CN101269797A - Vacuum concentration technique for dilute sulphuric acid containing high-solidification point organic matter - Google Patents
Vacuum concentration technique for dilute sulphuric acid containing high-solidification point organic matter Download PDFInfo
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- CN101269797A CN101269797A CNA2008100253349A CN200810025334A CN101269797A CN 101269797 A CN101269797 A CN 101269797A CN A2008100253349 A CNA2008100253349 A CN A2008100253349A CN 200810025334 A CN200810025334 A CN 200810025334A CN 101269797 A CN101269797 A CN 101269797A
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Abstract
The invention provides a vacuum concentration technics of dilute sulfuric acid containing high condensation point organic matters in connection with the deficiencies that when the condensation point of organic matters dissolved in the dilute sulfuric acid is high than 30 DEG C, the organic matters can be solidified in the temperature reduction process of a washing tower and a condenser to stop up a cold snap body channel or a heat exchange surface. The vacuum concentration technics is added with the high condensation point organic matters with 0.5-10 percent of raw material acid feed rate in the spray liquid of the washing tower, so the condensation point of the mixture is reduced because a plurality of organic matters are solidified at the same time in the condensation process, and the situation of solidification is avoided when the organic matters are solidified. The organic matters obtained by the condensation of the vacuum concentration technics return to a main device after separation, the mode is not increased with three wastes and well solves the problem that the organic matters are solidified to stop up the channel in the washing tower and the condenser at the same time, and the vacuum concentration technics obtains good effect in practical use.
Description
Technical field
The present invention relates to a kind of organic vacuum concentration technique for dilute sulphuric acid technology of high-solidification point (〉=30 ℃) that contains, solved the problem that the organism condensation after coagulation that carries in the sulfuric acid vapor stops up washing tower and condenser.
Background technology
Sulfuric acid is the base substance of chemical industry, and it is of many uses, and still, in most of purposes, exhausted sulfuric acid becomes impure dilute sulphuric acid.If the dilute sulphuric acid that produces does not deal with, will pollute the environment, become social effects of pollution.Past is often adopted processing modes such as doing gypsum, Tai-Ace S 150, even is used for producing phosphate fertilizer, along with the development of chemical industry and improving constantly of environmental requirement, these treatment processs can't meet the demands, dilute sulphuric acid is concentrated, get back to recycled in the production process, become the processing mode of main flow.Present state-of-the-art sulphuric acid concentration mode is exactly a vacuum concentration, this mode is compared with the obvious advantage with other modes, good operational environment at first, avoided the acid fume pollution fully, almost there is not three waste discharge, next has adopted the impregnating material of multiple superior performance, has avoided the frequent replacing behind the equipment corrosion, greatly reduces labour intensity; The 3rd concentration systems moves continuously, and operator are few, and energy consumption is low.But in some production processes, dissolved organism zero pour higher (〉=30 ℃) in the dilute sulphuric acid, in spray washing and condensation process, these organism can solidify, stop up fluid channel or heat-transfer surface, thereby the continuous operation of device is gone wrong.The measure that can only adopt the every operation of device just to stop and organism is melted in several hours at this problem at present with steaming out washing tower and condenser, this measure is wasted time and energy, and the operation of device impacted, be unfavorable for the stable of production process and operation continuously.
Summary of the invention
Purpose of the present invention then is at present above-mentioned the deficiencies in the prior art, and a kind of three wastes that do not increase are provided, and has solved the vacuum concentration technique for dilute sulphuric acid of organism frozen plug access issues in washing tower and condenser simultaneously well.
Technical scheme of the present invention is as follows:
A kind of vacuum concentration technique for dilute sulphuric acid that contains high-solidification point organic matter, its technological process is: the raw material acid that contains high-solidification point organic matter obtains finished acid through steaming after sour device heating evaporation concentrates, sulfuric acid vapor that wherein is evaporated and organism enter into washing tower and are absorbed by spray liquid, sulfuric acid vapor and the organism that is absorbed by spray liquid do not enter into the condenser condensation again, the liquid that uncooled sulfuric acid vapor waste gas and condensation obtain enters into gas-liquid separator again, vacuumize and take away thus the sulfuric acid vapor waste gas that enters into gas-liquid separator in the gas-liquid separator, the condensed liquid of sulfuric acid vapor then flows to the organism withdrawing can, phlegma reclaims through layering and obtains acid waste water and organism, acid waste water and organism return to generate participates in reaction in the raw material acid master's device that contains high-solidification point organic matter, it is characterized in that in the spray liquid of above-mentioned washing tower adding the organism of zero pour 〉=30 ℃ of raw material acid inlet amount 0.5～10%, this organism is a kind of in the organism composition that generates of the raw material that uses of above-mentioned main device or reaction.
Described condenser adopts board-like or spiral sheet condenser.
Described washing tower adopts the lass lining tower that the tetrafluoro filler is housed.
The organism of described zero pour 〉=30 ℃ is nitro-chlorobenzene, oil of mirbane, Benzene Chloride or nitrotoluene.
The present invention utilizes then depression of the freezing point this principle of organism purity decline, in the washing tower spray liquid, add and become owner of operating raw material of device or product, in condensation process because multiple organism mixes condensation simultaneously, its zero pour descends, the situation of having solidified when having avoided the organism condensation, the organism that condensation obtains returns main device again after separating, this mode does not increase the three wastes, well solve simultaneously the problem of organism frozen plug passage in Ta Nei and condenser, in practice, obtained good effect.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing the present invention is further described:
As shown in Figure 1, its technological process of the present invention is: the raw material acid that contains high-solidification point organic matter obtains finished acid through steaming after sour device heating evaporation concentrates, steam sour device and be thickener, its housing liner lass lining, (as China Patent No. is 02294114.2 to use bayonet formula tantalum pipe heater, name is called the structure of " a kind of sulfuric acid evaporator ") heating, simultaneously the thickener inner-use clapboard is separated into a plurality of concentration compartmentss, dilute sulphuric acid is mobile in proper order along the concentration compartmentss at different levels of thickener, concentration improves step by step, dividing plate in the concentration compartmentss at different levels has stoped the backflow of acid solution, guaranteed the maximum mean temperature difference between acid solution and the heating steam, make full use of the heating-surface area of tantalum tube-surface, thereby make the effusive sulfuric acid in last step concentration compartments reach aimed concn.Sulfuric acid vapor that is evaporated from steam sour device and organism enter into washing tower by the spray absorption in addition, and washing tower is the lass lining tower that the tetrafluoro filler is housed.The present invention adds the organism of zero pour 〉=30 ℃ of above-mentioned raw materials acid inlet amount 0.5～10% in the spray liquid of washing tower, this organism is one or more in the organism composition that generates of the raw material that uses of main device or reaction.Described organism specifically need satisfy following three conditions: 1, add-on is little; 2, the organic zero pour of mixing is descended obviously; 3, it is one of the raw material of main device or the composition in the product, and is recyclable to guarantee.Sulfuric acid vapor that is absorbed by spray liquid and organism do not enter into condenser again and are condensed, and condenser adopts board-like or spiral sheet condenser, and the liquid that uncooled sulfuric acid vapor waste gas and condensation obtain enters into gas-liquid separator again.Gas-liquid separator is a hollow tank body, its the upper end by pipe connection to vaccum-pumping equipment, take away the sulfuric acid vapor waste gas that enters into gas-liquid separator with vacuum mode, the condensed liquid of sulfuric acid vapor and organism then flows to the organism withdrawing can from the bottom of gas-liquid separator, obtain acid waste water and organism through the recovery of layering in the organism withdrawing can, acid waste water and organism return to generate in the raw material acid master's device that contains high-solidification point organic matter and recycle.
Below in conjunction with specific embodiment the organism that adds in the spray liquid of the present invention is described:
Embodiment 1: in the supporting sulphuric acid concentration device of nitro-chlorobenzene production equipment, dissolved para-nitrochloro-benzene in the dilute sulphuric acid, its zero pour is more than 80 ℃, in steaming sour device, carried by sulfuric acid vapor during heating and enter in washing tower and the condenser, by in the spray liquid of washing tower, adding the Benzene Chloride of raw material acid inlet amount 0.5%, effectively reduce organic zero pour, along with temperature reduces, the organism that from steam sour device, is evaporated not resolidification attached in washing tower filler and the condenser passages, thereby solved gas phase organism condensation after coagulation blocking problem, move more than half a year not blockage phenomenon continuously through single, satisfy the requirement of chemical plant installations long period maintenance fully.
Embodiment 2: in the supporting sulphuric acid concentration device of nitrotoluene production equipment, the nitrotoluene that adds raw material acid inlet amount 1% has solved organism and has solidified attached to the problem in washing tower filler and the condenser passages in the spray liquid of washing tower.
Embodiment 3: in the supporting sulphuric acid concentration device of dinitrotoluene (DNT) production equipment, the oil of mirbane that adds raw material acid inlet amount 5% has solved organism and has solidified attached to the problem in washing tower filler and the condenser passages in the spray liquid of washing tower.
Embodiment 4: in the supporting sulphuric acid concentration device of dinitrochlorobenzene production equipment, the Benzene Chloride that adds raw material acid inlet amount 7% has solved organism equally and has solidified attached to the problem in washing tower filler and the condenser passages in the spray liquid of washing tower.
Embodiment 5: in the supporting sulphuric acid concentration device of nitrophenol production equipment, the oil of mirbane that adds raw material acid inlet amount 10% has solved organism equally and has solidified attached to the problem in washing tower filler and the condenser passages in the spray liquid of washing tower.
The undeclared part of other that the present invention relates to is same as the prior art.
Claims (4)
1, a kind of vacuum concentration technique for dilute sulphuric acid that contains high-solidification point organic matter, its technological process is: the raw material acid that contains high-solidification point organic matter obtains finished acid through steaming after sour device heating evaporation concentrates, wherein the sulfuric acid vapor of evaporation generation and organism enter into washing tower by the spray liquid absorption under the cat head spray, sulfuric acid vapor that is absorbed by spray liquid and organism are not overflowed from cat head and are entered into condenser and be condensed, the liquid that uncooled sulfuric acid vapor waste gas and condensation obtain enters into gas-liquid separator again, vacuumize and take away thus the sulfuric acid vapor waste gas that enters into gas-liquid separator in the gas-liquid separator, the liquid that condensation obtains then flows to the organism withdrawing can, wherein contain a large amount of organism, obtain acid waste water and organism through the layering recovery, acid waste water that recovery obtains and organism are got back to respectively in the main device that generates the raw material acid that contains high-solidification point organic matter and are recycled, it is characterized in that in the spray liquid of above-mentioned washing tower adding the organism of zero pour 〉=30 ℃ of raw material acid inlet amount 0.5～10%, this organism is a kind of in the organism composition that generates of the raw material that uses of above-mentioned main device or reaction.
2, the vacuum concentration technique for dilute sulphuric acid that contains high-solidification point organic matter according to claim 1 is characterized in that described condenser adopts board-like or spiral sheet condenser.
3, the vacuum concentration technique for dilute sulphuric acid that contains high-solidification point organic matter according to claim 1 is characterized in that described washing tower adopts the lass lining tower that the tetrafluoro filler is housed.
4, the vacuum concentration technique for dilute sulphuric acid that contains high-solidification point organic matter according to claim 1 is characterized in that the organism of described zero pour 〉=30 ℃ is nitro-chlorobenzene, oil of mirbane, Benzene Chloride or nitrotoluene.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100253349A CN101269797A (en) | 2008-04-25 | 2008-04-25 | Vacuum concentration technique for dilute sulphuric acid containing high-solidification point organic matter |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109930010A (en) * | 2019-02-28 | 2019-06-25 | 昆明理工大学 | A method of organic matter in removing zinc hydrometallurgy solution |
| CN111773749A (en) * | 2020-07-13 | 2020-10-16 | 青岛海湾精细化工有限公司 | Vacuum concentration system for dilute sulfuric acid |
-
2008
- 2008-04-25 CN CNA2008100253349A patent/CN101269797A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109930010A (en) * | 2019-02-28 | 2019-06-25 | 昆明理工大学 | A method of organic matter in removing zinc hydrometallurgy solution |
| CN109930010B (en) * | 2019-02-28 | 2020-12-15 | 昆明理工大学 | Method for removing organic matters in zinc hydrometallurgy solution |
| CN111773749A (en) * | 2020-07-13 | 2020-10-16 | 青岛海湾精细化工有限公司 | Vacuum concentration system for dilute sulfuric acid |
| CN111773749B (en) * | 2020-07-13 | 2022-02-01 | 青岛海湾精细化工有限公司 | Vacuum concentration system for dilute sulfuric acid |
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Open date: 20080924 |