CN103966670A - Method for integrating waste sulfuric acid treatment engineering and gypsum crystal whisker production - Google Patents
Method for integrating waste sulfuric acid treatment engineering and gypsum crystal whisker production Download PDFInfo
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- CN103966670A CN103966670A CN201410196310.5A CN201410196310A CN103966670A CN 103966670 A CN103966670 A CN 103966670A CN 201410196310 A CN201410196310 A CN 201410196310A CN 103966670 A CN103966670 A CN 103966670A
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Abstract
The invention discloses a method for integrating waste sulfuric acid treatment engineering and gypsum crystal whisker production. According to the method, waste sulfuric acid treatment and gypsum crystal whisker production are combined, the waste sulfuric acid reacts with calcium carbonate, and a crystallizing agent and a stabilizing agent are added in the production process, thereby obtaining various gypsum crystal whisker products. The process is simple, multiple gypsum crystal whisker products can be prepared, the crystal structure of the gypsum crystal whisker is stable and not easy to break, meanwhile the waste sulfuric acid can be effectively utilized, and then environment protection and resource recycling and reuse can be effectively combined.
Description
Technical field
The present invention relates to a kind of crystal whisker of gypsum production method, particularly a kind of Waste Sulfuric Acid is processed the method for engineering and crystal whisker of gypsum production integration.
Background technology
Sulfuric acid is first of three large acid basis, and output is large, application is wide, for indelible contribution is made in human being's production, life.But in application process, inevitably discharge again vitriolated waste (waste water), serious environment pollution, endangers biological growth, human lives strongly.Therefore, these waste water must be processed after up to standard and can discharge.In the past both at home and abroad spent acid to process be all neutralisation, with Wingdale or lime, slaked lime neutralization, waste water ph reaches 7 left and right and can discharge.So each manufacturing enterprise will spend a lot of investment construction Waste Sulfuric Acid engineering of water treatment, spend human and material resources, financial resources to process.
Calcium sulfate crystal whiskers is again crystal whisker of gypsum, and it is the single crystal of ca sulphate fibre shape, diameter 1～6 μ m, length-to-diameter ratio is 5～1000, the same with gypsum have anhydrous, Ban Shui and two water minute.Calcium sulfate crystal whiskers has the granularity of granulated filler, dimensional stabilizing, intensity are high, good toughness, high temperature resistant, resist chemical, easily carry out surface treatment, strong with the avidity of the polymkeric substance such as rubber plastic, because its volume is fluffy, dispersed, heat retaining property is good, be the rare raw material of papermaking, coating and lagging material again.The characteristic that it is good and widely purposes, become generally acknowledged environment-friendly type novel material already at home and abroad.Existing calcium sulfate crystal whiskers manufacturing technology is mainly produced calcium sulfate crystal whiskers with dihydrate gypsum, and production technique be take hydrothermal method as main.But investment is large, high to gypsum raw material requirement, energy consumption is high, and cost is high, and price is also high, produces user in enormous quantities and is difficult to accept.Other method has: normal pressure acid solution is produced crystal whisker of gypsum; Normal pressure salts solution is produced crystal whisker of gypsum.Mainly acid under differing temps, calcium sulfate different solubility in salts solution, can form a certain amount of crystal whisker of gypsum after cooling.These two kinds of process yields are very low, also do not see that at present formal production line puts into production.
Summary of the invention
The object of the present invention is to provide a kind of Waste Sulfuric Acid to process the method for engineering and crystal whisker of gypsum production integration, solve Waste Sulfuric Acid simultaneously and process the problem of producing with crystal whisker of gypsum.
Technical scheme of the present invention is specific as follows:
Waste Sulfuric Acid is processed a method for engineering and crystal whisker of gypsum production integration, comprises the following steps:
(1) Waste Sulfuric Acid is filtered, and Waste Sulfuric Acid is added to water dilute and make sulphuric acid soln;
(2) get calcium carbonate and grind and add water, make calcium carbonate slurry;
(3) in described sulphuric acid soln, add crystal modifier, will add sulphuric acid soln and the described calcium carbonate slurry of crystal modifier to inject crystallizer, reaction generates CaSO42H2O;
(4) mixture in described crystallizer is dewatered, obtain CaSO42H2O slurry, and add stablizer in described CaSO42H2O slurry;
(5) the described CaSO42H2O slurry of stablizer that adds is dewatered, obtain wet dihydrate gypsum whisker;
(6) by described 100 ℃ of hot-air seasonings for wet dihydrate gypsum whisker, obtain dry dihydrate gypsum whisker; By described 150～170 ℃ of hot-air seasonings for dry dihydrate gypsum whisker, obtain semi-hydrated gypsum whisker; By described 280～320 ℃ of hot-air seasonings for dry dihydrate gypsum whisker, obtain dehydrated gyp-whisker.
Preferably, described in step (1), the concentration of sulphuric acid soln is 5～7%; Described in step (2), calcium carbonate slurry concentration is 30～50%.
Preferably, in step (2), described calcium carbonate is ground, levigate reach 325 orders more than.
Preferably, the temperature in step (3) in crystallizer is controlled at 40～70 degree, and mixing speed is 50～60 revs/min;
Preferably, the contained H2SO4 of sulphuric acid soln described in step (3) and the contained CaCO3 of described calcium carbonate slurry mix with mol ratio 1:1.
Preferably, crystal modifier described in step (3) is that concentration is 50% solution, and solute is a kind of or combination in citric acid and alkylbenzene sulfonate.
Preferably, described in step (4), stablizer is the solution of concentration 10～20%, and solute is a kind of or combination in oleate and polycarboxylate.
The obtained technique effect of the present invention is, realized Waste Sulfuric Acid simultaneously and processed with crystal whisker of gypsum and produce, and owing to adding crystal modifier, the crystal whisker of gypsum that CaSO42H2O crystallization is generated, rather than sheet, column dihydrate gypsum crystal; Add in process of production stablizer, make the whisker transforming keep whisker structure in follow-up dehydration, calcination process, and easy fracture not, and finally can obtain multiple crystal whisker of gypsum product.It is simple that the present invention produces crystal whisker of gypsum method, and can realize scale operation.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet that Waste Sulfuric Acid is processed the method for engineering and crystal whisker of gypsum production integration;
The crystal whisker of gypsum that Fig. 2 is production picture under the microscope;
Fig. 3 is that crystal whisker of gypsum unit length under Electronic Speculum of producing is the picture of 50 μ m;
Fig. 4 is that crystal whisker of gypsum unit length under Electronic Speculum of producing is the picture of 5 μ m.
Embodiment
Embodiment
In conjunction with Fig. 1, Fig. 2, Fig. 3, Fig. 4, a kind of Waste Sulfuric Acid is processed the method for engineering and crystal whisker of gypsum production integration, the Waste Sulfuric Acid that factory is discharged is collected, then filter and remove solid impurity, and to the Waste Sulfuric Acid dilution after filtering, make sulphuric acid soln, put into Waste Sulfuric Acid tank standby, the sulphuric acid soln that preferred Waste Sulfuric Acid dilution is 5～7% for concentration; Get calcium carbonate and grind and add water, make calcium carbonate slurry, can select the white calcium carbonate in one-level Yaan of Sichuan special product, grade 90～98%, whiteness 90～95, levigate reach 325 orders more than, described calcium carbonate slurry concentration 30～50%; In described sulphuric acid soln, add crystal modifier, described crystal modifier is that concentration is 50% solution, solute is a kind of or combination in citric acid and alkylbenzene sulfonate, crystal modifier is pumped into by micropump, with agitator, itself and sulphuric acid soln are fully stirred, as added 40～60 grams of 60～80 grams of the citric acids of concentration 50% and alkylbenzene sulfonates in 1 ton of sulphuric acid soln; By adding sulphuric acid soln and the described calcium carbonate slurry of crystal modifier, put into crystallizer, the contained H2SO4 of preferred described sulphuric acid soln and the contained CaCO3 of described calcium carbonate slurry mix with mol ratio 1:1, in crystallizer, be furnished with electric heater unit temperature and be controlled at 40～70 degree, 50～60 revs/min of stirrer rotating speeds are equipped with in central authorities; Crystallizer divides inner core and urceolus, stirring head blade is by two kinds of slurries mixing and by turning on inner core to urceolus, in the abundant hybrid reaction of urceolus, generate Dihydrate gypsum whiskers, in crystallizer outside, inspection window is housed, regularly detect whisker and whether generate, after crystal whisker of gypsum generates, by constantly mobile slurries, from crystallizer bottom, discharge; The mixture of discharging bottom crystallizer is dewatered by folding belt vacuum hydroextractor, obtain CaSO42H2O slurry; In described CaSO42H2O slurry, add stablizer, fully stir, described stablizer is the solution of concentration 10～20%, and solute is a kind of or combination in oleate and polycarboxylate; The described CaSO42H2O slurry of stablizer that adds is dewatered, can obtain the wet dihydrate gypsum whisker of product; By action of forced stirring dryer, wet dihydrate gypsum whisker is carried out to 100 ℃ of hot-air seasonings and stir, obtain the dry dihydrate gypsum whisker of product; By described 150～170 ℃ of hot-air seasonings for dry dihydrate gypsum whisker, obtain semi-hydrated gypsum whisker; By described 280～320 ℃ of hot-air seasonings for dry dihydrate gypsum whisker, obtain dehydrated gyp-whisker; Concrete can use Dual-barrel rotary kiln, the Dual-barrel rotary kiln patent No. 200820215929.6, and Dual-barrel rotary kiln is blown into 600 ° of left and right hot blasts from kiln hood inner core, and dry dihydrate gypsum whisker flows into inner core from urceolus, and hot blast is discharged from inner core reversed flow from urceolus vapor pipe.The outer tube length 6-8 of design Dual-barrel rotary kiln inner core rice, is opening discharge port No. 1 from 6-8 rice, combustion chamber, and material temperature is designed to 150～170 ℃ here, discharges product semi-hydrated gypsum whisker; Down 6 meters of left and right are opened discharge port again No. 2, and material temperature is discharged dehydrated gyp-whisker at 280～320 ℃ here.
It is simple that the present invention produces crystal whisker of gypsum method, and can realize scale operation.
Claims (7)
1. Waste Sulfuric Acid is processed a method for engineering and crystal whisker of gypsum production integration, it is characterized in that, comprises the following steps:
(1) Waste Sulfuric Acid is filtered, and Waste Sulfuric Acid is added to water dilute and make sulphuric acid soln;
(2) get calcium carbonate and grind and add water, make calcium carbonate slurry;
(3) in described sulphuric acid soln, add crystal modifier, will add sulphuric acid soln and the described calcium carbonate slurry of crystal modifier to inject crystallizer, reaction generates CaSO42H2O;
(4) mixture in crystallizer is dewatered, obtain CaSO42H2O slurry, and add stablizer in described CaSO42H2O slurry;
(5) the described CaSO42H2O slurry of stablizer that adds is dewatered, obtain wet dihydrate gypsum whisker;
(6) by described 100 ℃ of hot-air seasonings for wet dihydrate gypsum whisker, obtain dry dihydrate gypsum whisker; By described 150～170 ℃ of hot-air seasonings for dry dihydrate gypsum whisker, obtain semi-hydrated gypsum whisker; By described 280～320 ℃ of hot-air seasonings for dry dihydrate gypsum whisker, obtain dehydrated gyp-whisker.
2. Waste Sulfuric Acid according to claim 1 is processed the method for engineering and crystal whisker of gypsum production integration, it is characterized in that:
Described in step (1), the concentration of sulphuric acid soln is 5～7%; Described in step (2), calcium carbonate slurry concentration is 30～50%.
3. Waste Sulfuric Acid according to claim 1 is processed the method for engineering and crystal whisker of gypsum production integration, it is characterized in that:
In step (2), described calcium carbonate is ground, levigate reach 325 orders more than.
4. Waste Sulfuric Acid according to claim 1 is processed the method for engineering and crystal whisker of gypsum production integration, it is characterized in that:
Temperature in step (3) in crystallizer is controlled at 40～70 degree, and mixing speed is 50～60 revs/min.
5. Waste Sulfuric Acid according to claim 1 is processed the method for engineering and crystal whisker of gypsum production integration, it is characterized in that:
The contained H2SO4 of sulphuric acid soln described in step (3) and the contained CaCO3 of described calcium carbonate slurry mix with mol ratio 1:1.
6. Waste Sulfuric Acid according to claim 1 is processed the method for engineering and crystal whisker of gypsum production integration, it is characterized in that:
Crystal modifier described in step (3) is that concentration is 50% solution, and solute is a kind of or combination in citric acid and alkylbenzene sulfonate.
7. Waste Sulfuric Acid according to claim 1 is processed the method for engineering and crystal whisker of gypsum production integration, it is characterized in that:
Described in step (4), stablizer is the solution of concentration 10～20%, and solute is a kind of or combination in oleate and polycarboxylate.
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Cited By (14)
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| CN104499040A (en) * | 2014-12-05 | 2015-04-08 | 上海宝冶钢渣综合开发实业有限公司 | Method for preparing gypsum whisker |
| CN104928752A (en) * | 2015-07-06 | 2015-09-23 | 宁远县隆翔新型材料科技有限公司 | Method for preparing calcium sulphate dihydrate crystal whiskers at normal temperature and method thereof for converting calcium sulphate dihydrate crystal whiskers into anhydrous crystal whiskers at normal pressure |
| 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 |
| CN106007428A (en) * | 2016-05-18 | 2016-10-12 | 安徽工业大学 | Method for lowering moisture content of titanium gypsum |
| CN106395879A (en) * | 2016-08-29 | 2017-02-15 | 安徽六国化工股份有限公司 | Preparation method of large particle size calcium sulphate dihydrate in wet-process phosphoric acid technology |
| CN108707967A (en) * | 2018-08-13 | 2018-10-26 | 南京工业大学 | A method of preparing calcium sulfate crystal whiskers using the sulfate radical in sour dead-wood quality black liquor |
| 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 |
| CN111153615A (en) * | 2020-01-21 | 2020-05-15 | 广西大学 | Method for preparing building gypsum from sulfuric acid-containing wastewater |
| CN111960700A (en) * | 2020-07-16 | 2020-11-20 | 云锡文山锌铟冶炼有限公司 | Method for comprehensively utilizing waste water containing dilute sulfuric acid |
| WO2021000586A1 (en) * | 2019-07-04 | 2021-01-07 | 江苏一夫科技股份有限公司 | Method for preparing calcium sulfate dihydrate whiskers and calcium sulfate hemihydrate whiskers and product prepared therefrom |
| CN114808139A (en) * | 2022-04-18 | 2022-07-29 | 四川大学 | Method for preparing gypsum whiskers from titanium white waste acid by microwave hydrothermal method |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104499040B (en) * | 2014-12-05 | 2017-06-30 | 上海宝冶钢渣综合开发实业有限公司 | A kind of method for preparing crystal whisker of gypsum |
| CN104499040A (en) * | 2014-12-05 | 2015-04-08 | 上海宝冶钢渣综合开发实业有限公司 | Method for preparing gypsum whisker |
| CN104928752A (en) * | 2015-07-06 | 2015-09-23 | 宁远县隆翔新型材料科技有限公司 | Method for preparing calcium sulphate dihydrate crystal whiskers at normal temperature and method thereof for converting calcium sulphate dihydrate crystal whiskers into anhydrous crystal whiskers at normal pressure |
| 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 |
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| 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 |
| CN106007428A (en) * | 2016-05-18 | 2016-10-12 | 安徽工业大学 | Method for lowering moisture content of titanium gypsum |
| CN106395879A (en) * | 2016-08-29 | 2017-02-15 | 安徽六国化工股份有限公司 | Preparation method of large particle size calcium sulphate dihydrate in wet-process phosphoric acid technology |
| 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 |
| CN108707967A (en) * | 2018-08-13 | 2018-10-26 | 南京工业大学 | A method of preparing calcium sulfate crystal whiskers using the sulfate radical in sour dead-wood quality black liquor |
| WO2021000586A1 (en) * | 2019-07-04 | 2021-01-07 | 江苏一夫科技股份有限公司 | Method for preparing calcium sulfate dihydrate whiskers and calcium sulfate hemihydrate whiskers and product prepared therefrom |
| 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 |
| CN111153615A (en) * | 2020-01-21 | 2020-05-15 | 广西大学 | Method for preparing building gypsum from sulfuric acid-containing wastewater |
| CN111960700A (en) * | 2020-07-16 | 2020-11-20 | 云锡文山锌铟冶炼有限公司 | Method for comprehensively utilizing waste water containing dilute sulfuric acid |
| CN114808139A (en) * | 2022-04-18 | 2022-07-29 | 四川大学 | Method for preparing gypsum whiskers from titanium white waste acid by microwave hydrothermal method |
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