CN205170592U - A mother liquor processing system for clopyralid material separation is concentrated - Google Patents
A mother liquor processing system for clopyralid material separation is concentrated Download PDFInfo
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- CN205170592U CN205170592U CN201520958124.0U CN201520958124U CN205170592U CN 205170592 U CN205170592 U CN 205170592U CN 201520958124 U CN201520958124 U CN 201520958124U CN 205170592 U CN205170592 U CN 205170592U
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Abstract
The utility model discloses a mother liquor processing system for clopyralid material separation is concentrated, including first heavy jar, former water pitcher, reation kettle, gunbarrel, sand filtration tank, ultrafiltration filtration system and the superRO membrane ware that connects gradually to reach the evaporimeter of being connected with superRO membrane ware, wherein, clopyralid mother liquor raw water gets into just heavy jar, all is equipped with the doser on former water pitcher and the reation kettle, and just former water pitcher and reation kettle pass through the elevator pump intercommunication, the gunbarrel bottom is equipped with mud valve, sand filtration tank is equipped with the back flush pipe, and its recoil wash -out water end (W. E. ) and reation kettle intercommunication, ultrafiltration filtration system and reation kettle intercommunication. The utility model discloses characteristics to the clopyralid material design the improvement, soften earlier and filter through ultrafiltration and special reverse osmosis membrane except that hard again, and a small amount of dense water that will obtain at last evaporates the crystallization, reduces the evaporation cost, has also avoided the hot oxygen of whole in -process to act on the influence to the material, guarantees the mother liquor and retrieves the quality to can obviously reduce the energy consumption, thus the greatly reduced running cost.
Description
Technical field
The utility model relates to weeding agricultural chemicals and prepares mother liquid disposal field, and specifically, what relate to is a kind of mother liquid disposal system concentrated for clopyralid feed separation.
Background technology
Lontrel (3,6-DCP) (Bi Kecao) is a kind of novel nitrogen-containing weedicide, research and develop the nineties in last century, having unique texture, toxicity is low, activity is high, selectivity is good, environmentally friendly, is one of heterocyclic (pyridines) pesticide species in the ten large green novel pesticides endeavouring in the world at present to develop.
The main technique of current domestic production clopyralid has two kinds: one is chemical dechlorination method, with excessive hydrazine hydrate reduction 4 chloro pyridine formic acid in the aqueous solution of alkalescence, generate lontrel, this explained hereafter cost is low, but product yield is low, its the highest yield is 79%, product purity is also only 90%, and use violent in toxicity hydrazine hydrate due to a large amount of in technique, wastewater discharge is large, cause severe contamination as dealt with improperly by environment, current domestic and international most of producer still adopts the method to produce.
Another kind is electrochemical reducing, by being lontrel to the adjustment of electric current and voltage by 4 chloro pyridine formic acid electrolytic reduction in alkaline aqueous solution, this process stabilizing is reliable, production control only need control groove point source, product yield and quality are obviously high than chemical dechlorination method, the highest yield can reach 87%, product purity can reach more than 97%, not containing hydrazine hydrate in the mother liquor produced, composition is relatively simple, recycle more for convenience, to safety in production, protection of the environment is all highly beneficial, the method produces at present two pyridine carboxylic acids the most effectively and method the most advanced, but unique shortcoming that this method exists is that the product dichloropyridine acid content in the aqueous solution is lower, only have 4% ~ 6%, product separation recovery operation amount is large, need to adopt effective Separation and Recovery way.
Electrochemical reduction is produced to the method technique of clopyralid, after obtaining clopyralid dope, usually the feature that dichloropyridine acid solubility is low is utilized, adopt acid out technique, obtain most lontrel solid, but still containing part clopyralid in remaining mother liquor, separately due to production technique, also containing a large amount of salinities (mainly NaCl) in mother liquor.The COD of this mother liquor is higher, owing to also having pyridine structure in molecule, biodegradability is poor, the technique of multiple-effect evaporation is normally adopted to process mother liquor at present, thus reach decrement discharge object, but evaporation energy consumption is higher, investment and working cost high, the processing cost of mother liquor per ton is 150 yuan, higher concerning cost enterprise.
Membrane technique, due to its higher separation accuracy, is used to the separation of material, purification gradually and concentrates, without the need to heating, without chemical transformation, avoiding and alleviate hot oxygen effect to the impact of material.As shown in Figure 1, which employs " ultrafiltration+electrodialysis+two-stage concentrates " technique and process, dope enters existing vapo(u)rization system to current existing dichloropyridine acid mother liquor membrane technique concentration technology, and light liquid reuse is in production technique.Although so can realize the concentrating and separating of dichloropyridine acid mother liquor, it adopts in technique and uses electrodialysis and coiled reverse osmosis membrane, still existing defects.The limitation that traditional coiled reverse osmosis membrane designs because of its diaphragm and rolled structure, require higher to influent quality, be not suitable for sewage disposal, resistance to crocking is poor, the sewage rate of recovery is low, cleaning frequency is high, work-ing life is short, even if adopt ultrafiltration and electrodialysis to carry out pre-treatment above, but feed concentration in reverse osmosis membrane water inlet is still higher, long-time running, to the dirt of reverse osmosis membrane be caused to block up, flux depression, the rate of recovery reduces.In addition, although the running cost of this technique is 75 yuan/ton (film replacing construction was by 2 years), comparatively pervaporation technique 150 yuan/ton, relative cost decreases, for the low output of high investment enterprise, still not the most effective way.And electrodialysis appts is installed comparatively complicated, desalting effect is not too thorough, be generally 75%, Water Sproading rate is low, is generally 50%, and current consumption and water loss are all very high, and require also very strict for the turbidity of water inlet, easily fouling on negative electrode and film in operational process, thus affect effluent quality, and shorten the use of instrument.
In sum, enterprise needs a kind of mother liquid disposal technology of economical and efficient badly.
Utility model content
For overcoming prior art Problems existing, the utility model provides that a kind for the treatment of effect is good, cost is low, the mother liquid disposal system concentrated for clopyralid feed separation of efficient energy-saving.
To achieve these goals, the technical solution adopted in the utility model is as follows:
A kind of mother liquid disposal system concentrated for clopyralid feed separation, comprise the first heavy tank connected successively, former water pot, reactor, setting tank, sandfiltration pot, ultra-filtration filters system and SuperRO film device, and the vaporizer to be connected with SuperRO film device, wherein, the former water of dichloropyridine acid mother liquor enters just heavy tank, former water pot and reactor are equipped with doser, and former water pot is communicated with by lift pump with reactor; Be provided with mud valve bottom setting tank, described sandfiltration pot is provided with backwash tube, and its back flushing water side is communicated with reactor, and ultra-filtration filters system is communicated with reactor.
Further, stirrer is provided with in described reactor.
For the ease of sludge settling, bottom described setting tank, be provided with the bucket in back taper, be the tip of this taper bottom this bucket, and be communicated with mud valve.
Particularly, described ultra-filtration filters system comprises the tank connected ultrafiltration raw water box with sand filtration, is arranged at the second doser on ultrafiltration raw water box, and by ultra-filtration membrane device that transferpump is communicated with ultrafiltration raw water box, wherein, ultra-filtration membrane device is all communicated with SuperRO film device with reactor respectively.
Further, described SuperRO film device comprises the pressurized vessel that end is connected by flange seal, be arranged at the fluid inlet on pressurized vessel and the first liquid outlet, be arranged at the several flow guiding disc and filtration membrane that are also mutually stacked alternately in pressurized vessel, run through all flow guiding discs and filtration membrane from middle part and pass the center pull rod that pressurized vessel two end flanges arranges, wherein, center pull rod is tubular, and with the through hole be communicated with flow guiding disc on its wall, its end forms the second liquid outlet.
Compared with prior art, the utility model has following beneficial effect:
(1) the utility model carries out design improvement for the feature of clopyralid material, first soften except hard again through ultrafiltration and extraordinary reverse osmosis membrane filtration, finally a small amount of dense water obtained is carried out evaporative crystallization, reduce evaporation cost, to it also avoid in whole process hot oxygen effect to the impact of material, ensure disposing mother liquor quality, and obviously can reduce energy consumption, thus greatly reduce running cost, and the utility model is novel, structure is simple, with low cost, convenient and practical, safe and efficient, be with a wide range of applications, be applicable to applying.
(2) the utility model high energy consumption avoiding electrodialytic technique and hot oxygen effect that may bring, realizes the taking-up of foreign material and the recovery of clopyralid material by completely physico filter type, significantly reduces system energy consumption, thus reduce costs.
(3) the utility model also arranges uf processing before extraordinary reverse osmosis membrane processing, has effectively ensured the influent quality of reverse osmosis, improves the processing efficiency of reverse osmosis membrane device, extends its work-ing life.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of prior art.
Fig. 2 is process flow sheet of the present utility model.
Fig. 3 is structured flowchart of the present utility model.
Fig. 4 is the structural representation of SuperRO film device in the utility model.
Embodiment
Below in conjunction with drawings and Examples, the utility model is described in further detail, and embodiment of the present utility model includes but not limited to the following example.
Embodiment
As shown in Figures 2 to 4, the mother liquid disposal system that should concentrate in clopyralid feed separation, comprise the first heavy tank connected successively, former water pot, reactor, setting tank, sandfiltration pot, ultra-filtration filters system and SuperRO film device, and the vaporizer to be connected with SuperRO film device, wherein, the former water of dichloropyridine acid mother liquor enters just heavy tank, former water pot and reactor are equipped with doser, and former water pot is communicated with by lift pump with reactor; Be provided with mud valve bottom setting tank, described sandfiltration pot is provided with backwash tube, and its back flushing water side is communicated with reactor, and ultra-filtration filters system is communicated with reactor.Further, stirrer is provided with in described reactor.
For the ease of sludge settling, bottom described setting tank, be provided with the bucket in back taper, be the tip of this taper bottom this bucket, and be communicated with mud valve.
Particularly, described ultra-filtration filters system comprises the tank connected ultrafiltration raw water box with sand filtration, is arranged at the second doser on ultrafiltration raw water box, and by ultra-filtration membrane device that transferpump is communicated with ultrafiltration raw water box, wherein, ultra-filtration membrane device is all communicated with SuperRO film device with reactor respectively.
Further, described SuperRO film device comprises the pressurized vessel 10 that end is tightly connected by flange 11, be arranged at the fluid inlet 12 on pressurized vessel and the first liquid outlet 13, be arranged at the several flow guiding discs 14 and filtration membrane 15 that are also mutually stacked alternately in pressurized vessel, run through all flow guiding discs and filtration membrane from middle part and pass the center pull rod 16 that pressurized vessel two end flanges arranges, wherein, center pull rod is tubular, and with the through hole be communicated with flow guiding disc on its wall, its end forms the second liquid outlet 17.
Utilize said system to carry out the concentrated mother liquor treatment process of clopyralid feed separation, step is as follows:
(1) former for dichloropyridine acid mother liquor water is carried out centralized collection at former water pot after just sinking, carry out the even of water quality and quantity;
(2) in former water pot, liquid caustic soda is added by former water pH regulator to 8 ~ 9;
(3) entering reactor by lift pump by regulating the raw water pump after pH, in reactor, adding sodium carbonate solution, under low rate mixing, form flocculence alumen ustum and gravity flow enters setting tank;
(4) in setting tank, carry out sludge settling, then liquid enters sandfiltration pot and tentatively filters;
(5) liquid after preliminary filtration enters ultrafiltration raw water box, and adds acid for adjusting pH to 6.5 ~ 7, then pumps into ultra-filtration membrane device and filters;
(6) the light liquid after the filtration of ultra-filtration membrane device enters SuperRO film device, and dope is back to reactor;
(7) the product water after the filtration of SuperRO film device enters sewage plant, and dense water enters vaporizer and carries out evaporative crystallization.
For ensureing that sodium carbonate fully reacts in reactor, in described step (3), stirring velocity is 15 ~ 25round/min.
Further, for improving strainability and the abundant reuse of resource, in described step (4), regularly back flushing being carried out to sandfiltration pot and cleaning, and by the sewage backflow of back flushing to reactor.
Particularly, the ultra-filtration membrane aperture of described ultra-filtration membrane device is 0.002-0.1 micron, is 20% ~ 60% to the rejection of COD, water outlet SDI < 3, delivery turbidity < 0.1NTU.SDI(SiltingDensityIndex, pollution index), NTU is nephelometric turbidity unit, and SuperRO is extraordinary reverse osmosis membrane.
Certain clopyralid manufacturing enterprise carry out testing and the data obtained as shown in following table 1 and table 2:
Table 1 raw water quality analytical data
By the process of above-mentioned steps (1) ~ (4), original water hardness can be reduced to below 110mg/L by 480mg/L; Due to former water COD and salinity all very high, the common coiled reverse osmosis membrane that prior art adopts is limited to COD tolerance, when COD is greater than 100mg/L, film is just easy to pollute, and the former water COD of enterprise's material is up to more than 8000mg/L, and its highest working pressure is limited, is only 50bar, and the highest working pressure of the extraordinary reverse osmosis membrane that the utility model adopts can reach 160bar, and improve cycles of concentration, decrease dope amount, can make finally to produce water COD and be down to below 250mg/L.
The economic comparison of table 2 prior art processes and the utility model technique
As seen from the above comparison, the working cost of the utility model technique is significantly less than the working cost of prior art processes.
Above-described embodiment is only preferred embodiment of the present utility model; restriction not to the utility model protection domain; in every case principle of design of the present utility model being adopted, and the change carried out non-creativeness work on this basis and make, all should belong within protection domain of the present utility model.
Claims (5)
1. the mother liquid disposal system concentrated for clopyralid feed separation, it is characterized in that, comprise the first heavy tank connected successively, former water pot, reactor, setting tank, sandfiltration pot, ultra-filtration filters system and SuperRO film device, and the vaporizer to be connected with SuperRO film device, wherein, the former water of dichloropyridine acid mother liquor enters just heavy tank, former water pot and reactor are equipped with doser, and former water pot is communicated with by lift pump with reactor; Be provided with mud valve bottom setting tank, described sandfiltration pot is provided with backwash tube, and its back flushing water side is communicated with reactor, and ultra-filtration filters system is communicated with reactor.
2. a kind of mother liquid disposal system concentrated for clopyralid feed separation according to claim 1, is characterized in that, be provided with stirrer in described reactor.
3. a kind of mother liquid disposal system concentrated for clopyralid feed separation according to claim 1, is characterized in that, be provided with the bucket in back taper bottom described setting tank, be the tip of this taper, and be communicated with mud valve bottom this bucket.
4. a kind of mother liquid disposal system concentrated for clopyralid feed separation according to any one of claim 1 ~ 3, it is characterized in that, described ultra-filtration filters system comprises the tank connected ultrafiltration raw water box with sand filtration, be arranged at the second doser on ultrafiltration raw water box, and by ultra-filtration membrane device that transferpump is communicated with ultrafiltration raw water box, wherein, ultra-filtration membrane device is all communicated with SuperRO film device with reactor respectively.
5. a kind of mother liquid disposal system concentrated for clopyralid feed separation according to any one of claim 1 ~ 3, it is characterized in that, described SuperRO film device comprises the pressurized vessel that end is connected by flange seal, be arranged at the fluid inlet on pressurized vessel and the first liquid outlet, be arranged at the several flow guiding disc and filtration membrane that are also mutually stacked alternately in pressurized vessel, run through all flow guiding discs and filtration membrane from middle part and pass the center pull rod that pressurized vessel two end flanges arranges, wherein, center pull rod is tubular, and with the through hole be communicated with flow guiding disc on its wall, its end forms the second liquid outlet.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201520958124.0U CN205170592U (en) | 2015-11-27 | 2015-11-27 | A mother liquor processing system for clopyralid material separation is concentrated |
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| CN201520958124.0U CN205170592U (en) | 2015-11-27 | 2015-11-27 | A mother liquor processing system for clopyralid material separation is concentrated |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439347A (en) * | 2015-11-27 | 2016-03-30 | 成都美富特膜科技有限公司 | Mother liquor treatment process and system applied to clopyralid material separation and concentration |
| CN113620494A (en) * | 2021-08-18 | 2021-11-09 | 江苏艾科维科技有限公司 | Low COD treatment of waste water and method for recovering hexahydropyridine in waste water |
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2015
- 2015-11-27 CN CN201520958124.0U patent/CN205170592U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439347A (en) * | 2015-11-27 | 2016-03-30 | 成都美富特膜科技有限公司 | Mother liquor treatment process and system applied to clopyralid material separation and concentration |
| CN105439347B (en) * | 2015-11-27 | 2018-09-14 | 成都美富特环保产业集团有限公司 | A kind of mother liquor treatment process and system for the concentration of clopyralid feed separation |
| CN113620494A (en) * | 2021-08-18 | 2021-11-09 | 江苏艾科维科技有限公司 | Low COD treatment of waste water and method for recovering hexahydropyridine in waste water |
| CN113620494B (en) * | 2021-08-18 | 2023-06-13 | 江苏艾科维科技股份有限公司 | Method for reducing COD in wastewater and recovering piperidine in wastewater |
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| C14 | Grant of patent or utility model | ||
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Address after: Jintang County of Chengdu City, Sichuan province 610000 Huai town Jintang Industrial Park Green Avenue Patentee after: Chengdu Environmental Protection Industry Group Co.,Ltd. Foote Address before: Jintang County of Chengdu City, Sichuan province 610000 Huai town Jintang Industrial Park Green Avenue Patentee before: CHENGDU MEIFUTE MEMBRANE TECHNOLOGY Co.,Ltd. |
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| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 610000 environmental protection Avenue, Jintang Industrial Park, huaikou Town, Jintang County, Chengdu, Sichuan Patentee after: Chengdu Meifute Environmental Protection Industry Co.,Ltd. Address before: 610000 environmental protection Avenue, Jintang Industrial Park, huaikou Town, Jintang County, Chengdu, Sichuan Patentee before: Chengdu Environmental Protection Industry Group Co.,Ltd. Foote |