CN103304462A - Recovery method of sodium diethyldithiocarbamate - Google Patents
Recovery method of sodium diethyldithiocarbamate Download PDFInfo
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- CN103304462A CN103304462A CN2013102804050A CN201310280405A CN103304462A CN 103304462 A CN103304462 A CN 103304462A CN 2013102804050 A CN2013102804050 A CN 2013102804050A CN 201310280405 A CN201310280405 A CN 201310280405A CN 103304462 A CN103304462 A CN 103304462A
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Abstract
The invention discloses a recovery method of sodium diethyldithiocarbamate. The method comprises the steps of selecting diethyldithiocarbamic acid iron solution of which the pH is between 9 and 11; adding sodium hydroxide solution to the diethyldithiocarbamic acid iron solution, wherein the molar ratio of the diethyldithiocarbamic acid iron to the sodium hydroxide is 1 to 3, the temperature of the solution in reaction is controlled to be 70-80 DEG C and the reaction time is 25 minutes; simultaneously agitating continuously, and finally filtering the final reaction solution to obtain the sodium diethyldithiocarbamate solution.
Description
Technical field
The present invention relates to a kind of recycling of iron precipitation agent, more specifically, relate to a kind of recovery method of Thiocarb.
Background technology
Chinese patent application numbers 200410051386.5 discloses a kind of heavy metal precipitator, is N, N-two dithio piperazinecarboxylic acid sodium.The raw material availability that it has overcome existing heavy metal precipitator existence is not high, complex ability is strong, flco is loose and sedimentation speed waits slowly, particularly for the shortcoming of stable complexation heavy metal ion waste water without special effect agent, can effectively remove and fixing heavy metal ion, and in the precipitation of heavy metals ion function of can also decolouring simultaneously, can be applicable to the processing of heavy metal ions in wastewater.
The applicant finds by for many years research, when the preparation non-iron aluminium sulfate, with Thiocarb and iron ion reaction, generates the ferric diethyldithiocarbamate precipitation.In order to reuse Thiocarb, ferric diethyldithiocarbamate is processed, again obtain Thiocarb, the present invention adopts a kind of novel method, and is simple to operate, and the rate of recovery is high, and cost is low.
Summary of the invention
The purpose of this invention is to provide a kind of recovery method of Thiocarb, the rate of recovery is high, and cost is low.
A kind of recovery method of Thiocarb is chosen ferric diethyldithiocarbamate solution, makes between pH value of solution=9 to 11; Add sodium hydroxide solution in ferric diethyldithiocarbamate solution, wherein the molar ratio of ferric diethyldithiocarbamate and sodium hydroxide is 1:3; Solution temperature is controlled at 70-80 ℃ during reaction, and the reaction times constantly stirs simultaneously at 25min, and last reaction soln obtains Thiocarb solution by filtration.
As a kind of preferred, the pH value of ferric diethyldithiocarbamate solution is 10.
As a kind of preferred, the concentration of described sodium hydroxide solution is 10%.
As a kind of preferred, also obtain filter residue after the described filtration, described filter residue is ferric hydroxide precipitate.
Beneficial effect, device is simple, and easy to operate, expense is low.
Description of drawings
Fig. 1 is ferric diethyldithiocarbamate resolution of precipitate schematic diagram of the present invention;
Fig. 2 is filtration ferric hydroxide precipitate schematic diagram of the present invention.
Embodiment
Among Fig. 1,100g ferric diethyldithiocarbamate precipitation is placed container 8, add 300mL water, turn on agitator 9, the control solution temperature is 75 ℃, drip the sodium hydroxide solution 10 of 240g10%, obtain Thiocarb solution 11 and ferric hydroxide precipitate behind the reaction 25min.
Among Fig. 2, iron ring 2 is installed on the iron stand 1, filter paper 4 is placed funnel 3, funnel with filter paper is placed iron ring 2, place the funnel with filter paper to filter Thiocarb solution 7 and ferric hydroxide precipitate, obtain filtrate 6 and be Thiocarb solution, the filter residue in the funnel 7 is ferric hydroxide precipitate.
The testing data table
1. test method: get the 100g ferric diethyldithiocarbamate, place the container of 1000mL, add 300mL water, turn on agitator, the control solution temperature is 75 ℃, drip the sodium hydroxide solution of 240g10%, obtain Thiocarb solution and ferric hydroxide precipitate behind the reaction 25min.The Thiocarb rate of recovery sees Table 1.
The table 1 Thiocarb rate of recovery
| Project | The theoretical Thiocarb (g) that reclaims | Actual recovered Thiocarb (g) | The rate of recovery/% |
| ? | 102.6 | 101.06 | 98.5 |
2. the Thiocarb rate of recovery affects idealistic factor
(1) addition amount of sodium hydroxide is on the impact of the Thiocarb rate of recovery
Under the same conditions, change sodium hydroxide concentration.Get the 100g ferric diethyldithiocarbamate, place the container of 1000mL, add 300mL water, turn on agitator, the control solution temperature is 75 ℃, behind the reaction 25min, obtains Thiocarb solution and ferric hydroxide precipitate.The Thiocarb rate of recovery sees Table 2.
Table 2 addition amount of sodium hydroxide is on the impact of the Thiocarb rate of recovery
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 |
| Sodium hydroxide quality/g | 20 | 22 | 24 | 26 | 28 | 30 |
| The Thiocarb rate of recovery/% | 83.3 | 91.7 | 98.5 | 98.6 | 98.6 | 98.6 |
Can be found out by test-results, addition amount of sodium hydroxide is on the impact of the Thiocarb rate of recovery, and is best when the molar ratio of ferric diethyldithiocarbamate and sodium hydroxide is 1:3.
(2) reaction times is on the impact of the Thiocarb rate of recovery
Under the same conditions, change the reaction times.Get the 100g ferric diethyldithiocarbamate, place the container of 1000mL, add 300mL water, turn on agitator, the control solution temperature is 75 ℃, drips the sodium hydroxide solution of 240g10%, obtains Thiocarb solution and ferric hydroxide precipitate.The Thiocarb rate of recovery sees Table 3.
Table 3 reaction times is on the impact of the Thiocarb rate of recovery
| Reaction times (min) | Thiocarb quality (g) | The rate of recovery/% |
| 5 | 53 | 51.9 |
| 15 | 79 | 77.4 |
| 25 | 101.06 | 98.5 |
| 30 | 101.07 | 98.5 |
| 60 | 101.07 | 98.5 |
| 90 | 101.07 | 98.5 |
Can be found out by test-results, there is a Best Times in the Thiocarb rate of recovery, is the 25min best results in the reaction times namely.
(3) temperature of reaction is on the impact of the Thiocarb rate of recovery
Under the same conditions, change temperature of reaction.Get the 100g ferric diethyldithiocarbamate, place the container of 1000mL, add 300mL water, turn on agitator, the sodium hydroxide solution of dropping 240g10% obtains Thiocarb solution and ferric hydroxide precipitate.The Thiocarb rate of recovery sees Table 4.
The relation of table 4 temperature of reaction and iron level and aluminium content
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Solution temperature/℃ | 20 | 30 | 40 | 50 | 60 | 70 | 80 | 90 | 100 |
| The Thiocarb rate of recovery/% | 12.0 | 18.9 | 24.3 | 29.6 | 68.3 | 98.7 | 98.8 | 98.8 | 98.8 |
Along with the rising of temperature of reaction, the Thiocarb rate of recovery raises, and optimal temperature is 70 ~ 80 ℃.
(4) potential of hydrogen of solution is on the impact of the Thiocarb rate of recovery
Under the same conditions, change the potential of hydrogen of solution.Get the container that a certain amount of ferric diethyldithiocarbamate places 1000mL, add water 300mL, temperature of reaction is controlled at 75 ℃, add 10% hydrogen-oxygen sodium solution 240g, simultaneously continuous stirred solution, stop to stir behind the reaction 25min, solution acid alkalinity sees Table 5 to the impact of the Thiocarb rate of recovery.
Table 5 solution acid alkalinity is on the impact of the Thiocarb rate of recovery
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 |
| PH value of solution | 1 | 3 | 5 | 7 | 9 | 11 |
| The Thiocarb rate of recovery/% | 83.7 | 86.4 | 90.3 | 92.5 | 98.8 | 98.9 |
By above data presentation, the pH of solution is higher more favourable to reaction, when pH between 9.0 to 11, the Thiocarb rate of recovery is stable.
In sum, when reclaiming Thiocarb, add the amount (molar ratio is 1:3) of corresponding sodium hydroxide according to the amount of ferric diethyldithiocarbamate, between control pH value of solution=9-11, solution temperature is controlled at 70-80 ℃ during reaction, and the reaction times is at 25min.
This embodiment just embodies the preferred special case of spirit of the present invention, those skilled in the art fully can be according to the present invention the purport of patent, in addition flexible has reached best implementation result.The present invention is made amendment or is equal to replacement, and do not break away from the spirit and scope of patent of the present invention, it all should be encompassed in the middle of the claim scope of patent of the present invention.
Claims (4)
1. the recovery method of a Thiocarb is characterized in that: choose ferric diethyldithiocarbamate solution, make between pH value of solution=9 to 11; Add sodium hydroxide solution in ferric diethyldithiocarbamate solution, wherein the molar ratio of ferric diethyldithiocarbamate and sodium hydroxide is 1:3; Solution temperature is controlled at 70-80 ℃ during reaction, and the reaction times constantly stirs simultaneously at 25min, and last reaction soln obtains Thiocarb solution by filtration.
2. recovery method according to claim 1, it is characterized in that: the pH value of ferric diethyldithiocarbamate solution is 10.
3. recovery method according to claim 1, it is characterized in that: the concentration of described sodium hydroxide solution is 10%.
4. recovery method according to claim 1, it is characterized in that: also obtain filter residue after the described filtration, described filter residue is ferric hydroxide precipitate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922420A (en) * | 2014-04-28 | 2014-07-16 | 辽宁石化职业技术学院 | Rapid preparation method for iron oxide red |
| CN110950789A (en) * | 2019-12-12 | 2020-04-03 | 青岛惠城环保科技股份有限公司 | Regeneration method of nickel-removing chelating agent in aluminum sulfate production process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3966601A (en) * | 1972-11-01 | 1976-06-29 | Robinson Brothers Ltd. | Effluent treatment |
| JPS5321079A (en) * | 1976-08-11 | 1978-02-27 | Tokyo Yuuki Kagaku Kougiyou Kk | Method of treating aqueous waste liquid containing dithiocarbamate |
| JP2006299004A (en) * | 2005-04-18 | 2006-11-02 | Pollars Laboratory Corp | HEAVY METAL AND CHEMICALS FOR TREATING Cr (VI) INTO HARMLESS |
| US7390416B1 (en) * | 2004-01-26 | 2008-06-24 | American Airlines, Inc. | Method for the removal of metals, including a co-precipitation of molybdenum, from wastewater |
-
2013
- 2013-07-05 CN CN2013102804050A patent/CN103304462A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3966601A (en) * | 1972-11-01 | 1976-06-29 | Robinson Brothers Ltd. | Effluent treatment |
| JPS5321079A (en) * | 1976-08-11 | 1978-02-27 | Tokyo Yuuki Kagaku Kougiyou Kk | Method of treating aqueous waste liquid containing dithiocarbamate |
| US7390416B1 (en) * | 2004-01-26 | 2008-06-24 | American Airlines, Inc. | Method for the removal of metals, including a co-precipitation of molybdenum, from wastewater |
| JP2006299004A (en) * | 2005-04-18 | 2006-11-02 | Pollars Laboratory Corp | HEAVY METAL AND CHEMICALS FOR TREATING Cr (VI) INTO HARMLESS |
Non-Patent Citations (1)
| Title |
|---|
| 李秦川等: "DDTC络合去除硫酸铝中铁工艺条件的优化", 《化学与生物工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922420A (en) * | 2014-04-28 | 2014-07-16 | 辽宁石化职业技术学院 | Rapid preparation method for iron oxide red |
| CN110950789A (en) * | 2019-12-12 | 2020-04-03 | 青岛惠城环保科技股份有限公司 | Regeneration method of nickel-removing chelating agent in aluminum sulfate production process |
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Application publication date: 20130918 |