CN102070665A - Process for arsenic removal of 1-hydroxy ethylidene-1,1-diphosphonic acid - Google Patents
Process for arsenic removal of 1-hydroxy ethylidene-1,1-diphosphonic acid Download PDFInfo
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- CN102070665A CN102070665A CN2011100060329A CN201110006032A CN102070665A CN 102070665 A CN102070665 A CN 102070665A CN 2011100060329 A CN2011100060329 A CN 2011100060329A CN 201110006032 A CN201110006032 A CN 201110006032A CN 102070665 A CN102070665 A CN 102070665A
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- diphosphonic acid
- hydroxy ethylene
- ethylene diphosphonic
- arsenic removal
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Abstract
The invention discloses a process for the arsenic removal of 1-hydroxy ethylidene-1,1-diphosphonic acid, which ensures low production cost. The process comprises the following operating steps of: adding 400 to 1,000 weight parts of 1-hydroxy ethylidene-1,1-diphosphonic acid free from arsenic removal treatment into a reaction kettle, introducing vapor to adjust the temperature of the material in the kettle to 20 to 70 DEG C by using a reaction kettle clamping sleeve, adding 0.1 to 1 weight part of phosphorus pentasulfide serving as an arsenic removal agent, adding 0.2 to 2 weight parts of activated carbon, washing a charging hole by using 0.5 to 2 weight parts of pure water after the charging is finished, preserving the heat for 1 to 5 hours at the temperature of 20 to 70 DEG C, filtering the 1-hydroxy ethylidene-1,1-diphosphonic acid (HEDP), heating the filtered clean 1-hydroxy ethylidene-1,1-diphosphonic acid to 80 DEG C, performing external evaporation for 1 to 3 hours under negative pressure, and before the external evaporation is finished, performing activity analysis, adding the pure water for dilution according to an activity result, and introducing cooling water to reduce the temperature of the material in the kettle to 40 to 50 DEG C by using the reaction kettle clamping sleeve and performing discharging.
Description
Technical field
The present invention relates to a kind of arsenic removal technology, relate in particular to a kind of arsenic removal technology of hydroxy ethylene diphosphonic acid.
Background technology
Hydroxy ethylene diphosphonic acid has another name called 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, and molecular formula is C2H8O7P2, and its english abbreviation is HEDP.Hydroxy ethylene diphosphonic acid is a kind of organic phosphine acids anti-incrustation corrosion inhibitor, can form stable complex compound with multiple metal ions such as iron, copper, zinc, the oxide compound on dissolution of metals surface, under 250 ℃, still can play good corrosion-mitigation scale-inhibition effect, still very stable under high pH, facile hydrolysis, general light and heat condition are difficult for down decomposing, and resistance to acids and bases, anti-oxychlorination performance are good than other organic phospho acid (salt).Can belong to ion, especially calcium ion formation six-membered ring chelate, thereby tool scale inhibition effect and the tangible molten limit effect of tool preferably with underwater gold, when with the compound use of other water conditioner, have synergistic effect preferably.
HEDP also uses in industries such as medicine, weaving, papermaking except as the water conditioner, is specially adapted to the clean-out system and the household chemicals additive of electron trade.HEDP be widely used in industrial circulating cooling water systems such as electric power, chemical industry, metallurgy, chemical fertilizer and in, the scale inhibition and the inhibition of low pressure boiler, oil-field flooding and pipe laying; In light and textile industries, can be used as metal and nonmetallic clean-out system, can also be as the complexing agent of bleachinging and dyeing industrial peroxide stabiliser and laking agent, cyanideless electro-plating industry, pharmaceutical industries is done the agent of carrying of radioelement.
Used phosphorus trichloride in the raw materials for production of HEDP, it is that initial feed is produced with the phosphorus ore, owing to unavoidably contain arsenic in the Rock Phosphate (72Min BPL), so often there is arsenic to exist among the HEDP, expansion day by day along with the HEDP range of application, a lot of terminal users require to reduce as far as possible the content of heavy metal arsenic in fields such as makeup, articles for washing, so the HEDP market of low arsenic is just increasing, it is very important that the HEDP dearsenicating technology just seems.
In the prior art, there is not technology at Amino Trimethylene Phosphonic Acid dearsenification processing, hydroxy ethylene diphosphonic acid and the reparation technology thereof of a kind of arsenic content≤3ppm only in being 200810230638.9 patent, the patent No. are disclosed, this technology uses the thioacetic acid ammonium as the dearsenification reagent in the hydroxy ethylene diphosphonic acid production process, but the thioacetic acid ammonium costs an arm and a leg, be difficult to buy, domestic production producer seldom, basic by import, and the thioacetic acid ammonium consumption that uses in this method is too big, improve production cost greatly, be unfavorable for the practical application in the suitability for industrialized production.
Summary of the invention
The arsenic removal technology that the purpose of this invention is to provide the low hydroxy ethylene diphosphonic acid of a kind of production cost.
For achieving the above object, the technical solution used in the present invention is:
A kind of arsenic removal technology of hydroxy ethylene diphosphonic acid is characterized in that: comprise following operation steps:
The hydroxy ethylene diphosphonic acid that in reactor, adds 400～1000 weight parts without the dearsenification processing, temperature of charge to 20 in the reacting kettle jacketing feeding steam adjusting still～70 ℃, the arsenic removing agent thiophosphoric anhydride that adds 0.1～1 weight part then, the gac that adds 0.2～2 weight part again, with the pure water rinsing charging opening of 0.5～2 weight part, under 20～70 ℃ of temperature ranges, be incubated 1～5 hour then after reinforced the finishing; Afterwards hydroxy ethylene diphosphonic acid (being HEDP) is filtered, be heated to 80 ℃ with filtering the clean hydroxy ethylene diphosphonic acid in back, steamed 1～3 hour outside under negative pressure, the outer preceding elder generation of end of steaming analyzes active, add the pure water dilution according to active result, the logical water coolant of reacting kettle jacketing is cooled to 40～50 ℃ of blowings with material in the still.
This technology is by adding dearsenic agent thiophosphoric anhydride (P
2S
5) and gac remove arsenic in the hydroxy ethylene diphosphonic acid, the consumption of used dearsenic agent (thiophosphoric anhydride) is few, per 600 weight part HEDP use dearsenic agent thiophosphoric anhydride (P
2S
5) 0.15～0.5 weight part just can reach the dearsenification effect, because the thiophosphoric anhydride low price, therefore whole arsenic removal technology is with low cost, helps this technology large-scale industrialization and uses.
Description of drawings
Fig. 1 is an engineering process synoptic diagram of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is further described:
A kind of arsenic removing method of hydroxy ethylene diphosphonic acid comprises following operation steps:
The hydroxy ethylene diphosphonic acid that in reactor, adds 400～1000 weight parts without the dearsenification processing, temperature of charge to 20 in the reacting kettle jacketing feeding steam adjusting still～70 ℃, the arsenic removing agent thiophosphoric anhydride that adds 0.1～1 weight part then, the gac that adds 0.2～2 weight part again, with the pure water rinsing charging opening of 0.5～2 weight part, under 20～70 ℃ of temperature ranges, be incubated 1～5 hour then after reinforced the finishing; Afterwards hydroxy ethylene diphosphonic acid (being HEDP) is filtered, be heated to 80 ℃ with filtering the clean hydroxy ethylene diphosphonic acid in back, steamed 1～3 hour outside under negative pressure, the outer preceding elder generation of end of steaming analyzes active, add the pure water dilution according to the active result of HEDP, the logical water coolant of reacting kettle jacketing is cooled to 40～50 ℃ of blowings with material in the still.
The content of arsenic element is preferably 20～200ppm in the hydroxy ethylene diphosphonic acid of handling without dearsenification described in the above-mentioned steps, and more preferably 40～150ppm especially is preferably 60～100ppm, most preferably 70～80ppm.
The add-on of the hydroxy ethylene diphosphonic acid of handling without dearsenification described in the above-mentioned steps is preferably 450～900 weight parts, and more preferably 500～800 weight parts most preferably are 550～700 weight parts, the most are preferably 600 weight parts.
The add-on of thiophosphoric anhydride described in the above-mentioned steps is preferably 0.15～0.5 weight part, more preferably 0.2～0.4 weight part.
Temperature range described in the above-mentioned steps is preferably 20～70 ℃, more preferably 22～55 ℃, most preferably is 25 ± 2～50 ± 2 ℃.
The pure water consumption of the charging opening of flushing described in the above-mentioned steps is preferably 0.5～2 weight part, more preferably 1 weight part.
Soaking time described in the above-mentioned steps is preferably 2～4 hours, more preferably 2 hours or 4 hours.
The add-on of gac described in the above-mentioned steps is preferably 0.5～2 ‰ of the hydroxy ethylene diphosphonic acid add-on handled without dearsenification, and more preferably 1 ‰.
The time that to filter the clean hydroxy ethylene diphosphonic acid heating in back described in the above-mentioned steps is preferably 2～4 hours, more preferably 2 hours or 4 hours.
Embodiment recited above is described preferred implementation of the present invention; be not that design of the present invention and scope are limited; under the prerequisite that does not break away from design concept of the present invention; common engineering technical personnel make technical scheme of the present invention in this area various modification and improvement all should fall into protection scope of the present invention.
The present invention is a kind of arsenic removal technology cheaply, can effectively reduce the arsenic content among the HEDP, obtain the HEDP of arsenic content less than 1ppm, solve arsenic content height in the common HEDP product and caused the limited difficult problem of range of application, the HEDP that the gained arsenic content is extremely low can be used for clean-out system, the additive of household chemicals, makeup, the medicine and other fields of electron trade, the Application Areas of having widened product.
The used raw material of the present invention includes: (arsenic content is 70～80ppm) to HEDP, commercial grade else vulcanizes two phosphorus (P2S5), gac and pure water.
Principle of work of the present invention is:
Thiophosphoric anhydride can hydrolysis in water, slowly releases hydrogen sulfide, and hydrogen sulfide can react with trivalent arsenic or pentavalent arsenic, and the red arsenic that obtain can be adsorbed and remove, thereby obtain the extremely low HEDP of arsenic content.
The reaction equation that relates among the present invention has:
P
2S
5+8H
2O→5H
2S+2H
3PO
4
3H
2S+2As(III)→As
2S
3+6H
+
5H
2S+2As(IV)→As
2S
5+10H
+
Process characteristic of the present invention has:
At first, be that the arsenic removal technology described in 200810230638.9 the patent is to carry out under 50～60 ℃ of temperature in the patent No., the temperature range that technology is suitable for is narrow, is unfavorable for diversified operational condition and production environment in the actual production.Technology of the present invention is less demanding to used temperature, and the temperature range that technology is suitable for is wide, can react from 20～70 ℃, especially can finish the dearsenification operation under the room temperature about 20 ℃;
Secondly, the consumption of the used dearsenic agent thiophosphoric anhydride of this technology is few, and per 600 weight part HEDP use dearsenic agent thiophosphoric anhydride (P
2S
5) 0.15～0.5 weight part just can reach the dearsenification effect, because the thiophosphoric anhydride low price, therefore whole arsenic removal technology is with low cost, helps large-scale industrialization and uses; (thiophosphoric anhydride is not all used in existing water treatment field dearsenification, and the present invention uses thiophosphoric anhydride first in water conditioner dearsenification process, have unexpected good result.)
Once more, the speed of response of dearsenification operation is relatively gentleer in this technology, can not produce a large amount of deleterious hypertoxic gas vulcanization hydrogen, and production technique is controlled easily, and harm can be eliminated and be taken precautions against fully in advance to workers'health, is convenient to realize suitability for industrialized production and safety in production;
At last, this technology is little to the pollution of environment, the hydrogen sulfide (H of generation
2S) can be fully utilized unnecessary hydrogen sulfide (H
2S) can absorb with alkali lye, discharging waste gas does not produce environment and pollutes.
Among the present invention, " outer steam " is this area term commonly used, and the meaning is steamed the mode that the impurity of material the inside and moisture mix by heating next.
As shown in Figure 1, the present invention includes following operation steps:
1, early-stage preparations.
2, feed intake: get a certain amount of hydroxy ethylene diphosphonic acid, dearsenic agent, activated carbon in reactor, and start stirring.
3, dearsenification at a certain temperature.
4, insulation is 2～4 hours.
5, intensification is filtered.
6, sampling detects.
7, blowing, packing.
Specific embodiments of the invention have:
Embodiment 1:
Charging capacity HEDP is that 600kg, dearsenic agent thiophosphoric anhydride (P2S5) are 0.2kg, and the gac add-on is 0.6kg, maintains the temperature at 50 ℃, soaking time 2 hours.
In still, add 600kgHEDP, add the back and open stirring, reacting kettle jacketing feeds steam heating makes the interior temperature of charge of still be raised to 50 ± 2 ℃, once add 0.2kg dearsenic agent and 0.6kg gac from special-purpose charging opening, add back 1kg pure water rinsing charging opening, add back insulation 2 hours, holding temperature is 50 ± 2 ℃; Then HEDP is filled in another still with strainer, the HEDP after filtering is heated to 80 ℃, negative pressure is outer steamed 2 hours by drawing, and analyzed activity earlier before outer steaming finishes, and added the pure water dilution according to the HEDP active quantities, was cooled to 50 ℃ of blowings.Chemical examination arsenic content is less than 1mg/L.
Embodiment 2:
Charging capacity HEDP is that 600kg, dearsenic agent thiophosphoric anhydride (P2S5) are that 0.4kg, gac are 0.6kg, maintains the temperature at 25 ℃, 4 hours time.
In still, add 600kgHEDP, add the back and open stirring, reacting kettle jacketing feeds steam heating makes the interior temperature of charge of still be raised to 25 ± 2 ℃, once add 0.4kg dearsenic agent and 0.6kg gac from special-purpose charging opening, add back 1kg pure water rinsing charging opening, add back insulation 4 hours, holding temperature is 25 ± 2 ℃; Then HEDP is filled in another still with strainer, clean HEDP is heated to 80 ℃ with the filtration back, and negative pressure is outer steamed 2 hours by drawing, and analyzed activity earlier before outer steaming finishes, and added the pure water dilution according to the HEDP activity, was cooled to 40 ℃ of blowings.Chemical examination arsenic content is less than 1mg/L.
Embodiment 3:
Charging capacity HEDP is that 600kg, dearsenic agent thiophosphoric anhydride (P2S5) are that 0.6kg, gac are 0.6kg, maintains the temperature at 25 ℃, 2 hours time.
In still, add 600kgHEDP, add the back and open stirring, reacting kettle jacketing feeds steam heating makes the interior temperature of charge of still be raised to 25 ± 2 ℃, once add 0.4kg dearsenic agent and 0.6kg gac from special-purpose charging opening, add back 1kg pure water rinsing charging opening, add back insulation 2 hours, holding temperature is 25 ± 2 ℃; Then HEDP is filled in another still with strainer, clean HEDP is heated to 80 ℃ with the filtration back, and negative pressure is outer steamed 2 hours by drawing, and analyzed activity earlier before outer steaming finishes, and added the pure water dilution according to the HEDP activity, was cooled to 45 ℃ of blowings.Chemical examination arsenic content is less than 1mg/L.
Embodiment 4:
Charging capacity HEDP is that 600kg, dearsenic agent thiophosphoric anhydride (P2S5) are that 0.3kg, gac are 0.6kg, maintains the temperature at 35 ℃, 4 hours time.
In still, add 600kgHEDP, add the back and open stirring, reacting kettle jacketing feeds steam heating makes the interior temperature of charge of still be raised to 35 ± 2 ℃, once add 0.3kg dearsenic agent and 0.6kg gac from special-purpose charging opening, add back 1kg pure water rinsing charging opening, add back insulation 3 hours, holding temperature is 35 ± 2 ℃; Then HEDP is filled in another still with strainer, clean HEDP is heated to 80 ℃ with the filtration back, and negative pressure is outer steamed 2 hours by drawing, and analyzed activity earlier before outer steaming finishes, and added the pure water dilution according to the HEDP activity, was cooled to 45 ℃ of blowings.Chemical examination arsenic content 0.5mg/L.
Embodiment 5:
Charging capacity HEDP is that 600kg, dearsenic agent thiophosphoric anhydride (P2S5) are that 0.3kg, gac are 0.6kg, maintains the temperature at 40 ℃, 3 hours time.
In still, add 600kgHEDP, add the back and open stirring, reacting kettle jacketing feeds steam heating makes the interior temperature of charge of still be raised to 40 ± 2 ℃, once add 0.3kg dearsenic agent and 0.6kg gac from special-purpose charging opening, add back 1kg pure water rinsing charging opening, add back insulation 3 hours, holding temperature is 40 ± 2 ℃; Then HEDP is filled in another still with strainer, clean HEDP is heated to 80 ℃ with the filtration back, and negative pressure is outer steamed 2 hours by drawing, and analyzed activity earlier before outer steaming finishes, and added the pure water dilution according to the HEDP activity, was cooled to 50 ℃ of blowings.Chemical examination arsenic content is less than 0.3～0.6mg/L.
Embodiment 6:
Charging capacity HEDP is that 5000kg, dearsenic agent thiophosphoric anhydride (P2S5) are 2.7kg, and gac is 5.0kg, maintains the temperature at 30 ℃, 3 hours time.
In still, add 5000kgHEDP, add the back and open stirring, reacting kettle jacketing feeds steam heating makes the interior temperature of charge of still be raised to 40 ± 2 ℃, once add 0.3kg dearsenic agent and 0.6kg gac from special-purpose charging opening, add back 1kg pure water rinsing charging opening, add back insulation 3 hours, holding temperature is 40 ± 2 ℃; Then HEDP is filled in another still with strainer, is heated to 80 ℃ with filtering the clean HEDP in back, negative pressure is outer steamed 2 hours by drawing, and steamed outward and finished to analyze earlier activity, added the pure water dilution according to the HEDP activity, was cooled to 40 ℃ of blowings.Chemical examination arsenic content is less than 0.5mg/L.
The present invention is not limited to the scope of disclosed embodiment, and the foregoing description only is the simple examples of all respects of the present invention, and any have the embodiment of same function all within the scope of application of the present invention.
Claims (10)
1. the arsenic removal technology of a hydroxy ethylene diphosphonic acid is characterized in that: comprise following operation steps:
The hydroxy ethylene diphosphonic acid that in reactor, adds 400～1000 weight parts without the dearsenification processing, temperature of charge to 20 in the reacting kettle jacketing feeding steam adjusting still～70 ℃, the arsenic removing agent thiophosphoric anhydride that adds 0.1～1 weight part then, the gac that adds 0.2～2 weight part again, with the pure water rinsing charging opening of 0.5～2 weight part, under 20～70 ℃ of temperature ranges, be incubated 1～5 hour then after reinforced the finishing; Afterwards hydroxy ethylene diphosphonic acid is filtered, be heated to 80 ℃ with filtering the clean hydroxy ethylene diphosphonic acid in back, the outer steaming 1～3 hour under negative pressure, the outer steaming analyzed activity earlier before finishing, add the pure water dilution according to active result, the logical water coolant of reacting kettle jacketing is cooled to 40～50 ℃ of blowings with material in the still.
2. the arsenic removal technology of a kind of hydroxy ethylene diphosphonic acid according to claim 1 is characterized in that: the content of arsenic element is 20～200ppm in the described hydroxy ethylene diphosphonic acid of handling without dearsenification.
3. the arsenic removal technology of a kind of hydroxy ethylene diphosphonic acid according to claim 2 is characterized in that: the content of arsenic element is 40～150ppm in the described hydroxy ethylene diphosphonic acid of handling without dearsenification.
4. the arsenic removal technology of a kind of hydroxy ethylene diphosphonic acid according to claim 1 is characterized in that: the add-on of the described hydroxy ethylene diphosphonic acid of handling without dearsenification is 450～900 weight parts.
5. the arsenic removal technology of a kind of hydroxy ethylene diphosphonic acid according to claim 1, it is characterized in that: the add-on of described arsenic removing agent thiophosphoric anhydride is 0.15～0.5 weight part.
6. the arsenic removal technology of a kind of hydroxy ethylene diphosphonic acid according to claim 1, it is characterized in that: the temperature range of described reaction is 22～55 ℃.
7. the arsenic removal technology of a kind of hydroxy ethylene diphosphonic acid according to claim 1, it is characterized in that: the pure water consumption of described flushing charging opening is 1 weight part.
8. the arsenic removal technology of a kind of hydroxy ethylene diphosphonic acid according to claim 1, it is characterized in that: described soaking time is 2～4 hours.
9. the arsenic removal technology of a kind of hydroxy ethylene diphosphonic acid according to claim 1 is characterized in that: the add-on of described gac is 1 ‰ of the hydroxy ethylene diphosphonic acid add-on handled without dearsenification.
10. the arsenic removal technology of a kind of hydroxy ethylene diphosphonic acid according to claim 1 is characterized in that: the described time that will filter the clean hydroxy ethylene diphosphonic acid heating in back is 2～4 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043744A (en) * | 2012-12-07 | 2013-04-17 | 常州大学 | Method for treating industrial waste water with coal cinder ash |
| CN103694274A (en) * | 2014-01-16 | 2014-04-02 | 山东省泰和水处理有限公司 | Preparation method of low-chloride low-ammonia amino trimethylene phosphonic acid |
| CN106186116A (en) * | 2016-08-28 | 2016-12-07 | 张伟 | Wastewater purificant being added with hydroxy ethylene diphosphonic acid and preparation method thereof |
| CN106366125A (en) * | 2016-08-31 | 2017-02-01 | 南通联膦化工有限公司 | Production technique of low-arsenic solid hydroxyethylidenediphosphonic acid |
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| CN101676201A (en) * | 2008-09-19 | 2010-03-24 | 胡金来 | Technology for removing arsenic in polyphosphoric acid |
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| CN101676201A (en) * | 2008-09-19 | 2010-03-24 | 胡金来 | Technology for removing arsenic in polyphosphoric acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043744A (en) * | 2012-12-07 | 2013-04-17 | 常州大学 | Method for treating industrial waste water with coal cinder ash |
| CN103043744B (en) * | 2012-12-07 | 2014-06-11 | 常州大学 | Method for treating industrial waste water with coal cinder ash |
| CN103694274A (en) * | 2014-01-16 | 2014-04-02 | 山东省泰和水处理有限公司 | Preparation method of low-chloride low-ammonia amino trimethylene phosphonic acid |
| CN106186116A (en) * | 2016-08-28 | 2016-12-07 | 张伟 | Wastewater purificant being added with hydroxy ethylene diphosphonic acid and preparation method thereof |
| CN106366125A (en) * | 2016-08-31 | 2017-02-01 | 南通联膦化工有限公司 | Production technique of low-arsenic solid hydroxyethylidenediphosphonic acid |
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Application publication date: 20110525 |