CN100560491C - Change into the recovery and treatment method and the treatment system thereof of waste liquid mesoboric acid - Google Patents
Change into the recovery and treatment method and the treatment system thereof of waste liquid mesoboric acid Download PDFInfo
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- CN100560491C CN100560491C CNB2007100755232A CN200710075523A CN100560491C CN 100560491 C CN100560491 C CN 100560491C CN B2007100755232 A CNB2007100755232 A CN B2007100755232A CN 200710075523 A CN200710075523 A CN 200710075523A CN 100560491 C CN100560491 C CN 100560491C
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Abstract
The present invention relates to a kind of recovery and treatment method and treatment system that changes into the waste liquid mesoboric acid, method comprises the steps: to add ammoniacal liquor in waste liquid, impels waste liquid to separate out aluminum hydroxide precipitation, and isolates aluminum hydroxide precipitation obtain separatory just from waste liquid; In first separatory, add hydrochloric acid or nitric acid, impel the ammonium pentaborate in the first separatory to be hydrolyzed to boric acid, obtain acidizing fluid; Acidizing fluid is carried out underpressure distillation, steam ammonium root, acid solution and moisture, separate out until solid boric acid; With the solid boric acid of separating out carry out vacuum-drying or constant pressure and dry, recovery is used again.Treatment process of the present invention and system can isolate aluminium and ammonium root efficiently from aging waste liquid; and ammonium pentaborate is converted into boric acid and the high efficiente callback utilization; can better protect environment, guarantee to reclaim the purity of boric acid product and changing into recycling of paper tinsel industry again, and can enhance productivity, reduce cost recovery.
Description
Technical field
The present invention relates to a kind of Chemical Manufacture treatment technology, more particularly, the present invention relates to a kind of purification and environmental protection reutilization technology and treatment system of industrial boric acid waste liquid.
Background technology
Along with the develop rapidly of electronic industry, the employing of electrical condenser is more and more.Make a living the changing in the paper tinsel industry of electrogenesis container aluminium foil, mesohigh change into the boric acid that needs to use a large amount of capacitor stage purity as changing into tank liquor, and the preparation tank liquor generally also needs to add ammoniacal liquor or ammonium pentaborate is regulated the pH value.
In changing into production process, constantly have small amount of aluminum above the aluminium foil and be dissolved in the tank liquor, cause formation efficiency to reduce at last and quality product decline, just tank liquor is aging.Need prepare the new tank liquor that changes into again when the aged tank liquor can not continue to use, the aged tank liquor can only be as liquid waste disposal.Yet, contain a large amount of boric acid and some aluminum ions in the aged waste liquid, discharge factory and can cause that natural water pollutes, the infringement of environment, so reclaim after preferably related substance in the waste liquid being separated, recycle.
Yet treatment process in the past is directly boric acid waste liquid to be heated to boiling, separates out boric acid after cooling, and the separation of waste liquid suction filtration, drying are obtained boric acid and get final product.The shortcoming of traditional method is: 1, do not remove aluminium and ammonium pentaborate in the waste liquid, not only aluminium and ammonium pentaborate can not obtain collect reclaiming, and filtrate still can damage to the environment; 2, the ammonium pentaborate in the waste liquid does not obtain separating, cause the boric acid that reclaims because ammonium pentaborate is residual purity not high enough, the boric acid of recovery can't recycle changing into the paper tinsel industry, processing remains big problem; 3, the traditional treatment method heating cost is too high, and is uneconomical economically.
Summary of the invention
Above-mentioned shortcoming at prior art; the objective of the invention is to provide a kind of recovery and treatment method and treatment system thereof that changes into the waste liquid mesoboric acid; this treatment process and system have following advantage: can isolate aluminium and ammonium root efficiently from aging waste liquid; and ammonium pentaborate is converted into boric acid and the high efficiente callback utilization; can better protect environment, guarantee to reclaim the purity of boric acid product and changing into recycling of paper tinsel industry again, and can enhance productivity, reduce cost recovery.
For this reason, one of technical solution of the present invention is a kind of recovery and treatment method that changes into the waste liquid mesoboric acid, comprise ammonium root, aluminum ion and five borates in the described waste liquid, and the treating method comprises following steps: (A) in described waste liquid, add ammoniacal liquor, impel waste liquid to separate out aluminum hydroxide precipitation, and from described waste liquid, isolate aluminum hydroxide precipitation and obtain separatory just; (B) in first separatory, add hydrochloric acid or nitric acid, impel the ammonium pentaborate in the first separatory to be hydrolyzed to boric acid, obtain acidizing fluid; (C) acidizing fluid is carried out underpressure distillation, steam ammonium root, acid solution and moisture, separate out until solid boric acid; (D) the solid boric acid of separating out is carried out vacuum-drying or constant pressure and dry, recovery is used again.
Waste liquid recovery and treatment method of the present invention, do not contained ammonia and phenomenon and idea that aluminum ion still freely exists confuse by waste liquid, one confrontational separation ammonium root and aluminum ions electrolytic electrophoresis method, in containing ammonia solution, attempt continuing to add ammoniacal liquor, the hydroxyl of attempting to increase in the waste liquid precipitates the removal aluminum ion, evidence, this steps A can be with the content of the aluminum ion in the waste liquid by original 500mg/L to 5000mg/L, be reduced to the content of the 5mg/L to 20mg/L after handling, aluminum ions decreasing ratio is up to 99.99%; On the basis that aluminum ion efficiently removes, consider the requirement of later separation, purification, the present invention adopts lower boiling hydrochloric acid of interpolation or nitric acid acid solution to carry out acidifying step B, try hard to change the balance of ammonium pentaborate and boric acid in the first separatory, most ammonium pentaborates are converted into boric acid, guarantee simultaneously after evaporative process can remove ammonium root, acid solution and moisture.Evidence, this step B can guarantee that the purity that reclaims boric acid reaches 99.9%, the outward appearance of boric acid is rendered as white powder, and muriate (Cl wherein
-), vitriol (SO4
2-), molysite (Fe
3+) content and capacitor stage boric acid basic identical (capacitor stage boric acid, outward appearance: white powder or transparent crystallization; Boric acid content (%): 〉=99.5.The high-content (%) of impurity: muriate (Cl
-)≤0.0001; Vitriol (SO
4 2-)≤0.0005; Molysite (Fe
3+)≤0.0002), guaranteed to reclaim the purity of boric acid product; The boric acid that adopts the inventive method to reclaim is made purification experiment: do not have hot spot on the formed aluminum foil, no flakes dirt settling.The boric acid that reclaims can be competent at fully and change into recycling of paper tinsel industry.And; aluminum hydroxide precipitation, ammonium root and the acid solution of the higher degree of removing from mix stoste and acidizing fluid utilized easily again and the pollution hazard of environment reduced; the inventive method is removed and has been guaranteed to reclaim the purity of boric acid product and changing into recycling of paper tinsel industry, has also protected environment better.In addition, what the inventive method was used is that distillation under vacuum is removed moisture, and power consumption mainly is the power consumption of a. vacuum pump, the heating during b. vacuum-evaporation; Because need not to be heated to 100 ℃ of the boiling points of water, so these energy consumptions are smaller, about boric acid per ton reclaims power consumption 200 to 400 degree.C. the exsiccant energy consumption is littler: 100 to 200 degree/tons.This shows that the inventive method has improved organic efficiency, reduced cost recovery.
The improvement of the inventive method also comprises the following content of determining through experiment:
In the described steps A, interpolation ammoniacal liquor to the pH value of waste liquid reaches 5.5-6.5, leaves standstill then or centrifugation, impels aluminum hydroxide precipitation to separate out.
In the described steps A, adopt the method for suction filtration or centrifuging that aluminum hydroxide precipitation is separated from described waste liquid.
Among the described step B, add described acid solution to the pH value of described acidizing fluid less than 4.0.
Among the described step B, preferred nitric acid, among the described step C, the temperature of described underpressure distillation is controlled at 20 ℃ to 50 ℃ scopes, pressure-controlling in 2.5kPa to 4.2kPa scope.Consider with acid for adjusting pH value and need in evaporative process, again acid be removed, so the inventive method only adopts lower boiling acid, example hydrochloric acid, nitric acid; But in changing into the paper tinsel industry, chlorion definitely will be avoided, so generally do not use hydrochloric acid, if the boric acid that reclaims is used for other purposes, can certainly use hydrochloric acid.The hydrofluoric acid boiling point is not high but toxicity is too strong, does not intend using.Sour as for high boiling points such as phosphoric acid, sulfuric acid because of being difficult to evaporative removal, so be not used.
Among the described step D, described vacuum drying temperature is controlled at 30-40 ℃ of scope, pressure-controlling is 1-3 hour scope in 4.0kPa-8.5kPa scope, vacuum drying time.
Among the described step D, it is 3-6 hour scope that the temperature of described constant pressure and dry is controlled at 60-80 ℃ of scope, exsiccant time.
Aluminum ions content is in the 500mg/L-5000mg/L scope in the described waste liquid before handling; In the described separatory just, aluminum ions content is at 5mg/L-20mg/L.This improvement can reduce waste liquid greatly pollutes environment water, is convenient to recycle the high concentration of hydrogen precipitation of alumina.
Correspondingly, another technical solution of the present invention is a kind of system that is used for changing into as mentioned above the recycling of waste liquid mesoboric acid, and this system comprises and being mutually related on position and the operation as lower device: the filtration unit that adds the ammoniacal liquor adding set of ammoniacal liquor in the tank liquor, aluminum hydroxide precipitation is separated from waste liquid, add acid solution adding set, the vacuum distillation apparatus of acid solution in the tank liquor.
Described filtration unit comprises suction filtration device and/or centrifugation device, and level also comprises solid boric acid is carried out the exsiccant Minton dryer behind described vacuum distillation apparatus.
As previously mentioned; the present invention changes into the apparatus system of the recycling of waste liquid mesoboric acid; can from aging waste liquid, separate aluminium and ammonium pentaborate efficiently; ammonium pentaborate efficiently is converted into boric acid and recycles; can better protect environment, guarantee that the purity and the recovery boric acid that reclaim the boric acid product are changing into recycling of paper tinsel industry again, and production efficiency improves, cost recovery reduces.
The present invention will be further described below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is the structural representation block diagram of system embodiment of the present invention.
Embodiment
System embodiment:
As Fig. 1, be depicted as a kind of structural representation block diagram that is used to change into the recovery and processing system embodiment of waste liquid mesoboric acid, this system comprises and being mutually related on position and the operation as lower device: the filtration unit 3 that adds the ammoniacal liquor adding set 2 of ammoniacal liquor in the tank liquor 1, aluminum hydroxide precipitation is separated from waste liquid, add acid solution adding set 4, the vacuum distillation apparatus 5 of acid solution in the tank liquor 1.
Described filtration unit 3 comprises the centrifugation device, also comprises in described vacuum distillation apparatus 5 back levels solid boric acid is carried out exsiccant Minton dryer 6.
Method embodiment 1:
Get boric acid waste liquid 10L, know about 500 grams of its boronic acid containing according to tank liquor concentration.Add ammoniacal liquor and regulate pH value to 6.0, consume ammoniacal liquor 50mL.Left standstill after stirring 5 hours, the adularescent flocks of waste liquid bottom is separated out, and its suction filtration is separated.Add concentrated nitric acid 30mL in the mother liquor, stir, its pH value is 3.5.Under the room temperature (25 ℃) with its underpressure distillation, pressure is 3kPa (22mmHg).The boric acid crystal of separating out is put into vacuum drying oven, under 35 ℃, dry 2 hours of 6kPa (45mmHg).Weighing boric acid quality is 485 grams.
Method embodiment 2:
Get boric acid waste liquid 10L, know about 700 grams of its boronic acid containing according to tank liquor concentration.Add ammoniacal liquor and regulate pH value to 6.0, consume ammoniacal liquor 52mL.Stirred 500 rev/mins of rotating speeds back centrifugal 5 minutes.The adularescent flocks of waste liquid bottom is separated out, and its suction filtration is separated.Add concentrated nitric acid 38mL in the mother liquor, stir, its pH value is 2.5.Under the room temperature (25 ℃) with its underpressure distillation, pressure is 3.5kPa (26mmHg).The boric acid crystal of separating out is put into vacuum drying oven, under 35 ℃, dry 2 hours of 6.5kPa (48mmHg).Weighing boric acid quality is 695 grams.
Claims (10)
1, a kind of recovery and treatment method that changes into the waste liquid mesoboric acid, comprise ammonium root, aluminum ion and five borates in the described waste liquid, it is characterized in that: the treating method comprises following steps: (A) in described waste liquid, add ammoniacal liquor, impel waste liquid to separate out aluminum hydroxide precipitation, and from described waste liquid, isolate aluminum hydroxide precipitation and obtain separatory just; (B) in first separatory, add hydrochloric acid or nitric acid, impel the ammonium pentaborate in the first separatory to be hydrolyzed to boric acid, obtain acidizing fluid; (C) acidizing fluid is carried out underpressure distillation, steam ammonium root, acid solution and moisture, separate out until solid boric acid; (D) the solid boric acid of separating out is carried out vacuum-drying or constant pressure and dry, recovery is used again.
2, change into the recovery and treatment method of waste liquid mesoboric acid according to claim 1, it is characterized in that: in the described steps A, interpolation ammoniacal liquor to the pH value of waste liquid reaches 5.5-6.5, leaves standstill then or centrifugation, impels aluminum hydroxide precipitation to separate out.
3, change into the recovery and treatment method of waste liquid mesoboric acid according to claim 1, it is characterized in that: in the described steps A, adopt the method for suction filtration or centrifuging that aluminum hydroxide precipitation is separated from described waste liquid.
4, change into the recovery and treatment method of waste liquid mesoboric acid according to claim 1, it is characterized in that: among the described step B, add described acid solution to the pH value of described acidizing fluid less than 4.0.
5, as changing into the recovery and treatment method of waste liquid mesoboric acid as described in one of claim 1-4, it is characterized in that: among the described step C, the temperature of described underpressure distillation is controlled at 20 ℃ to 50 ℃ scopes, pressure-controlling in 2.5kPa to 4.2kPa scope.
6, change into the recovery and treatment method of waste liquid mesoboric acid according to claim 1, it is characterized in that: among the described step D, described vacuum drying temperature is controlled at 30-40 ℃ of scope, pressure-controlling is 1-3 hour scope in 4.0kPa-8.5kPa scope, vacuum drying time.
7, change into the recovery and treatment method of waste liquid mesoboric acid according to claim 1, it is characterized in that: among the described step D, it is 3-6 hour scope that the temperature of described constant pressure and dry is controlled at 60-80 ℃ of scope, exsiccant time.
8, change into the recovery and treatment method of waste liquid mesoboric acid according to claim 1, it is characterized in that: aluminum ions content is in the 500mg/L-5000mg/L scope in the described waste liquid before handling; In the described separatory just, aluminum ions content is at 5mg/L-20mg/L.
9, a kind of system that is used for changing into the recycling of waste liquid mesoboric acid as described in claim 1-8 is characterized in that: this system comprises and being mutually related on position and the operation as lower device: the filtration unit that adds the ammoniacal liquor adding set of ammoniacal liquor in the tank liquor, aluminum hydroxide precipitation is separated from waste liquid, add acid solution adding set, the vacuum distillation apparatus of acid solution in the tank liquor.
10, the system of recycling as claimed in claim 9 is characterized in that: described filtration unit comprises suction filtration device and/or centrifugation device, and level also comprises solid boric acid is carried out the exsiccant Minton dryer behind described vacuum distillation apparatus.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100755232A CN100560491C (en) | 2007-08-03 | 2007-08-03 | Change into the recovery and treatment method and the treatment system thereof of waste liquid mesoboric acid |
Applications Claiming Priority (1)
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|---|---|---|---|
| CNB2007100755232A CN100560491C (en) | 2007-08-03 | 2007-08-03 | Change into the recovery and treatment method and the treatment system thereof of waste liquid mesoboric acid |
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| CN101139097A CN101139097A (en) | 2008-03-12 |
| CN100560491C true CN100560491C (en) | 2009-11-18 |
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| CN108083528A (en) * | 2016-11-21 | 2018-05-29 | 江苏同禾药业有限公司 | A kind of method that waste water containing boron is handled in 6- hydroxyl -8- Lipase Catalyzed Resolution of Racemic Ethyl preparation process |
| CN111498861B (en) * | 2020-04-23 | 2022-07-26 | 无锡中天固废处置有限公司 | Polarizing plate waste liquid treatment method |
| CN114956436B (en) * | 2022-08-01 | 2022-11-01 | 江苏同禾药业有限公司 | Method for recovering boron element from production wastewater |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4196177A (en) * | 1978-07-24 | 1980-04-01 | Sallay Stephen I | Process for producing boron compounds from borate ores |
| CN1309082A (en) * | 2001-03-19 | 2001-08-22 | 李洪岭 | Process for recovering boric acid from boron mud |
| CN1528666A (en) * | 2003-10-08 | 2004-09-15 | 四川石油管理局川西北矿区 | Process for preparing kali salt and boric acid from bittern |
| CN1654326A (en) * | 2004-12-23 | 2005-08-17 | 大连理工大学 | Manufacturing method of calcium borate by dissociating ulexite in limebase prooess |
-
2007
- 2007-08-03 CN CNB2007100755232A patent/CN100560491C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4196177A (en) * | 1978-07-24 | 1980-04-01 | Sallay Stephen I | Process for producing boron compounds from borate ores |
| CN1309082A (en) * | 2001-03-19 | 2001-08-22 | 李洪岭 | Process for recovering boric acid from boron mud |
| CN1528666A (en) * | 2003-10-08 | 2004-09-15 | 四川石油管理局川西北矿区 | Process for preparing kali salt and boric acid from bittern |
| CN1654326A (en) * | 2004-12-23 | 2005-08-17 | 大连理工大学 | Manufacturing method of calcium borate by dissociating ulexite in limebase prooess |
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| CN101139097A (en) | 2008-03-12 |
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Granted publication date: 20091118 Termination date: 20160803 |