slag |
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