CN103332666A - Settling agent in wet-method phosphoric acid concentration processing process - Google Patents

Settling agent in wet-method phosphoric acid concentration processing process Download PDF

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Publication number
CN103332666A
CN103332666A CN2013102883118A CN201310288311A CN103332666A CN 103332666 A CN103332666 A CN 103332666A CN 2013102883118 A CN2013102883118 A CN 2013102883118A CN 201310288311 A CN201310288311 A CN 201310288311A CN 103332666 A CN103332666 A CN 103332666A
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phosphoric acid
wet
parts
agent
sinking agent
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CN2013102883118A
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CN103332666B (en
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罗宝瑞
吴保全
段利中
虞康浩
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Hubei Xingfa Chemicals Group Co Ltd
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Hubei Xingfa Chemicals Group Co Ltd
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Abstract

An excellent settling agent used for processing the concentration of wet-method phosphoric acid is prepared by sending 40-93 parts by mass of an anionic flocculating agent, 1-30 parts by mass of a non-ionic flocculating agent, 1-40 parts by mass of an adsorbent and 0-20 parts by mass of a fluorine removal agent to a stirring tank, controlling the temperature of the stirring tank in a range of 60-80DEG C through heating and heat insulation via a jacket, and allowing the solution obtained after stirring ending to stand for 10-40min. The excellent settling agent has the advantages of low prices and easy purchasing of the above used raw materials, simple preparation, less consumption, obvious shortening of the settling time of the concentration of wet-method phosphoric acid, effective reduction of the fluorine content, reduction of the contents of cations comprising Al<3+>, Fe<3+>, Ca<2+>, Mg<2+>, Si<4+> and the like, and realization of the clear texture and low impurity content of the produced concentrated wet-method phosphoric acid, and provides a high-quality raw material for subsequent production.

Description

Sinking agent in a kind of phosphoric acid by wet process concentration process
Technical field
The present invention relates to a kind of sedimentation removal of impurities production technical field of concentrated wet-process phosphoric acid, be specifically related to the good sinking agent in a kind of phosphoric acid by wet process concentration process.
Background technology
After the phosphoric acid by wet process that makes by the sulfuric acid to leach phosphorus ore concentrates at present, make finished product through natural subsidence in subsider.Because the phosphoric acid by wet process viscosity after concentrating is bigger, shearing stress suffered in the natural subsidence process is bigger, has increased the frictional force of fluid inside, has hindered the subsidence rate of phosphoric acid, has reduced production efficiency, has improved production cost.
The use of phosphoric acid by wet process sinking agent can obviously be shortened the settling time and improve settling efficiency, reduces storage tank quantity, conserve space, reduce production costs, simplified the production management program, the phosphoric acid by wet process turbidity that makes is descended, become limpid, wherein part metals foreign ion Fe 3+, Al 3+, Ca 2+, Mg 2+, Si 4+Deng can catch by the net of sinking agent, build bridge, roll up sweep, effect such as charge neutrality removes along with reunion, the sedimentation of flco is able to part, the quality that has improved phosphoric acid by wet process has reduced the loaded down with trivial details property of subsequent handling and the use of medicament, also reduced the refining difficulty of phosphoric acid, reduced the discharging of tailings, be conducive to improve subsequent product quality, reduce production costs.
The flocculation agent kind of development research both at home and abroad roughly can be divided three classes at present: inorganic flocculating agent, organic polymer coargulator and biological flocculant.Wherein inorganic flocculating agent is generally inorganic salt and the inorganic polymer salt of Fe and Al; Organic polymer coargulator comprises two kinds of natural organic high-molecular flocculant and synthetic organic polymer coargulators; Biological flocculant generally is to utilize biotechnology to extract from the meta-bolites of microorganism and secretory product, because the costliness of the immature and cost of technology does not have large-scale promotion application at present.
At the foreign ion in the phosphoric acid by wet process with positively charged ion such as Al 3+, Fe 3+, Ca 2+, Mg 2+, Si 4+Etc. in the majority, avoid secondary pollution and bring new foreign ion into, should select the flocculation agent of anionic or non-ionic type for use.Therefore, inorganic flocculating agent such as bodied ferric sulfate (PFS) and polymerize aluminum chloride (PAC) are not done naturally and are considered, and biological flocculant is owing to hysteresis and the more high factor of Financial cost of technological development also will not adopt then.
The present situation of phosphorous chemical industry production at present, the phosphorus ore grade is not high relatively, and the concentration of the concentrated wet-process phosphoric acid of producing is 46 ~ 48%P 2O 5About, viscosity is bigger, the content of solid content and foreign ion is higher, longer by the time that natural subsidence needs, need the quantity of storage tank more, the space that occupies is bigger, production efficiency is low, the concentrated wet-process phosphoric acid that production obtains of low quality increased the difficulty that subsequent technique is handled, and influenced the quality of derived product.
Summary of the invention
Concrete grammar of the present invention is as follows:
Good sinking agent in a kind of phosphoric acid by wet process concentration process is by anionic flocculant, flocculant in non-ion type, sorbent material and form except fluorine reagent four parts, with anionic flocculant, flocculant in non-ion type, sorbent material and except fluorine reagent be 40 ~ 93 parts with mass fraction respectively, 1 ~ 30 part, 1 ~ 40 part, send in the oar formula steel basin for 0 ~ 20 part, steel basin is by the chuck heat tracing, temperature control is between 60 ~ 80 ℃, stirring rake stirs 5 ~ 15min fast with the stir speed (S.S.) of 200 ~ 500r/min, stir speed (S.S.) with 50 ~ 80r/min stirs 10 ~ 30min at a slow speed again, stirring finishes solution left standstill 10 ~ 40min, makes this sinking agent.
Above-mentioned anionic flocculant is one or more in sodium laurylsulfonate, sodium polyacrylate, polyacrylic acid, alkyl benzene sulphonate (ABS), the sodium alkyl benzene sulfonate.
Above-mentioned flocculant in non-ion type is one or more in non-ionic polyacrylamide, polyoxyethylene, polyvinyl alcohol, the Natvosol.
Above-mentioned sorbent material is one or more in diatomite, wilkinite, gac, the molecular sieve.
Above-mentioned except fluorine reagent be in sodium-chlor, sodium hydroxide, calcium oxide, calcium hydroxide, yellow soda ash, potassium hydroxide, the salt of wormwood one or more.
Advantage of the present invention: the employed raw material of good sinking agent is more cheap relatively, and raw material is buied easily, prepares easyly, and consumption is few, can obviously shorten the settling time of concentrated wet-process phosphoric acid, reduces fluorine content effectively, reduces Al simultaneously 3+, Fe 3+, Ca 2+, Mg 2+, Si 4+Etc. cationic content, make the concentrated wet-process phosphoric acid quality produce limpid bright, foreign matter content is low to provide high-quality raw materials for follow-up production.
Embodiment
Embodiment 1:
Sinking agent is 40 parts with mass fraction respectively by sodium laurylsulfonate, polyacrylamide, diatomite and yellow soda ash, and 16 parts, 25 parts, 12 parts mix formulated in steel basin.With 0.23kg/t (P 2O 5Meter) amount of concentrated wet-process phosphoric acid adds, and sedimentation is after 14 hours, and the clearance of fluorine reaches 87%, Fe 3+Clearance reaches 17%, Al 3+Clearance reach 15%, Mg 2+Clearance reach 22%, Ca 2+Clearance reach 10%, Si 4+Clearance reach 19%, the phosphoric acid by wet process that obtains is limpid bright.
Embodiment 2:
Sinking agent is 85 parts with mass fraction respectively by sodium polyacrylate, polyvinyl alcohol, wilkinite and sodium hydroxide, and 20 parts, 35 parts, 16 parts mix formulated in steel basin.With 0.27kg/t (P 2O 5Meter) amount of concentrated wet-process phosphoric acid adds, and sedimentation is after 12 hours, and the clearance of fluorine reaches 92%, Fe 3+Clearance reaches 18%, Al 3+Clearance reach 21%, Mg 2+Clearance reach 24%, Ca 2+Clearance reach 27%, Si 4+Clearance reach 16%, the phosphoric acid by wet process that obtains is limpid bright.
Embodiment 3:
Sinking agent is 92 parts with mass fraction respectively by alkyl benzene sulphonate (ABS), polyoxyethylene, gac and sodium-chlor, and 28 parts, 35 parts, 18 parts mix formulated in steel basin.With 0.29kg/t (P 2O 5Meter) amount of concentrated wet-process phosphoric acid adds, and sedimentation is after 10 hours, and the clearance of fluorine reaches 88%, Fe 3+Clearance reaches 13%, Al 3+Clearance reach 16%, Mg 2+Clearance reach 21%, Ca 2+Clearance reach 18%, Si 4+Clearance reach 23%, the phosphoric acid by wet process that obtains is limpid bright.
Embodiment 4:
Sinking agent is 67 parts with mass fraction respectively by sodium alkyl benzene sulfonate, Natvosol, molecular sieve and calcium hydroxide, and 23 parts, 19 parts, 12 parts mix formulated in steel basin.With 0.36kg/t (P 2O 5Meter) amount of concentrated wet-process phosphoric acid adds, and sedimentation is after 14 hours, and the clearance of fluorine reaches 85%, Fe 3+Clearance reaches 11%, Al 3+Clearance reach 9%, Mg 2+Clearance reach 15%, Ca 2+Clearance reach 19%, Si 4+Clearance reach 20%, the phosphoric acid by wet process that obtains is limpid bright.
Embodiment 5:
Sinking agent is 52 parts with mass fraction respectively by polyacrylic acid, polyvinyl alcohol, wilkinite, and 5 parts, 5 parts mix formulated in steel basin.With 0.30kg/t (P 2O 5Meter) amount of concentrated wet-process phosphoric acid adds, and sedimentation is after 14 hours, and the clearance of fluorine reaches 55%, Fe 3+Clearance reaches 6.4%, Al 3+Clearance reach 3.4%, Mg 2+Clearance reach 4.5%, Ca 2+Clearance reach 10%, Si 4+Clearance reach 4.8%, the phosphoric acid by wet process that obtains is limpider bright.
Embodiment 6:
Sinking agent is 89 parts with mass fraction respectively by polyacrylic acid, polyvinyl alcohol, wilkinite: 15 parts: 18 parts mix formulated in steel basin.With 0.30kg/t (P 2O 5Meter) amount of concentrated wet-process phosphoric acid adds, and sedimentation is after 14 hours, and the clearance of fluorine reaches 68%, Fe 3+Clearance reaches 8.4%, Al 3+Clearance reach 6%, Mg 2+Clearance reach 12.2%, Ca 2+Clearance reach 13.5%, Si 4+Clearance reach 10.6%, the phosphoric acid by wet process that obtains is limpider bright.
Embodiment 7:
Sinking agent is 90 parts with mass fraction respectively by polyacrylic acid, polyvinyl alcohol, wilkinite: 28 parts: 38 parts mix formulated in steel basin.With 0.30kg/t (P 2O 5Meter) amount of concentrated wet-process phosphoric acid adds, and sedimentation is after 14 hours, and the clearance of fluorine reaches 77%, Fe 3+Clearance reaches 9.5%, Al 3+Clearance reach 7.5%, Mg 2+Clearance reach 13.8%, Ca 2+Clearance reach 15%, Si 4+Clearance reach 11%, the phosphoric acid by wet process that obtains is limpider bright.

Claims (5)

1. the sinking agent in the phosphoric acid by wet process concentration process, it is characterized in that: the preparation method is, with anionic flocculant, flocculant in non-ion type, sorbent material and except fluorine reagent be respectively 40-93 part with the mass fraction, 1-30 part, 1-40 part, 0-20 part is sent into oar formula steel basin, steel basin is by the chuck heat tracing, temperature control is at 60-80 ℃, stirring rake stirs 5-15min fast with the stir speed (S.S.) of 200-500r/min, stir speed (S.S.) with 50-80r/min stirs 10-30min at a slow speed again, stirs to finish solution left standstill 10-40min, makes sinking agent.
2. the sinking agent in the phosphoric acid by wet process concentration process according to claim 1, it is characterized in that: anionic flocculant is one or more in sodium laurylsulfonate, sodium polyacrylate, polyacrylic acid, alkyl benzene sulphonate (ABS), the sodium alkyl benzene sulfonate.
3. the sinking agent in the phosphoric acid by wet process concentration process according to claim 1, it is characterized in that: flocculant in non-ion type is one or more in non-ionic polyacrylamide, polyoxyethylene, polyvinyl alcohol, the Natvosol.
4. the sinking agent in the phosphoric acid by wet process concentration process according to claim 1, it is characterized in that: above-mentioned sorbent material is one or more in diatomite, wilkinite, gac, the molecular sieve.
5. the sinking agent in the phosphoric acid by wet process concentration process according to claim 1 is characterized in that: above-mentioned except fluorine reagent be in sodium-chlor, sodium hydroxide, yellow soda ash, calcium oxide, calcium hydroxide, potassium hydroxide, the salt of wormwood one or more.
CN201310288311.8A 2013-07-10 2013-07-10 Sinking agent in a kind of wet-process phosphoric acid concentration treating processes Active CN103332666B (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104310328A (en) * 2014-10-09 2015-01-28 瓮福(集团)有限责任公司 Method for primary purification of phosphoric acid by using wet process
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
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
CN106744760A (en) * 2016-05-03 2017-05-31 湖北大峪口化工有限责任公司 The sedimentation agent and method of solids in rapid subsidence phosphoric acid by wet process
CN107043094A (en) * 2017-04-18 2017-08-15 云南佳贝节能科技有限公司 A kind of system of processing of concentrated phosphoric acid
CN109437135A (en) * 2018-11-09 2019-03-08 湖北富邦科技股份有限公司 A kind of method of phosphoric acid by wet process decoloration
CN109987594A (en) * 2019-04-01 2019-07-09 太仓沪试试剂有限公司 A kind of preparation method of potassium dihydrogen phosphate
CN113413643A (en) * 2021-07-26 2021-09-21 中建西部建设建材科学研究院有限公司 Efficient settling method for waste slurry of concrete mixing plant
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

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1757988A (en) * 2004-10-08 2006-04-12 潘戈 Converging pipe connecting structure of heat pipe type solar energy collector
CN102219198A (en) * 2011-05-03 2011-10-19 湖北富邦科技股份有限公司 Multifunctional sinking agent used in production of phosphoric acid by wet method
CN102267691A (en) * 2011-07-05 2011-12-07 侯炎学 Settling agent for wet phosphoric acid refining desulfuration and using method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1757988A (en) * 2004-10-08 2006-04-12 潘戈 Converging pipe connecting structure of heat pipe type solar energy collector
CN102219198A (en) * 2011-05-03 2011-10-19 湖北富邦科技股份有限公司 Multifunctional sinking agent used in production of phosphoric acid by wet method
CN102267691A (en) * 2011-07-05 2011-12-07 侯炎学 Settling agent for wet phosphoric acid refining desulfuration and using method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104310328A (en) * 2014-10-09 2015-01-28 瓮福(集团)有限责任公司 Method for primary purification of phosphoric acid by using wet process
CN106744760A (en) * 2016-05-03 2017-05-31 湖北大峪口化工有限责任公司 The sedimentation agent and method of solids in rapid subsidence phosphoric acid by wet process
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
CN107043094A (en) * 2017-04-18 2017-08-15 云南佳贝节能科技有限公司 A kind of system of processing of concentrated phosphoric acid
CN109437135A (en) * 2018-11-09 2019-03-08 湖北富邦科技股份有限公司 A kind of method of phosphoric acid by wet process decoloration
CN109987594A (en) * 2019-04-01 2019-07-09 太仓沪试试剂有限公司 A kind of preparation method of potassium dihydrogen phosphate
CN113413643A (en) * 2021-07-26 2021-09-21 中建西部建设建材科学研究院有限公司 Efficient settling method for waste slurry of concrete mixing plant
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

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