CN112877777A - Method for preparing calcium sulfate hemihydrate crystal whisker by using semidry desulfurization ash - Google Patents
Method for preparing calcium sulfate hemihydrate crystal whisker by using semidry desulfurization ash Download PDFInfo
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- CN112877777A CN112877777A CN202110238158.2A CN202110238158A CN112877777A CN 112877777 A CN112877777 A CN 112877777A CN 202110238158 A CN202110238158 A CN 202110238158A CN 112877777 A CN112877777 A CN 112877777A
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- calcium sulfate
- sulfate hemihydrate
- desulfurization ash
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- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 31
- 230000023556 desulfurization Effects 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 27
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 title claims abstract description 22
- 239000013078 crystal Substances 0.000 title description 3
- 239000000243 solution Substances 0.000 claims abstract description 29
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 239000002351 wastewater Substances 0.000 claims abstract description 12
- 239000002699 waste material Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011593 sulfur Substances 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- 239000003546 flue gas Substances 0.000 claims description 3
- 239000010842 industrial wastewater Substances 0.000 claims description 3
- 150000007522 mineralic acids Chemical class 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 239000002956 ash Substances 0.000 claims 11
- 239000002585 base Substances 0.000 claims 7
- 239000000203 mixture Substances 0.000 claims 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- 239000003637 basic solution Substances 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 238000009713 electroplating Methods 0.000 claims 1
- 239000010881 fly ash Substances 0.000 claims 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002910 solid waste Substances 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 238000010335 hydrothermal treatment Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- GBAOBIBJACZTNA-UHFFFAOYSA-L calcium sulfite Chemical compound [Ca+2].[O-]S([O-])=O GBAOBIBJACZTNA-UHFFFAOYSA-L 0.000 description 1
- 235000010261 calcium sulphite Nutrition 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention belongs to the technical field of solid waste resource utilization, and particularly relates to a method for preparing calcium sulfate hemihydrate whiskers by using semidry desulfurization ash. The method takes powdery semi-dry desulfurization ash as a raw material, fully oxidizes hexavalent chromium wastewater under an acidic condition, and dehydrates and dries the hexavalent chromium wastewater to obtain oxidized desulfurization ash. Respectively with CaCl2-HCl mixed solution or MgCl2‑H2SO4And (3) adding a certain amount of oxidized desulfurized ash into the mixed solution serving as a base solution, and performing hydrothermal treatment to obtain a calcium sulfate hemihydrate finished product, wherein the base solution can be repeatedly used. The invention realizes the resource utilization of the waste while performing harmless treatment on the waste, thereby producing the effect of improving the quality of the productObvious economic benefit, social benefit and environmental benefit.
Description
Technical Field
The invention belongs to the technical field of solid waste resource utilization, and particularly relates to a method for preparing calcium sulfate hemihydrate whiskers by using semidry desulfurization ash.
Background
The semi-dry flue gas desulfurization technology is a flue gas desulfurization technology with the advantages of a wet method and a dry method, compared with the wet method, the method has the advantages of high desulfurization efficiency, simple process system, low capital cost and small occupied area, and the desulfurization product is similar to the dry method and is dry powder without wastewater. However, the desulfurization product components are complex and variable (the main components are calcium sulfite, calcium carbonate, calcium hydroxide, a small amount of calcium sulfate and the like), are strong in basicity and are easy to decompose, so that the comprehensive utilization is very difficult. The invention utilizes hexavalent chromium wastewater to fully oxidize semi-dry desulfurized ash, and then utilizes a hydrothermal method to prepare the calcium sulfate hemihydrate crystal whisker. The method has simple process and low cost, and realizes high value-added resource utilization of various wastes.
Disclosure of Invention
The invention provides a method for preparing calcium sulfate hemihydrate whiskers by using semidry desulfurization ash, which comprises the steps of fully oxidizing the semidry desulfurization ash by using hexavalent chromium wastewater, synthesizing the calcium sulfate hemihydrate whiskers by using a hydrothermal method, performing harmless treatment on the wastewater and wastes, realizing high added value resource utilization of the wastes, and having remarkable economic, social and environmental benefits.
A method for preparing calcium sulfate hemihydrate whiskers by using semidry desulfurization ash is characterized by comprising the following steps:
(1) putting powdery semi-dry desulfurization ash into an oxidation reaction tank, and adding a certain amount of hexavalent chromium wastewater into the reaction tank, wherein the mass of the hexavalent chromium added into the reaction tank is about 50-70% of the mass of the sulfur in the desulfurization ash. Adding inorganic acid, continuously stirring, adjusting the pH to be 2.0-4.5, continuously stirring for 10-30 min, standing for precipitation for 5-20 min, press-filtering for dehydration, repeatedly washing the precipitate, and drying to obtain oxidized desulfurized ash;
(2) preparing CaCl with the mass fraction of 0.5-5.0%2The solution is adjusted with HCl to pH =1.0-4.5, whereby CaCl is added2-HCl mixed solution as base solution; or MgCl with the mass fraction of 0.5-5.0 percent is prepared2In solution with H2SO4Adjusting the pH of the solution to 1.0-4.5 to obtain MgCl2-H2SO4The mixed solution is used as a base solution;
(3) adding 5.0-15% of desulfurized ash after oxidation treatment into the base solution, adding the mixed solution into a hydrothermal reaction kettle, and reacting for 1.0-3.0h at the temperature of 120-. And (4) taking out the sample after the reaction kettle is cooled to room temperature, filtering and washing, and reusing the supernatant as the substrate liquid.
Compared with the prior art, the invention has the characteristics and beneficial effects that:
the method solves the problems of secondary pollution and land occupation of the semidry desulfurization ash, reduces the treatment cost of the chromium-containing wastewater and the semidry desulfurization ash, and realizes the low-cost and high-added-value resource utilization of wastes.
Drawings
Fig. 1 is a photograph of a calcium sulfate hemihydrate whisker product prepared in an example of the invention.
Fig. 2 is an SEM image of calcium sulfate hemihydrate whiskers prepared in an example of the present invention.
Detailed Description
The method and technique of the present invention are described below by way of example, but not limitation in practical applications.
Example 1
The method for preparing the calcium sulfate hemihydrate whiskers by using the semidry desulfurization ash comprises the following steps:
(1) and (2) placing powdery semi-dry desulfurization ash into an oxidation reaction tank, and adding a certain amount of vanadium industrial wastewater into the reaction tank, wherein the mass of hexavalent chromium added into the reaction tank is about 60% of the mass of sulfur in the desulfurization ash. Adjusting pH =2.5 with sulfuric acid, stirring for 15 min, standing for 20 min, press-filtering and dehydrating the precipitate, washing repeatedly and drying;
(2) preparing CaCl with the mass fraction of 2.0 percent2The solution is adjusted to pH =3.0 with HCl, whereby CaCl is added2-HCl mixed solution as base solution;
(3) adding 10% of desulfurized ash after oxidation treatment into the base solution, adding the mixed solution into a hydrothermal reaction kettle, and reacting for 2.0 h at 140 ℃. And (3) taking out the sample after the reaction kettle is cooled to room temperature, filtering, washing and drying to obtain a calcium sulfate hemihydrate finished product, wherein the average length-diameter ratio of the calcium sulfate hemihydrate finished product can reach more than 25.
Example 2
The method for preparing the calcium sulfate hemihydrate whiskers by using the semidry desulfurization ash comprises the following steps:
(1) and (2) placing powdery semi-dry desulfurization ash into an oxidation reaction tank, and adding a certain amount of vanadium industrial wastewater into the reaction tank, wherein the mass of hexavalent chromium added into the reaction tank is about 70% of the mass of sulfur in the desulfurization ash. Adjusting pH =3.0 with sulfuric acid, stirring for 15 min, standing for 20 min, press-filtering and dehydrating the precipitate, washing repeatedly and drying;
(2) or MgCl with the mass fraction of 5.0 percent is prepared2In solution with H2SO4Adjusting the solution pH =2.0 to obtain MgCl2-H2SO4The mixed solution is used as a base solution;
(3) adding 5 mass percent of desulfurized ash after oxidation treatment into the base solution, adding the mixed solution into a hydrothermal reaction kettle, and reacting for 1.5 h at 130 ℃. And (3) taking out the sample after the reaction kettle is cooled to room temperature, filtering, washing and drying to obtain a calcium sulfate hemihydrate finished product, wherein the average length-diameter ratio of the calcium sulfate hemihydrate finished product can reach more than 20.
The above description is only a preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto,
technical solutions according to the present invention and methods thereof within the technical scope of the present disclosure
The inventive concept is intended to cover such alternatives, modifications and equivalents as may be included within the spirit and scope of the invention.
Claims (5)
1. A method for preparing calcium sulfate hemihydrate whiskers by using semidry desulfurization ash is characterized by comprising the following steps:
(1) powdery semi-dry desulfurized fly ash (the main component is CaSO)3·0.5H2O) is placed in an oxidation reaction tank, a certain amount of hexavalent chromium wastewater is added into the reaction tank, wherein the mass of the hexavalent chromium added into the reaction tank is about 50-70% of the mass of the sulfur in the desulfurization ash, inorganic acid is added, the mixture is continuously stirred, the pH =2.0-4.5 is adjusted, the mixture is continuously stirred for 10-30 min, then the mixture is kept stand and deposited for 5-20 min, filter pressing and dehydration are carried out, and the deposit is repeatedly washed and dried to obtain the oxidized desulfurization ash (the main component of CaSO)4·2H2O）；
(2) Preparing CaCl with the mass fraction of 0.5-5.0%2The solution is adjusted with HCl to pH =1.0-4.5, whereby CaCl is added2-HCl mixed solution as base solution; or MgCl with the mass fraction of 0.5-5.0 percent is prepared2In solution with H2SO4Adjusting the pH of the solution to 1.0-4.5 to obtain MgCl2-H2SO4The mixed solution is used as a base solution;
(3) adding 5.0-15% of desulfurized ash after oxidation treatment into the base solution, adding the mixed solution into a hydrothermal reaction kettle, reacting at the temperature of 120-160 ℃ for 1.0-3.0h, taking out a sample after the reaction kettle is cooled to room temperature, filtering and washing, and reusing the supernatant as the base solution.
2. The method for preparing the calcium sulfate hemihydrate whiskers by using the semidry desulfurization ash according to claim 1, wherein the semidry desulfurization ash belongs to waste generated by semidry calcium flue gas desulfurization, and the hexavalent chromium wastewater is one or more of vanadium industrial wastewater, electroplating wastewater and tanning wastewater.
3. The method for preparing calcium sulfate hemihydrate whiskers by using semi-dry desulfurized ash according to claim 1, wherein the mass of hexavalent chromium added in the reaction tank is about 50-70% of the mass of sulfur in the desulfurized ash, and the pH is adjusted to be 2.0-4.5 by using inorganic acid during the oxidation process.
4. The method for preparing the calcium sulfate hemihydrate whiskers by using the semidry desulfurization ash as claimed in claim 1, wherein the two basic solutions are mainly prepared by the following steps: (1) CaCl2-HCl base solution: CaCl with mass fraction of 0.5-5.0%2Solution, and adjusting the solution pH =1.0-4.5 with HCl; (2) MgCl2-H2SO4Base solution: MgCl with mass fraction of 0.5-5.0%2In solution with H2SO4Adjusting the solution pH = 1.0-4.5.
5. The method for preparing calcium sulfate hemihydrate whiskers by using semi-dry desulfurized ash as claimed in claim 1, wherein the amount of desulfurized ash added after oxidation treatment is 5.0-15% of the mass of the base liquid, the reaction temperature is 120-.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114226421A (en) * | 2021-12-23 | 2022-03-25 | 上海电气电站环保工程有限公司 | Treatment method of semidry desulfurization ash |
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2021
- 2021-03-04 CN CN202110238158.2A patent/CN112877777A/en active Pending
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114226421A (en) * | 2021-12-23 | 2022-03-25 | 上海电气电站环保工程有限公司 | Treatment method of semidry desulfurization ash |
| CN114226421B (en) * | 2021-12-23 | 2024-03-15 | 上海电气电站环保工程有限公司 | Treatment method of semi-dry desulfurization ash |
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