CN103641092B - A kind of purifying phosphoric acid in a wet process and phosphoric anhydride are the method for Material synthesis polyphosphoric acid - Google Patents
A kind of purifying phosphoric acid in a wet process and phosphoric anhydride are the method for Material synthesis polyphosphoric acid Download PDFInfo
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- CN103641092B CN103641092B CN201310708008.9A CN201310708008A CN103641092B CN 103641092 B CN103641092 B CN 103641092B CN 201310708008 A CN201310708008 A CN 201310708008A CN 103641092 B CN103641092 B CN 103641092B
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Abstract
A kind of purifying phosphoric acid in a wet process of the present invention and phosphoric anhydride are the method for Material synthesis polyphosphoric acid, belong to technical field of phosphorous chemical industry.Be characterized in be placed in there-necked flask by Vanadium Pentoxide in FLAKES is disposable, slowly add Wet Phosphoric Acid Market, and constantly stirring makes Vanadium Pentoxide in FLAKES powder dissolve as far as possible, the temperature of setting heat collecting type constant-temperature heating magnetic stirring apparatus and rotating speed are with abundant batch mixing.After batch mixing is even, is warming up to design temperature, adds dispersion agent, after constant temperature polyreaction 2 ~ 6h, obtain the transparent polyphosphoric acid of colourless flowing shape that phosphoric acid quality concentration is 114 ~ 120%.Advantage of the present invention, adopts wet purification acid to be raw material, greatly reduces the production energy consumption of polyphosphoric acid, and operational safety is simple, has and promotes practicality preferably.
Description
Technical field
The present invention relates to a kind of method that purifying phosphoric acid in a wet process and phosphoric anhydride are Material synthesis polyphosphoric acid.Belong to technical field of phosphorous chemical industry.
Background technology
The acid of existing phosphorous chemical industry basic material is mainly industrial phosphoric acid, and its industrial production mainly comprises Re Fa and wet method two kinds of routes.Be that the hot method route in direction has good product quality, the features such as foreign matter content is low, expensive with yellow phosphorus, may be used for the processing of the higher food grade of purity requirement, electron-level phosphoric acid; Be that the wet route in direction has the industrialized feature of low, the easy enforcement of cost with sulfuric acid dissolution, but phosphoric acid foreign matter content prepared by wet route is high, and purification process difficulty is large, by restriction to a certain extent.Along with continually developing in recent years to phosphor resource, the advantage of polyphosphoric acid manifests gradually.Compare industrial phosphoric acid, it has superfusibility matter, and still keep liquid even if store under cryogenic, corrodibility is little; Transport equivalent P
2o
5trucking costs to economize the advantage such as 40% than common phosphoric acid.Polyphosphoric acid just progressively becomes the substitute of industrial phosphoric acid, is widely used in producing agricultural chemical fertilizer and producing in the fields such as feed phosphate.
The industrial process of polyphosphoric acid is equally also divided into Re Fa and wet method.Hot method is mainly based on traditional phosphorous acid production by BEP device, and difference is only the technology mode supplementing cooling; Phosphoric acid by wet process mainly concentrates through single-stage or multi-step evaporator heating by wet method, and removing moisture obtains.Prior art mainly adopts Wet-process Phosphoric Acid Production polyphosphoric acid, and due to reasons such as polyphosphoric acid preparation method maintain secrecy, domestic and international pertinent data report is relatively less, generally uses high temperature method of enrichment.This method in process of production, the slip that Rock Phosphate (72Min BPL) and sulfuric acid reaction produce after filtration, concentrate the concentration improving phosphoric acid.Although the high temperature of concentration process and heat transfer ununiformity, acid can produce local superheating unavoidably in concentration process, makes heating unit inwall occur white precipitate fouling.Meanwhile, the temperature that this method requires reaches 800 ~ 1000 DEG C, vacuum tightness 0.1 ~ 0.3atm, requires higher, be difficult to cleaning, affect the production driving of polyphosphoric acid after device inwall generation fouling the material of device and sealing property.Therefore, how to develop a kind of polyphosphoric acid synthetic route that is efficient, less energy-consumption necessary, in order to increase the extent of polymerization of phosphoric acid, improving the concentration of phosphoric acid, having carried out research of the present invention.
Summary of the invention
The object of the invention is to overcome above-mentioned prior art Problems existing, provide a kind of method that purifying phosphoric acid in a wet process and phosphoric anhydride are Material synthesis polyphosphoric acid, the method is intended to the concentration improving polyphosphoric acid, reduces polyphosphoric acid synthesis cost.
The present invention in a wet process purifying phosphoric acid and phosphoric anhydride to be the technical scheme of the method for Material synthesis polyphosphoric acid be: the method comprises the following steps:
There-necked flask is placed in by disposable for Vanadium Pentoxide in FLAKES, there-necked flask is fixed in oil bath pan, the temperature of oil bath pan setting heat collecting type constant-temperature heating magnetic stirring apparatus is 100 ~ 150 DEG C, rotating speed is 225r/min, in the there-necked flask that Vanadium Pentoxide in FLAKES is housed, Wet Phosphoric Acid Market is added with constant pressure funnel, and carry out mechanical stirring until dropwise, abundant batch mixing, obtain Vanadium Pentoxide in FLAKES and Wet Phosphoric Acid Market mixing solutions, intensification Vanadium Pentoxide in FLAKES and Wet Phosphoric Acid Market mixing solutions, add dispersion agent, after polyreaction 2 ~ 6h, obtain the transparent polyphosphoric acid of colourless flowing shape that phosphoric acid quality concentration is 114 ~ 120%.
Described Vanadium Pentoxide in FLAKES and Wet Phosphoric Acid Market mass ratio are 0.4 ~ 0.8, and wherein the mass concentration of Wet Phosphoric Acid Market is between 74 ~ 79%.
Described dispersion agent is one or more in Yatall MA, tributyl phosphate, tannin and xylogen benzene sulfonic acid sodium salt, and its massfraction accounts for 0.01 ~ 0.03% of raw material total mass.
Beneficial effect of the present invention is: (1) temperature of reaction reduces greatly than traditional technology, saves production energy consumption.(2) reaction pressure is normal pressure, safe and simple to operate.(3) reaction need not produce a large amount of water vapor, can reduce the heat energy that water vapour is taken away, and is convenient to produce simultaneously.(4) reaction process adopts one-step synthesis, shortens the reaction times.
Embodiment
Further illustrate the present invention by embodiment below, but the present invention is in no way limited to these embodiments.
Purifying phosphoric acid and phosphoric anhydride are that the method for Material synthesis polyphosphoric acid comprises the following steps: in a wet process
There-necked flask is placed in by disposable for Vanadium Pentoxide in FLAKES, there-necked flask is fixed in oil bath pan, the temperature of oil bath pan setting heat collecting type constant-temperature heating magnetic stirring apparatus is 100 ~ 150 DEG C, rotating speed is 225r/min, in the there-necked flask that Vanadium Pentoxide in FLAKES is housed, Wet Phosphoric Acid Market is added with constant pressure funnel, and carry out mechanical stirring until dropwise, abundant batch mixing, obtain Vanadium Pentoxide in FLAKES and Wet Phosphoric Acid Market mixing solutions, intensification Vanadium Pentoxide in FLAKES and Wet Phosphoric Acid Market mixing solutions, add dispersion agent, after polyreaction 2 ~ 6h, obtain the transparent polyphosphoric acid of colourless flowing shape that phosphoric acid quality concentration is 114 ~ 120%.
Described Vanadium Pentoxide in FLAKES and Wet Phosphoric Acid Market mass ratio are 0.4 ~ 0.8, and wherein the mass concentration of Wet Phosphoric Acid Market is 74 ~ 79% scopes.
Described dispersion agent is one or more in Yatall MA, tributyl phosphate, tannin and xylogen benzene sulfonic acid sodium salt, and its massfraction accounts for 0.01 ~ 0.03% of raw material total mass.
embodiment 1
To be that 150g Vanadium Pentoxide in FLAKES is disposable be placed in there-necked flask to quality, slowly add the Wet Phosphoric Acid Market that 100g massfraction is 76%, and constantly stirring makes Vanadium Pentoxide in FLAKES powder dissolve as far as possible, then there-necked flask is made to be fixed in oil bath pan, the temperature of setting heat collecting type constant-temperature heating magnetic stirring apparatus is 150 DEG C, rotating speed is 225 rpms, with abundant batch mixing, after being warming up to design temperature, add mass concentration 0.01% viscosity-depression agent Yatall MA, after constant temperature polyreaction 4h, Vanadium Pentoxide in FLAKES powder dissolves completely, obtain the transparent polyphosphoric acid of colourless flowing shape that phosphoric acid mass concentration is 116%.
embodiment 2
To be that 150g Vanadium Pentoxide in FLAKES is disposable be placed in there-necked flask to quality, slowly add the Wet Phosphoric Acid Market that 85g massfraction is 74%, and constantly stirring makes Vanadium Pentoxide in FLAKES powder dissolve as far as possible, then there-necked flask is made to be fixed in oil bath pan, the temperature of setting heat collecting type constant-temperature heating magnetic stirring apparatus is 100 DEG C, rotating speed is 225 rpms, with abundant batch mixing, after being warming up to design temperature, add mass concentration 0.02% viscosity-depression agent tributyl phosphate, after constant temperature polyreaction 5h, Vanadium Pentoxide in FLAKES powder dissolves completely, obtain the transparent polyphosphoric acid of colourless flowing shape that phosphoric acid quality concentration is 116%.
embodiment 3
To be that 150g Vanadium Pentoxide in FLAKES is disposable be placed in there-necked flask to quality, slowly adding 60g massfraction is 78% Wet Phosphoric Acid Market, and constantly stirring makes Vanadium Pentoxide in FLAKES powder dissolve as far as possible, then there-necked flask is made to be fixed in oil bath pan, the temperature of setting heat collecting type constant-temperature heating magnetic stirring apparatus is 140 DEG C, rotating speed is 225 rpms, with abundant batch mixing, after being warming up to design temperature, add mass concentration 0.03% viscosity-depression agent tannin, after constant temperature polyreaction 6h, Vanadium Pentoxide in FLAKES powder dissolves completely, obtain the transparent polyphosphoric acid of colourless flowing shape that phosphoric acid quality concentration is 115%.
embodiment 4
To be that 150g Vanadium Pentoxide in FLAKES is disposable be placed in there-necked flask to quality, slowly add 120g, massfraction is 79% Wet Phosphoric Acid Market, and constantly stirring makes Vanadium Pentoxide in FLAKES powder dissolve as far as possible, then there-necked flask is made to be fixed in oil bath pan, the temperature of setting heat collecting type constant-temperature heating magnetic stirring apparatus is 110 DEG C, rotating speed is 225 rpms, with abundant batch mixing, after being warming up to design temperature, adding mass concentration is 0.02% viscosity-depression agent xylogen benzene sulfonic acid sodium salt, after constant temperature polyreaction 2h, Vanadium Pentoxide in FLAKES powder dissolves completely, obtain the transparent polyphosphoric acid of colourless flowing shape that phosphoric acid quality concentration is 114%.
embodiment 5
To be that 150g Vanadium Pentoxide in FLAKES is disposable be placed in there-necked flask to quality, slowly add 90g, massfraction is 75% Wet Phosphoric Acid Market, and constantly stirring makes Vanadium Pentoxide in FLAKES powder dissolve as far as possible, then there-necked flask is made to be fixed in oil bath pan, the temperature of setting heat collecting type constant-temperature heating magnetic stirring apparatus is 120 DEG C, rotating speed is 225 rpms, with abundant batch mixing, after being warming up to design temperature, add the tannin that viscosity-depression agent mass concentration is 0.01% Yatall MA and 0.01%, after constant temperature polyreaction 2h, Vanadium Pentoxide in FLAKES powder dissolves completely, obtain the transparent polyphosphoric acid of colourless flowing shape that phosphoric acid quality concentration is 116%.
Present invention process is compared than traditional technology, and energy consumption greatly reduces, and safety is easy to operate, specifically in table 1:
Claims (2)
1. purifying phosphoric acid and phosphoric anhydride are a method for Material synthesis polyphosphoric acid in a wet process, it is characterized in that the method comprises the following steps:
There-necked flask is placed in by disposable for Vanadium Pentoxide in FLAKES, there-necked flask is fixed in oil bath pan, the temperature of oil bath pan setting heat collecting type constant-temperature heating magnetic stirring apparatus is 100 ~ 150 DEG C, rotating speed is 225r/min, in the there-necked flask that Vanadium Pentoxide in FLAKES is housed, Wet Phosphoric Acid Market is added with constant pressure funnel, and carry out mechanical stirring until dropwise, abundant batch mixing, obtain Vanadium Pentoxide in FLAKES and Wet Phosphoric Acid Market mixing solutions, intensification Vanadium Pentoxide in FLAKES and Wet Phosphoric Acid Market mixing solutions, add dispersion agent, after polyreaction 2 ~ 6h, obtain the transparent polyphosphoric acid of colourless flowing shape that phosphoric acid quality concentration is 114 ~ 120%,
Described Vanadium Pentoxide in FLAKES and Wet Phosphoric Acid Market mass ratio are 0.4 ~ 0.8, and wherein the mass concentration of Wet Phosphoric Acid Market is between 74 ~ 79%,
Described dispersion agent is one or more in Yatall MA, tributyl phosphate, tannin and xylogen benzene sulfonic acid sodium salt.
2. the purifying phosphoric acid in a wet process according to right 1 and phosphoric anhydride are the method for Material synthesis polyphosphoric acid, it is characterized in that: described dispersion agent massfraction accounts for 0.01 ~ 0.03% of raw material total mass.
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| CN101269805A (en) * | 2008-05-07 | 2008-09-24 | 瓮福（集团）有限责任公司 | Method for producing polyphosphoric acid |
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| 湿法磷酸净化酸制多聚磷酸的工艺研究;刘飞等;《化工矿物与加工》;20101231(第10期);第11-13页 * |
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