CN101435082A - Method for processing pickle liquor by negative pressure outer circulation continuous evaporation continuous freezing crystallization process - Google Patents
Method for processing pickle liquor by negative pressure outer circulation continuous evaporation continuous freezing crystallization process Download PDFInfo
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- CN101435082A CN101435082A CNA2008102041443A CN200810204144A CN101435082A CN 101435082 A CN101435082 A CN 101435082A CN A2008102041443 A CNA2008102041443 A CN A2008102041443A CN 200810204144 A CN200810204144 A CN 200810204144A CN 101435082 A CN101435082 A CN 101435082A
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Abstract
The invention relates to a method for adopting negative pressure external circulating continuous evaporation and continuous freezing crystallization method to treat pickling waste liquid. A triple effect negative pressure external circulating continuous evaporator is utilized to carry out evaporation concentration to pickling waste liquid; the sour vapour generated by evaporation forms recovered acid by condensation; the restored acid is used as a follow-up evaporator heat source; the concentrated solution is treated by heat exchange, cooling and freezing crystallization, and then is separated by a vacuum belt type solid-liquid separator so as to obtain solid particles; and the mother liquid is returned to a waste acid tank so as to complete the whole circulation and realize the zero discharging of waste acid liquid. A first effect evaporator is heated by vapour, a second effect evaporator is heated by the sour vapour generated by the first effect evaporator and a triple effect evaporator is heated by the sour vapour generated by the second effect evaporator, thus utilizing the heat energy furthest. The technique method of the invention has high efficiency, fast speed, stable production and low cost and also realizes the zero discharge of waste liquid.
Description
Technical field
The invention belongs to chemical field, relate to the technology of a kind of steel mill spent pickle liquor processing technology field, specifically is that the acid washing rolled steel waste liquid recycles by the evaporation concentration regenerating acid, and freezing and crystallizing is separated out ferrous crystal, obtains solid phase prod, realizes the spent acid solution zero release.
Background technology
Because iron and steel enterprise is extensive use of acid as the acid washing rolled steel medium, consequent waste liquid is many to enter rivers after general neutralizing treatment, and this becomes one of comparatively serious source of pollution in waters, and is the waste of resource.
Along with the raising of people's environmental consciousness, the development of recycling economy if can be with these spent acid efficient recovery regenerations, produce useful Chemicals, not only can reduce environmental pollution, can reduce the waste of resource simultaneously, be a good thing that meets the energy-saving and emission-reduction beneficial to national welfare and the people's livelihood.So the processing method that development and Design one cover can address the above problem is necessary in fact.
Summary of the invention
The object of the present invention is to provide a kind of technology of handling spent pickle liquor, make the spent acid resource utilization, regenerating acid repeats pickling, and it is ferrous to obtain solid phase prod simultaneously, thereby reaches the minimizing environmental pollution, reduces the wasting of resources, realizes the purpose of recycling economy.
For reaching above purpose, solution of the present invention is:
A kind of negative pressure outer circulation continuous evaporation continuous freezing crystallization process is handled the technology of spent pickle liquor, utilize triple effect negative pressure outer circulation continuous evaporator that spent pickle liquor is carried out evaporation concentration, the acid vapour that evaporation produces forms regenerating acid through condensation, regenerating acid is as subsequent evaporation device thermal source, concentrated solution is through continuous acid heat exchange, cooling, freezing and crystallizing, maximally utilise heat energy and separate out ferrous crystal, separate through the vacuum belt solid-liquid separating machine, obtain solid particulate, mother liquor returns the spent acid pond, finish full cycle, realize the spent acid solution zero release.
One imitates and to be evaporated to normal pressure, two imitate be evaporated to-0.01～-0.03MPa, triple effect evaporation is-0.06～-0.08MPa.
One imitates 100～110 ℃ of evaporation operation temperature, and two imitate 85～95 ℃ of evaporation operation temperature, 70～80 ℃ of triple effect evaporation service temperatures.
Spent acid to be evaporated carries out preheating with giving birth to steam condensate and high temperature evaporation concentrated solution earlier, 1st effective evaporator is by steam heating, the acid vapour heating that 2nd effect evaporator is produced by 1st effective evaporator, triple-effect evaporator gets to the limit heat energy and is utilized by the acid vapour heating that 2nd effect evaporator produces.
Cooled concentrated solution is freezing continuously through the continuous freezing and crystallizing jar of particular design, crystallization, growing the grain, and carries out solid-liquid separation continuously with the vacuum belt solid-liquid separating machine, discharges ferrous particle continuously.
0～8 ℃ of freezing and crystallizing temperature, rearing crystal time 0.5～1.5 hour.
Through the continuous freezing and crystallizing jar of particular design, good effect of heat exchange, the crystal of separating out is difficult for occluding device, favorable anti-corrosion effect, the anacidity gas leakage can the continous-stable operation.
Through the continuous secondary cooling of the interchanger of particular design, good effect of heat exchange is difficult for stopping up, and technical process is succinct, and is easy to operate, and floor space is little.
Owing to adopted such scheme, the present invention to have following characteristics:
1. efficient height, speed is fast
Continuous freeze crystallization, material only need finish in the continuous freezing and crystallizing still of particular design at one from high temperature to low temperature, have made full use of the low-temperature receiver of equipment, and crystalline rate is fast at a high speed;
2. produce stable
Because continuity production makes material turnover flow obtain balance, continuous and stable production is simple to operate;
3. consume and lack, cost is low
Need not add eo-acid, heat utilization ratio height in the treating processes, equipment anticorrosion is durable, running cost is low.
4. realization Zero discharge
The regenerating acid that this technology obtains after evaporation can directly enter acid-washing stainless steel, through obtaining ferrous crystal behind the freezing and crystallizing continuously, and can be with barreled or packed sale.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The present invention is further illustrated below in conjunction with the accompanying drawing illustrated embodiment.
Spent acid by after the under meter metering, is successively entered triple effect, two and imitates, one imitates negative pressure outer circulation continuous evaporator, control certain input speed and heating steam temperature, the acid vapour that heating evaporation produces reclaims after cooling off, the spent acid mother liquor after two sections coolings of continous way solution cooling tower, enters continuous freezing and crystallizing jar after concentrating again, separate out ferrous crystal, advance the vacuum belt solid-liquid separating machine afterwards, solid-liquid separates continuously, obtains solid particulate, mother liquor returns the spent acid pond, finishes full cycle.
Wherein, 1st effective evaporator is an atmospheric operation, by steam heating, 105 ℃ of working temperatures, 2nd effect evaporator is negative pressure-0.02MPa operation, by the HCl steam heating that 1st effective evaporator produces, 90 ℃ of working temperatures, triple-effect evaporator also is a negative-pressure operation, operating pressure is-0.08MPa, by the HCl steam heating that 2nd effect evaporator produces, 75 ℃ of working temperatures, in the consecutive evaporation process, energy is fully utilized.Whole crystallisation process is finished by continous way solution cooling tower and continuous freezing and crystallizing jar, concrete operations are: at first with spent acid concentrated solution is cooled to 75 ℃ from 105 ℃, with water coolant material is cooled to 30 ℃ from 75 ℃ then, with refrigerant material is cooled to 5 ℃ at last, finish refrigeration crystallization process.In continuous refrigeration crystallization process, energy also is fully utilized.
Negative pressure outer circulation continuous evaporation continuous freezing crystallization process of the present invention is handled the technology of spent pickle liquor, uses checking in certain spent acid solution processing enter, by the effect behind the actual motion, has realized the spent acid resource utilization, Zero discharge.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (7)
1. method of handling spent pickle liquor, it is characterized in that: utilize triple effect negative pressure outer circulation continuous evaporator that spent pickle liquor is carried out evaporation concentration, the acid vapour that evaporation produces forms regenerating acid through condensation, regenerating acid is as subsequent evaporation device thermal source, and concentrated solution separates through the vacuum belt solid-liquid separating machine through heat exchange, cooling, freezing and crystallizing again, obtain solid particulate, mother liquor returns the spent acid pond, finishes full cycle, realizes the spent acid solution zero release.
2. the method for processing spent pickle liquor according to claim 1 is characterized in that: one imitates and to be evaporated to normal pressure, two imitate be evaporated to-0.01～-0.03MPa, triple effect evaporation is-0.06～-0.08MPa.
3. the method for processing spent pickle liquor according to claim 1 is characterized in that: one imitates 100～110 ℃ of evaporation operation temperature, and two imitate 85～95 ℃ of evaporation operation temperature, 70～80 ℃ of triple effect evaporation service temperatures.
4. the method for processing spent pickle liquor according to claim 1, it is characterized in that: spent acid to be evaporated carries out preheating with giving birth to steam condensate and high temperature evaporation concentrated solution earlier, 1st effective evaporator is by steam heating, the acid vapour heating that 2nd effect evaporator is produced by 1st effective evaporator, the acid vapour heating that triple-effect evaporator is produced by 2nd effect evaporator.
5. the method for processing spent pickle liquor according to claim 1, it is characterized in that: cooled concentrated solution is freezing continuously through freezing and crystallizing jar continuously, crystallization, growing the grain, and carry out solid-liquid separation continuously with the vacuum belt solid-liquid separating machine, discharge ferrous particle continuously.
6. the method for processing spent pickle liquor according to claim 5 is characterized in that: 0～8 ℃ of freezing and crystallizing temperature, rearing crystal time 0.5～1.5 hour.
7. the method for processing spent pickle liquor according to claim 1 is characterized in that: concentrated solution is through the continuous secondary cooling of interchanger.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102041443A CN101435082A (en) | 2008-12-05 | 2008-12-05 | Method for processing pickle liquor by negative pressure outer circulation continuous evaporation continuous freezing crystallization process |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008102041443A CN101435082A (en) | 2008-12-05 | 2008-12-05 | Method for processing pickle liquor by negative pressure outer circulation continuous evaporation continuous freezing crystallization process |
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| CN101435082A true CN101435082A (en) | 2009-05-20 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863036A (en) * | 2012-09-24 | 2013-01-09 | 蒙自矿冶有限责任公司 | Method for regeneration of hydrochloric acid containing waste liquid by means of microwave heating |
| CN104548634A (en) * | 2013-10-28 | 2015-04-29 | 南通醋酸纤维有限公司 | Solid-liquid separation process for combining multiple-effect evaporation and agitated evaporation |
| CN104692575A (en) * | 2014-12-22 | 2015-06-10 | 内蒙古久科康瑞环保科技有限公司 | Crystallization treatment method and device of high salt wastewater |
| CN104711617A (en) * | 2015-04-09 | 2015-06-17 | 南通晨光石墨设备有限公司 | Regeneration method of acid washing waste acids |
| CN108726615A (en) * | 2018-08-01 | 2018-11-02 | 江苏泰特联合环保科技有限公司 | A kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique and device |
| CN111498884A (en) * | 2020-06-01 | 2020-08-07 | 江苏泰特联合环保科技有限公司 | Treatment process and device for fluorine-containing waste hydrochloric acid |
-
2008
- 2008-12-05 CN CNA2008102041443A patent/CN101435082A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863036A (en) * | 2012-09-24 | 2013-01-09 | 蒙自矿冶有限责任公司 | Method for regeneration of hydrochloric acid containing waste liquid by means of microwave heating |
| CN104548634A (en) * | 2013-10-28 | 2015-04-29 | 南通醋酸纤维有限公司 | Solid-liquid separation process for combining multiple-effect evaporation and agitated evaporation |
| WO2015062393A1 (en) * | 2013-10-28 | 2015-05-07 | 南通醋酸纤维有限公司 | Solid-liquid separation process with multi-effect evaporation in combination with stirring evaporation |
| CN104548634B (en) * | 2013-10-28 | 2016-08-17 | 南通醋酸纤维有限公司 | A kind of multiple-effect evaporation combines the solid-liquid separation process of stirring evaporation |
| CN104692575A (en) * | 2014-12-22 | 2015-06-10 | 内蒙古久科康瑞环保科技有限公司 | Crystallization treatment method and device of high salt wastewater |
| CN104692575B (en) * | 2014-12-22 | 2017-02-22 | 内蒙古久科康瑞环保科技有限公司 | Crystallization treatment method and device of high salt wastewater |
| CN104711617A (en) * | 2015-04-09 | 2015-06-17 | 南通晨光石墨设备有限公司 | Regeneration method of acid washing waste acids |
| CN108726615A (en) * | 2018-08-01 | 2018-11-02 | 江苏泰特联合环保科技有限公司 | A kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique and device |
| CN111498884A (en) * | 2020-06-01 | 2020-08-07 | 江苏泰特联合环保科技有限公司 | Treatment process and device for fluorine-containing waste hydrochloric acid |
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Open date: 20090520 |