CN103288240B - High-purity barium hydroxide production wastewater recycling technology and equipment - Google Patents
High-purity barium hydroxide production wastewater recycling technology and equipment Download PDFInfo
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Abstract
The invention relates to a high-purity barium hydroxide production wastewater recycling technology and equipment. The equipment is characterized in that an outlet of a barium hydroxide reactor is connected with a separator; the wastewater outlet of the separator is connected with a barium chloride reactor through a pipeline; a discharge pipe of the barium chloride reactor is connected with a filter; a liquid outlet pipe of the filter is connected with an alkaline liquor reactor; the discharge pipe of the alkaline liquor reactor is connected with a centrifugal machine; the centrifugal machine is provided with a finished product discharge pipe and a mother liquid discharge pipe; and the mother liquid discharge pipe is connected with the separator, wherein an acid inlet, a barium carbonate inlet, a barium carbonate inlet and a tap water inlet are also formed in the barium chloride reactor, an exhaust gas outlet is also formed in the top end of the barium chloride reactor and is connected with a wastewater outlet pipeline of the separator through an elbow. By utilizing the technology, barium ions in the wastewater can be fully recycled and are utilized to re-prepare high-purity barium hydroxide, so that resource recycling is realized, the environmental pollution is greatly reduced, resource consumption is reduced, the production cost is lowered, and the technology has a better economic benefit and a better environmental benefit.
Description
Technical field
The present invention relates to technical field of waste water processing in the barytic production of High Purity Hydrogen, be specifically related to utilization process and the equipment of waste water in a kind of High Purity Hydrogen barium oxide production.
Background technology
Hydrated barta is an important kind in barium salt, be widely used in sewage purification, it in water treatment field, is effective remover of carbonic acid gas and sulfate ion, at medicine, plastics, glass, pottery, it in electron trade, is also necessary chemical, can be used for manufacturing organic barium compound, barium based grease, also for refining animals and plants oils, sucrose, beet, also for stabilizer for plastics, additive for paper making, sealing component, vulcanization of rubber catalyzer, anti-tarnish paper component, coating dispersant, polyurethane foam foam extinguishing agent, silk and artificial silk treatment agent, boiler Ethylene Diaminetetra Acetic Acid and neutralizing agent, glass is warded off the industrial raw material as production glass and enamel etc., along with the developing of the new purposes of hydrated barta, hydrated barta market demand increases year by year.Because German and Italian barium resource have been tending towards exhausted, so China is transferred in the main place of production of global hydrated barta gradually.
Hydrated barta product main raw material is barium resource, and the explored barite deposit in the whole world (major ingredient: BaSO4) reserves have 2,000,000,000 T, and the reserves of China approximately 900,000,000 T, account for 45% of global total reserves, are mainly distributed in the provinces such as Hubei, Shaanxi, Hunan.Witherite mineral's (major ingredient: BaCO3) is rare mineral, China has verified witherite mineral's reserves 3,800 ten thousand T, ore bed is stable, the BaCO3 of the witherite mineral content of exploiting out is 65%～75%, through the exploitation of more than ten years, ore deposit grade is reduced year by year trend, and the production cost of hydrated barta is constantly raise, You Ji family enterprise because of production cost high in end-of-life state.
Tradition hydrated barta industrialized producing technology has two kinds:
1, adopt and first barium sulphide and hydrochloric acid reaction are made to bariumchloride, then carry out replacement(metathesis)reaction with sodium hydroxide.Through crystallisation by cooling, after separating, washing, packing is finished product.
For guaranteeing well carrying out of reaction, reaction need be carried out under comparatively high temps He under excessive sodium hydrate condition.
This method advantage: flow process is short, simple to operate.
This method shortcoming: production cost is high, raw material availability is only 70%, and resource utilization is low, and chloride containing barium, hydrated barta, sodium-chlor, sodium hydroxide in crystalline mother solution reclaim difficulty, usually used as waste water, directly drain.
2, adopt witherite under isolated air conditions, under 1400 ℃ of high temperature, react with carbon, produce barium oxide, the reaction of reusable heat water soaking, separation, concentrated, crystallization, make hydrated barta.
This method advantage: flow process is short, simple to operate.
This method shortcoming:
1. production cost is high, and ingredient requirement witherite quality is good, but the heavy Mineral resources of high-quality poison are increasingly exhausted at present, and raw materials technology utilization ratio is only 50% simultaneously, and resource utilization is low;
2. the pyroreaction time long, energy consumption is large, 1400 ℃ of pyroreaction time remainings just can complete for tens hours.
3. the pincers alms bowl life cycle only 2-3 time of splendid attire reaction mass, cost is high, and waste water is directly drained, and is difficult to reclaim the barium in waste water.
The patent of invention that a name is called " processing method of combination producing hydrated barta and manganous sulfate " is disclosed in CN1202013C, the main method of this patent is: (1) is by solid barium sulphide water-soluble barium sulfide solution that obtains at 60 ℃～85 ℃ temperature, then cooling, obtain hydrated barta and barium sulphide crystalline mixture, filter, obtain product hydrated barta crystal, wash and wash away barium sulphide 1～3 time, washings returns to use.(2) in filtrate, add Manganse Dioxide, make Ba(HS in itself and solution)
2reaction generates MnO precipitation with BaS.(3) filter, obtain MnO washing 1～3 time, remove Ba
2+, HS
2+, S
2+after ion, MnO dissolves in sulfuric acid again; Remove by filter S, obtain manganese sulfate solution; Described sulfuric acid is 6mol/L.(4) concentrated vitriol manganese solution, cooling, crystallization, obtain manganous sulfate crystal.(5), by the filtrate of (3), concentrated, crystallisation by cooling, obtains hydrated barta crystal.
The weak point that this patent of invention exists is: in actual production, the hydrated barta making described in its step (1) cannot reach national correlated quality standard, cannot make qualified product.Its reason is: the cocrystallization mixture that the hydrated barta making contains hydrated barta and barium sulphide, method by washing, recrystallization all cannot be removed barium sulphide, thereby in prepared hydrated barta product, sulphur content is too high, causes in process of production, a large amount of raw-material wastes.In addition, the waste water such as filtrate, concentrated solution are directly drained, and cannot recycle the barium in waste water.
The patent of invention that a name is called " a kind of preparation method of hydrated barta " is disclosed in CN1962451C, the principal feature of this patent is: first barium sulfide solution is mixed with to required concentration, temperature, by Manganse Dioxide oxidation of sulfureted barium, make barium hydroxide solution again, barium hydroxide solution makes finished product barium hydroxide through concentrated, crystallisation by cooling.In process, after Manganse Dioxide oxidation of sulfureted barium, become manganese monoxide at a low price, manganese monoxide changes into Manganse Dioxide by atmospheric oxygen again, is cycled to used in the oxidation of barium sulphide, and Manganse Dioxide only plays intermediation, takes away part consumption while only separating sulphur.This scheme method is simple, it is clean, with low cost to produce, and Manganse Dioxide recycles, and consumption is very little, but there is no equally wastewater treatment link, the waste water of link such as filters, concentrated and directly drains, and cannot fully reclaim barium ion wherein.
Approximately 30,000 tons of China's hydrated barta annual production, the barytic market share of High Purity Hydrogen is increasing, and High Purity Hydrogen barium oxide produces a large amount of waste water in producing, barium ion wherein cannot be fully recycled, mostly directly drain, increased environmental pollution, cause the wasting of resources.
Summary of the invention
For the existing deficiency of prior art, the present invention proposes utilization process and the equipment of waste water in a kind of High Purity Hydrogen barium oxide production, this technique has fully been recycled barium ion in waste water, again be prepared as High Purity Hydrogen barium oxide, realize the recycle of resource, greatly reduced environmental pollution, reduced resource consumption, reduce production cost, there is good economic benefit and environmental benefit.
In a kind of High Purity Hydrogen barium oxide production of the present invention, utilization process and the equipment of waste water are achieved by the following technical measures:
The recycling device of waste water in a kind of High Purity Hydrogen barium oxide production, its feature is that the outlet of hydrated barta reactor connects separator, separator wastewater outlet connects bariumchloride reactor by pipeline, bariumchloride reactor discharge nozzle connects strainer, strainer drain pipe connects alkaline reaction still, alkaline reaction still discharge nozzle connects whizzer, whizzer is provided with finished product discharge nozzle and mother liquor discharge nozzle, mother liquor discharge nozzle connects separator, wherein in bariumchloride reactor, be provided with agitator, on bariumchloride reactor, be also provided with sour entrance, sodium bicarbonate entrance, barium carbonate entrance, tap water entrance, dilute hydrochloric acid tank is connected with bariumchloride reactor acid entrance by acid tube, and hydrochloride buffer tank, concentrated hydrochloric acid tank, graphite hydrochloric acid dilution water cooler, dilute hydrochloric acid tank is connected in series successively, sodium bicarbonate entrance connects sodium bicarbonate storing pump, wherein the top of bariumchloride reactor is also provided with a waste gas outlet, waste gas outlet connects separator wastewater outlet pipeline by a bend pipe.
Waterwater entrance pipeline on the above bariumchloride reactor is extended into be bent downwardly by sidewall and extends to agitator one side, and sour inlet duct is located at waterwater entrance pipeline bottom, parallel with waterwater entrance pipeline.Waterwater entrance pipeline on described bariumchloride reactor and sour inlet duct, around the circumferential wall setting of reactor, are provided with 1～5 group.
Above-described waste gas outlet bend pipe extends into separator wastewater outlet pipeline.
In the above strainer, have filter screen, screen specification is 300 orders.
The utilization process of waste water in a kind of High Purity Hydrogen barium oxide production, its processing step is as follows: the separator of the barytic waste water of production High Purity Hydrogen after by hydrated barta reactor separates, waste water is pumped into bariumchloride reactor, simultaneously to waste water in mass ratio in bariumchloride reactor: sodium bicarbonate is 7:0.1～0.2, add sodium bicarbonate, agitator stirs after 5～10min, tap water in mass ratio: hydrochloric acid: barium carbonate is that 4～5:0.5～1:1.8～2.5 pump into tap water, hydrochloric acid and barium carbonate, agitator stirs 10～30min, exporting strainer to filters, filtrate pumps into alkaline reaction still, filtrate in mass ratio: alkali lye is that 15～20:8～15 add alkali lye, stirring reaction 5～20min, be discharged to whizzer centrifugal, centrifugal mother liquor out pumps into separator by mother liquor discharge nozzle, High Purity Hydrogen barium oxide finished product is by the discharging of finished product discharge nozzle.
The stir speed (S.S.) of the above agitator is 50～300rpm.
Above-described centrifuge speed is 1000 revs/min.
Above-described alkali lye is sodium hydroxide.
Useful technique effect of the present invention is:
High Purity Hydrogen barium oxide produces a large amount of waste water in producing, the a set of sewage treatment equipment of our designed, designed, by to adding hydrochloric acid in waste water, sodium bicarbonate is produced 20% barium chloride solution supply chlor-alkali plant use, the barium chloride solution that chlor-alkali plant was used is in the past all the solution of oneself buying bariumchloride modulation 20%, cause like this cost up, the solution that chlor-alkali plant is produced with our hydrated barta waste water now, reduce costs more than 50%, and our waste water has also obtained fine recycling, so both created good economic benefit, also reduced environmental pollution simultaneously, kill two birds with one stone.Can continue in addition to add alkali lye to process waste water, make it regenerate High Purity Hydrogen barium oxide finished product, reduced production cost, after centrifugal, wastewater mother liquor out again pumps into separator processing and does barium carbonate, realized the recycle of waste water, the zero release of waste water, has fundamentally avoided environmental pollution.
Our waste water treatment process equipment is reasonable in design in addition, makes wastewater treatment realize serialization, has improved waste water treatment efficiency; Bariumchloride reactor is provided with carbon dioxide recovery bend pipe, and bend pipe passes into separator rising pipe, utilizes wastewater mother liquor to reclaim carbonic acid gas, realizes carbon dioxide and recycles, and realizes carbon dioxide zero release; Wastewater inlet pipe on bariumchloride reactor and acid inlet tube are set up in parallel on still wall circumference, go deep into tank body and agitator with neat, make waste water and sour short mix even, fully reaction, many groups arrange in addition, can gather the waste water of different location simultaneously, and guarantee the continuity to wastewater treatment in bariumchloride reactor.
As can be seen here, the present invention compared with prior art, has substantive distinguishing features and progress, and the beneficial effect of its enforcement is also apparent.
figure of description
Fig. 1 is the utilization process of waste water and the schematic flow sheet of equipment during a kind of High Purity Hydrogen barium oxide of the present invention is produced, wherein 1 is hydrated barta reactor, 2 is separator, 3 is hydrochloride buffer tank, 4 is concentrated hydrochloric acid tank, 5 is graphite hydrochloric acid dilution water cooler, 6 is dilute hydrochloric acid tank, 7 is sodium bicarbonate storing pump, 8 is strainer, 9 is alkaline reaction still, 10 is whizzer, 11 is waste gas outlet, 12 is bend pipe, 13 is waterwater entrance, 14 is sour entrance, 15 is agitator, 16 is sodium bicarbonate entrance, 17 is bariumchloride reactor, 18 is mother liquor discharge nozzle, 19 is finished product discharge nozzle, 20 is barium carbonate entrance, 21 is tap water entrance.
Embodiment
For clearly demonstrating the present invention program's technical characterstic, below in conjunction with specific embodiment, the present invention is further elaborated.
As shown in Figure 1, the recycling device of waste water in a kind of High Purity Hydrogen barium oxide production, its feature is that 1 outlet of hydrated barta reactor connects separator 2, separator 2 wastewater outlets connect bariumchloride reactor 17 by pipeline, bariumchloride reactor 17 discharge nozzles connect strainer 8, strainer 8 drain pipes connect alkaline reaction still 9, alkaline reaction still 9 discharge nozzles connect whizzer 10, whizzer 10 is provided with finished product discharge nozzle 19 and mother liquor discharge nozzle 18, mother liquor discharge nozzle 18 connects separator 2, wherein in bariumchloride reactor 17, be provided with agitator 15, on bariumchloride reactor 17, be also provided with sour entrance 14, sodium bicarbonate entrance 16, barium carbonate entrance 20, tap water entrance 21, dilute hydrochloric acid tank 6 is connected by the sour entrance 14 of acid tube and bariumchloride reactor 17, hydrochloride buffer tank 3, concentrated hydrochloric acid tank 4, graphite hydrochloric acid dilution water cooler 5, dilute hydrochloric acid tank 6 is connected in series successively, sodium bicarbonate entrance 16 connects sodium bicarbonate storing pump 7, wherein the top of bariumchloride reactor 17 is also provided with a waste gas outlet 11, waste gas outlet 11 connects separator 2 wastewater outlet pipelines by a bend pipe 12.
The pipeline of the waterwater entrance 13 on the above bariumchloride reactor 17 is extended into be bent downwardly by sidewall and extends to agitator 15 1 sides, and sour entrance 14 pipelines are located at waterwater entrance 13 pipeline bottoms, parallel with waterwater entrance 13 pipelines.
Above-described waste gas outlet 11 bend pipes extend into separator 2 wastewater outlet pipelines.
In the above strainer 8, have filter screen, screen specification is 300 orders.
Embodiment 1: the separator of the barytic waste water of production High Purity Hydrogen after by hydrated barta reactor separates, waste water is pumped into bariumchloride reactor, simultaneously to waste water in mass ratio in bariumchloride reactor: sodium bicarbonate is 7:0.1, add sodium bicarbonate, after agitator stirs 5, tap water in mass ratio: hydrochloric acid: barium carbonate is that 4:0.5:1.8 pumps into tap water, hydrochloric acid and barium carbonate, agitator stirs 10min, exporting strainer to filters, filtrate pumps into alkaline reaction still, filtrate in mass ratio: sodium hydroxide is that 15:8 adds sodium hydroxide, stirring reaction 5min, be discharged to whizzer centrifugal, centrifugal mother liquor out pumps into separator by mother liquor discharge nozzle, High Purity Hydrogen barium oxide finished product is by the discharging of finished product discharge nozzle.
The stir speed (S.S.) of the above agitator is 50rpm.
Above-described centrifuge speed is 1000 revs/min.
Embodiment 2: the separator of the barytic waste water of production High Purity Hydrogen after by hydrated barta reactor separates, waste water is pumped into bariumchloride reactor, simultaneously to waste water in mass ratio in bariumchloride reactor: sodium bicarbonate is 7:0.2, add sodium bicarbonate, agitator stirs after 10min, tap water in mass ratio: hydrochloric acid: barium carbonate is that 5:1:2.5 pumps into tap water, hydrochloric acid and barium carbonate, agitator stirs 30min, exporting strainer to filters, filtrate pumps into alkaline reaction still, filtrate in mass ratio: sodium hydroxide is that 20:15 adds sodium hydroxide, stirring reaction 20min, be discharged to whizzer centrifugal, centrifugal mother liquor out pumps into separator by mother liquor discharge nozzle, High Purity Hydrogen barium oxide finished product is by the discharging of finished product discharge nozzle.
The stir speed (S.S.) of the above agitator is 300rpm.
Above-described centrifuge speed is 1000 revs/min.
Embodiment 3: the separator of the barytic waste water of High Purity Hydrogen after by hydrated barta reactor separates, waste water is pumped into bariumchloride reactor, simultaneously to waste water in mass ratio in bariumchloride reactor: sodium bicarbonate is 7:0.14, add sodium bicarbonate, agitator stirs after 8min, tap water in mass ratio: hydrochloric acid: barium carbonate is that 4.5:0.6:2 pumps into tap water, hydrochloric acid and barium carbonate, agitator stirs 25min, exporting strainer to filters, filtrate pumps into alkaline reaction still, filtrate in mass ratio: sodium hydroxide is that 20:10 adds sodium hydroxide, stirring reaction 10min, be discharged to whizzer centrifugal, centrifugal mother liquor out pumps into separator by mother liquor discharge nozzle, High Purity Hydrogen barium oxide finished product is by the discharging of finished product discharge nozzle.
The stir speed (S.S.) of the above agitator is 50～300rpm.
Above-described centrifuge speed is 1000 revs/min.
We utilize in above processing step and the production of device processes High Purity Hydrogen barium oxide and produce a large amount of waste water, to waste water, adding hydrochloric acid, sodium bicarbonate produces 20% barium chloride solution and supplies with chlor-alkali plant and use, the barium chloride solution that before comparing, chlor-alkali plant is used is all the solution of oneself buying bariumchloride modulation 20%, the solution that chlor-alkali plant is produced with our hydrated barta waste water now, reduces costs more than 50%.Continue to add sodium hydroxide lye to process waste water, make it regenerate High Purity Hydrogen barium oxide finished product, reduced production cost, after centrifugal, wastewater mother liquor out again pumps into separator processing and does barium carbonate, realized the recycle of waste water, the zero release of waste water, has fundamentally avoided environmental pollution.
Claims (9)
1. the recycling device of waste water in a High Purity Hydrogen barium oxide production, it is characterized in that: the outlet of hydrated barta reactor connects separator, separator wastewater outlet connects bariumchloride reactor by pipeline, bariumchloride reactor discharge nozzle connects strainer, strainer drain pipe connects alkaline reaction still, alkaline reaction still discharge nozzle connects whizzer, whizzer is provided with finished product discharge nozzle and mother liquor discharge nozzle, mother liquor discharge nozzle connects separator, wherein in bariumchloride reactor, be provided with agitator, on bariumchloride reactor, be also provided with sour entrance, sodium bicarbonate entrance, barium carbonate entrance, tap water entrance, dilute hydrochloric acid tank is connected with bariumchloride reactor acid entrance by acid tube, and hydrochloride buffer tank, concentrated hydrochloric acid tank, graphite hydrochloric acid dilution water cooler, dilute hydrochloric acid tank is connected in series successively, sodium bicarbonate entrance connects sodium bicarbonate storing pump, wherein the top of bariumchloride reactor is also provided with a waste gas outlet, waste gas outlet connects separator wastewater outlet pipeline by a bend pipe.
2. the recycling device of waste water in a kind of High Purity Hydrogen barium oxide production according to claim 1, it is characterized in that: the waterwater entrance pipeline on bariumchloride reactor is extended into be bent downwardly by sidewall and extends to agitator one side, acid inlet duct is located at waterwater entrance pipeline bottom, parallel with waterwater entrance pipeline.
3.
?in a kind of High Purity Hydrogen barium oxide production according to claim 2, the recycling device of waste water, is characterized in that: the waterwater entrance pipeline on described bariumchloride reactor and sour inlet duct, around the circumferential wall setting of reactor, are provided with 1～5 group.
4.
?in a kind of High Purity Hydrogen barium oxide production according to claim 1, the recycling device of waste water, is characterized in that: described waste gas outlet bend pipe extends into separator wastewater outlet pipeline.
5. the recycling device of waste water in a kind of High Purity Hydrogen barium oxide production according to claim 1, is characterized in that: in described strainer, have filter screen, screen specification is 300 orders.
6. the utilization process of waste water in a High Purity Hydrogen barium oxide production, it is characterized in that processing step is as follows: the separator of the barytic waste water of production High Purity Hydrogen after by hydrated barta reactor separates, waste water is pumped into bariumchloride reactor, simultaneously to waste water in mass ratio in bariumchloride reactor: sodium bicarbonate is 7:0.1～0.2, add sodium bicarbonate, agitator stirs after 5～10min, tap water in mass ratio: hydrochloric acid: barium carbonate is that 4～5:0.5～1:1.8～2.5 pump into tap water, hydrochloric acid and barium carbonate, agitator stirs 10～30min, exporting strainer to filters, filtrate pumps into alkaline reaction still, filtrate in mass ratio: alkali lye is that 15～20:8～15 add alkali lye, stirring reaction 5～20min, be discharged to whizzer centrifugal, centrifugal mother liquor out pumps into separator by mother liquor discharge nozzle, High Purity Hydrogen barium oxide finished product is by the discharging of finished product discharge nozzle.
7. the utilization process of waste water in a kind of High Purity Hydrogen barium oxide production according to claim 6, is characterized in that: the stir speed (S.S.) of described agitator is 50～300rpm.
8.
?in a kind of High Purity Hydrogen barium oxide production according to claim 6, the utilization process of waste water, is characterized in that: described centrifuge speed is 1000 revs/min.
9.
?in a kind of High Purity Hydrogen barium oxide production according to claim 6, the utilization process of waste water, is characterized in that: described alkali lye is sodium hydroxide.
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| C06 | Publication | ||
| PB01 | Publication | ||
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