CN102093415A - Process for removing arsenic from diethylene triamine penta(methylene phosphonic acid) (DTPMPA) - Google Patents
Process for removing arsenic from diethylene triamine penta(methylene phosphonic acid) (DTPMPA) Download PDFInfo
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- CN102093415A CN102093415A CN2011100060102A CN201110006010A CN102093415A CN 102093415 A CN102093415 A CN 102093415A CN 2011100060102 A CN2011100060102 A CN 2011100060102A CN 201110006010 A CN201110006010 A CN 201110006010A CN 102093415 A CN102093415 A CN 102093415A
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- pentamethylene phosphonic
- diethylenetriamine pentamethylene
- dtpmpa
- arsenic
- removal technology
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Abstract
The invention provides a process for removing arsenic from diethylene triamine penta(methylene phosphonic acid) (DTPMPA). The process has the advantage of low production cost and comprises the following steps: adding 400-1000 parts by weight of DTPMPA which does not undergo arsenic removal treatment to a reaction kettle, pumping steam from the jacket of the reaction kettle to adjust the temperature of the materials in the kettle to 20-70 DEG C, then adding 0.1-1 part by weight of arsenic removing agent phosphorus pentasulfide, then adding 0.2-2 parts by weight of active carbon, washing the charging hole with 0.5-2 parts by weight of pure water after charging and then preserving the heat in the temperature range of 20-70 DEG C for 1-5 hours; and later filtering the DTPMPA, heating the clean DTPMPA after filtration to 80 DEG C, externally steaming the clean DTPMPA under negative pressure for 1-3 hours, before completing external steaming, firstly analyzing the activity, adding pure water for dilution according to the activity result, pumping cooling water from the jacket of the reaction kettle to cool the materials in the kettle to 40-50 DEG C and discharging the DTPMPA.
Description
Technical field
The present invention relates to a kind of arsenic removal technology, relate in particular to a kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology.
Background technology
Diethylenetriamine pentamethylene phosphonic acids has another name called diethylene triamine pentamethylene phosphonic, molecular formula is C9H28015N3P5, its english abbreviation is DTPMPA, it 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 not, general light and heat condition is 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 with underwater gold, especially calcium ion formation six-membered ring chelate, thereby tool is scale inhibition effect and the tangible molten limit effect of tool preferably, when with the compound use of other water conditioner, shows synergistic effect preferably.
DTPMPA can be applicable to the winter severe cold area, be specially adapted to the clean-out system and the household chemicals additive of electron trade, DTPMPA 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, DTPMPA can be used as metal and nonmetallic clean-out system, bleaching and dyeing the peroxide stabiliser of industry and laking agent, the complexing agent of cyanideless electro-plating industry, and pharmaceutical industries is as the agent of carrying of radioelement.
Used phosphorus trichloride in the raw materials for production of DTPMPA, it is that initial feed is produced with the phosphorus ore, because unavoidably contain arsenic in the Rock Phosphate (72Min BPL), so often there is arsenic to exist among the DTPMPA, expansion day by day along with the DTPMPA 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 DTPMPA market of low arsenic is just increasing, it is very important that the DTPMPA 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 purpose of this invention is to provide the low diethylenetriamine pentamethylene phosphonic arsenic removal technology of a kind of production cost.
For achieving the above object, the technical solution used in the present invention is:
A kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology is characterized in that: comprise following operation steps:
The diethylenetriamine pentamethylene phosphonic acids 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 diethylenetriamine pentamethylene phosphonic acids (being DTPMPA) is filtered, be heated to 80 ℃ with filtering the clean diethylenetriamine pentamethylene phosphonic acids 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 diethylenetriamine pentamethylene phosphonic acids, the consumption of used dearsenic agent (thiophosphoric anhydride) is few, per 600 weight part DTPMPA use 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 a process flow diagram of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is further described:
A kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology comprises following operation steps:
The diethylenetriamine pentamethylene phosphonic acids 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 diethylenetriamine pentamethylene phosphonic acids (being DTPMPA) is filtered, be heated to 80 ℃ with filtering the clean diethylenetriamine pentamethylene phosphonic acids 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 DTPMPA, the logical water coolant of reacting kettle jacketing is cooled to 40～50 ℃ of blowings with material in the still.
The diethylenetriamine pentamethylene phosphonic arsenic element content of handling without dearsenification described in the above-mentioned steps is preferably 20～200ppm, and more preferably 40～150ppm especially is preferably 60～100ppm, most preferably is 70～80ppm.
The diethylenetriamine pentamethylene phosphonic add-on 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, is 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 diethylenetriamine pentamethylene phosphonic acids add-on handled without dearsenification, and more preferably 1 ‰.
The time that to filter the clean diethylenetriamine pentamethylene phosphonic acids 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 diethylenetriamine pentamethylene phosphonic arsenic removal technology, by adding dearsenic agent thiophosphoric anhydride (P
2S
5) and gac remove arsenic among the DTPMPA, provide a kind of efficiently, dearsenicating technology cheaply, can effectively reduce the arsenic content among the DTPMPA, it is high and cause the limited difficult problem of range of application to have solved in the common DTPMPA product arsenic content.This technology can access the DTPMPA of arsenic content less than 1ppm, and the DTPMPA 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 present invention is raw materials used to be included: (arsenic content is 70～80ppm) to DTPMPA, other thiophosphoric anhydride of commercial grade (P
2S
5), 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 DTPMPA 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, the patent No. is that arsenic removal technology is to carry out under 50～60 ℃ of temperature in 200810230638.9 the described method of patent, the temperature range that technology is suitable for is narrow, be unfavorable for diversified operational condition and production environment in the actual production, technology of the present invention is less demanding to used temperature, the temperature range that technology is suitable for is wide, and 20～70 ℃ can be reacted, and especially can finish the dearsenification operation under the room temperature about 20 ℃;
Secondly, the consumption of the used dearsenic agent of this technology (thiophosphoric anhydride) is few, per 600 weight part DTPMPA use thiophosphoric anhydride (P2S5) 0.15～0.5 weight part just can reach the dearsenification effect, the thiophosphoric anhydride low price, whole arsenic removal technology with low cost helps this technology 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 effect.)
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, and the hydrogen sulfide of generation (H2S) can be fully utilized, and unnecessary hydrogen sulfide (H2S) can absorb with alkali lye, and 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 diethylenetriamine pentamethylene phosphonic acids, dearsenic agent, activated carbon in reactor, and start stirring.
3, dearsenification at a certain temperature (AS).
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 DTPMPA 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 600kgDTPMPA, 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 DTPMPA is filled in another still with strainer, the DTPMPA 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 DTPMPA active quantities, was cooled to 50 ℃ of blowings.Chemical examination arsenic content is less than 1mg/L.
Embodiment 2:
Charging capacity DTPMPA 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 600kgDTPMPA, 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 DTPMPA is filled in another still with strainer, clean DTPMPA 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 DTPMPA activity, was cooled to 40 ℃ of blowings.Chemical examination arsenic content is less than 1mg/L.
Embodiment 3:
Charging capacity DTPMPA 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 600kgDTPMPA, 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 DTPMPA is filled in another still with strainer, clean DTPMPA 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 DTPMPA activity, was cooled to 45 ℃ of blowings.Chemical examination arsenic content is less than 1mg/L.
Embodiment 4:
Charging capacity DTPMPA 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 600kgDTPMPA, 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 DTPMPA is filled in another still with strainer, clean DTPMPA 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 DTPMPA activity, was cooled to 45 ℃ of blowings.Chemical examination arsenic content 0.5mg/L.
Embodiment 5:
Charging capacity DTPMPA 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 600kgDTPMPA, 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 DTPMPA is filled in another still with strainer, clean DTPMPA 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 DTPMPA activity, was cooled to 50 ℃ of blowings.Chemical examination arsenic content is less than 0.3～0.6mg/L.
Embodiment 6:
Charging capacity DTPMPA 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 5000kgDTPMPA, 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 DTPMPA is filled in another still with strainer, is heated to 80 ℃ with filtering the clean DTPMPA 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 DTPMPA 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. diethylenetriamine pentamethylene phosphonic arsenic removal technology is characterized in that: comprise following operation steps:
The diethylenetriamine pentamethylene phosphonic acids 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 diethylenetriamine pentamethylene phosphonic acids is filtered, be heated to 80 ℃ with filtering the clean diethylenetriamine pentamethylene phosphonic acids 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.
2. a kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology according to claim 1 is characterized in that: described content without arsenic element in the diethylenetriamine pentamethylene phosphonic acids of dearsenification processing is 20～200ppm.
3. a kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology according to claim 2 is characterized in that: described content without arsenic element in the diethylenetriamine pentamethylene phosphonic acids of dearsenification processing is 40～150ppm.
4. a kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology according to claim 1 is characterized in that: the described diethylenetriamine pentamethylene phosphonic add-on of handling without dearsenification is 450～900 weight parts.
5. a kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology 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. a kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology according to claim 1, it is characterized in that: the temperature range of described reaction is 22～55 ℃.
7. a kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology according to claim 1, it is characterized in that: the pure water consumption of described flushing charging opening is 1 weight part.
8. a kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology according to claim 1, it is characterized in that: described soaking time is 2～4 hours.
9. a kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology according to claim 1 is characterized in that: the add-on of described gac is without 1 ‰ of the diethylenetriamine pentamethylene phosphonic acids add-on of dearsenification processing.
10. a kind of diethylenetriamine pentamethylene phosphonic arsenic removal technology according to claim 1 is characterized in that: the described time that will filter the clean diethylenetriamine pentamethylene phosphonic acids heating in back is 2～4 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114534651A (en) * | 2022-01-13 | 2022-05-27 | 宁夏天霖新材料科技有限公司 | Reactor temperature control method |
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| CN101676201A (en) * | 2008-09-19 | 2010-03-24 | 胡金来 | Technology for removing arsenic in polyphosphoric acid |
| CN101786744A (en) * | 2010-03-08 | 2010-07-28 | 昆明理工大学 | Method for directly utilizing waste liquor containing phosphoric acid and phosphorous acid |
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2011
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676201A (en) * | 2008-09-19 | 2010-03-24 | 胡金来 | Technology for removing arsenic in polyphosphoric acid |
| CN101786744A (en) * | 2010-03-08 | 2010-07-28 | 昆明理工大学 | Method for directly utilizing waste liquor containing phosphoric acid and phosphorous acid |
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| 汤长青等: "低含量砷羟基亚乙基二膦酸的制备", 《精细化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114534651A (en) * | 2022-01-13 | 2022-05-27 | 宁夏天霖新材料科技有限公司 | Reactor temperature control method |
| CN114534651B (en) * | 2022-01-13 | 2024-03-12 | 宁夏天霖新材料科技有限公司 | Reactor temperature control method |
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Application publication date: 20110615 |