CN113698038A - Utilization and treatment method of gluconolactone high-salt ion exchange wastewater - Google Patents
Utilization and treatment method of gluconolactone high-salt ion exchange wastewater Download PDFInfo
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- CN113698038A CN113698038A CN202111021913.8A CN202111021913A CN113698038A CN 113698038 A CN113698038 A CN 113698038A CN 202111021913 A CN202111021913 A CN 202111021913A CN 113698038 A CN113698038 A CN 113698038A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/02—Methods and apparatus for dehydrating gypsum
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/26—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
- C04B11/266—Chemical gypsum
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02F2101/00—Nature of the contaminant
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- C02F2101/101—Sulfur compounds
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Abstract
The invention relates to the technical field of wastewater treatment, in particular to a utilization and treatment method of gluconolactone high-salt ion exchange wastewater. The method comprehensively utilizes sewage resources, cancels the addition of sodium hydroxide to adjust the pH value in the prior art, produces sodium hydroxide through double decomposition reaction to adjust the low-pH wastewater of enterprises, effectively removes sulfate ions, reduces the pressure of sewage treatment, and simultaneously reduces the sewage treatment cost.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a utilization and treatment method of gluconolactone high-salt ion exchange wastewater.
Background
In the production of gluconolactone, the used raw material is sodium gluconate, ion exchange is needed in the process of converting the sodium gluconate into the gluconolactone, and the resin needs to be regenerated after the ion exchange. Generally, the regenerant is dilute sulfuric acid and hydrochloric acid, the regenerated resin needs to be washed, the water after washing contains 5% of sodium sulfate, 0.5% of gluconolactone and pH of 1-6, and biochemical treatment is directly carried out through an A/O system, so that anaerobic and aerobic bacteria cannot survive, and a sewage treatment system cannot operate. The existing method for treating gluconolactone mainly comprises the steps of adjusting the pH to 7.5-8.0 by using sodium hydroxide, then adding calcium chloride, and controlling the concentration of sulfate ions to be 5000 ppm. After filtering, entering an A/O system for biochemical treatment, discharging after reaching the standard, adding water for dilution once in the treatment process, and entering the A/O system for biochemical treatment after diluting to the conductivity of less than or equal to 4000 mus/cm. And the other method is that the pH value of the sewage is adjusted to 7-8 by using sodium hydroxide, then the sewage is concentrated and crystallized, and sodium sulfate crystals are separated. However, the process has high investment and operation cost, and the sodium sulfate obtained by separation has low market price, so the overall benefit is extremely poor. The first process is generally adopted for the current stage of sewage treatment.
Disclosure of Invention
Aiming at the problems of high treatment cost of the gluconolactone production wastewater and the like in the prior art, the invention provides a utilization and treatment method of the gluconolactone high-salt ion exchange wastewater, so as to solve the problems. The method comprehensively utilizes sewage resources, cancels the addition of sodium hydroxide to adjust the pH value in the prior art, produces sodium hydroxide through double decomposition reaction to adjust the low-pH wastewater of enterprises, effectively removes sulfate ions, reduces the pressure of sewage treatment, and simultaneously reduces the sewage treatment cost.
The technical scheme of the invention is as follows:
a utilization and treatment method of gluconolactone high-salt ion exchange wastewater comprises the following steps:
(1) collecting high-salt ion exchange wastewater with pH less than or equal to 5;
(2) carrying out decoloring treatment on the high-salinity wastewater collected in the step (1);
(3) after the high-salinity wastewater decolorized in the step (2) is collected, adding calcium oxide or calcium hydroxide or a mixture of the calcium oxide and the calcium hydroxide into the high-salinity wastewater decolorized for reaction;
(4) performing suction filtration on the material reacted in the step (3) by using a vacuum belt filter, and installing four paths of washing water above filter cloth of the vacuum belt filter for washing;
(5) adding the filter cake obtained in the step (4) into a dissolving tank, adding water, and stirring at a rotating speed of 40-60 revolutions per minute;
(6) performing suction filtration on the crystal slurry obtained in the step (5) through a vacuum belt filter again, installing four paths of washing water above filter cloth of the vacuum belt filter for washing to obtain a filter cake and filtrate, and combining and mixing the obtained filtrate with the filtrate obtained in the step (4);
(7) drying the filter cake obtained in the step (6) in airflow;
(8) drying the airflow dried calcium sulfate obtained in the step (7) in a fluidized bed furnace to obtain semi-hydrated gypsum;
(9) packaging the semi-hydrated gypsum obtained in the step (8) to obtain finished gypsum powder;
(10) and (3) adding the filtrate obtained in the step (6) into low-pH condensed water generated by the triple-effect concentration of the gluconolactone, adjusting the pH of the condensed water to 6-9, then carrying out A/O sewage biochemical treatment (anaerobic-aerobic process), and discharging after reaching the standard.
Preferably, in the step (2), the decolorizing agent is selected from activated carbon, granular carbon or carbon fiber.
Preferably, in the step (2), the decoloring temperature is 40-70 ℃, and the decoloring time is 0.5-2 h.
Preferably, in the step (3), the mesh number of the calcium oxide is 200-300 meshes. When the mesh number of the used calcium oxide is small, the generated calcium sulfate is easy to attach to the surface of the granular calcium oxide when the granular calcium oxide reacts with wastewater, and the calcium oxide is coated, so that the prepared calcium sulfate contains calcium oxide or calcium hydroxide, and the purity of the recovered calcium sulfate is influenced.
Preferably, in the step (3), the reaction temperature is 50-80 ℃, the stirring speed is 40-80 r/min, and the reaction time is 1-5 h.
Preferably, in the step (3), after calcium oxide and/or calcium hydroxide are added, the reaction pH of the high-salinity wastewater is 6-14.
Preferably, in the step (5), the water addition amount is 0.2-0.5 kg/kg based on the weight of the filter cake.
Preferably, in the step (7), the temperature of the drying gas is 80-120 ℃, and the moisture of the dried calcium sulfate is 17-28%.
Preferably, in the step (8), the air temperature at the bottom of the fluidized bed furnace is controlled to be 135-145 ℃, the material retention time is 2 hours, and the water content is controlled to be 5-6.2%.
The invention has the beneficial effects that:
(1) according to the method, calcium sulfate is formed by the neutralization reaction of calcium oxide and sulfuric acid in the wastewater, the calcium sulfate is removed, and then excessive calcium oxide is added to react with sodium sulfate in the wastewater to form calcium sulfate and sodium hydroxide, so that sulfate radicals are further removed. The gluconic acid solution concentration is concentrated from 35% to 70%, and a triple effect evaporator is adopted, so that a large amount of wastewater with the pH value of 3-5 is generated. Because the filtrate remained after removing the sulfate radicals contains a large amount of sodium hydroxide, the low-pH material condensed water generated by the triple-effect evaporator is treated. Replaces the commercial sodium hydroxide used in the original treatment process, and reduces the sewage treatment cost.
(2) According to the invention, calcium oxide and sulfuric acid in wastewater are subjected to neutralization reaction to form calcium sulfate, the calcium sulfate is removed, excess calcium oxide is added to react with sodium sulfate in the wastewater to form calcium sulfate and sodium hydroxide, the excess calcium oxide replaces calcium chloride added in the original process, so that a large amount of sodium chloride is avoided, the formed high-salinity wastewater causes difficulty in sewage treatment, a large amount of primary water is added to dilute the wastewater, then the sewage treatment is carried out, and meanwhile, the unit price of the calcium hydroxide is lower than that of the calcium chloride, so that the sewage treatment cost is reduced.
(3) The formed calcium sulfate is deeply processed to produce building gypsum, the added value of the calcium sulfate is improved, the environmental protection risk of enterprises is reduced, and the aim of changing waste into valuables is fulfilled.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A utilization and treatment method of gluconolactone high-salt ion exchange wastewater comprises the following steps:
(1) collecting 201m of wastewater with pH less than or equal to 5 by interlocking an ion exchange wastewater pH meter with an automatic valve3(ii) a Wherein SO4 2-The content was 3.5g/100 ml.
(2) Heating the wastewater to 65 ℃, adding 40.2kg of powdered activated carbon, adding 20.2kg of diatomite, stirring at the rotating speed of 60 revolutions per minute for 30min, filtering by a plate frame,
(3) putting the clear solution into a tank, wherein the pH is 3.2, and SO4 2-The content is 3.4g/100 dL; stirring for 60 r/min, slowly adding powdered calcium oxide for 3.51t, adjusting pH of the solution to 13, maintaining for 60min, and fine-adjusting pH to 13.8 with 0.2t calcium hydroxide.
(4) Pumping the feed liquid obtained in the step (3) into a vacuum belt filter for filtering, wherein the vacuum degree is less than or equal to-0.085 Mpa, the water pressure is 0.25Mpa, washing water is used for four ways, filtrate is separately collected, and a filter cake is added into a calcium sulfate dissolving tank. At this time, SO was contained in the filtrate4 2-The content is 0.35g/100 ml.
(5) Sulfuric acidDissolving calcium, adding water 12m into calcium sulfate dissolving tank3Stirring for 40 r/min, automatically adding the filter cake of the belt filter into a calcium sulfate dissolving tank, and stirring for 1h after the calcium sulfate filter cake is completely fed.
(6) Pumping the feed liquid treated by the calcium sulfate dissolving tank into a vacuum belt filter, wherein the filtering temperature is as follows: 75 ℃, feeding amount: 20m3H, vacuum degree less than or equal to-0.085 Mpa, water pressure 0.25Mpa, four-way washing water, total washing water amount of 10.5m3And (4) combining the filtrate with the filtrate in the step (4) after separately collecting the filtrate, and transporting the filter cake to an air flow drying inlet through a flood dragon.
(7) Drying the washed calcium sulfate in airflow, wherein the feeding amount is 2t per hour, the temperature of the drying gas is 120 ℃, the drying time is 25s, and the feeding amount is measured as follows: 26.35t, the discharge amount is 10.31t, and the water content is 17.3%.
(8) Transporting the calcium sulfate dried in the step (7) to a feed inlet of a fluidized bed furnace through a flood dragon, controlling the feeding flow to be 1.5t/h, controlling the air temperature at the bottom of the fluidized bed furnace to be 140 ℃, controlling the material detention time to be 2h, discharging to obtain semi-hydrated gypsum, and measuring the product discharging: 9.025t, 5.5% moisture was detected by sampling.
The produced gypsum is detected, and the national standard GB/T9776-2008 is met.
(9) Combining the filtrates in the steps (4) and (6), measuring the pH value to be 13.58, measuring the pH value of the gluconolactone triple-effect concentrated condensed water to be 3.2, adjusting the pH value of the condensed water to be 7.9 by using the filtrate, and measuring the indexes of the waste water as follows: COD: 4800ppm, sulfate: 2500ppm, the sewage enters an A/O system for biochemical treatment (anaerobic-aerobic process method), and the system normally operates.
The invention can recover 9.025t of hemihydrate gypsum every day, the water content is 5.5 percent, and the actual calcium sulfate content is 9.025 x (1-5.5 percent) which is 8.52 t. The amount of sulfate radical contained in the treated wastewater is as follows: (3.4-0.35) × 10 × 1000 × 201 ≈ 6130500g ≈ 6.13t, and when the conversion is 8.68t to calcium sulfate, the recovery rate of calcium sulfate is 8.52 ÷ 8.68 × 100% ═ 98.3%. The complete recovery of sulfate radical is basically realized.
Comparative example
Adopts the existing high-salt ion exchange wastewater treatment method to treat 201m3The wastewater is treated. Firstly adding sodium hydroxide to adjust the pH value to 7.5-8And 0, then adding calcium chloride, controlling the concentration of sulfate ions to be less than or equal to 5000ppm, and feeding the filtered filtrate into an A/O system for biochemical treatment.
Compared with the benefit aspect, the raw material cost of the wastewater treatment method is about 9.5 yuan per ton of wastewater treated. The original treatment method has the raw material cost of about 25 yuan per ton of waste water. The treatment method reduces the cost of raw materials by 60 percent
Although the present invention has been described in detail by referring to the drawings in connection with the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A method for utilizing and treating gluconolactone high-salt ion exchange wastewater is characterized by comprising the following steps:
(1) collecting high-salt ion exchange wastewater with pH less than or equal to 5;
(2) carrying out decoloring treatment on the high-salinity wastewater collected in the step (1);
(3) after the high-salinity wastewater decolorized in the step (2) is collected, adding calcium oxide and/or calcium hydroxide into the high-salinity wastewater decolorized for reaction;
(4) performing suction filtration on the material reacted in the step (3) by using a vacuum belt filter, and installing four paths of washing water above filter cloth of the vacuum belt filter for washing;
(5) adding the filter cake obtained in the step (4) into a dissolving tank, adding water, and stirring at a rotating speed of 40-60 revolutions per minute;
(6) performing suction filtration on the crystal slurry obtained in the step (5) through a vacuum belt filter again, installing four paths of washing water above filter cloth of the vacuum belt filter for washing to obtain a filter cake and filtrate, and combining and mixing the obtained filtrate with the filtrate obtained in the step (4);
(7) drying the filter cake obtained in the step (6) in airflow;
(8) drying the airflow dried calcium sulfate obtained in the step (7) in a fluidized bed furnace to obtain semi-hydrated gypsum;
(9) packaging the semi-hydrated gypsum obtained in the step (8) to obtain finished gypsum powder;
(10) and (3) adding the filtrate obtained in the step (6) into low-pH condensed water generated by the triple-effect concentration of the gluconolactone, adjusting the pH of the condensed water to 6-9, then carrying out A/O sewage biochemical treatment, and discharging after reaching the standard.
2. The method for utilizing and treating gluconolactone high-salt ion exchange wastewater as claimed in claim 1, wherein in the step (2), the decolorizing agent is selected from activated carbon, granular carbon or carbon fiber.
3. The utilization and treatment method of gluconolactone high-salt ion exchange wastewater as claimed in claim 1, wherein in the step (2), the decolorizing temperature is 40-70 ℃ and the decolorizing time is 0.5-2 h.
4. The method for utilizing and treating gluconolactone high-salt ion exchange wastewater according to claim 1, wherein the mesh number of calcium oxide in the step (3) is 200-300 meshes.
5. The utilization and treatment method of gluconolactone high-salt ion exchange wastewater according to claim 1, wherein in the step (3), the reaction temperature is 50-80 ℃, the stirring speed is 40-80 r/min, and the reaction time is 1-5 h.
6. The utilization and treatment method of gluconolactone high-salt ion exchange wastewater as claimed in claim 1, wherein in the step (3), after calcium oxide and/or calcium hydroxide is added, the reaction pH of the high-salt wastewater is 6-14.
7. The method for utilizing and treating gluconolactone high-salt ion exchange wastewater as claimed in claim 1, wherein the water addition amount in the step (5) is 0.2-0.5 kg/kg based on the weight of the filter cake.
8. The utilization and treatment method of gluconolactone high-salt ion exchange wastewater according to claim 1, wherein in the step (7), the temperature of the drying gas is 80-120 ℃, and the moisture of the dried calcium sulfate is 17-28%.
9. The utilization and treatment method of gluconolactone high-salt ion exchange wastewater as claimed in claim 1, wherein in the step (8), the air temperature at the bottom of the fluidized bed furnace is controlled to be 135-145 ℃, the material retention time is 2h, and the water content is controlled to be 5-6.2%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1532149A (en) * | 2003-03-18 | 2004-09-29 | 李晓里 | Utilizing method for waste sulfuric radical |
| CN1884173A (en) * | 2005-06-24 | 2006-12-27 | 王嘉兴 | Method for combined production of gypsum, active carbon, and copperas by using waste sulfuric acid and carbide slag |
| CN109205921A (en) * | 2017-06-29 | 2019-01-15 | 开封市隆兴化工有限公司 | Align treatment method for high-salinity wastewater in ester production process |
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- 2021-09-01 CN CN202111021913.8A patent/CN113698038A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1532149A (en) * | 2003-03-18 | 2004-09-29 | 李晓里 | Utilizing method for waste sulfuric radical |
| CN1884173A (en) * | 2005-06-24 | 2006-12-27 | 王嘉兴 | Method for combined production of gypsum, active carbon, and copperas by using waste sulfuric acid and carbide slag |
| CN109205921A (en) * | 2017-06-29 | 2019-01-15 | 开封市隆兴化工有限公司 | Align treatment method for high-salinity wastewater in ester production process |
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