CN1373243A - Process for treating waste pickling liquid of hydrochloric acid by negative-pressure external-circulation evaporation-concentrating crystallization method - Google Patents
Process for treating waste pickling liquid of hydrochloric acid by negative-pressure external-circulation evaporation-concentrating crystallization method Download PDFInfo
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- CN1373243A CN1373243A CN 01138382 CN01138382A CN1373243A CN 1373243 A CN1373243 A CN 1373243A CN 01138382 CN01138382 CN 01138382 CN 01138382 A CN01138382 A CN 01138382A CN 1373243 A CN1373243 A CN 1373243A
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- liquid
- hydrochloric acid
- waste
- evaporation chamber
- crystallization
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000007788 liquid Substances 0.000 title claims abstract description 22
- 239000002699 waste material Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000002425 crystallisation Methods 0.000 title claims abstract description 12
- 238000005554 pickling Methods 0.000 title claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 23
- 238000001704 evaporation Methods 0.000 claims abstract description 21
- 230000008020 evaporation Effects 0.000 claims abstract description 18
- 230000008025 crystallization Effects 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 239000012452 mother liquor Substances 0.000 claims abstract description 4
- 229960002089 ferrous chloride Drugs 0.000 claims abstract 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000013505 freshwater Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims 2
- 238000000926 separation method Methods 0.000 claims 2
- 238000001816 cooling Methods 0.000 claims 1
- 230000005484 gravity Effects 0.000 claims 1
- 238000005086 pumping Methods 0.000 claims 1
- 230000008929 regeneration Effects 0.000 claims 1
- 238000011069 regeneration method Methods 0.000 claims 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- -1 outward transport Substances 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 235000021110 pickles Nutrition 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- SQVRNKJHWKZAKO-UHFFFAOYSA-N beta-N-Acetyl-D-neuraminic acid Natural products CC(=O)NC1C(O)CC(O)(C(O)=O)OC1C(O)C(O)CO SQVRNKJHWKZAKO-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- SQVRNKJHWKZAKO-OQPLDHBCSA-N sialic acid Chemical compound CC(=O)N[C@@H]1[C@@H](O)C[C@@](O)(C(O)=O)OC1[C@H](O)[C@H](O)CO SQVRNKJHWKZAKO-OQPLDHBCSA-N 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
一种负压外循环蒸发浓缩结晶法处理盐酸酸洗废液的工艺,包括以下步骤:将废酸液用泵输送到蒸发室,开启蒸汽阀门使加热器开始加热蒸发废酸液,废酸液在加热器和蒸发室之间循环加热蒸发浓缩,得到氯化亚铁的结晶体,之后进离心机分离,得到固体氯化亚铁晶体,母液回到废酸池,完成整个循环。使该技术稳定可靠。设备使用寿命延长。现场氯化氢外泄少,使环境大为改善。
A process for treating waste hydrochloric acid pickling liquid by evaporation, concentration and crystallization in a negative pressure external circulation, comprising the following steps: transporting the waste acid liquid to an evaporation chamber with a pump, opening a steam valve so that a heater starts to heat and evaporate the waste acid liquid, and the waste acid liquid is Circulate heating, evaporation and concentration between the heater and the evaporation chamber to obtain crystals of ferrous chloride, which are then separated in a centrifuge to obtain solid ferrous chloride crystals, and the mother liquor is returned to the waste acid pool to complete the entire cycle. Make the technology stable and reliable. The service life of the equipment is extended. On-site leakage of hydrogen chloride is less, greatly improving the environment.
Description
Technical field
The present invention relates to crystallization process and handle the technology of hydrochloric acid pickling waste liquor.
Background technology
The surface can produce ferric oxide in the System on Rolling Steel, in order to improve surface quality of steel, must carry out pickling.For ordinary steel and general low alloy steel, the past sulfuric acid washings that adopt more, China is since the later stage eighties, and having used hydrochloric acid on the basis of using for reference industrially developed country's advanced experience instead is main pickle solution.Steel can produce a large amount of spent pickle liquors after pickling, nearly hundred ten thousand steres of this type of waste liquid approximately will be discharged every year in the whole nation at present, and it just increases along with the raising of steel output and quality.Remove in this waste liquid and contain a considerable amount of remaining acid, also be rich in ferrous salt, other contains a small amount of sialic acid non-soluble substance.As not carrying out processing and utilizing, both environmental pollution can be caused to it, precious resources will be wasted again.The method that adopts at present mainly contains both at home and abroad: FeCl
3Method, FeSO
4Method, neutralisation, direct roasting method and atmospheric evaporation method of enrichment.FeCl
3Method is free HCl and FeCl
2All change into FeCl
3, because of FeCl
3Unmarketable and consume Cl
2Now seldom adopt FeSO
4Method H
2SO
4Replacement of fe Cl
2Become FeSO
4, because of FeSO
4Tc is low, needs to add a cover ice maker system, and it is higher that investment strengthens running cost.Neutralisation is to obtain solid slag, secondary pollution and serious waste of resources with the lime neutralization.The direct roasting method is an oxydrolysis ferrous salt at high temperature, and water is evaporated, thereby obtains ferric oxide and regenerating acid, and investment that this method is too high and working cost, medium-sized and small enterprises are difficult to bear.Atmospheric evaporation condensing crystal method adopts common two to imitate evaporating and concentrating process, in use, has the problem that equipment easily stops up and equipment life is short.This is because liquid passes through the too slow and vaporization temperature height of the flow velocity of vaporizer.
Summary of the invention
The object of the present invention is to provide a kind of at atmospheric evaporation shortcoming and the technology of improved treating waste pickling liquid of hydrochloric acid by negative-pressure external-circulation evaporation-concentrating crystallization method.
The present invention includes following steps: earlier spent acid solution is arrived evaporator room with pump delivery, when waiting to reach the charging liquid level, open hydraulic jet pump, make the system vacuum degree reach 550-650mmHg, opening steam valve makes well heater begin the heating evaporation spent acid solution, spent acid solution circulation heating evaporation between well heater and evaporator room concentrates, and HCl that evaporator room steams and water vapor reclaim and obtain dilute hydrochloric acid through condenser condenses, acid tank advances to regenerate, overflow is to the hydrochloric acid storage pool, and non-condensable gases and small amount of H Cl enter hydraulic jet pump, and circulation absorbs, when HCl reaches the working concentration requirement in the pond to be recycled, with being pumped to the hydrochloric acid storage pool, replenish fresh water afterwards, treat to absorb next time.Evaporation concentration liquid is put into crystallization kettle, and the iron protochloride xln that obtains under water-cooled and stirring condition advances whizzer afterwards and separates, and obtains the solid iron protochloride, outward transport, and mother liquor is got back to the spent acid pond, finishes full cycle.
The following characteristics of process program tool of the present invention:
(1) under the system vacuum condition, evaporator room liquid material descends, and the cyclic motion of scurrying on the heating chamber material has fundamentally been stopped material possibility of jamming in well heater, evaporator room.Make this consistent reliable.
(2) adopt the heating under vacuum evaporation, the material boiling point is descended, working temperature reduces, thereby the equipment corrosion degree is reduced greatly, and this makes has a lot of favourable conditions and extensive possibility aspect the material choosing.Because vacuum-evaporation, service temperature reduce greatly, thereby can prolong service life of equipment.Because heating evaporation condensation and store operation such as regenerating acid and be in vacuum state, make the minimizing that leaks of on-the-spot hydrogenchloride, environment is greatly improved.
(3) whole process flow is simple in operation, and number of devices is few, and facility investment is lower.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
A specific embodiment of the present invention as shown in drawings, it may further comprise the steps: earlier spent acid solution is arrived evaporator room with pump delivery, when waiting to reach the charging liquid level, open hydraulic jet pump, make the system vacuum degree reach 600mmHg, opening steam valve makes well heater begin the heating evaporation spent acid solution, spent acid solution circulation heating evaporation between well heater and evaporator room concentrates, HCl that evaporator room steams and water vapor are through the graphite condenser condensation, recovery obtains dilute hydrochloric acid, the acid tank that advances to regenerate, and overflow is to the hydrochloric acid storage pool, non-condensable gases and small amount of H Cl enter hydraulic jet pump, circulation absorbs, when HCl reaches the working concentration requirement in the pond to be recycled, with being pumped to the hydrochloric acid storage pool, replenish fresh water afterwards, treat to absorb next time.Evaporation concentration liquid is put into crystallization kettle, and the iron protochloride xln that obtains under water-cooled and stirring condition advances whizzer afterwards and separates, and obtains the solid iron protochloride, outward transport, and mother liquor is got back to the spent acid pond, finishes full cycle.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01138382 CN1373243A (en) | 2001-12-31 | 2001-12-31 | Process for treating waste pickling liquid of hydrochloric acid by negative-pressure external-circulation evaporation-concentrating crystallization method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01138382 CN1373243A (en) | 2001-12-31 | 2001-12-31 | Process for treating waste pickling liquid of hydrochloric acid by negative-pressure external-circulation evaporation-concentrating crystallization method |
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| Publication Number | Publication Date |
|---|---|
| CN1373243A true CN1373243A (en) | 2002-10-09 |
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ID=4674579
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01138382 Pending CN1373243A (en) | 2001-12-31 | 2001-12-31 | Process for treating waste pickling liquid of hydrochloric acid by negative-pressure external-circulation evaporation-concentrating crystallization method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1373243A (en) |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787537B (en) * | 2009-12-11 | 2011-11-16 | 北京天泰兴工程科技有限公司 | Method for recovering waste nitric-hydrofluoric acid from stainless steel annealing-pickling by micro- and negative-pressure evaporation and crystallization processes |
| CN102660751A (en) * | 2012-04-28 | 2012-09-12 | 浙江大学 | Resourceful treating method and resourceful treating device for metal pickling effluent |
| CN101891259B (en) * | 2009-05-20 | 2012-10-10 | 北京紫光英力化工技术有限公司 | New process for recycling pickling waste liquid |
| CN102066262B (en) * | 2008-06-19 | 2013-08-28 | Sms西马格股份公司 | Processing method for recovering iron oxide and hydrochloric acid |
| CN103288232A (en) * | 2013-04-17 | 2013-09-11 | 浙江大学 | Resourceful treatment apparatus and method for waste liquid of chlorohydric acid pickling of steel |
| CN103553256A (en) * | 2013-11-04 | 2014-02-05 | 云南农业大学 | Recycling treatment process for chlorohydric acid pickling liquid waste |
| CN104047009A (en) * | 2014-06-28 | 2014-09-17 | 南通久信石墨科技开发有限公司 | Recovery process device of ferrous chloride in steel pickling liquid |
| CN104098213A (en) * | 2014-06-29 | 2014-10-15 | 扬州祥发资源综合利用有限公司 | Comprehensive recycling and utilizing method and device for ferrum-containing waste hydrochloric acid |
| CN104828995A (en) * | 2015-05-20 | 2015-08-12 | 中冶东方工程技术有限公司 | Treatment method of ferrous waste hydrochloric acid |
| CN105439362A (en) * | 2014-09-02 | 2016-03-30 | 天津市天利达环保科技有限公司 | Method for treating pickling wastewater and recovering byproducts through reduced pressure and low temperature catalytic fractionation |
| CN106086914A (en) * | 2016-08-25 | 2016-11-09 | 天津市润杰创新环保科技股份公司 | Online hydrochloric acid circulation utilization method on acid washing rolled steel line and device thereof |
| CN106830488A (en) * | 2017-03-23 | 2017-06-13 | 彭春来 | A kind of steel galvanization spent acid auto purification environment-friendly disposal system and method |
| CN107651793A (en) * | 2016-07-26 | 2018-02-02 | 重庆大学 | A kind of chlorohydric acid pickling Waste Water Treatment |
| CN108383187A (en) * | 2018-05-10 | 2018-08-10 | 西安热工研究院有限公司 | A kind of station boiler citric acid wastewater enrichment facility and application method |
| CN108557765A (en) * | 2018-05-07 | 2018-09-21 | 桐乡市思远环保科技有限公司 | A kind of pickle liquor post-processing approach including zinc and iron ion |
| CN110172704A (en) * | 2019-06-17 | 2019-08-27 | 江阴市欧姆机械设备有限公司 | A kind of online recycling system of acid circulation |
| CN111020633A (en) * | 2019-12-23 | 2020-04-17 | 广东臻鼎环境科技有限公司 | Treatment method of acidic etching waste liquid |
| CN111233239A (en) * | 2020-02-17 | 2020-06-05 | 浙江天蓝环保技术股份有限公司 | Zero-discharge process and system for resource utilization of desulfurization wastewater |
| CN112897589A (en) * | 2021-02-09 | 2021-06-04 | 鞍钢股份有限公司 | Method for separating iron ions in low-alloy steel corrosion product chemical cleaning solution |
| CN114014480A (en) * | 2021-11-09 | 2022-02-08 | 洛阳昊冶分离环保科技有限公司 | Hydrochloric acid pickling waste water concentration crystallization separation zero release equipment |
-
2001
- 2001-12-31 CN CN 01138382 patent/CN1373243A/en active Pending
Cited By (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102066262B (en) * | 2008-06-19 | 2013-08-28 | Sms西马格股份公司 | Processing method for recovering iron oxide and hydrochloric acid |
| CN101891259B (en) * | 2009-05-20 | 2012-10-10 | 北京紫光英力化工技术有限公司 | New process for recycling pickling waste liquid |
| CN101787537B (en) * | 2009-12-11 | 2011-11-16 | 北京天泰兴工程科技有限公司 | Method for recovering waste nitric-hydrofluoric acid from stainless steel annealing-pickling by micro- and negative-pressure evaporation and crystallization processes |
| CN102660751A (en) * | 2012-04-28 | 2012-09-12 | 浙江大学 | Resourceful treating method and resourceful treating device for metal pickling effluent |
| CN102660751B (en) * | 2012-04-28 | 2014-05-21 | 浙江大学 | Resourceful treating method and resourceful treating device for metal pickling effluent |
| CN103288232B (en) * | 2013-04-17 | 2014-12-31 | 浙江大学 | Resourceful treatment apparatus and method for waste liquid of chlorohydric acid pickling of steel |
| CN103288232A (en) * | 2013-04-17 | 2013-09-11 | 浙江大学 | Resourceful treatment apparatus and method for waste liquid of chlorohydric acid pickling of steel |
| CN103553256A (en) * | 2013-11-04 | 2014-02-05 | 云南农业大学 | Recycling treatment process for chlorohydric acid pickling liquid waste |
| CN104047009B (en) * | 2014-06-28 | 2016-07-27 | 南通久信石墨科技开发有限公司 | The recovery process device of ferrous chloride in acid washing rolled steel liquid |
| CN104047009A (en) * | 2014-06-28 | 2014-09-17 | 南通久信石墨科技开发有限公司 | Recovery process device of ferrous chloride in steel pickling liquid |
| CN104098213A (en) * | 2014-06-29 | 2014-10-15 | 扬州祥发资源综合利用有限公司 | Comprehensive recycling and utilizing method and device for ferrum-containing waste hydrochloric acid |
| CN105439362B (en) * | 2014-09-02 | 2018-10-16 | 天津市天利达环保科技有限公司 | It is a kind of to depressurize low-temperature catalyzed fractionation processing pickling waste waters and byproduct recovery process |
| CN105439362A (en) * | 2014-09-02 | 2016-03-30 | 天津市天利达环保科技有限公司 | Method for treating pickling wastewater and recovering byproducts through reduced pressure and low temperature catalytic fractionation |
| CN104828995A (en) * | 2015-05-20 | 2015-08-12 | 中冶东方工程技术有限公司 | Treatment method of ferrous waste hydrochloric acid |
| CN107651793A (en) * | 2016-07-26 | 2018-02-02 | 重庆大学 | A kind of chlorohydric acid pickling Waste Water Treatment |
| CN106086914A (en) * | 2016-08-25 | 2016-11-09 | 天津市润杰创新环保科技股份公司 | Online hydrochloric acid circulation utilization method on acid washing rolled steel line and device thereof |
| CN106086914B (en) * | 2016-08-25 | 2019-06-14 | 天津市润杰创新环保科技股份公司 | Online hydrochloric acid circulation utilization method and its device on acid washing rolled steel line |
| CN106830488A (en) * | 2017-03-23 | 2017-06-13 | 彭春来 | A kind of steel galvanization spent acid auto purification environment-friendly disposal system and method |
| CN108557765A (en) * | 2018-05-07 | 2018-09-21 | 桐乡市思远环保科技有限公司 | A kind of pickle liquor post-processing approach including zinc and iron ion |
| CN108383187A (en) * | 2018-05-10 | 2018-08-10 | 西安热工研究院有限公司 | A kind of station boiler citric acid wastewater enrichment facility and application method |
| CN110172704A (en) * | 2019-06-17 | 2019-08-27 | 江阴市欧姆机械设备有限公司 | A kind of online recycling system of acid circulation |
| CN111020633A (en) * | 2019-12-23 | 2020-04-17 | 广东臻鼎环境科技有限公司 | Treatment method of acidic etching waste liquid |
| CN111233239A (en) * | 2020-02-17 | 2020-06-05 | 浙江天蓝环保技术股份有限公司 | Zero-discharge process and system for resource utilization of desulfurization wastewater |
| CN112897589A (en) * | 2021-02-09 | 2021-06-04 | 鞍钢股份有限公司 | Method for separating iron ions in low-alloy steel corrosion product chemical cleaning solution |
| CN114014480A (en) * | 2021-11-09 | 2022-02-08 | 洛阳昊冶分离环保科技有限公司 | Hydrochloric acid pickling waste water concentration crystallization separation zero release equipment |
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