CN102030354A - Treatment method of waste sulfuric acid - Google Patents
Treatment method of waste sulfuric acid Download PDFInfo
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- CN102030354A CN102030354A CN 201010509465 CN201010509465A CN102030354A CN 102030354 A CN102030354 A CN 102030354A CN 201010509465 CN201010509465 CN 201010509465 CN 201010509465 A CN201010509465 A CN 201010509465A CN 102030354 A CN102030354 A CN 102030354A
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Abstract
The invention relates to a treatment method of waste sulfuric acid, which is characterized by comprising the following steps: crushing heavy calcium carbonate ore or fine ore into 100 meshes to obtain heavy calcium carbonate dry powder, or pulping to obtain the heavy calcium carbonate pulp the weight percent concentration of which is not higher than 70%; simultaneously, controlling the weight percent concentration of the waste sulfuric acid to be treated to be not higher than 20%; adding the waste sulfuric acid and the heavy calcium carbonate dry powder or the heavy calcium carbonate pulp into the reaction zone of a salt chemical engineering reactor, wherein the molar ratio of the waste sulfuric acid to the heavy calcium carbonate is (50-90):(70-100); after reaction, discharging gypsum ore pulp through the underflow of the salt chemical engineering reactor, and filtering to obtain fibrous gypsum products; and discharging the treated water and gypsum crystals through the overflow of the salt chemical engineering reactor. The pH value of the waste acid water treated by the method provided by the invention reaches 6-9, thereby meeting the requirement for the pH value of the discharge water; and the by-product gypsum crystals are fibrous, the purity of the gypsum crystals reaches more than 85%, and the gypsum crystals can be widely applied to the fields such as medicine, agriculture, light industry, building material industry and the like.
Description
Technical field
The present invention relates to a kind of recovery and treatment method of chemical spent material, particularly a kind of useless vitriolic treatment process.
Background technology
Sulfuric acid is in industry widespread uses such as chemical industry, iron and steel.In many production processes, sulfuric acid often can not be utilized completely, and remaining sulfuric acid emits in company with big water gaging, forms the lower waste acid water of concentration.These waste acid waters can make water body or soil acidification as being discharged in the environment without processing, and ecotope is caused serious harm.Many in recent years countries have formulated strict emission control standards, and meanwhile, advanced improvement technology also develops rapidly all over the world.
Useless vitriolic treatment process is more in the prior art, forms and the difference of management goal according to waste acid water, and the improvement method that adopts both at home and abroad is broadly divided into following 3 big classes at present: recovery is used again, comprehensive utilization and neutralizing treatment.In China, concentrate absorption method and neutralizing treatment method and be still most widely used method at present.The sulfur waste sour water very low for sulfuric acid concentration, that the water yield is bigger, reclaim(ed) sulfuric acid and with in the caustic soda and cost higher, should select to invest the treatment process less, that cost is low as the case may be.
Waste water of flue gas desulfurization of the prior art heavy calcium carbonate also commonly used is handled, but because coarse whiting and vitriolic speed of response are very fast, gypsum with coarse whiting and the direct hybrid reaction generation of sulfur waste acid under the normal condition is a microcrystal, granularity mostly is below ten microns, sedimentation, filtration, dehydration be difficulty very, and processing cost is higher.Discharging and stacking produce new environmental pollution again.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, provides that a kind of technology is more reasonable, treatment effect is good, the useless vitriolic treatment process of by-product fibrous gypsum crystalline simultaneously.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of useless vitriolic treatment process, is characterized in that its step is as follows:
(1) get water-ground limestone ore or fine ore and be crushed to-100 orders and get ground whiting dry powder, perhaps the ground whiting dry powder water being sized mixing is not higher than 70% water-ground limestone slurry again to weight percent concentration; Simultaneously pending useless vitriolic weight percent concentration is controlled at and is not higher than 20%;
(2) sulfur waste acid and ground whiting dry powder or water-ground limestone slurry are added in the reaction zone of salt chemical engineering reactor, sulfur waste acid is 50-90: 70-100 with the mol ratio of water-ground limestone; The stirring intensity linear velocity of salt chemical engineering reactor is the 1.4-2.50 meter per second during reaction, and rotating speed is 300-1200 rev/min; The time that material stops in the salt chemical engineering reactor is 0.5-2.5 hour; The current lift velocity in salt chemical engineering reactor overflow district is the 0.03-0.50 mm/second; Reaction back salt chemical engineering reactor underflow is discharged the gypsum ore pulp, filters and obtains the fibrous gypsum product; Water and gypsum that the salt chemical engineering reactor overflow is discharged after handling are carefully brilliant.
In the step (2) of above-described useless vitriolic treatment process technical scheme, before sulfur waste acid and ground whiting dry powder or water-ground limestone slurry adding salt chemical engineering reactor, can in the salt chemical engineering reactor, add part fibrous gypsum product earlier and make crystal seed.This, the crystallization of the fibrous gypsum product in can the accelerated reaction process.When no crystal seed, can produce crystal seed earlier, and then handle sulfur waste acid by technical solution of the present invention.
In the step (2) of above-described useless vitriolic treatment process technical scheme, water and the gypsum thin crystalline substance of part after the processing that the salt chemical engineering reactor overflow is discharged can be returned the salt chemical engineering reactor after concentrating.
" salt chemical engineering reactor " of the present invention is meant that the patent No. is 01237973.5, publication number is " the salt chemical engineering reactor " put down in writing in the Chinese publication document of CN2485020.
The sulfur waste acid that the inventive method was suitable for can absorb the sulfur waste sour water that the back is produced for the waste gas water that full scale plant produced or full scale plant produces.
Compared with prior art, the present invention can overcome the directly problem of the gypsum crystal of the microfine of hybrid reaction generation of coarse whiting and sulfur waste acid of handling in the useless vitriolic process effectively, in the process of handling spent acid, use the salt chemical engineering reactor, by the salt chemical engineering reactor, make the gypsum crystal of microfine grow up to fibrous coarse crystal, when handling the sulfur waste sour water, by-product fibrous gypsum crystal.
Through experiment test, the pH value of the waste acid water after the inventive method is handled reaches 6-9, meets the requirement of the pH value of discharge water; By-produced gypsum (terra alba) crystal shape is fibrous, and purity reaches more than 85%; Planar water content is less than 20% in the product, and by the control raw materials quality, further the correlation parameter of preferably salt chemical reactor can be produced purity and reach 95% gypsum product simultaneously; The mean particle size of gypsum reaches 0.1 millimeter, has extensive use in fields such as medical science, agricultural, light industry, building materials.
Embodiment
Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.
Embodiment 1.A kind of useless vitriolic treatment process, its step is as follows:
(1) get water-ground limestone ore or fine ore and be crushed to-100 orders and get ground whiting dry powder, perhaps the ground whiting dry powder water being sized mixing is not higher than 70% water-ground limestone slurry again to weight percent concentration; Simultaneously pending useless vitriolic weight percent concentration is controlled at and is not higher than 20%;
(2) sulfur waste acid and ground whiting dry powder or water-ground limestone slurry are added in the reaction zone of salt chemical engineering reactor, sulfur waste acid is 50: 70 with the mol ratio of water-ground limestone; The stirring intensity linear velocity of salt chemical engineering reactor is 1.4 meter per seconds during reaction, and rotating speed is 300 rev/mins; The time that material stops in the salt chemical engineering reactor is 0.5 hour; The current lift velocity in salt chemical engineering reactor overflow district is 0.03 mm/second; Reaction back salt chemical engineering reactor underflow is discharged the gypsum ore pulp, filters and obtains the fibrous gypsum product; Water and gypsum that the salt chemical engineering reactor overflow is discharged after handling are carefully brilliant.
Embodiment 2.A kind of useless vitriolic treatment process, its step is as follows:
(1) get water-ground limestone ore or fine ore and be crushed to-100 orders and get ground whiting dry powder, perhaps the ground whiting dry powder water being sized mixing is not higher than 70% water-ground limestone slurry again to weight percent concentration; Simultaneously pending useless vitriolic weight percent concentration is controlled at and is not higher than 20%;
Sulfur waste acid and ground whiting dry powder or water-ground limestone slurry are added in the reaction zone of salt chemical engineering reactor, and sulfur waste acid is 90: 100 with the mol ratio of water-ground limestone; The stirring intensity linear velocity of salt chemical engineering reactor is 2.50 meter per seconds during reaction, and rotating speed is 1200 rev/mins; The time that material stops in the salt chemical engineering reactor is 2.5 hours; The current lift velocity in salt chemical engineering reactor overflow district is 0.50 mm/second; Reaction back salt chemical engineering reactor underflow is discharged the gypsum ore pulp, filters and obtains the fibrous gypsum product; Water and gypsum that the salt chemical engineering reactor overflow is discharged after handling are carefully brilliant.
Embodiment 3.A kind of useless vitriolic treatment process, its step is as follows:
(1) get water-ground limestone ore or fine ore and be crushed to-100 orders and get ground whiting dry powder, perhaps the ground whiting dry powder water being sized mixing is not higher than 70% water-ground limestone slurry again to weight percent concentration; Simultaneously pending useless vitriolic weight percent concentration is controlled at and is not higher than 20%;
(2) sulfur waste acid and ground whiting dry powder or water-ground limestone slurry are added in the reaction zone of salt chemical engineering reactor, sulfur waste acid is 70: 85 with the mol ratio of water-ground limestone; The stirring intensity linear velocity of salt chemical engineering reactor is 2.00 meter per seconds during reaction, and rotating speed is 800 rev/mins; The time that material stops in the salt chemical engineering reactor is 1.5 hours; The current lift velocity in salt chemical engineering reactor overflow district is 0.20 mm/second; Reaction back salt chemical engineering reactor underflow is discharged the gypsum ore pulp, filters and obtains the fibrous gypsum product; Water and gypsum that the salt chemical engineering reactor overflow is discharged after handling are carefully brilliant.
Embodiment 4.In embodiment 1 or the 2 or 3 described useless vitriolic treatment processs: in step (2), before sulfur waste acid and ground whiting dry powder or water-ground limestone slurry adding salt chemical engineering reactor, in the salt chemical engineering reactor, add part fibrous gypsum product earlier and make crystal seed.
Embodiment 5.In embodiment 1 or 2 or the 3 or 4 described useless vitriolic treatment processs: water and the gypsum thin crystalline substance of part after the processing that the salt chemical engineering reactor overflow is discharged returned the salt chemical engineering reactor after concentrating.
Embodiment 6.A kind of sulfur waste acid treatment method, its step is as follows: water-ground limestone ore reduction is to-100 orders, and dry powder is not sized mixing; The sulfur waste acid concentration is 5%; Sulfur waste acid is 55: 70 with coarse whiting reaction mole number proportioning, adds the part crystal seed earlier in the salt chemical engineering reactor, and spent acid and coarse whiting are added in the salt chemical engineering reactor reaction zone.Salt chemical engineering reactor underflow is discharged the gypsum ore pulp, filters to obtain the striate gypsum product.Water and gypsum that the salt chemical engineering reactor overflow is discharged after handling are carefully brilliant, return the salt chemical engineering reactor after thin brilliant the concentrating.Salinization reactor stirring intensity linear velocity is 1.8 meter per seconds, and rotating speed is 700 rev/mins, and material residence time in the salinization reactor is 2.2 hours, and the current lift velocity in salinization reactor overflow district is 0.30 mm/second.The pH value of the waste acid water after the processing reaches 7.5; The by-produced gypsum crystal shape is fibrous, and purity reaches 92.1%; Planar water content is less than 19% in the product.
Embodiment 7.A kind of sulfur waste acid treatment method, its step is as follows: water-ground limestone ore reduction is sized mixing to 70% concentration to-120 orders, and acid-spending strength is 7%; Spent acid and coarse whiting reaction mole number proportioning are 60: 80, add the part crystal seed earlier in the salinization reactor, and spent acid and coarse whiting are added in the salinization reactor reaction zone.Salinization reactor underflow is discharged the gypsum ore pulp, filters to obtain the striate gypsum product.Water and gypsum that the salinization reactor overflow is discharged after handling are carefully brilliant, return the salinization reactor after thin brilliant the concentrating; Salinization reactor stirring intensity linear velocity is 2.20 meter per seconds, and rotating speed is 1000 rev/mins, and material residence time in the salinization reactor is 1.7 hours, and the current lift velocity in salinization reactor overflow district is 0.10 mm/second.The pH value of the waste acid water after the processing reaches 7.1; The by-produced gypsum crystal shape is fibrous, and purity reaches 93.1%; Planar water content is less than 17.5% in the product.
Embodiment 8.A kind of sulfur waste acid treatment method, its step is as follows: water-ground limestone ore reduction is sized mixing to 55% concentration to-150 orders; Acid-spending strength is 10%; Spent acid and coarse whiting reaction mole number proportioning are 70: 90, add the part crystal seed earlier in the salinization reactor, and spent acid and coarse whiting are added in the salinization reactor reaction zone.Salinization reactor underflow is discharged the gypsum ore pulp, filters to obtain the striate gypsum product.Water and gypsum that the salinization reactor overflow is discharged after handling are carefully brilliant, return the salinization reactor after thin brilliant the concentrating.Salinization reactor stirring intensity linear velocity is 2.1 meter per seconds, and rotating speed is 900 rev/mins, and material residence time in the salinization reactor is 0.8 hour, and the current lift velocity in salinization reactor overflow district is 0.08 mm/second.The ph value of the waste acid water after the processing reaches 6.5; The by-produced gypsum crystal shape is fibrous, and purity reaches 94.5%; Planar water content is less than 16% in the product.
Claims (3)
1. useless vitriolic treatment process is characterized in that its step is as follows:
(1) get water-ground limestone ore or fine ore and be crushed to-100 orders and get ground whiting dry powder, perhaps the ground whiting dry powder water being sized mixing is not higher than 70% water-ground limestone slurry again to weight percent concentration; Simultaneously pending useless vitriolic weight percent concentration is controlled at and is not higher than 20%;
(2) sulfur waste acid and ground whiting dry powder or water-ground limestone slurry are added in the reaction zone of salt chemical engineering reactor, sulfur waste acid is 50-90: 70-100 with the mol ratio of water-ground limestone; The stirring intensity linear velocity of salt chemical engineering reactor is the 1.4-2.50 meter per second during reaction, and rotating speed is 300-1200 rev/min; The time that material stops in the salt chemical engineering reactor is 0.5-2.5 hour; The current lift velocity in salt chemical engineering reactor overflow district is the 0.03-0.50 mm/second; Reaction back salt chemical engineering reactor underflow is discharged the gypsum ore pulp, filters and obtains the fibrous gypsum product; Water and gypsum that the salt chemical engineering reactor overflow is discharged after handling are carefully brilliant.
2. a kind of useless vitriolic treatment process according to claim 1, it is characterized in that: in step (2), before sulfur waste acid and ground whiting dry powder or water-ground limestone slurry adding salt chemical engineering reactor, in the salt chemical engineering reactor, add part fibrous gypsum product earlier and make crystal seed.
3. a kind of useless vitriolic treatment process according to claim 1 is characterized in that: in step (2), water and the gypsum thin crystalline substance of part after the processing that the salt chemical engineering reactor overflow is discharged returned the salt chemical engineering reactor after concentrating.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103395816A (en) * | 2013-07-22 | 2013-11-20 | 蓝星（成都）新材料有限公司 | Process for producing calcium sulphate dihydrate by utilizing aramid fiber II spinning acid pickle |
| CN103966670A (en) * | 2014-05-12 | 2014-08-06 | 江苏一夫科技股份有限公司 | Method for integrating waste sulfuric acid treatment engineering and gypsum crystal whisker production |
| CN104692443A (en) * | 2015-03-24 | 2015-06-10 | 枣庄市泰瑞精细化工有限公司 | Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate |
| CN104828851A (en) * | 2015-04-21 | 2015-08-12 | 南通南辉电子材料股份有限公司 | Production method and production device of calcium sulphate dihydrate |
| CN105819485A (en) * | 2016-03-29 | 2016-08-03 | 云南华联锌铟股份有限公司 | Method and device for producing gypsum from zinc smelting acid-containing solution |
| CN105858705A (en) * | 2016-03-30 | 2016-08-17 | 东南大学 | Method for preparing dihydrate gypsum with low free water content by using waste sulfuric acid solution |
| CN106241849A (en) * | 2016-06-27 | 2016-12-21 | 枣庄市泰瑞精细化工有限公司 | A kind of method utilizing the waste water producing naphthalenedisulfonic acid to prepare gypsum for cement |
| CN106477616A (en) * | 2015-08-25 | 2017-03-08 | 住友大阪水泥株式会社 | The manufacture method of Gypsum Fibrosum and the manufacture method of cement composition |
| CN107055586A (en) * | 2016-12-30 | 2017-08-18 | 宁夏东吴农化有限公司 | A kind of preparation method of calcium sulfate |
| CN109134007A (en) * | 2017-06-17 | 2019-01-04 | 新疆丰泰化工科技有限公司 | Utilize the method for spent acid production calcium humate |
| CN110204028A (en) * | 2019-07-10 | 2019-09-06 | 孙宝成 | Handle gypsum rotating crystal device, processing method and the dihydrate gypsum of dilute sulfuric acid waste water |
| CN110330047A (en) * | 2019-07-10 | 2019-10-15 | 孙宝成 | Gypsum rotating crystal device, the method for preparing dihydrate gypsum, α high strength gypsum and plasterboard |
| CN111018382A (en) * | 2019-12-30 | 2020-04-17 | 中芳特纤股份有限公司 | Method for preparing high-strength gypsum by using para-aramid spinning waste acid and waste silk |
| CN111362292A (en) * | 2020-03-17 | 2020-07-03 | 中国科学院过程工程研究所 | Continuous production system and method for producing low-water-content calcium sulfate from waste sulfuric acid |
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| CN2485020Y (en) * | 2001-05-24 | 2002-04-10 | 化学工业部连云港设计研究院 | Salt chemical reactor |
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| CN2485020Y (en) * | 2001-05-24 | 2002-04-10 | 化学工业部连云港设计研究院 | Salt chemical reactor |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103395816A (en) * | 2013-07-22 | 2013-11-20 | 蓝星（成都）新材料有限公司 | Process for producing calcium sulphate dihydrate by utilizing aramid fiber II spinning acid pickle |
| CN103395816B (en) * | 2013-07-22 | 2015-04-22 | 蓝星（成都）新材料有限公司 | Process for producing calcium sulphate dihydrate by utilizing aramid fiber II spinning acid pickle |
| CN103966670A (en) * | 2014-05-12 | 2014-08-06 | 江苏一夫科技股份有限公司 | Method for integrating waste sulfuric acid treatment engineering and gypsum crystal whisker production |
| CN104692443A (en) * | 2015-03-24 | 2015-06-10 | 枣庄市泰瑞精细化工有限公司 | Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate |
| CN104828851A (en) * | 2015-04-21 | 2015-08-12 | 南通南辉电子材料股份有限公司 | Production method and production device of calcium sulphate dihydrate |
| CN106477616A (en) * | 2015-08-25 | 2017-03-08 | 住友大阪水泥株式会社 | The manufacture method of Gypsum Fibrosum and the manufacture method of cement composition |
| CN106477616B (en) * | 2015-08-25 | 2020-05-19 | 住友大阪水泥株式会社 | Method for producing gypsum and method for producing cement composition |
| CN105819485A (en) * | 2016-03-29 | 2016-08-03 | 云南华联锌铟股份有限公司 | Method and device for producing gypsum from zinc smelting acid-containing solution |
| CN105819485B (en) * | 2016-03-29 | 2018-06-22 | 云南华联锌铟股份有限公司 | The method and apparatus of output gypsum from the acid-containing solution of zinc abstraction |
| CN105858705A (en) * | 2016-03-30 | 2016-08-17 | 东南大学 | Method for preparing dihydrate gypsum with low free water content by using waste sulfuric acid solution |
| CN106241849A (en) * | 2016-06-27 | 2016-12-21 | 枣庄市泰瑞精细化工有限公司 | A kind of method utilizing the waste water producing naphthalenedisulfonic acid to prepare gypsum for cement |
| CN107055586A (en) * | 2016-12-30 | 2017-08-18 | 宁夏东吴农化有限公司 | A kind of preparation method of calcium sulfate |
| CN109134007A (en) * | 2017-06-17 | 2019-01-04 | 新疆丰泰化工科技有限公司 | Utilize the method for spent acid production calcium humate |
| CN110204028A (en) * | 2019-07-10 | 2019-09-06 | 孙宝成 | Handle gypsum rotating crystal device, processing method and the dihydrate gypsum of dilute sulfuric acid waste water |
| CN110330047A (en) * | 2019-07-10 | 2019-10-15 | 孙宝成 | Gypsum rotating crystal device, the method for preparing dihydrate gypsum, α high strength gypsum and plasterboard |
| CN111018382A (en) * | 2019-12-30 | 2020-04-17 | 中芳特纤股份有限公司 | Method for preparing high-strength gypsum by using para-aramid spinning waste acid and waste silk |
| CN111362292A (en) * | 2020-03-17 | 2020-07-03 | 中国科学院过程工程研究所 | Continuous production system and method for producing low-water-content calcium sulfate from waste sulfuric acid |
| CN111362292B (en) * | 2020-03-17 | 2021-05-07 | 中国科学院过程工程研究所 | Continuous production system and method for producing low-water-content calcium sulfate from waste sulfuric acid |
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