CN102515125B - Arsenic-removing filtering method for high-concentration polyphosphoric acid - Google Patents
Arsenic-removing filtering method for high-concentration polyphosphoric acid Download PDFInfo
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Abstract
The invention provides an arsenic-removing filtering method for high-concentration polyphosphoric acid, which includes: using industrial polyphosphoric acid as the raw material, adding water-soluble phosphorus pentasulfide emulsion used as arsenic-removing agent to enable arsenic contained in the polyphosphoric acid to form sulfide precipitate under the acidic condition, and purifying and refining the polyphosphoric acid by means of filtering, aerating and the like to produce low-arsenic polyphosphoric acid. By the low-arsenic polyphosphoric acid production method that filter cakes are formed on filter media from the dilute polyphosphoric acid containing arsenic residue first, and then the polyphosphoric acid with added arsenic-removing agent is filtered, the technical problem of filtering in the low-arsenic polyphosphoric acid preparation process is solved, and low-arsenic polyphosphoric acid production can be industrialized. Further, the arsenic-removing filtering method for high-concentration polyphosphoric acid is low in operating cost and simple in operating process, and low-arsenic polyphosphoric acid products, which cannot be obtained by conventional methods and are 105%-118% in concentration, namely percentage composition of P2O5 ranges from 76.1% to 85.5%, and arsenic content is no more than 10ppm, can be obtained by the arsenic-removing filtering method.
Description
Technical field
The present invention relates to polyphosphoric acid dearsenification and filter the method for producing low arsenic polyphosphoric acid, the method can effectively reduce arsenic content and the heavy metal content in polyphosphoric acid, and obtaining thus comparatively pure low arsenic polyphosphoric acid, it is expected to be used widely in weaving, food, medicine and other fields.
Background technology
Produce the method for polyphosphoric acid, industrial conventional have two kinds, and it is similar that a kind of method and thermal phosphoric acid are produced, and produce Vanadium Pentoxide in FLAKES by burning yellow phosphorus, and use water cycle absorption, until product acid concentration reaches 100%, i.e. P
2o
5percentage composition is more than 72.45%, and direct production goes out the polyphosphoric acid product that the polymerization degree is higher, another kind of method be by use finished product phosphoric acid (concentration is lower than 100%) with finished product Vanadium Pentoxide in FLAKES Hybrid Heating polycondensation production concentration higher than 100% polyphosphoric acid product.Owing to containing arsenic in Rock Phosphate (72Min BPL), therefore, the polyphosphoric acid that above-mentioned two kinds of methods are produced all may be brought the impurity such as arsenic into by phosphoric acid or Vanadium Pentoxide in FLAKES, is generally 50-150ppm.Due to reasons such as arsenic are harmful, the arsenic containing in polyphosphoric acid, is unfavorable at food, medicine, and electronic materials etc. need the application in highly purified field.And owing to having given great attention to environmental problem, need to have the polyphosphoric acid of low arsenic content as industrialization passivation or cleaning articles for use recent years, for metal finishing, dyestuff processing etc.Therefore, polyphosphoric acid market and the application prospect of low arsenic content are better, need a kind of arsenic removing method that can carry out with low cost effective running in phosphoric acid industry.
Using sulfide dearsenification is one of method conventional in phosphoric acid industry, but the method is only 85% for concentration at present, i.e. P
2o
5the phosphoric acid of percentage composition 61.6% left and right or concentration, lower than 100%, are also P
2o
5the phosphoric acid of percentage composition 72.45% is not used in the polyphosphoric acid of high density 105%-118%, and its major cause is that polyphosphoric acid viscosity is excessive, poor fluidity, and arsenic slag and polyphosphoric acid mix, and cannot adopt conventional dearsenicating method that arsenic is separated.Therefore,, owing to there is above-mentioned technical barrier, add at present the method for sulfide dearsenification also not for low arsenic polyphosphoric acid industrial production.
At present, oneself knows that the method for dearsenification comprises from polyphosphoric acid:
(1) sulfide dearsenification method;
(2) halogenide dearsenification method;
(3) solvent extration;
(4) ion exchange method;
(5) Vanadium Pentoxide in FLAKES preparation method.
Wherein, solvent extration and ion exchange method due to equipment and processing cost too high, do not possess the feasibility of large-scale commercial production.
Sulfide dearsenification method, is used in the production of concentration lower than 100% phosphoric acid, at polyphosphoric acid, particularly in the production of high density polyphosphoric acid, because dearsenification polyphosphoric acid after treatment is difficult to filtering, be difficult to obtain qualified product, the method is not also applied in industrial production.The Hu gold of Haian County of Jiangsu Province discloses a kind of technology for removing arsenic in polyphosphoric acid, number of patent application: 200810157176.2, the method is carried out dearsenification processing as dearsenic agent to polyphosphoric acid with sulfide, the polyphosphoric acid after to dearsenification filters as flocculating aids to use gac, and uses degassing tower to remove excess hydrogen sulfide.The concentration range of the polyphosphoric acid that the undeclared the method for this patent can be processed, does not illustrate polyphosphoric acid arsenic content after treatment yet and can be reduced to what level, and not mentioned any production exercise control process parameter, and industrial production is not had to practical significance.The method is for the filtration process link of difficulty maximum in polyphosphoric acid dearsenification process, there is no concrete technical specification and technical requirements, not proposing concrete Technology requirement to how using degassing tower to remove hydrogen sulfide, not possessing actual directive significance to producing yet.In addition, the method is used tower to remove hydrogen sulfide, compares with the method for aeration, and higher for equipment and process manipulation request, production cost is higher, is unfavorable for using in actual production.
Halogenide dearsenification method, the method that uses hydrogen halide to deviate from arsenic in polyphosphoric acid has been invented by Toyo Boseki K.K of Japan, patent publication No.: CN1332698A, CN1817790A, the method by passing into hydrogen halide or adding the muriate that can form iron, copper or the tin of hydrogen halide under acidic conditions to deviate from the arsenic in polyphosphoric acid in polyphosphoric acid.Arsenic is converted into the gaseous substance that volatilization point is not high by this method, can realize separating of arsenide and polyphosphoric acid by the mode of heating evaporation, thereby produce low arsenic polyphosphoric acid.The shortcoming of this method is that the produced vent gas treatment difficulty containing gaseous state arsenide is large, processing cost is high, easily cause work safety accident and environmental accident, particularly larger to human injury, simultaneously, the method is easily introduced haloid element impurity in polyphosphoric acid product, as chlorion etc., this has considerable influence to polyphosphoric acid quality product, under chlorion effect, the corrodibility of polyphosphoric acid also can strengthen greatly, thereby causes this technique in industrialization process, equipment material requirement raising, production cost to be improved.This technology is not also applied at present in industrialization is produced.
Vanadium Pentoxide in FLAKES preparation method refers to use phosphoric acid for food and low arsenic Vanadium Pentoxide in FLAKES product, and under certain temperature, stirring velocity condition, polycondensation is the method for synthetic low arsenic polyphosphoric acid product directly.The method is the main method of the low arsenic polyphosphoric acid of current domestic production product, its advantage is that production technique is simple, production handiness is good, but the defect of this technique is also very outstanding: first, the low arsenic polyphosphoric acid concentration that the method can be produced is subject to the restriction of Vanadium Pentoxide in FLAKES arsenic content, under present condition, the highest polyphosphoric acid that only can production concentration 105%, its arsenic content is lower than 10PPm; Secondly, the polyphosphoric acid that the method is produced, the polyphosphoric acid of polymerization degree method of specific heat explained hereafter is low; The 3rd, the low arsenic phosphorus pentoxide raw material of this process using is purchased difficulty on market, still there is no the full scale plant of the low arsenic Vanadium Pentoxide in FLAKES of scale operation at present, and production cost is higher, the restriction that production is subject to is a lot, does not possess economy and the practicality of the low arsenic polyphosphoric acid of the suitability for industrialized production of realizing.
Summary of the invention
Object of the present invention is intended to overcome the defect of prior art, provides a kind of by polyphosphoric acid is carried out to dearsenification filtration, the dearsenification filter method of a kind of high density polyphosphoric acid that the high arsenic content of production concentration is low.
The dearsenification filter method of a kind of high density polyphosphoric acid of the present invention, use industrial polyphosphoric acid for raw material, add wherein water-soluble thiophosphoric anhydride emulsion as dearsenic agent, make arsenic contained in polyphosphoric acid form sulfide under acidic conditions, and by means such as filtration, aerations, polyphosphoric acid is carried out to purifying, produce thus the method for low arsenic polyphosphoric acid.
The invention provides a kind of method of producing low arsenic polyphosphoric acid, adopting industrial polyphosphoric acid is that raw material is produced, and its method is as follows:
A use the warm water of 28-45 DEG C and thiophosphoric anhydride be configured to concentration be the emulsion of mass percent 0.2%-4% as dearsenic agent, by dearsenic agent join 100-140 DEG C of temperature, concentration is 105%-118%, i.e. P
2o
5in the polyphosphoric acid of percentage composition 76.1%-85.5%, under agitation react 20-40 minutes reaction times;
After b reaction finishes, first total amount 4-15% polyphosphoric acid product is diluted with water to concentration 95%-105%, i.e. P
2o
5percentage composition is between 68.8%-76.1%, the filtration particle diameter of selecting tolerate P-levels acid corrosion is that the high-temperature resistance plastice of 0.5-1 μ m or glass fiber material are as filtration medium, use this part diluted acid on filtration medium, to carry out circulating filtration, till forming the uniform filter cake of a layer thickness 0.5-2mm on medium to be filtered;
C sends into the reaction mass of other not diluted to filter with pressure filter or suction filtration machine that the method for step b has formed filter cake, and after filtering, filtrate is 105%-118%, its P
2o
5the low arsenic polyphosphoric acid of percentage composition 76.1%-85.5%, the low arsenic polyphosphoric acid after filtering, through Air Exposure, makes polyphosphoric acid colourity (once black) <40, when concentration is lower than 115%, i.e. P
2o
5percentage composition is lower than 83.3% polyphosphoric acid colourity (once black) <20), arsenic content is less than 10PPm.
In step a, use thiophosphoric anhydride and water to be configured to emulsion as dearsenic agent, with respect to the arsenic content in raw material polyphosphoric acid, the add-on of thiophosphoric anhydride is with P
2s
5: As meter, between its mol ratio 0.7:1-2:1.
In step b and c, described high-temperature resistance plastice is the one in polytetrafluoroethylene PTFE, polyvinylidene difluoride (PVDF) PVDF, organic system nylon 66, nylon 6.
In step c, after finishing, filtration removes hydrogen sulfide residual in polyphosphoric acid by aeration, aeration time 20-60min.The hydrogen sulfide tail gas that aeration produces uses high alkali liquid and water to absorb and processes.
In step a to c, the concentration of described polyphosphoric acid is 105%-118%.
The present invention proposes a kind of dearsenification filter method of polyphosphoric acid, the method that uses the present invention to propose can production concentration reach 105%-118%, and arsenic content is lower than the polyphosphoric acid of 10ppm.
The invention provides a kind of dearsenification filter method of brand-new polyphosphoric acid, different with the method for directly adding thiophosphoric anhydride from traditional interpolation sodium sulphite, the emulsion that the warm water that present method use is 28-45 DEG C and thiophosphoric anhydride are configured to concentration 2-5% is as dearsenic agent, can in polyphosphoric acid product, not introduce sodium ion impurity, simultaneously, be separated into more tiny particle by the water-soluble thiophosphoric anhydride that makes, make it in full-bodied polyphosphoric acid, can better disperse, more effectively contact with polyphosphoric acid, thereby improve reaction dearsenification efficiency, make reaction more abundant.
Present method is selected, filtration temperature, filter type is control effectively by the material to filtration medium and filtration particle diameter, and first part polyphosphoric acid product is diluted with water to concentration 95%-105%, its P
2o
5percentage composition is between 68.8%-76.1%, make it first on filtration medium, carry out circulating filtration, on medium to be filtered, form after the uniform filter cake of a layer thickness 0.5-2mm, again polyphosphoric acid product is filtered, solve arsenic slag in high density polyphosphoric acid, it is the problem that reacted sulfide is difficult to filtering, the product concentration of producing is more than or equal to 115% polyphosphoric acid colourity (once black) can reach <40, and product concentration is less than 115% polyphosphoric acid colourity (once black) and can reaches even the quality index of <20.
Present method adopts the mode of pressurized air aeration, has effectively removed the excess hydrogen sulfide gas that remains in polyphosphoric acid inside in dearsenification process, produces colory low arsenic polyphosphoric acid product.
The polyphosphoric acid dearsenification filter method that this patent provides, solve a filtering technique difficult problem of preparing in low arsenic polyphosphoric acid technique, make to produce low arsenic polyphosphoric acid and be achieved industrialization, and operating cost is low, operating procedure is simple, the low arsenic polyphosphoric acid of high density that reaches 105%-118% by the not getable concentration of ordinary method can be provided, this polyphosphoric acid has the arsenic content that is no more than 10ppm, the chromaticity index of <40 or <20 and the heavy metal of low levels and other impurity.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but be not limited to embodiment.
Embodiment 1
Working concentration is 115.87%, its P
2o
5percentage composition 83.95%, colourity <40, arsenic content 60ppm, iron level 6ppm, lead content 9ppm, the polyphosphoric acid of cl content 1ppm is as raw material, and the thiophosphoric anhydride emulsion 95ml that interpolation concentration is 0.2% reacts 30 minutes under the stirring velocitys of 250 revs/min and 100 DEG C of temperature of reaction conditions.By 5% product polyphosphoric acid, thin up arrives to concentration 95%, using these diluted acids is that 0.5 micron, material carry out circulating filtration pre-treatment on for the filter cloth of organic system nylon 6 filtering particle diameter, after forming the filter cake of 0.5mm on filter cloth, adopt the mode of suction filtration to carry out filtering containing arsenic slag polyphosphoric acid reacted, filter 110 DEG C of initial temperatures, after polyphosphoric acid filtering, use the dried pressurized air of cooling driers it to be carried out to Air Exposure, aeration time 20 minutes.After aeration finishes, make low arsenic polyphosphoric acid product, detect by analysis, the concentration of product polyphosphoric acid is 105.0%, i.e. P
2o
5percentage composition 76.1%, colourity <20, arsenic content <1ppm, iron level 6ppm, lead content <3ppm, cl content <1ppm.
Embodiment 2
Working concentration is 116.11%, its P
2o
5percentage composition 84.12%, colourity <20, arsenic content 73ppm, iron level 3ppm, lead content 5ppm, the polyphosphoric acid of cl content 2ppm is as raw material, and the thiophosphoric anhydride emulsion 95ml that interpolation concentration is 0.2% reacts 30 minutes under the stirring velocitys of 250 revs/min and 110 DEG C of temperature of reaction conditions.By 10% product polyphosphoric acid, thin up arrives to concentration 100%, using these diluted acids is to carry out circulating filtration pre-treatment on 0.5 micron, the material filter cloth that is PTFE filtering particle diameter, after forming the filter cake of 1mm on filter cloth, adopt the mode of press filtration to carry out filtering containing arsenic slag polyphosphoric acid reacted, filter 120 DEG C of initial temperatures, after polyphosphoric acid filtering, use the dried pressurized air of cooling driers it to be carried out to Air Exposure, aeration time 30 minutes.After aeration finishes, make low arsenic polyphosphoric acid product, detect by analysis, the concentration of product polyphosphoric acid is 106.0%, its P
2o
5percentage composition 76.8%, colourity <20, arsenic content <1ppm, iron level 3ppm, lead content <3ppm, cl content <1ppm.
Embodiment 3
Working concentration is 115.87%, its P
2o
5percentage composition 83.95%, colourity <40, arsenic content 60ppm, iron level 6ppm, lead content 9ppm, the polyphosphoric acid of cl content 1ppm is as raw material, and the thiophosphoric anhydride emulsion 45ml that interpolation concentration is 0.44% reacts 20 minutes under the stirring velocitys of 250 revs/min and 120 DEG C of temperature of reaction conditions.By 5% product polyphosphoric acid, thin up arrives to concentration 95%, be to carry out circulating filtration pre-treatment on 0.5 micron, the material filter cloth that is PVDF filtering particle diameter, after forming the filter cake of 0.5mm on filter cloth, adopt the mode of press filtration to carry out filtering containing arsenic slag polyphosphoric acid reacted, filter 130 DEG C of initial temperatures, after polyphosphoric acid filtering, use the dried pressurized air of cooling driers it to be carried out to Air Exposure, aeration time 1 hour.After aeration finishes, make low arsenic polyphosphoric acid product, detect by analysis, the concentration of product polyphosphoric acid is 109.2%, its P
2o
5percentage composition is 79.1%, colourity <20, arsenic content <2ppm, iron level 5ppm, lead content 1ppm, cl content <1ppm.
Embodiment 4
Working concentration is 116.11%, its P
2o
5percentage composition is 84.12%, colourity <20, arsenic content 73ppm, iron level 3ppm, lead content 5ppm, the polyphosphoric acid of cl content 2ppm is as raw material, and the thiophosphoric anhydride emulsion 45ml that interpolation concentration is 0.44% reacts 30 minutes under the stirring velocitys of 250 revs/min and 120 DEG C of temperature of reaction conditions.By 4% product polyphosphoric acid, thin up arrives to concentration 105%, be to carry out circulating filtration pre-treatment on 0.5 micron, the material filter cloth that is PTFE filtering particle diameter, after forming the filter cake of 0.5mm on filter cloth, adopt the mode of suction filtration to carry out filtering containing arsenic slag polyphosphoric acid reacted, filter 130 DEG C of initial temperatures, after polyphosphoric acid filtering, use the dried pressurized air of cooling driers it to be carried out to Air Exposure, aeration time 1 hour.After aeration finishes, make low arsenic polyphosphoric acid product, detect by analysis, the concentration of product polyphosphoric acid is 110.4%, its P
2o
5percentage composition is 80%, colourity <20, arsenic content <1ppm, iron level 63ppm, lead content 1ppm, cl content <1ppm.
Embodiment 5
Working concentration is 117.8%, its P
2o
5percentage composition is 85.3%, colourity <40, arsenic content 60ppm, iron level 6ppm, lead content 9ppm, the polyphosphoric acid of cl content 1ppm is as raw material, and the thiophosphoric anhydride emulsion 20ml that interpolation concentration is 1% reacts 30 minutes under the stirring velocitys of 250 revs/min and 140 DEG C of temperature of reaction conditions.By 12% product polyphosphoric acid, thin up arrives to concentration 95%, be that 0.5 micron, material are to carry out circulating filtration pre-treatment on the filter cloth of organic system nylon 66 filtering particle diameter, after forming the filter cake of 1.5mm on filter cloth, adopt the mode of press filtration to carry out filtering containing arsenic slag polyphosphoric acid reacted, filter 140 DEG C of initial temperatures, after polyphosphoric acid filtering, use the dried pressurized air of cooling driers it to be carried out to Air Exposure, aeration time 1 hour.After aeration finishes, make low arsenic polyphosphoric acid product, detect by analysis, the concentration of product polyphosphoric acid is 116.0%, its P
2o
5percentage composition is 84%, colourity <40, arsenic content 8ppm, iron level 6ppm, lead content 1ppm, cl content <1ppm.
Embodiment 6
Working concentration is 118%, its P
2o
5percentage composition is 85.5%, colourity <40, arsenic content 60ppm, iron level 6ppm, lead content 9ppm, the polyphosphoric acid of cl content 1ppm is as raw material, and the thiophosphoric anhydride emulsion 10ml that interpolation concentration is 2% reacts 30 minutes under the stirring velocitys of 250 revs/min and 120 DEG C of temperature of reaction conditions.By 15% product polyphosphoric acid, thin up arrives to concentration 100%, be to carry out circulating filtration pre-treatment on 0.5 micron, the material filter cloth that is PVDF filtering particle diameter, after forming the filter cake of 2mm on filter cloth, adopt the mode of suction filtration to carry out filtering containing arsenic slag polyphosphoric acid reacted, filter 130 DEG C of initial temperatures, after polyphosphoric acid filtering, use the dried pressurized air of cooling driers it to be carried out to Air Exposure, aeration time 1 hour.After aeration finishes, make low arsenic polyphosphoric acid product, detect by analysis, the concentration of product polyphosphoric acid is 116.9%, its P
2o
5percentage composition is 84.7%, colourity <40, arsenic content 8ppm, iron level 5ppm, lead content <1ppm, cl content 1ppm.
Embodiment 7
Working concentration is 116.11%, is also P
2o
5percentage composition is 84.12%, colourity <20, arsenic content 73ppm, iron level 3ppm, lead content 5ppm, the polyphosphoric acid of cl content 2ppm is as raw material, and the thiophosphoric anhydride emulsion 10ml that interpolation concentration is 2% reacts 40 minutes under the stirring velocitys of 250 revs/min and 130 DEG C of temperature of reaction conditions.By 5% product polyphosphoric acid, thin up arrives to concentration 95%, be to carry out circulating filtration pre-treatment on 0.5 micron, the material filter cloth that is PTFE filtering particle diameter, after forming the filter cake of 0.5mm on filter cloth, adopt the mode of press filtration to carry out filtering containing arsenic slag polyphosphoric acid reacted, filter 130 DEG C of initial temperatures, after polyphosphoric acid filtering, use the dried pressurized air of cooling driers it to be carried out to Air Exposure, aeration time 1 hour.After aeration finishes, make low arsenic polyphosphoric acid product, detect by analysis, the concentration of product polyphosphoric acid is 115%, is also P
2o
5percentage composition is 83.3%, colourity <40, arsenic content 10ppm, iron level 4ppm, lead content <1ppm, cl content 1ppm.
Claims (5)
1. a dearsenification filter method for high density polyphosphoric acid, adopting industrial polyphosphoric acid is raw material, it is characterized in that, its method is as follows:
A. using the warm water of 28-45 DEG C and thiophosphoric anhydride to be configured to concentration is that the emulsion of mass percent 0.2%-4% is as dearsenic agent, dearsenic agent is joined in the polyphosphoric acid that 100-140 DEG C of temperature, concentration are 105%-118%, under agitation react 20-40 minutes reaction times;
B. after reaction finishes, first total amount 4-15% polyphosphoric acid product is diluted with water between concentration 95%-105%, the filtration particle diameter of selecting tolerate P-levels acid corrosion is that the high-temperature resistance plastice of 0.5-1 μ m or glass fiber material are as filtration medium, use this part diluted acid on filtration medium, to carry out circulating filtration, till forming a layer thickness on medium to be filtered and be the uniform filter cake of 0.5-2mm;
C. the reaction mass of other not diluted is sent into and filtered with pressure filter or suction filtration machine that the method for step b has formed filter cake, the low arsenic polyphosphoric acid that after filtering, filtrate is 105%-118%, low arsenic polyphosphoric acid after filtering is through Air Exposure, make polyphosphoric acid colourity <40, the unit of colourity is once black, and arsenic content is less than 10ppm.
2. the dearsenification filter method of high density polyphosphoric acid according to claim 1, is characterized in that, after the filtration described in step c filter liquor concentration lower than 115% time, polyphosphoric acid colourity <20, the unit of colourity is once black.
3. the dearsenification filter method of high density polyphosphoric acid according to claim 1, is characterized in that, uses thiophosphoric anhydride and water to be configured to emulsion as dearsenic agent, and with respect to the arsenic content in raw material polyphosphoric acid, the add-on of thiophosphoric anhydride is with P
2s
5: As meter, its mol ratio is between 0.7:1-2:1.
4. the dearsenification filter method of high density polyphosphoric acid according to claim 1, is characterized in that, described high-temperature resistance plastice is the one in polytetrafluoroethylene PTFE, polyvinylidene difluoride (PVDF) PVDF, organic system nylon 66, nylon 6.
5. the dearsenification filter method of high density polyphosphoric acid according to claim 1, is characterized in that, after filtration finishes, removes hydrogen sulfide residual in polyphosphoric acid by aeration, and aeration time is 20-60 minutes.
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